# 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 #TrackingRef '- C2DT30785E_ccdc_876455_876458_cif-rev.CIF' #=================================================================== # SUBMISSION DETAILS loop_ _publ_contact_author_name 'Dr. Hui-Zhong Kou' _publ_contact_author_address ; Department of Chemistry Tsinghua University Beijing 100084 People's Republic of China ; _publ_contact_author_email kouhz@mail.tsinghua.edu.cn _publ_contact_author_Phone 86-10-62771748 _publ_requested_category FM _publ_requested_coeditor_name ? _publ_contact_letter ; ; loop_ _publ_author_name 'Qi-Wei Xie' 'Ai-Li Cui' 'Jun Tao' 'Hui-Zhong Kou' #====================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 876455' #TrackingRef '- C2DT30785E_ccdc_876455_876458_cif-rev.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H90 Mn2 N12 O24 Y4' _chemical_formula_weight 1756.90 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' Mn Mn 0.3368 0.7283 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7841(10) _cell_length_b 12.0352(12) _cell_length_c 14.532(3) _cell_angle_alpha 101.582(2) _cell_angle_beta 111.507(2) _cell_angle_gamma 93.569(2) _cell_volume 1857.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4168 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.48 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 3.496 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.405 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _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 R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17671 _diffrn_reflns_av_R_equivalents 0.0836 _diffrn_reflns_av_sigmaI/netI 0.1231 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8281 _reflns_number_gt 4168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1165P)^2^+7.5357P] 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 SHELXL _refine_ls_extinction_coef 0.020(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8281 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1644 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.2833 _refine_ls_wR_factor_gt 0.1844 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _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 Mn1 Mn 1.13346(13) 0.86655(13) 0.41491(12) 0.0526(4) Uani 1 1 d . . . Y1 Y 0.87693(8) 0.86650(8) 0.46115(7) 0.0468(3) Uani 1 1 d . . . Y2 Y 0.94237(9) 0.99007(9) 0.26057(8) 0.0541(3) Uani 1 1 d . . . C1 C 0.8683(9) 0.7600(9) 0.6550(8) 0.055(2) Uani 1 1 d . . . C2 C 0.9353(10) 0.6887(9) 0.7116(8) 0.062(3) Uani 1 1 d . . . H2A H 1.0195 0.6943 0.7261 0.075 Uiso 1 1 calc R . . C3 C 0.8842(12) 0.6116(9) 0.7466(9) 0.072(3) Uani 1 1 d . . . C4 C 0.7546(12) 0.6005(10) 0.7193(10) 0.076(3) Uani 1 1 d . . . C5 C 0.6872(11) 0.6677(10) 0.6595(9) 0.074(3) Uani 1 1 d . . . H5A H 0.6020 0.6582 0.6404 0.088 Uiso 1 1 calc R . . C6 C 0.7410(9) 0.7489(9) 0.6267(9) 0.062(3) Uani 1 1 d . . . C7 C 0.9594(14) 0.5416(11) 0.8172(10) 0.094(4) Uani 1 1 d . . . H7A H 1.0450 0.5589 0.8291 0.141 Uiso 1 1 calc R . . H7B H 0.9314 0.4613 0.7862 0.141 Uiso 1 1 calc R . . H7C H 0.9493 0.5604 0.8809 0.141 Uiso 1 1 calc R . . C8 C 0.6869(15) 0.5156(13) 0.7562(12) 0.108(5) Uani 1 1 d . . . H8A H 0.6001 0.5194 0.7291 0.162 Uiso 1 1 calc R . . H8B H 0.7181 0.5357 0.8293 0.162 Uiso 1 1 calc R . . H8C H 0.7007 0.4391 0.7331 0.162 Uiso 1 1 calc R . . C9 C 0.6654(9) 0.8223(10) 0.5637(7) 0.057(2) Uani 1 1 d . . . H9A H 0.7006 0.9021 0.5961 0.068 Uiso 1 1 calc R . . H9B H 0.5827 0.8120 0.5629 0.068 Uiso 1 1 calc R . . C10 C 0.5720(8) 0.8689(9) 0.3975(9) 0.061(3) Uani 1 1 d . . . H10A H 0.4924 0.8556 0.4019 0.074 Uiso 1 1 calc R . . H10B H 0.5601 0.8460 0.3263 0.074 Uiso 1 1 calc R . . C11 C 0.6238(9) 0.9967(10) 0.4388(9) 0.066(3) Uani 1 1 d . . . H11A H 0.5786 1.0389 0.3903 0.079 Uiso 1 1 calc R . . H11B H 0.6133 1.0250 0.5021 0.079 Uiso 1 1 calc R . . C12 C 0.6054(9) 0.6772(9) 0.4055(9) 0.062(3) Uani 1 1 d . . . H12A H 0.5565 0.6712 0.3341 0.074 Uiso 1 1 calc R . . H12B H 0.5510 0.6510 0.4357 0.074 Uiso 1 1 calc R . . C13 C 0.7033(9) 0.5999(9) 0.4137(9) 0.062(3) Uani 1 1 d . . . H13A H 0.7377 0.5903 0.4828 0.074 Uiso 1 1 calc R . . H13B H 0.6649 0.5250 0.3688 0.074 Uiso 1 1 calc R . . C14 C 0.9115(9) 0.5896(9) 0.4366(9) 0.065(3) Uani 1 1 d . . . H14A H 0.8954 0.5083 0.4043 0.078 Uiso 1 1 calc R . . H14B H 0.9252 0.5978 0.5078 0.078 Uiso 1 1 calc R . . C15 C 1.0292(10) 0.6452(9) 0.4287(10) 0.069(3) Uani 1 1 d . . . H15A H 1.1017 0.6195 0.4724 0.083 Uiso 1 1 calc R . . H15B H 1.0239 0.6231 0.3591 0.083 Uiso 1 1 calc R . . C16 C 0.7755(10) 0.6156(9) 0.2759(8) 0.064(3) Uani 1 1 d . . . H16A H 0.7532 0.5331 0.2498 0.077 Uiso 1 1 calc R . . H16B H 0.8501 0.6376 0.2661 0.077 Uiso 1 1 calc R . . C17 C 0.6718(9) 0.6731(9) 0.2117(8) 0.062(3) Uani 1 1 d . . . C18 C 0.5576(12) 0.6137(12) 0.1466(9) 0.083(4) Uani 1 1 d . . . H18A H 0.5404 0.5362 0.1434 0.100 Uiso 1 1 calc R . . C19 C 0.4666(12) 0.6658(13) 0.0853(10) 0.087(4) Uani 1 1 d . . . C20 C 0.4948(11) 0.7812(13) 0.0901(10) 0.086(4) Uani 1 1 d . . . C21 C 0.6086(10) 0.8395(11) 0.1566(9) 0.076(3) Uani 1 1 d . . . H21A H 0.6256 0.9173 0.1607 0.091 Uiso 1 1 calc R . . C22 C 0.7005(9) 0.7878(10) 0.2189(7) 0.058(3) Uani 1 1 d . . . C23 C 0.3396(12) 0.5981(16) 0.0170(12) 0.125(6) Uani 1 1 d . . . H23A H 0.2878 0.6479 -0.0172 0.188 Uiso 1 1 calc R . . H23B H 0.3035 0.5674 0.0577 0.188 Uiso 1 1 calc R . . H23C H 0.3476 0.5365 -0.0326 0.188 Uiso 1 1 calc R . . C24 C 0.3991(15) 0.8450(17) 0.0236(14) 0.144(8) Uani 1 1 d . . . H24A H 0.3243 0.7929 -0.0171 0.217 Uiso 1 1 calc R . . H24B H 0.4316 0.8741 -0.0200 0.217 Uiso 1 1 calc R . . H24C H 0.3823 0.9076 0.0669 0.217 Uiso 1 1 calc R . . C25 C 0.8750(18) 0.7304(14) 0.0859(14) 0.130(7) Uani 1 1 d . . . H25A H 0.8376 0.6939 0.0144 0.196 Uiso 1 1 calc R . . H25B H 0.8349 0.6947 0.1216 0.196 Uiso 1 1 calc R . . H25C H 0.9609 0.7225 0.1114 0.196 Uiso 1 1 calc R . . C26 C 0.7534(19) 1.199(2) 0.2978(16) 0.205(14) Uani 1 1 d . . . H26A H 0.6899 1.2082 0.3241 0.308 Uiso 1 1 calc R . . H26B H 0.7215 1.2018 0.2275 0.308 Uiso 1 1 calc R . . H26C H 0.8218 1.2589 0.3362 0.308 Uiso 1 1 calc R . . C27 C 1.1836(15) 0.8684(15) 0.2258(11) 0.110(5) Uani 1 1 d . . . H27A H 1.2491 0.8303 0.2616 0.165 Uiso 1 1 calc R . . H27B H 1.2179 0.9370 0.2155 0.165 Uiso 1 1 calc R . . H27C H 1.1327 0.8184 0.1610 0.165 Uiso 1 1 calc R . . N1 N 1.2560(9) 0.7647(9) 0.4053(8) 0.075(3) Uani 1 1 d . . . N2 N 1.3080(9) 0.7158(9) 0.4671(9) 0.080(3) Uani 1 1 d . . . N3 N 1.3609(11) 0.6644(14) 0.5253(13) 0.130(6) Uani 1 1 d . . . N4 N 0.8042(6) 0.6430(7) 0.3878(6) 0.0508(19) Uani 1 1 d . . . N5 N 0.6570(7) 0.7974(7) 0.4559(6) 0.0535(19) Uani 1 1 d . . . N6 N 0.9420(11) 1.1097(10) 0.1060(8) 0.081(3) Uani 1 1 d . . . O1 O 0.9268(5) 0.8404(5) 0.6253(5) 0.0498(15) Uani 1 1 d . . . O2 O 0.8081(6) 0.8492(6) 0.2851(5) 0.0559(17) Uani 1 1 d . . . O3 O 0.7514(6) 1.0150(6) 0.4561(5) 0.0564(17) Uani 1 1 d . . . O4 O 1.0379(5) 0.7654(5) 0.4596(5) 0.0495(15) Uani 1 1 d . . . O5 O 1.0175(5) 0.9643(5) 0.4176(4) 0.0440(14) Uani 1 1 d . . . O6 O 0.7947(8) 1.0869(7) 0.3064(7) 0.073(2) Uani 1 1 d . . . O7 O 0.8622(9) 0.8520(7) 0.1012(7) 0.090(3) Uani 1 1 d . . . O8 O 1.1099(7) 0.8976(7) 0.2851(6) 0.068(2) Uani 1 1 d . . . O9 O 0.8527(8) 1.1012(8) 0.1366(6) 0.083(2) Uani 1 1 d . . . O10 O 1.0329(8) 1.0606(7) 0.1485(6) 0.074(2) Uani 1 1 d . . . O11 O 0.9403(10) 1.1631(9) 0.0437(7) 0.105(3) Uani 1 1 d . . . O1W O 0.7772(14) 0.8937(14) -0.0786(10) 0.093(6) Uani 0.65(3) 1 d P . . O1W' O 0.662(4) 0.871(3) -0.140(2) 0.111(15) Uani 0.35(3) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0473(8) 0.0568(9) 0.0641(10) 0.0233(7) 0.0276(7) 0.0158(7) Y1 0.0391(5) 0.0529(6) 0.0532(6) 0.0210(4) 0.0185(4) 0.0105(4) Y2 0.0503(6) 0.0621(7) 0.0546(6) 0.0234(5) 0.0205(4) 0.0113(4) C1 0.054(5) 0.057(6) 0.055(6) 0.018(5) 0.021(5) 0.002(5) C2 0.057(6) 0.066(7) 0.063(7) 0.025(5) 0.021(5) -0.004(5) C3 0.084(8) 0.056(6) 0.074(8) 0.022(6) 0.026(6) 0.014(6) C4 0.086(8) 0.068(7) 0.082(8) 0.033(6) 0.036(7) -0.007(6) C5 0.060(6) 0.081(8) 0.085(9) 0.025(7) 0.033(6) -0.001(6) C6 0.049(5) 0.069(7) 0.073(7) 0.028(6) 0.026(5) 0.003(5) C7 0.130(12) 0.080(9) 0.088(10) 0.044(8) 0.046(9) 0.028(8) C8 0.117(12) 0.117(12) 0.105(12) 0.053(10) 0.050(10) 0.001(10) C9 0.048(5) 0.075(7) 0.052(6) 0.016(5) 0.023(4) 0.015(5) C10 0.031(4) 0.077(7) 0.076(7) 0.022(6) 0.019(4) 0.011(5) C11 0.051(6) 0.088(8) 0.070(7) 0.027(6) 0.028(5) 0.032(6) C12 0.048(5) 0.065(7) 0.066(7) 0.011(5) 0.020(5) 0.002(5) C13 0.048(5) 0.063(6) 0.080(8) 0.028(6) 0.027(5) -0.008(5) C14 0.059(6) 0.051(6) 0.081(8) 0.022(5) 0.021(5) 0.006(5) C15 0.067(7) 0.053(6) 0.095(9) 0.028(6) 0.032(6) 0.029(5) C16 0.061(6) 0.063(7) 0.067(7) 0.021(6) 0.021(5) 0.002(5) C17 0.053(6) 0.064(6) 0.068(7) 0.017(5) 0.025(5) -0.008(5) C18 0.087(8) 0.088(9) 0.063(8) 0.016(6) 0.021(7) -0.019(7) C19 0.069(7) 0.110(11) 0.058(8) 0.015(7) 0.004(6) -0.008(7) C20 0.057(7) 0.110(11) 0.081(9) 0.032(8) 0.012(6) 0.007(7) C21 0.060(6) 0.088(9) 0.067(8) 0.025(7) 0.008(6) 0.010(6) C22 0.044(5) 0.082(7) 0.042(5) 0.022(5) 0.007(4) 0.008(5) C23 0.066(8) 0.164(16) 0.102(12) 0.016(11) -0.001(8) -0.030(10) C24 0.092(11) 0.185(19) 0.119(14) 0.061(14) -0.016(10) 0.036(12) C25 0.167(17) 0.108(13) 0.122(15) -0.005(11) 0.088(13) -0.026(12) C26 0.119(16) 0.36(4) 0.129(18) 0.02(2) 0.074(14) -0.06(2) C27 0.121(12) 0.162(15) 0.091(11) 0.061(11) 0.067(10) 0.069(11) N1 0.066(6) 0.090(7) 0.100(8) 0.051(6) 0.046(6) 0.040(5) N2 0.054(5) 0.084(7) 0.113(9) 0.032(7) 0.040(6) 0.020(5) N3 0.075(8) 0.169(14) 0.179(15) 0.107(12) 0.047(9) 0.049(9) N4 0.037(4) 0.058(5) 0.062(5) 0.021(4) 0.021(4) 0.008(4) N5 0.046(4) 0.059(5) 0.055(5) 0.017(4) 0.016(4) 0.015(4) N6 0.093(8) 0.093(8) 0.063(6) 0.036(6) 0.030(6) 0.012(6) O1 0.047(3) 0.058(4) 0.047(4) 0.020(3) 0.018(3) 0.002(3) O2 0.049(4) 0.071(4) 0.047(4) 0.022(3) 0.014(3) 0.009(3) O3 0.049(3) 0.070(4) 0.057(4) 0.022(3) 0.022(3) 0.027(3) O4 0.039(3) 0.047(4) 0.069(4) 0.020(3) 0.024(3) 0.006(3) O5 0.042(3) 0.045(3) 0.044(3) 0.013(3) 0.016(3) 0.004(3) O6 0.077(5) 0.066(5) 0.096(6) 0.036(5) 0.042(5) 0.044(4) O7 0.117(7) 0.073(6) 0.075(6) 0.003(4) 0.042(5) -0.009(5) O8 0.073(5) 0.086(5) 0.071(5) 0.035(4) 0.047(4) 0.036(4) O9 0.075(5) 0.105(7) 0.077(6) 0.042(5) 0.027(4) 0.020(5) O10 0.075(5) 0.091(6) 0.070(5) 0.036(5) 0.034(4) 0.018(4) O11 0.136(9) 0.120(8) 0.079(7) 0.058(6) 0.045(6) 0.024(7) O1W 0.075(11) 0.155(14) 0.052(9) 0.030(8) 0.028(8) 0.005(9) O1W' 0.14(4) 0.12(3) 0.08(2) 0.006(18) 0.06(2) 0.02(2) _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 Mn1 O5 1.864(6) . ? Mn1 O8 1.921(7) . ? Mn1 O4 1.963(6) . ? Mn1 N1 1.977(9) . ? Mn1 O3 2.052(7) 2_776 ? Mn1 Y2 3.2192(17) . ? Mn1 Y1 3.3286(16) . ? Mn1 Y1 3.3865(18) 2_776 ? Y1 O5 2.314(6) . ? Y1 O4 2.321(6) . ? Y1 O1 2.330(6) . ? Y1 O5 2.332(6) 2_776 ? Y1 O2 2.342(6) . ? Y1 O3 2.385(6) . ? Y1 N5 2.641(8) . ? Y1 N4 2.645(8) . ? Y1 Mn1 3.3865(18) 2_776 ? Y1 Y2 3.7806(15) 2_776 ? Y1 Y2 3.8143(13) . ? Y2 O5 2.218(6) . ? Y2 O8 2.275(7) . ? Y2 O6 2.371(8) . ? Y2 O1 2.380(6) 2_776 ? Y2 O7 2.382(9) . ? Y2 O2 2.415(6) . ? Y2 O9 2.429(8) . ? Y2 O10 2.496(7) . ? Y2 Y1 3.7806(15) 2_776 ? C1 O1 1.379(11) . ? C1 C2 1.388(14) . ? C1 C6 1.393(14) . ? C2 C3 1.353(14) . ? C2 H2A 0.9300 . ? C3 C4 1.420(17) . ? C3 C7 1.523(16) . ? C4 C5 1.378(16) . ? C4 C8 1.549(16) . ? C5 C6 1.384(14) . ? C5 H5A 0.9300 . ? C6 C9 1.496(14) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N5 1.500(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N5 1.497(12) . ? C10 C11 1.530(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O3 1.426(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N5 1.462(13) . ? C12 C13 1.513(14) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.467(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.464(12) . ? C14 C15 1.554(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O4 1.412(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.494(13) . ? C16 C17 1.541(15) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C22 1.373(14) . ? C17 C18 1.376(15) . ? C18 C19 1.393(18) . ? C18 H18A 0.9300 . ? C19 C20 1.389(19) . ? C19 C23 1.524(17) . ? C20 C21 1.373(16) . ? C20 C24 1.549(18) . ? C21 C22 1.404(14) . ? C21 H21A 0.9300 . ? C22 O2 1.335(11) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O7 1.462(18) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O6 1.47(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O8 1.443(14) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N1 N2 1.175(13) . ? N2 N3 1.166(15) . ? N6 O11 1.205(12) . ? N6 O10 1.273(12) . ? N6 O9 1.290(13) . ? O1 Y2 2.380(6) 2_776 ? O3 Mn1 2.052(7) 2_776 ? O5 Y1 2.332(6) 2_776 ? O1W O1W' 1.29(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 O8 85.2(3) . . ? O5 Mn1 O4 85.2(3) . . ? O8 Mn1 O4 133.3(3) . . ? O5 Mn1 N1 177.0(3) . . ? O8 Mn1 N1 91.8(4) . . ? O4 Mn1 N1 97.1(3) . . ? O5 Mn1 O3 84.2(3) . 2_776 ? O8 Mn1 O3 118.1(3) . 2_776 ? O4 Mn1 O3 106.2(3) . 2_776 ? N1 Mn1 O3 97.0(4) . 2_776 ? O5 Mn1 Y2 42.01(18) . . ? O8 Mn1 Y2 44.1(2) . . ? O4 Mn1 Y2 107.75(18) . . ? N1 Mn1 Y2 135.1(3) . . ? O3 Mn1 Y2 110.56(19) 2_776 . ? O5 Mn1 Y1 42.17(17) . . ? O8 Mn1 Y1 112.3(2) . . ? O4 Mn1 Y1 43.06(18) . . ? N1 Mn1 Y1 139.9(3) . . ? O3 Mn1 Y1 98.62(18) 2_776 . ? Y2 Mn1 Y1 71.24(4) . . ? O5 Mn1 Y1 41.15(18) . 2_776 ? O8 Mn1 Y1 98.2(2) . 2_776 ? O4 Mn1 Y1 103.9(2) . 2_776 ? N1 Mn1 Y1 139.5(3) . 2_776 ? O3 Mn1 Y1 44.04(18) 2_776 2_776 ? Y2 Mn1 Y1 69.77(4) . 2_776 ? Y1 Mn1 Y1 70.43(4) . 2_776 ? O5 Y1 O4 68.0(2) . . ? O5 Y1 O1 121.7(2) . . ? O4 Y1 O1 85.2(2) . . ? O5 Y1 O5 67.1(2) . 2_776 ? O4 Y1 O5 101.5(2) . 2_776 ? O1 Y1 O5 69.4(2) . 2_776 ? O5 Y1 O2 67.7(2) . . ? O4 Y1 O2 91.2(2) . . ? O1 Y1 O2 167.1(2) . . ? O5 Y1 O2 123.5(2) 2_776 . ? O5 Y1 O3 94.5(2) . . ? O4 Y1 O3 162.3(2) . . ? O1 Y1 O3 103.0(2) . . ? O5 Y1 O3 67.8(2) 2_776 . ? O2 Y1 O3 83.9(2) . . ? O5 Y1 N5 156.2(2) . . ? O4 Y1 N5 130.6(2) . . ? O1 Y1 N5 78.6(2) . . ? O5 Y1 N5 115.2(2) 2_776 . ? O2 Y1 N5 94.5(2) . . ? O3 Y1 N5 66.9(2) . . ? O5 Y1 N4 121.6(2) . . ? O4 Y1 N4 67.1(2) . . ? O1 Y1 N4 89.3(2) . . ? O5 Y1 N4 157.0(2) 2_776 . ? O2 Y1 N4 78.0(2) . . ? O3 Y1 N4 127.8(2) . . ? N5 Y1 N4 66.3(2) . . ? O5 Y1 Mn1 32.73(15) . . ? O4 Y1 Mn1 35.28(14) . . ? O1 Y1 Mn1 107.31(15) . . ? O5 Y1 Mn1 83.92(15) 2_776 . ? O2 Y1 Mn1 75.80(16) . . ? O3 Y1 Mn1 127.20(17) . . ? N5 Y1 Mn1 160.63(19) . . ? N4 Y1 Mn1 94.97(16) . . ? O5 Y1 Mn1 82.84(15) . 2_776 ? O4 Y1 Mn1 133.10(16) . 2_776 ? O1 Y1 Mn1 79.86(16) . 2_776 ? O5 Y1 Mn1 31.74(15) 2_776 2_776 ? O2 Y1 Mn1 111.21(18) . 2_776 ? O3 Y1 Mn1 36.72(17) . 2_776 ? N5 Y1 Mn1 89.50(18) . 2_776 ? N4 Y1 Mn1 155.13(16) . 2_776 ? Mn1 Y1 Mn1 109.57(4) . 2_776 ? O5 Y1 Y2 90.23(15) . 2_776 ? O4 Y1 Y2 89.97(17) . 2_776 ? O1 Y1 Y2 37.07(15) . 2_776 ? O5 Y1 Y2 32.86(14) 2_776 2_776 ? O2 Y1 Y2 155.53(17) . 2_776 ? O3 Y1 Y2 87.55(17) . 2_776 ? N5 Y1 Y2 103.14(18) . 2_776 ? N4 Y1 Y2 124.58(17) . 2_776 ? Mn1 Y1 Y2 91.50(4) . 2_776 ? Mn1 Y1 Y2 53.03(3) 2_776 2_776 ? O5 Y1 Y2 31.93(14) . . ? O4 Y1 Y2 83.96(15) . . ? O1 Y1 Y2 153.41(15) . . ? O5 Y1 Y2 89.14(14) 2_776 . ? O2 Y1 Y2 37.35(16) . . ? O3 Y1 Y2 81.86(16) . . ? N5 Y1 Y2 126.17(17) . . ? N4 Y1 Y2 108.57(17) . . ? Mn1 Y1 Y2 53.05(3) . . ? Mn1 Y1 Y2 90.03(4) 2_776 . ? Y2 Y1 Y2 118.69(3) 2_776 . ? O5 Y2 O8 69.5(2) . . ? O5 Y2 O6 87.1(3) . . ? O8 Y2 O6 156.5(3) . . ? O5 Y2 O1 70.4(2) . 2_776 ? O8 Y2 O1 89.6(3) . 2_776 ? O6 Y2 O1 80.5(3) . 2_776 ? O5 Y2 O7 129.7(3) . . ? O8 Y2 O7 82.6(3) . . ? O6 Y2 O7 115.5(3) . . ? O1 Y2 O7 152.4(3) 2_776 . ? O5 Y2 O2 68.0(2) . . ? O8 Y2 O2 99.0(2) . . ? O6 Y2 O2 72.7(3) . . ? O1 Y2 O2 130.9(2) 2_776 . ? O7 Y2 O2 76.6(3) . . ? O5 Y2 O9 153.2(3) . . ? O8 Y2 O9 129.4(3) . . ? O6 Y2 O9 72.1(3) . . ? O1 Y2 O9 89.3(3) 2_776 . ? O7 Y2 O9 75.8(3) . . ? O2 Y2 O9 118.9(3) . . ? O5 Y2 O10 135.0(2) . . ? O8 Y2 O10 78.1(3) . . ? O6 Y2 O10 120.1(3) . . ? O1 Y2 O10 79.2(2) 2_776 . ? O7 Y2 O10 73.3(3) . . ? O2 Y2 O10 149.9(3) . . ? O9 Y2 O10 52.1(3) . . ? O5 Y2 N6 152.8(3) . . ? O8 Y2 N6 103.7(3) . . ? O6 Y2 N6 96.3(3) . . ? O1 Y2 N6 83.5(3) 2_776 . ? O7 Y2 N6 72.8(3) . . ? O2 Y2 N6 138.8(3) . . ? O9 Y2 N6 26.1(3) . . ? O10 Y2 N6 25.9(3) . . ? O5 Y2 Mn1 34.22(16) . . ? O8 Y2 Mn1 36.01(17) . . ? O6 Y2 Mn1 121.0(2) . . ? O1 Y2 Mn1 82.84(15) 2_776 . ? O7 Y2 Mn1 104.8(2) . . ? O2 Y2 Mn1 77.17(15) . . ? O9 Y2 Mn1 163.0(2) . . ? O10 Y2 Mn1 111.4(2) . . ? N6 Y2 Mn1 137.2(2) . . ? O5 Y2 Y1 34.78(15) . 2_776 ? O8 Y2 Y1 81.8(2) . 2_776 ? O6 Y2 Y1 77.7(2) . 2_776 ? O1 Y2 Y1 36.16(14) 2_776 2_776 ? O7 Y2 Y1 162.0(2) . 2_776 ? O2 Y2 Y1 97.16(16) . 2_776 ? O9 Y2 Y1 121.3(2) . 2_776 ? O10 Y2 Y1 111.9(2) . 2_776 ? N6 Y2 Y1 119.7(2) . 2_776 ? Mn1 Y2 Y1 57.19(4) . 2_776 ? O5 Y2 Y1 33.49(14) . . ? O8 Y2 Y1 89.69(17) . . ? O6 Y2 Y1 70.55(19) . . ? O1 Y2 Y1 96.47(14) 2_776 . ? O7 Y2 Y1 109.8(2) . . ? O2 Y2 Y1 36.05(15) . . ? O9 Y2 Y1 140.6(2) . . ? O10 Y2 Y1 167.05(19) . . ? N6 Y2 Y1 166.6(2) . . ? Mn1 Y2 Y1 55.72(3) . . ? Y1 Y2 Y1 61.31(3) 2_776 . ? O1 C1 C2 120.4(9) . . ? O1 C1 C6 119.8(9) . . ? C2 C1 C6 119.7(9) . . ? C3 C2 C1 123.2(10) . . ? C3 C2 H2A 118.4 . . ? C1 C2 H2A 118.4 . . ? C2 C3 C4 117.4(10) . . ? C2 C3 C7 123.2(12) . . ? C4 C3 C7 119.3(11) . . ? C5 C4 C3 119.4(10) . . ? C5 C4 C8 119.0(12) . . ? C3 C4 C8 121.6(11) . . ? C4 C5 C6 122.6(11) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C1 117.5(10) . . ? C5 C6 C9 121.2(9) . . ? C1 C6 C9 121.3(9) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 N5 114.3(8) . . ? C6 C9 H9A 108.7 . . ? N5 C9 H9A 108.7 . . ? C6 C9 H9B 108.7 . . ? N5 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? N5 C10 C11 111.3(8) . . ? N5 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N5 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? O3 C11 C10 110.5(8) . . ? O3 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? O3 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N5 C12 C13 112.9(8) . . ? N5 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? N5 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? N4 C13 C12 113.9(8) . . ? N4 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? N4 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? N4 C14 C15 111.3(8) . . ? N4 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N4 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? O4 C15 C14 108.0(8) . . ? O4 C15 H15A 110.1 . . ? C14 C15 H15A 110.1 . . ? O4 C15 H15B 110.1 . . ? C14 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? N4 C16 C17 116.0(9) . . ? N4 C16 H16A 108.3 . . ? C17 C16 H16A 108.3 . . ? N4 C16 H16B 108.3 . . ? C17 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C22 C17 C18 120.7(11) . . ? C22 C17 C16 116.4(9) . . ? C18 C17 C16 122.8(10) . . ? C17 C18 C19 122.2(12) . . ? C17 C18 H18A 118.9 . . ? C19 C18 H18A 118.9 . . ? C20 C19 C18 118.0(11) . . ? C20 C19 C23 121.4(13) . . ? C18 C19 C23 120.6(14) . . ? C21 C20 C19 119.0(12) . . ? C21 C20 C24 119.9(13) . . ? C19 C20 C24 121.1(12) . . ? C20 C21 C22 123.3(12) . . ? C20 C21 H21A 118.3 . . ? C22 C21 H21A 118.3 . . ? O2 C22 C17 122.1(9) . . ? O2 C22 C21 121.0(10) . . ? C17 C22 C21 116.8(10) . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 C27 H27A 109.5 . . ? O8 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O8 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 N1 Mn1 125.3(9) . . ? N3 N2 N1 177.2(16) . . ? C14 N4 C13 107.6(7) . . ? C14 N4 C16 108.0(8) . . ? C13 N4 C16 113.7(8) . . ? C14 N4 Y1 105.4(5) . . ? C13 N4 Y1 113.3(6) . . ? C16 N4 Y1 108.4(6) . . ? C12 N5 C10 107.3(8) . . ? C12 N5 C9 109.9(8) . . ? C10 N5 C9 110.1(8) . . ? C12 N5 Y1 116.3(6) . . ? C10 N5 Y1 105.7(5) . . ? C9 N5 Y1 107.5(5) . . ? O11 N6 O10 122.8(11) . . ? O11 N6 O9 122.1(12) . . ? O10 N6 O9 115.0(9) . . ? O11 N6 Y2 177.3(10) . . ? O10 N6 Y2 59.0(5) . . ? O9 N6 Y2 56.0(5) . . ? C1 O1 Y1 127.4(6) . . ? C1 O1 Y2 123.7(6) . 2_776 ? Y1 O1 Y2 106.8(2) . 2_776 ? C22 O2 Y1 122.8(6) . . ? C22 O2 Y2 129.3(6) . . ? Y1 O2 Y2 106.6(3) . . ? C11 O3 Mn1 117.7(6) . 2_776 ? C11 O3 Y1 124.1(6) . . ? Mn1 O3 Y1 99.2(2) 2_776 . ? C15 O4 Mn1 120.2(6) . . ? C15 O4 Y1 126.2(6) . . ? Mn1 O4 Y1 101.7(3) . . ? Mn1 O5 Y2 103.8(3) . . ? Mn1 O5 Y1 105.1(3) . . ? Y2 O5 Y1 114.6(2) . . ? Mn1 O5 Y1 107.1(3) . 2_776 ? Y2 O5 Y1 112.4(2) . 2_776 ? Y1 O5 Y1 112.9(2) . 2_776 ? C26 O6 Y2 133.5(9) . . ? C25 O7 Y2 125.7(9) . . ? C27 O8 Mn1 127.0(7) . . ? C27 O8 Y2 133.1(7) . . ? Mn1 O8 Y2 99.9(3) . . ? N6 O9 Y2 97.8(6) . . ? N6 O10 Y2 95.1(6) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.113 _refine_diff_density_min -1.745 _refine_diff_density_rms 0.186 #===End data_2 _database_code_depnum_ccdc_archive 'CCDC 876456' #TrackingRef '- C2DT30785E_ccdc_876455_876458_cif-rev.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H90 Gd4 Mn2 N12 O24' _chemical_formula_weight 2030.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mn Mn 0.3368 0.7283 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8167(14) _cell_length_b 12.0190(14) _cell_length_c 14.5700(17) _cell_angle_alpha 101.724(3) _cell_angle_beta 111.523(3) _cell_angle_gamma 93.206(3) _cell_volume 1865.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5523 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.49 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 3.910 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.465 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _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 R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18422 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8444 _reflns_number_gt 5523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0531P)^2^+4.8627P] 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 8444 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Mn1 Mn 1.13617(12) 0.86448(11) 0.41501(10) 0.0464(3) Uani 1 1 d . . . Gd1 Gd 0.87672(3) 0.86507(3) 0.46072(3) 0.04037(13) Uani 1 1 d . . . Gd2 Gd 0.94157(4) 0.98909(4) 0.25735(3) 0.04758(14) Uani 1 1 d . . . C1 C 0.8674(9) 0.7584(7) 0.6548(7) 0.052(2) Uani 1 1 d . . . C2 C 0.9347(10) 0.6881(8) 0.7135(7) 0.060(2) Uani 1 1 d . . . H2A H 1.0190 0.6934 0.7298 0.072 Uiso 1 1 calc R . . C3 C 0.8780(11) 0.6094(8) 0.7484(8) 0.065(3) Uani 1 1 d . . . C4 C 0.7509(11) 0.5980(8) 0.7201(8) 0.069(3) Uani 1 1 d . . . C5 C 0.6876(10) 0.6663(9) 0.6588(8) 0.067(3) Uani 1 1 d . . . H5A H 0.6026 0.6579 0.6383 0.080 Uiso 1 1 calc R . . C6 C 0.7420(9) 0.7463(8) 0.6259(7) 0.056(2) Uani 1 1 d . . . C7 C 0.9566(13) 0.5394(10) 0.8173(9) 0.088(4) Uani 1 1 d . . . H7A H 1.0412 0.5582 0.8279 0.132 Uiso 1 1 calc R . . H7B H 0.9300 0.4591 0.7859 0.132 Uiso 1 1 calc R . . H7C H 0.9480 0.5569 0.8815 0.132 Uiso 1 1 calc R . . C8 C 0.6875(14) 0.5168(11) 0.7573(10) 0.103(4) Uani 1 1 d . . . H8A H 0.6008 0.5202 0.7306 0.154 Uiso 1 1 calc R . . H8B H 0.7191 0.5381 0.8302 0.154 Uiso 1 1 calc R . . H8C H 0.7020 0.4402 0.7349 0.154 Uiso 1 1 calc R . . C9 C 0.6670(9) 0.8203(9) 0.5620(7) 0.060(2) Uani 1 1 d . . . H9A H 0.5849 0.8119 0.5621 0.072 Uiso 1 1 calc R . . H9B H 0.7032 0.8999 0.5938 0.072 Uiso 1 1 calc R . . C10 C 0.5726(8) 0.8677(8) 0.3978(7) 0.056(2) Uani 1 1 d . . . H10A H 0.4928 0.8535 0.4013 0.068 Uiso 1 1 calc R . . H10B H 0.5617 0.8460 0.3269 0.068 Uiso 1 1 calc R . . C11 C 0.6217(8) 0.9955(8) 0.4398(8) 0.060(2) Uani 1 1 d . . . H11A H 0.5745 1.0380 0.3924 0.072 Uiso 1 1 calc R . . H11B H 0.6121 1.0223 0.5037 0.072 Uiso 1 1 calc R . . C12 C 0.6061(8) 0.6731(7) 0.4045(7) 0.056(2) Uani 1 1 d . . . H12A H 0.5563 0.6668 0.3334 0.068 Uiso 1 1 calc R . . H12B H 0.5531 0.6464 0.4354 0.068 Uiso 1 1 calc R . . C13 C 0.7049(8) 0.5966(8) 0.4118(8) 0.056(2) Uani 1 1 d . . . H13A H 0.7397 0.5866 0.4806 0.067 Uiso 1 1 calc R . . H13B H 0.6672 0.5216 0.3668 0.067 Uiso 1 1 calc R . . C14 C 0.9137(8) 0.5879(7) 0.4316(8) 0.055(2) Uani 1 1 d . . . H14A H 0.8978 0.5071 0.3975 0.066 Uiso 1 1 calc R . . H14B H 0.9269 0.5932 0.5022 0.066 Uiso 1 1 calc R . . C15 C 1.0297(9) 0.6416(7) 0.4270(8) 0.059(2) Uani 1 1 d . . . H15A H 1.1004 0.6148 0.4715 0.071 Uiso 1 1 calc R . . H15B H 1.0266 0.6188 0.3582 0.071 Uiso 1 1 calc R . . C16 C 0.7708(9) 0.6101(8) 0.2730(7) 0.061(2) Uani 1 1 d . . . H16A H 0.7442 0.5279 0.2485 0.073 Uiso 1 1 calc R . . H16B H 0.8439 0.6265 0.2598 0.073 Uiso 1 1 calc R . . C17 C 0.6721(9) 0.6694(8) 0.2121(7) 0.059(2) Uani 1 1 d . . . C18 C 0.5574(11) 0.6118(10) 0.1448(8) 0.077(3) Uani 1 1 d . . . H18A H 0.5404 0.5337 0.1395 0.092 Uiso 1 1 calc R . . C19 C 0.4669(11) 0.6642(11) 0.0850(8) 0.084(4) Uani 1 1 d . . . C20 C 0.4918(10) 0.7790(12) 0.0876(9) 0.083(3) Uani 1 1 d . . . C21 C 0.6075(10) 0.8396(10) 0.1535(8) 0.070(3) Uani 1 1 d . . . H21A H 0.6248 0.9167 0.1557 0.084 Uiso 1 1 calc R . . C22 C 0.6969(8) 0.7877(8) 0.2153(7) 0.055(2) Uani 1 1 d . . . C23 C 0.3378(12) 0.5982(14) 0.0162(11) 0.130(6) Uani 1 1 d . . . H23A H 0.2873 0.6492 -0.0174 0.195 Uiso 1 1 calc R . . H23B H 0.3014 0.5684 0.0569 0.195 Uiso 1 1 calc R . . H23C H 0.3445 0.5359 -0.0336 0.195 Uiso 1 1 calc R . . C24 C 0.3986(14) 0.8397(15) 0.0210(13) 0.143(7) Uani 1 1 d . . . H24A H 0.3245 0.7871 -0.0193 0.214 Uiso 1 1 calc R . . H24B H 0.4312 0.8674 -0.0229 0.214 Uiso 1 1 calc R . . H24C H 0.3809 0.9033 0.0628 0.214 Uiso 1 1 calc R . . C25 C 0.8719(19) 0.7250(12) 0.0793(12) 0.149(8) Uani 1 1 d . . . H25A H 0.8340 0.6902 0.0078 0.224 Uiso 1 1 calc R . . H25B H 0.8296 0.6910 0.1142 0.224 Uiso 1 1 calc R . . H25C H 0.9564 0.7131 0.1046 0.224 Uiso 1 1 calc R . . C26 C 0.7533(18) 1.1998(14) 0.3005(12) 0.138(6) Uani 1 1 d . . . H26A H 0.6899 1.2102 0.3266 0.206 Uiso 1 1 calc R . . H26B H 0.7223 1.2042 0.2307 0.206 Uiso 1 1 calc R . . H26C H 0.8223 1.2587 0.3396 0.206 Uiso 1 1 calc R . . C27 C 1.1839(13) 0.8597(13) 0.2257(9) 0.101(5) Uani 1 1 d . . . H27A H 1.2489 0.8217 0.2626 0.152 Uiso 1 1 calc R . . H27B H 1.2184 0.9253 0.2117 0.152 Uiso 1 1 calc R . . H27C H 1.1314 0.8075 0.1629 0.152 Uiso 1 1 calc R . . N1 N 1.2561(8) 0.7622(8) 0.4053(7) 0.070(2) Uani 1 1 d . . . N2 N 1.3069(8) 0.7124(8) 0.4663(9) 0.077(3) Uani 1 1 d . . . N3 N 1.3623(11) 0.6618(11) 0.5252(11) 0.125(5) Uani 1 1 d . . . N4 N 0.8056(7) 0.6408(6) 0.3855(6) 0.0529(18) Uani 1 1 d . . . N5 N 0.6565(6) 0.7950(6) 0.4549(6) 0.0516(18) Uani 1 1 d . . . N6 N 0.9426(10) 1.1119(8) 0.1029(6) 0.072(2) Uani 1 1 d . . . O1 O 0.9270(6) 0.8390(5) 0.6280(4) 0.0526(15) Uani 1 1 d . . . O2 O 0.8083(5) 0.8479(5) 0.2818(4) 0.0520(15) Uani 1 1 d . . . O3 O 0.7482(5) 1.0166(5) 0.4558(4) 0.0467(14) Uani 1 1 d . . . O4 O 1.0414(5) 0.7619(5) 0.4570(5) 0.0492(14) Uani 1 1 d . . . O5 O 1.0215(5) 0.9635(4) 0.4177(4) 0.0420(12) Uani 1 1 d . . . O6 O 0.7914(6) 1.0892(5) 0.3073(5) 0.0644(18) Uani 1 1 d . . . O7 O 0.8651(8) 0.8473(7) 0.0966(6) 0.090(3) Uani 1 1 d . . . O8 O 1.1134(6) 0.8962(6) 0.2857(5) 0.0645(18) Uani 1 1 d . . . O9 O 0.8533(8) 1.1041(7) 0.1324(6) 0.081(2) Uani 1 1 d . . . O10 O 1.0305(7) 1.0600(6) 0.1429(5) 0.0700(19) Uani 1 1 d . . . O11 O 0.9429(10) 1.1675(8) 0.0404(6) 0.103(3) Uani 1 1 d . . . O1W O 0.7722(14) 0.8909(13) -0.0834(9) 0.101(6) Uani 0.67(2) 1 d P . . O1W' O 0.656(3) 0.875(3) -0.142(2) 0.099(12) Uani 0.33(2) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0370(7) 0.0519(7) 0.0564(8) 0.0181(6) 0.0220(6) 0.0083(6) Gd1 0.0295(2) 0.0466(2) 0.0450(2) 0.01472(18) 0.01296(18) 0.00096(16) Gd2 0.0409(3) 0.0575(3) 0.0438(3) 0.0177(2) 0.0137(2) 0.00224(19) C1 0.054(6) 0.052(5) 0.057(5) 0.020(4) 0.023(5) 0.008(4) C2 0.058(6) 0.062(6) 0.058(6) 0.015(5) 0.022(5) -0.003(5) C3 0.077(8) 0.057(6) 0.059(6) 0.020(5) 0.023(6) -0.006(5) C4 0.082(8) 0.062(6) 0.058(6) 0.017(5) 0.026(6) -0.026(5) C5 0.046(6) 0.085(7) 0.066(6) 0.024(6) 0.019(5) -0.009(5) C6 0.052(6) 0.065(6) 0.055(5) 0.014(4) 0.027(5) -0.003(4) C7 0.115(11) 0.087(8) 0.071(7) 0.041(6) 0.033(7) 0.019(7) C8 0.114(12) 0.096(9) 0.099(10) 0.032(8) 0.043(9) -0.029(8) C9 0.046(5) 0.073(6) 0.065(6) 0.017(5) 0.027(5) 0.003(5) C10 0.030(4) 0.075(6) 0.065(6) 0.025(5) 0.016(4) 0.005(4) C11 0.029(4) 0.073(6) 0.075(7) 0.023(5) 0.014(5) 0.011(4) C12 0.045(5) 0.056(5) 0.059(6) 0.009(4) 0.016(5) -0.011(4) C13 0.044(5) 0.054(5) 0.066(6) 0.018(4) 0.017(5) -0.008(4) C14 0.038(5) 0.053(5) 0.073(6) 0.024(5) 0.017(5) 0.000(4) C15 0.056(6) 0.041(5) 0.086(7) 0.020(5) 0.030(5) 0.014(4) C16 0.056(6) 0.059(6) 0.068(6) 0.018(5) 0.024(5) 0.004(5) C17 0.061(6) 0.061(5) 0.044(5) 0.013(4) 0.009(5) -0.016(5) C18 0.069(7) 0.088(7) 0.060(7) 0.011(6) 0.018(6) -0.016(6) C19 0.059(7) 0.105(9) 0.059(7) 0.012(6) 0.000(6) -0.026(6) C20 0.042(6) 0.121(10) 0.070(7) 0.037(7) -0.002(5) 0.006(6) C21 0.055(6) 0.085(7) 0.062(6) 0.028(5) 0.009(5) 0.011(5) C22 0.042(5) 0.073(6) 0.042(5) 0.010(4) 0.009(4) -0.006(4) C23 0.064(9) 0.187(16) 0.093(10) 0.032(10) -0.012(8) -0.046(9) C24 0.084(11) 0.178(16) 0.135(14) 0.062(12) -0.006(10) 0.023(11) C25 0.25(2) 0.086(10) 0.137(14) -0.016(9) 0.135(16) -0.016(12) C26 0.178(19) 0.137(14) 0.117(13) 0.040(11) 0.073(13) 0.026(13) C27 0.108(11) 0.153(13) 0.076(8) 0.038(8) 0.063(8) 0.063(10) N1 0.068(6) 0.078(6) 0.089(7) 0.037(5) 0.048(5) 0.031(5) N2 0.044(5) 0.079(6) 0.117(8) 0.032(6) 0.036(6) 0.007(4) N3 0.077(8) 0.142(11) 0.186(13) 0.105(10) 0.047(9) 0.040(8) N4 0.041(4) 0.059(4) 0.058(5) 0.022(4) 0.014(4) 0.004(3) N5 0.035(4) 0.065(5) 0.057(5) 0.020(4) 0.019(4) 0.006(3) N6 0.079(7) 0.083(6) 0.051(5) 0.023(5) 0.019(5) 0.004(5) O1 0.051(4) 0.057(3) 0.057(4) 0.024(3) 0.023(3) 0.000(3) O2 0.045(4) 0.055(3) 0.047(3) 0.017(3) 0.007(3) -0.006(3) O3 0.026(3) 0.057(3) 0.056(3) 0.016(3) 0.014(3) 0.004(2) O4 0.042(3) 0.045(3) 0.064(4) 0.019(3) 0.022(3) 0.005(3) O5 0.031(3) 0.050(3) 0.041(3) 0.017(2) 0.008(2) 0.000(2) O6 0.063(4) 0.060(4) 0.075(5) 0.028(3) 0.025(4) 0.015(3) O7 0.112(7) 0.081(5) 0.062(5) -0.001(4) 0.032(5) -0.025(5) O8 0.062(4) 0.092(5) 0.057(4) 0.030(4) 0.035(4) 0.029(4) O9 0.073(5) 0.110(6) 0.069(5) 0.041(4) 0.026(4) 0.026(5) O10 0.061(5) 0.082(5) 0.067(5) 0.031(4) 0.019(4) 0.006(4) O11 0.137(9) 0.117(7) 0.076(5) 0.062(5) 0.043(6) 0.020(6) O1W 0.085(12) 0.174(14) 0.049(7) 0.036(8) 0.029(8) -0.003(9) O1W' 0.08(2) 0.14(2) 0.071(18) 0.013(16) 0.033(18) 0.024(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 1.859(5) . ? Mn1 O8 1.923(6) . ? Mn1 O4 1.950(6) . ? Mn1 N1 1.952(8) . ? Mn1 O3 2.062(6) 2_776 ? Mn1 Gd2 3.2734(13) . ? Mn1 Gd1 3.3677(14) . ? Mn1 Gd1 3.4254(14) 2_776 ? Gd1 O5 2.347(5) 2_776 ? Gd1 O5 2.362(6) . ? Gd1 O4 2.377(5) . ? Gd1 O1 2.379(6) . ? Gd1 O2 2.389(6) . ? Gd1 O3 2.431(5) . ? Gd1 N4 2.654(7) . ? Gd1 N5 2.655(7) . ? Gd1 Mn1 3.4254(14) 2_776 ? Gd1 Gd2 3.8390(7) 2_776 ? Gd1 Gd2 3.8629(7) . ? Gd2 O5 2.270(5) . ? Gd2 O8 2.316(6) . ? Gd2 O1 2.409(6) 2_776 ? Gd2 O2 2.418(6) . ? Gd2 O7 2.420(7) . ? Gd2 O6 2.441(7) . ? Gd2 O9 2.471(7) . ? Gd2 O10 2.525(7) . ? Gd2 Gd1 3.8390(7) 2_776 ? C1 O1 1.367(11) . ? C1 C6 1.374(13) . ? C1 C2 1.396(13) . ? C2 C3 1.406(13) . ? C2 H2A 0.9300 . ? C3 C4 1.394(15) . ? C3 C7 1.524(14) . ? C4 C5 1.381(14) . ? C4 C8 1.496(14) . ? C5 C6 1.383(13) . ? C5 H5A 0.9300 . ? C6 C9 1.504(13) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N5 1.485(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N5 1.491(11) . ? C10 C11 1.526(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O3 1.426(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N5 1.478(11) . ? C12 C13 1.513(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.481(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.457(11) . ? C14 C15 1.512(13) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O4 1.406(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.494(12) . ? C16 C17 1.499(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.386(14) . ? C17 C22 1.424(13) . ? C18 C19 1.384(16) . ? C18 H18A 0.9300 . ? C19 C20 1.384(16) . ? C19 C23 1.543(16) . ? C20 C21 1.401(15) . ? C20 C24 1.510(16) . ? C21 C22 1.385(13) . ? C21 H21A 0.9300 . ? C22 O2 1.367(10) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O7 1.452(15) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O6 1.437(16) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O8 1.439(11) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N1 N2 1.172(12) . ? N2 N3 1.175(14) . ? N6 O11 1.234(11) . ? N6 O10 1.258(11) . ? N6 O9 1.283(12) . ? O1 Gd2 2.409(6) 2_776 ? O3 Mn1 2.062(6) 2_776 ? O5 Gd1 2.347(5) 2_776 ? O1W O1W' 1.30(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 O8 85.0(2) . . ? O5 Mn1 O4 86.2(2) . . ? O8 Mn1 O4 132.8(3) . . ? O5 Mn1 N1 177.0(3) . . ? O8 Mn1 N1 92.0(3) . . ? O4 Mn1 N1 95.9(3) . . ? O5 Mn1 O3 84.2(2) . 2_776 ? O8 Mn1 O3 117.7(3) . 2_776 ? O4 Mn1 O3 107.3(2) . 2_776 ? N1 Mn1 O3 97.2(3) . 2_776 ? O5 Mn1 Gd2 42.17(16) . . ? O8 Mn1 Gd2 44.05(18) . . ? O4 Mn1 Gd2 107.62(17) . . ? N1 Mn1 Gd2 134.9(3) . . ? O3 Mn1 Gd2 111.04(16) 2_776 . ? O5 Mn1 Gd1 42.58(17) . . ? O8 Mn1 Gd1 112.4(2) . . ? O4 Mn1 Gd1 43.71(16) . . ? N1 Mn1 Gd1 139.5(3) . . ? O3 Mn1 Gd1 99.05(16) 2_776 . ? Gd2 Mn1 Gd1 71.12(3) . . ? O5 Mn1 Gd1 40.52(16) . 2_776 ? O8 Mn1 Gd1 97.9(2) . 2_776 ? O4 Mn1 Gd1 104.82(17) . 2_776 ? N1 Mn1 Gd1 140.2(3) . 2_776 ? O3 Mn1 Gd1 44.52(15) 2_776 2_776 ? Gd2 Mn1 Gd1 69.89(3) . 2_776 ? Gd1 Mn1 Gd1 70.32(3) . 2_776 ? O5 Gd1 O5 67.6(2) 2_776 . ? O5 Gd1 O4 102.65(19) 2_776 . ? O5 Gd1 O4 66.68(19) . . ? O5 Gd1 O1 69.33(19) 2_776 . ? O5 Gd1 O1 121.2(2) . . ? O4 Gd1 O1 86.2(2) . . ? O5 Gd1 O2 123.16(19) 2_776 . ? O5 Gd1 O2 67.82(19) . . ? O4 Gd1 O2 90.2(2) . . ? O1 Gd1 O2 167.5(2) . . ? O5 Gd1 O3 66.82(18) 2_776 . ? O5 Gd1 O3 95.26(18) . . ? O4 Gd1 O3 161.84(19) . . ? O1 Gd1 O3 102.7(2) . . ? O2 Gd1 O3 84.2(2) . . ? O5 Gd1 N4 157.9(2) 2_776 . ? O5 Gd1 N4 120.8(2) . . ? O4 Gd1 N4 67.0(2) . . ? O1 Gd1 N4 90.0(2) . . ? O2 Gd1 N4 77.6(2) . . ? O3 Gd1 N4 127.9(2) . . ? O5 Gd1 N5 114.6(2) 2_776 . ? O5 Gd1 N5 157.0(2) . . ? O4 Gd1 N5 130.8(2) . . ? O1 Gd1 N5 78.6(2) . . ? O2 Gd1 N5 94.8(2) . . ? O3 Gd1 N5 67.0(2) . . ? N4 Gd1 N5 66.5(2) . . ? O5 Gd1 Mn1 84.74(14) 2_776 . ? O5 Gd1 Mn1 32.17(13) . . ? O4 Gd1 Mn1 34.54(14) . . ? O1 Gd1 Mn1 107.28(15) . . ? O2 Gd1 Mn1 75.62(15) . . ? O3 Gd1 Mn1 127.43(14) . . ? N4 Gd1 Mn1 94.52(16) . . ? N5 Gd1 Mn1 160.44(16) . . ? O5 Gd1 Mn1 30.96(13) 2_776 2_776 ? O5 Gd1 Mn1 83.22(13) . 2_776 ? O4 Gd1 Mn1 133.39(14) . 2_776 ? O1 Gd1 Mn1 79.81(14) . 2_776 ? O2 Gd1 Mn1 111.02(14) . 2_776 ? O3 Gd1 Mn1 36.48(13) . 2_776 ? N4 Gd1 Mn1 155.56(16) . 2_776 ? N5 Gd1 Mn1 89.61(16) . 2_776 ? Mn1 Gd1 Mn1 109.68(3) . 2_776 ? O5 Gd1 Gd2 33.10(13) 2_776 2_776 ? O5 Gd1 Gd2 89.91(13) . 2_776 ? O4 Gd1 Gd2 90.58(14) . 2_776 ? O1 Gd1 Gd2 36.97(14) . 2_776 ? O2 Gd1 Gd2 155.25(14) . 2_776 ? O3 Gd1 Gd2 87.43(13) . 2_776 ? N4 Gd1 Gd2 125.09(16) . 2_776 ? N5 Gd1 Gd2 103.24(16) . 2_776 ? Mn1 Gd1 Gd2 91.41(3) . 2_776 ? Mn1 Gd1 Gd2 53.19(2) 2_776 2_776 ? O5 Gd1 Gd2 89.55(13) 2_776 . ? O5 Gd1 Gd2 32.74(12) . . ? O4 Gd1 Gd2 83.16(14) . . ? O1 Gd1 Gd2 153.64(15) . . ? O2 Gd1 Gd2 36.77(14) . . ? O3 Gd1 Gd2 82.04(14) . . ? N4 Gd1 Gd2 107.74(16) . . ? N5 Gd1 Gd2 126.00(16) . . ? Mn1 Gd1 Gd2 53.30(2) . . ? Mn1 Gd1 Gd2 90.13(3) 2_776 . ? Gd2 Gd1 Gd2 118.944(14) 2_776 . ? O5 Gd2 O8 67.7(2) . . ? O5 Gd2 O1 70.06(19) . 2_776 ? O8 Gd2 O1 88.7(2) . 2_776 ? O5 Gd2 O2 68.79(19) . . ? O8 Gd2 O2 98.9(2) . . ? O1 Gd2 O2 131.2(2) 2_776 . ? O5 Gd2 O7 129.3(2) . . ? O8 Gd2 O7 82.5(3) . . ? O1 Gd2 O7 151.7(2) 2_776 . ? O2 Gd2 O7 76.9(2) . . ? O5 Gd2 O6 86.8(2) . . ? O8 Gd2 O6 154.5(2) . . ? O1 Gd2 O6 80.1(2) 2_776 . ? O2 Gd2 O6 72.6(2) . . ? O7 Gd2 O6 117.4(3) . . ? O5 Gd2 O9 153.1(2) . . ? O8 Gd2 O9 129.6(2) . . ? O1 Gd2 O9 88.4(2) 2_776 . ? O2 Gd2 O9 119.8(2) . . ? O7 Gd2 O9 76.9(3) . . ? O6 Gd2 O9 73.3(2) . . ? O5 Gd2 O10 134.6(2) . . ? O8 Gd2 O10 79.2(2) . . ? O1 Gd2 O10 79.3(2) 2_776 . ? O2 Gd2 O10 149.5(2) . . ? O7 Gd2 O10 72.6(3) . . ? O6 Gd2 O10 120.5(2) . . ? O9 Gd2 O10 50.9(2) . . ? O5 Gd2 N6 151.5(2) . . ? O8 Gd2 N6 104.3(3) . . ? O1 Gd2 N6 82.7(2) 2_776 . ? O2 Gd2 N6 139.3(2) . . ? O7 Gd2 N6 73.6(3) . . ? O6 Gd2 N6 97.0(3) . . ? O9 Gd2 N6 25.7(3) . . ? O10 Gd2 N6 25.3(2) . . ? O5 Gd2 Mn1 33.35(14) . . ? O8 Gd2 Mn1 35.25(15) . . ? O1 Gd2 Mn1 82.68(14) 2_776 . ? O2 Gd2 Mn1 77.20(14) . . ? O7 Gd2 Mn1 104.2(2) . . ? O6 Gd2 Mn1 119.81(16) . . ? O9 Gd2 Mn1 162.2(2) . . ? O10 Gd2 Mn1 111.99(17) . . ? N6 Gd2 Mn1 137.0(2) . . ? O5 Gd2 Gd1 34.39(13) . 2_776 ? O8 Gd2 Gd1 80.70(16) . 2_776 ? O1 Gd2 Gd1 36.43(14) 2_776 2_776 ? O2 Gd2 Gd1 97.13(13) . 2_776 ? O7 Gd2 Gd1 161.1(2) . 2_776 ? O6 Gd2 Gd1 76.69(16) . 2_776 ? O9 Gd2 Gd1 120.82(19) . 2_776 ? O10 Gd2 Gd1 112.38(17) . 2_776 ? N6 Gd2 Gd1 119.14(18) . 2_776 ? Mn1 Gd2 Gd1 56.92(3) . 2_776 ? O5 Gd2 Gd1 34.24(14) . . ? O8 Gd2 Gd1 88.97(16) . . ? O1 Gd2 Gd1 96.52(14) 2_776 . ? O2 Gd2 Gd1 36.27(13) . . ? O7 Gd2 Gd1 110.11(19) . . ? O6 Gd2 Gd1 69.79(15) . . ? O9 Gd2 Gd1 141.27(19) . . ? O10 Gd2 Gd1 167.49(17) . . ? N6 Gd2 Gd1 166.7(2) . . ? Mn1 Gd2 Gd1 55.58(3) . . ? Gd1 Gd2 Gd1 61.057(14) 2_776 . ? O1 C1 C6 121.0(8) . . ? O1 C1 C2 119.6(9) . . ? C6 C1 C2 119.4(9) . . ? C1 C2 C3 121.5(10) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C4 C3 C2 119.2(9) . . ? C4 C3 C7 121.3(10) . . ? C2 C3 C7 119.5(11) . . ? C5 C4 C3 117.3(9) . . ? C5 C4 C8 122.0(12) . . ? C3 C4 C8 120.7(11) . . ? C4 C5 C6 124.4(10) . . ? C4 C5 H5A 117.8 . . ? C6 C5 H5A 117.8 . . ? C1 C6 C5 118.2(9) . . ? C1 C6 C9 120.4(9) . . ? C5 C6 C9 121.3(9) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 C6 115.4(8) . . ? N5 C9 H9A 108.4 . . ? C6 C9 H9A 108.4 . . ? N5 C9 H9B 108.4 . . ? C6 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? N5 C10 C11 112.3(7) . . ? N5 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N5 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? O3 C11 C10 110.8(7) . . ? O3 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N5 C12 C13 112.9(7) . . ? N5 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? N5 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? N4 C13 C12 114.3(7) . . ? N4 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? N4 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? N4 C14 C15 113.9(7) . . ? N4 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N4 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? O4 C15 C14 109.9(7) . . ? O4 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? O4 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N4 C16 C17 116.5(8) . . ? N4 C16 H16A 108.2 . . ? C17 C16 H16A 108.2 . . ? N4 C16 H16B 108.2 . . ? C17 C16 H16B 108.2 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C22 116.8(10) . . ? C18 C17 C16 122.7(9) . . ? C22 C17 C16 120.3(8) . . ? C19 C18 C17 123.5(11) . . ? C19 C18 H18A 118.2 . . ? C17 C18 H18A 118.2 . . ? C20 C19 C18 119.5(10) . . ? C20 C19 C23 119.0(12) . . ? C18 C19 C23 121.6(12) . . ? C19 C20 C21 118.6(10) . . ? C19 C20 C24 121.9(12) . . ? C21 C20 C24 119.5(12) . . ? C22 C21 C20 121.9(11) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? O2 C22 C21 121.7(9) . . ? O2 C22 C17 118.5(8) . . ? C21 C22 C17 119.7(9) . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 C27 H27A 109.5 . . ? O8 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O8 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 N1 Mn1 125.3(8) . . ? N1 N2 N3 176.5(12) . . ? C14 N4 C13 108.7(7) . . ? C14 N4 C16 108.0(7) . . ? C13 N4 C16 110.8(7) . . ? C14 N4 Gd1 105.2(5) . . ? C13 N4 Gd1 113.0(5) . . ? C16 N4 Gd1 110.8(5) . . ? C12 N5 C9 110.2(7) . . ? C12 N5 C10 108.4(7) . . ? C9 N5 C10 110.2(7) . . ? C12 N5 Gd1 116.2(5) . . ? C9 N5 Gd1 106.3(5) . . ? C10 N5 Gd1 105.3(5) . . ? O11 N6 O10 122.3(11) . . ? O11 N6 O9 122.3(10) . . ? O10 N6 O9 115.4(9) . . ? O11 N6 Gd2 177.5(8) . . ? O10 N6 Gd2 58.9(5) . . ? O9 N6 Gd2 56.5(5) . . ? C1 O1 Gd1 125.9(5) . . ? C1 O1 Gd2 125.3(5) . 2_776 ? Gd1 O1 Gd2 106.6(2) . 2_776 ? C22 O2 Gd1 121.8(5) . . ? C22 O2 Gd2 129.4(5) . . ? Gd1 O2 Gd2 107.0(2) . . ? C11 O3 Mn1 118.2(5) . 2_776 ? C11 O3 Gd1 122.6(5) . . ? Mn1 O3 Gd1 99.0(2) 2_776 . ? C15 O4 Mn1 123.0(5) . . ? C15 O4 Gd1 124.2(5) . . ? Mn1 O4 Gd1 101.8(2) . . ? Mn1 O5 Gd2 104.5(2) . . ? Mn1 O5 Gd1 108.5(2) . 2_776 ? Gd2 O5 Gd1 112.5(2) . 2_776 ? Mn1 O5 Gd1 105.2(2) . . ? Gd2 O5 Gd1 113.0(2) . . ? Gd1 O5 Gd1 112.4(2) 2_776 . ? C26 O6 Gd2 132.5(8) . . ? C25 O7 Gd2 127.8(8) . . ? C27 O8 Mn1 125.8(6) . . ? C27 O8 Gd2 133.3(6) . . ? Mn1 O8 Gd2 100.7(3) . . ? N6 O9 Gd2 97.8(6) . . ? N6 O10 Gd2 95.9(6) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.058 _refine_diff_density_min -2.537 _refine_diff_density_rms 0.183 #===End data_3 _database_code_depnum_ccdc_archive 'CCDC 876457' #TrackingRef '- C2DT30785E_ccdc_876455_876458_cif-rev.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H90 Mn2 N12 O24 Tb4' _chemical_formula_weight 2036.94 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7884(5) _cell_length_b 11.9961(6) _cell_length_c 14.5876(6) _cell_angle_alpha 101.876(2) _cell_angle_beta 111.5430(10) _cell_angle_gamma 93.304(2) _cell_volume 1857.51(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6885 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.42 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 4.163 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.269 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _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 R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18064 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.42 _reflns_number_total 8279 _reflns_number_gt 6885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0547P)^2^+0.9536P] 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 8279 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Mn1 Mn 1.13581(6) 0.86492(7) 0.41495(6) 0.03662(17) Uani 1 1 d . . . Tb1 Tb 0.876920(18) 0.864876(19) 0.460641(16) 0.03118(8) Uani 1 1 d . . . Tb2 Tb 0.94195(2) 0.98918(2) 0.258698(17) 0.03745(9) Uani 1 1 d . . . C1 C 0.8694(4) 0.7582(5) 0.6542(4) 0.0383(11) Uani 1 1 d . . . C2 C 0.9353(5) 0.6873(5) 0.7131(4) 0.0476(13) Uani 1 1 d . . . H2A H 1.0198 0.6921 0.7294 0.057 Uiso 1 1 calc R . . C3 C 0.8794(6) 0.6098(5) 0.7484(4) 0.0546(14) Uani 1 1 d . . . C4 C 0.7511(6) 0.5992(6) 0.7198(4) 0.0583(16) Uani 1 1 d . . . C5 C 0.6866(5) 0.6665(5) 0.6593(4) 0.0527(14) Uani 1 1 d . . . H5A H 0.6015 0.6579 0.6396 0.063 Uiso 1 1 calc R . . C6 C 0.7413(5) 0.7474(5) 0.6255(4) 0.0452(12) Uani 1 1 d . . . C7 C 0.9583(7) 0.5421(6) 0.8195(5) 0.074(2) Uani 1 1 d . . . H7A H 1.0432 0.5609 0.8301 0.111 Uiso 1 1 calc R . . H7B H 0.9321 0.4611 0.7896 0.111 Uiso 1 1 calc R . . H7C H 0.9494 0.5617 0.8834 0.111 Uiso 1 1 calc R . . C8 C 0.6873(8) 0.5169(7) 0.7586(6) 0.087(3) Uani 1 1 d . . . H8A H 0.6002 0.5198 0.7322 0.131 Uiso 1 1 calc R . . H8B H 0.7194 0.5392 0.8316 0.131 Uiso 1 1 calc R . . H8C H 0.7019 0.4400 0.7367 0.131 Uiso 1 1 calc R . . C9 C 0.6668(5) 0.8216(5) 0.5631(4) 0.0465(12) Uani 1 1 d . . . H9A H 0.5843 0.8128 0.5627 0.056 Uiso 1 1 calc R . . H9B H 0.7031 0.9015 0.5953 0.056 Uiso 1 1 calc R . . C10 C 0.5722(4) 0.8675(5) 0.3974(4) 0.0459(12) Uani 1 1 d . . . H10A H 0.4923 0.8535 0.4010 0.055 Uiso 1 1 calc R . . H10B H 0.5611 0.8445 0.3265 0.055 Uiso 1 1 calc R . . C11 C 0.6211(4) 0.9949(5) 0.4380(5) 0.0489(13) Uani 1 1 d . . . H11A H 0.5744 1.0365 0.3896 0.059 Uiso 1 1 calc R . . H11B H 0.6106 1.0230 0.5012 0.059 Uiso 1 1 calc R . . C12 C 0.6056(4) 0.6734(5) 0.4037(4) 0.0474(13) Uani 1 1 d . . . H12A H 0.5573 0.6678 0.3325 0.057 Uiso 1 1 calc R . . H12B H 0.5506 0.6468 0.4330 0.057 Uiso 1 1 calc R . . C13 C 0.7035(5) 0.5950(5) 0.4117(4) 0.0461(12) Uani 1 1 d . . . H13A H 0.7385 0.5859 0.4807 0.055 Uiso 1 1 calc R . . H13B H 0.6652 0.5196 0.3670 0.055 Uiso 1 1 calc R . . C14 C 0.9151(4) 0.5875(5) 0.4342(5) 0.0464(12) Uani 1 1 d . . . H14A H 0.9003 0.5058 0.4019 0.056 Uiso 1 1 calc R . . H14B H 0.9286 0.5956 0.5051 0.056 Uiso 1 1 calc R . . C15 C 1.0301(5) 0.6424(5) 0.4276(5) 0.0504(14) Uani 1 1 d . . . H15A H 1.1022 0.6169 0.4719 0.061 Uiso 1 1 calc R . . H15B H 1.0258 0.6188 0.3586 0.061 Uiso 1 1 calc R . . C16 C 0.7697(5) 0.6085(5) 0.2720(4) 0.0497(13) Uani 1 1 d . . . H16A H 0.8432 0.6241 0.2588 0.060 Uiso 1 1 calc R . . H16B H 0.7415 0.5264 0.2471 0.060 Uiso 1 1 calc R . . C17 C 0.6726(5) 0.6696(5) 0.2129(4) 0.0458(12) Uani 1 1 d . . . C18 C 0.5561(6) 0.6102(6) 0.1450(4) 0.0606(16) Uani 1 1 d . . . H18A H 0.5388 0.5321 0.1400 0.073 Uiso 1 1 calc R . . C19 C 0.4659(6) 0.6632(7) 0.0850(5) 0.071(2) Uani 1 1 d . . . C20 C 0.4946(5) 0.7802(7) 0.0885(5) 0.072(2) Uani 1 1 d . . . C21 C 0.6102(5) 0.8399(6) 0.1543(4) 0.0546(14) Uani 1 1 d . . . H21A H 0.6286 0.9171 0.1565 0.065 Uiso 1 1 calc R . . C22 C 0.6992(5) 0.7874(5) 0.2172(4) 0.0451(12) Uani 1 1 d . . . C23 C 0.3371(7) 0.5964(9) 0.0171(6) 0.107(4) Uani 1 1 d . . . H23A H 0.2860 0.6469 -0.0168 0.160 Uiso 1 1 calc R . . H23B H 0.3010 0.5669 0.0581 0.160 Uiso 1 1 calc R . . H23C H 0.3438 0.5336 -0.0325 0.160 Uiso 1 1 calc R . . C24 C 0.4007(7) 0.8399(9) 0.0202(8) 0.120(4) Uani 1 1 d . . . H24A H 0.3265 0.7865 -0.0200 0.180 Uiso 1 1 calc R . . H24B H 0.4337 0.8668 -0.0238 0.180 Uiso 1 1 calc R . . H24C H 0.3824 0.9041 0.0612 0.180 Uiso 1 1 calc R . . C25 C 0.8761(12) 0.7278(9) 0.0834(8) 0.123(4) Uani 1 1 d . . . H25A H 0.8389 0.6910 0.0122 0.185 Uiso 1 1 calc R . . H25B H 0.8358 0.6926 0.1189 0.185 Uiso 1 1 calc R . . H25C H 0.9619 0.7195 0.1091 0.185 Uiso 1 1 calc R . . C26 C 0.7527(8) 1.1965(8) 0.3009(7) 0.093(3) Uani 1 1 d . . . H26A H 0.6893 1.2057 0.3272 0.140 Uiso 1 1 calc R . . H26B H 0.7211 1.2014 0.2313 0.140 Uiso 1 1 calc R . . H26C H 0.8215 1.2561 0.3403 0.140 Uiso 1 1 calc R . . C27 C 1.1833(7) 0.8620(8) 0.2255(5) 0.087(3) Uani 1 1 d . . . H27A H 1.2487 0.8239 0.2617 0.130 Uiso 1 1 calc R . . H27B H 1.2177 0.9283 0.2120 0.130 Uiso 1 1 calc R . . H27C H 1.1305 0.8100 0.1625 0.130 Uiso 1 1 calc R . . N1 N 1.2568(4) 0.7623(5) 0.4061(4) 0.0567(13) Uani 1 1 d . . . N2 N 1.3078(4) 0.7123(5) 0.4662(5) 0.0617(14) Uani 1 1 d . . . N3 N 1.3606(6) 0.6604(8) 0.5227(7) 0.106(3) Uani 1 1 d . . . N4 N 0.8043(4) 0.6400(4) 0.3847(3) 0.0391(9) Uani 1 1 d . . . N5 N 0.6572(3) 0.7960(4) 0.4557(3) 0.0407(9) Uani 1 1 d . . . N6 N 0.9414(5) 1.1104(5) 0.1043(4) 0.0614(14) Uani 1 1 d . . . O1 O 0.9267(3) 0.8388(3) 0.6260(3) 0.0408(8) Uani 1 1 d . . . O2 O 0.8095(3) 0.8469(3) 0.2824(2) 0.0406(8) Uani 1 1 d . . . O3 O 0.7482(3) 1.0159(3) 0.4550(2) 0.0379(7) Uani 1 1 d . . . O4 O 1.0404(3) 0.7627(3) 0.4567(3) 0.0392(8) Uani 1 1 d . . . O5 O 1.0205(3) 0.9639(3) 0.4179(2) 0.0326(7) Uani 1 1 d . . . O6 O 0.7908(4) 1.0889(3) 0.3065(3) 0.0517(9) Uani 1 1 d . . . H6 H 0.7739 1.0410 0.3455 0.07(2) Uiso 1 1 d R . . O7 O 0.8640(5) 0.8474(4) 0.0984(3) 0.0748(14) Uani 1 1 d . . . O8 O 1.1139(4) 0.8972(4) 0.2854(3) 0.0568(11) Uani 1 1 d . . . O9 O 0.8519(4) 1.1030(4) 0.1336(3) 0.0682(12) Uani 1 1 d . . . O10 O 1.0308(4) 1.0602(4) 0.1450(3) 0.0562(10) Uani 1 1 d . . . O11 O 0.9398(6) 1.1666(5) 0.0428(4) 0.0896(17) Uani 1 1 d . . . O1W O 0.7755(8) 0.8897(9) -0.0807(5) 0.091(4) Uani 0.665(14) 1 d P . . O1W' O 0.6606(18) 0.8739(16) -0.1402(13) 0.095(7) Uani 0.335(14) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0333(3) 0.0395(4) 0.0414(4) 0.0130(3) 0.0171(3) 0.0087(3) Tb1 0.02668(12) 0.03518(15) 0.03100(14) 0.00985(10) 0.00983(10) 0.00219(9) Tb2 0.03654(13) 0.04529(17) 0.02955(14) 0.01242(11) 0.01032(11) 0.00365(10) C1 0.039(2) 0.044(3) 0.033(3) 0.012(2) 0.015(2) 0.001(2) C2 0.046(3) 0.054(4) 0.042(3) 0.017(3) 0.015(2) 0.002(2) C3 0.075(4) 0.044(3) 0.045(3) 0.016(3) 0.022(3) 0.003(3) C4 0.070(4) 0.059(4) 0.043(3) 0.014(3) 0.022(3) -0.012(3) C5 0.043(3) 0.073(4) 0.041(3) 0.015(3) 0.017(2) -0.008(3) C6 0.042(3) 0.054(3) 0.038(3) 0.010(2) 0.017(2) -0.003(2) C7 0.102(5) 0.059(4) 0.057(4) 0.031(3) 0.018(4) 0.008(4) C8 0.103(6) 0.083(6) 0.075(5) 0.026(4) 0.035(5) -0.026(5) C9 0.039(2) 0.057(4) 0.047(3) 0.011(2) 0.023(2) 0.000(2) C10 0.027(2) 0.062(4) 0.048(3) 0.016(3) 0.013(2) 0.006(2) C11 0.030(2) 0.060(4) 0.062(4) 0.022(3) 0.019(2) 0.014(2) C12 0.035(2) 0.051(3) 0.052(3) 0.007(3) 0.018(2) -0.005(2) C13 0.045(3) 0.043(3) 0.051(3) 0.011(2) 0.020(3) -0.004(2) C14 0.043(3) 0.031(3) 0.062(4) 0.016(2) 0.014(3) 0.004(2) C15 0.045(3) 0.038(3) 0.075(4) 0.023(3) 0.025(3) 0.013(2) C16 0.054(3) 0.044(3) 0.049(3) 0.005(2) 0.021(3) 0.001(2) C17 0.050(3) 0.044(3) 0.034(3) 0.001(2) 0.011(2) -0.006(2) C18 0.058(3) 0.068(4) 0.043(3) 0.003(3) 0.015(3) -0.015(3) C19 0.044(3) 0.102(6) 0.045(4) 0.012(4) 0.000(3) -0.019(3) C20 0.040(3) 0.108(6) 0.054(4) 0.030(4) -0.001(3) 0.005(3) C21 0.045(3) 0.066(4) 0.045(3) 0.021(3) 0.006(3) 0.004(3) C22 0.042(3) 0.060(4) 0.032(3) 0.011(2) 0.013(2) 0.004(2) C23 0.058(4) 0.174(10) 0.049(4) 0.005(5) -0.003(4) -0.040(5) C24 0.069(5) 0.150(10) 0.107(8) 0.048(7) -0.016(5) 0.028(5) C25 0.188(12) 0.087(8) 0.108(8) -0.003(6) 0.092(8) -0.008(7) C26 0.100(6) 0.114(8) 0.079(6) 0.036(5) 0.041(5) 0.028(5) C27 0.093(5) 0.147(8) 0.055(4) 0.042(5) 0.052(4) 0.061(5) N1 0.056(3) 0.062(3) 0.071(4) 0.029(3) 0.036(3) 0.026(2) N2 0.040(2) 0.069(4) 0.084(4) 0.026(3) 0.029(3) 0.010(2) N3 0.060(4) 0.138(7) 0.143(7) 0.090(6) 0.032(4) 0.033(4) N4 0.038(2) 0.036(2) 0.043(2) 0.0120(18) 0.0146(19) 0.0011(17) N5 0.0277(18) 0.045(3) 0.048(3) 0.0119(19) 0.0125(18) 0.0027(16) N6 0.079(4) 0.069(4) 0.036(3) 0.022(2) 0.018(3) 0.007(3) O1 0.0385(17) 0.049(2) 0.0364(19) 0.0188(16) 0.0132(15) 0.0007(15) O2 0.0376(16) 0.049(2) 0.0287(18) 0.0096(15) 0.0063(14) -0.0021(15) O3 0.0271(15) 0.049(2) 0.0366(18) 0.0128(15) 0.0101(14) 0.0064(14) O4 0.0366(16) 0.037(2) 0.050(2) 0.0164(16) 0.0197(16) 0.0090(14) O5 0.0318(15) 0.0389(19) 0.0317(17) 0.0136(14) 0.0145(14) 0.0070(13) O6 0.058(2) 0.053(3) 0.058(3) 0.027(2) 0.030(2) 0.0206(18) O7 0.104(4) 0.059(3) 0.051(3) -0.007(2) 0.033(3) -0.018(3) O8 0.061(2) 0.076(3) 0.052(2) 0.027(2) 0.035(2) 0.030(2) O9 0.064(3) 0.096(4) 0.055(3) 0.037(3) 0.024(2) 0.023(2) O10 0.061(2) 0.065(3) 0.048(2) 0.020(2) 0.024(2) 0.010(2) O11 0.119(4) 0.101(4) 0.059(3) 0.044(3) 0.035(3) 0.007(3) O1W 0.075(6) 0.167(9) 0.033(4) 0.026(4) 0.025(4) 0.000(5) O1W' 0.103(16) 0.112(15) 0.064(11) -0.004(9) 0.039(11) 0.022(11) _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 Mn1 O5 1.862(3) . ? Mn1 O8 1.934(4) . ? Mn1 O4 1.947(3) . ? Mn1 N1 1.959(5) . ? Mn1 O3 2.065(3) 2_776 ? Mn1 Tb2 3.2566(8) . ? Mn1 Tb1 3.3544(7) . ? Mn1 Tb1 3.4143(8) 2_776 ? Tb1 O5 2.337(3) 2_776 ? Tb1 O5 2.347(3) . ? Tb1 O4 2.354(3) . ? Tb1 O1 2.356(3) . ? Tb1 O2 2.381(3) . ? Tb1 O3 2.424(3) . ? Tb1 N5 2.643(4) . ? Tb1 N4 2.654(4) . ? Tb1 Mn1 3.4143(8) 2_776 ? Tb1 Tb2 3.8191(3) 2_776 ? Tb1 Tb2 3.8502(3) . ? Tb2 O5 2.256(3) . ? Tb2 O8 2.309(4) . ? Tb2 O1 2.403(4) 2_776 ? Tb2 O2 2.409(3) . ? Tb2 O7 2.410(4) . ? Tb2 O6 2.430(4) . ? Tb2 O9 2.468(4) . ? Tb2 O10 2.515(4) . ? Tb2 Tb1 3.8191(3) 2_776 ? C1 O1 1.362(5) . ? C1 C2 1.397(7) . ? C1 C6 1.400(7) . ? C2 C3 1.393(7) . ? C2 H2A 0.9300 . ? C3 C4 1.403(9) . ? C3 C7 1.525(8) . ? C4 C5 1.371(9) . ? C4 C8 1.524(8) . ? C5 C6 1.401(7) . ? C5 H5A 0.9300 . ? C6 C9 1.493(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N5 1.492(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N5 1.497(6) . ? C10 C11 1.515(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O3 1.424(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N5 1.486(7) . ? C12 C13 1.516(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.490(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.488(6) . ? C14 C15 1.516(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O4 1.403(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.491(8) . ? C16 N4 1.498(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.404(7) . ? C17 C22 1.413(8) . ? C18 C19 1.387(10) . ? C18 H18A 0.9300 . ? C19 C20 1.411(10) . ? C19 C23 1.535(8) . ? C20 C21 1.391(8) . ? C20 C24 1.519(10) . ? C21 C22 1.396(8) . ? C21 H21A 0.9300 . ? C22 O2 1.345(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O7 1.430(11) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O6 1.399(9) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O8 1.423(6) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N1 N2 1.167(7) . ? N2 N3 1.155(8) . ? N6 O11 1.223(6) . ? N6 O10 1.260(7) . ? N6 O9 1.279(7) . ? O1 Tb2 2.403(4) 2_776 ? O3 Mn1 2.065(3) 2_776 ? O5 Tb1 2.337(3) 2_776 ? O6 H6 0.9484 . ? O1W O1W' 1.289(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 O8 85.28(15) . . ? O5 Mn1 O4 85.79(14) . . ? O8 Mn1 O4 133.15(19) . . ? O5 Mn1 N1 177.44(18) . . ? O8 Mn1 N1 92.17(19) . . ? O4 Mn1 N1 96.08(18) . . ? O5 Mn1 O3 84.20(14) . 2_776 ? O8 Mn1 O3 117.76(17) . 2_776 ? O4 Mn1 O3 106.89(14) . 2_776 ? N1 Mn1 O3 96.89(19) . 2_776 ? O5 Mn1 Tb2 42.20(9) . . ? O8 Mn1 Tb2 44.30(11) . . ? O4 Mn1 Tb2 107.45(10) . . ? N1 Mn1 Tb2 135.33(16) . . ? O3 Mn1 Tb2 111.10(10) 2_776 . ? O5 Mn1 Tb1 42.51(9) . . ? O8 Mn1 Tb1 112.75(12) . . ? O4 Mn1 Tb1 43.33(10) . . ? N1 Mn1 Tb1 139.26(15) . . ? O3 Mn1 Tb1 98.81(9) 2_776 . ? Tb2 Mn1 Tb1 71.220(15) . . ? O5 Mn1 Tb1 40.55(10) . 2_776 ? O8 Mn1 Tb1 97.83(13) . 2_776 ? O4 Mn1 Tb1 104.50(11) . 2_776 ? N1 Mn1 Tb1 140.04(17) . 2_776 ? O3 Mn1 Tb1 44.58(9) 2_776 2_776 ? Tb2 Mn1 Tb1 69.802(16) . 2_776 ? Tb1 Mn1 Tb1 70.293(15) . 2_776 ? O5 Tb1 O5 67.43(12) 2_776 . ? O5 Tb1 O4 102.46(11) 2_776 . ? O5 Tb1 O4 66.97(11) . . ? O5 Tb1 O1 69.44(12) 2_776 . ? O5 Tb1 O1 121.45(11) . . ? O4 Tb1 O1 86.27(12) . . ? O5 Tb1 O2 123.26(11) 2_776 . ? O5 Tb1 O2 67.54(11) . . ? O4 Tb1 O2 89.86(12) . . ? O1 Tb1 O2 167.29(12) . . ? O5 Tb1 O3 67.24(11) 2_776 . ? O5 Tb1 O3 94.84(11) . . ? O4 Tb1 O3 161.75(11) . . ? O1 Tb1 O3 103.01(12) . . ? O2 Tb1 O3 84.17(12) . . ? O5 Tb1 N5 114.32(12) 2_776 . ? O5 Tb1 N5 156.68(12) . . ? O4 Tb1 N5 131.16(12) . . ? O1 Tb1 N5 78.30(12) . . ? O2 Tb1 N5 95.34(12) . . ? O3 Tb1 N5 66.75(12) . . ? O5 Tb1 N4 157.94(12) 2_776 . ? O5 Tb1 N4 121.14(12) . . ? O4 Tb1 N4 67.28(12) . . ? O1 Tb1 N4 89.93(12) . . ? O2 Tb1 N4 77.42(12) . . ? O3 Tb1 N4 127.53(12) . . ? N5 Tb1 N4 66.68(13) . . ? O5 Tb1 Mn1 84.56(7) 2_776 . ? O5 Tb1 Mn1 32.42(8) . . ? O4 Tb1 Mn1 34.58(8) . . ? O1 Tb1 Mn1 107.42(8) . . ? O2 Tb1 Mn1 75.25(8) . . ? O3 Tb1 Mn1 127.26(7) . . ? N5 Tb1 Mn1 160.88(10) . . ? N4 Tb1 Mn1 94.75(8) . . ? O5 Tb1 Mn1 31.20(8) 2_776 2_776 ? O5 Tb1 Mn1 83.05(8) . 2_776 ? O4 Tb1 Mn1 133.44(9) . 2_776 ? O1 Tb1 Mn1 79.87(9) . 2_776 ? O2 Tb1 Mn1 111.28(9) . 2_776 ? O3 Tb1 Mn1 36.72(8) . 2_776 ? N5 Tb1 Mn1 89.15(10) . 2_776 ? N4 Tb1 Mn1 155.32(8) . 2_776 ? Mn1 Tb1 Mn1 109.707(15) . 2_776 ? O5 Tb1 Tb2 33.07(7) 2_776 2_776 ? O5 Tb1 Tb2 90.04(8) . 2_776 ? O4 Tb1 Tb2 90.69(9) . 2_776 ? O1 Tb1 Tb2 37.06(9) . 2_776 ? O2 Tb1 Tb2 155.29(8) . 2_776 ? O3 Tb1 Tb2 87.68(8) . 2_776 ? N5 Tb1 Tb2 102.79(9) . 2_776 ? N4 Tb1 Tb2 125.19(9) . 2_776 ? Mn1 Tb1 Tb2 91.544(14) . 2_776 ? Mn1 Tb1 Tb2 53.158(13) 2_776 2_776 ? O5 Tb1 Tb2 89.43(7) 2_776 . ? O5 Tb1 Tb2 32.49(8) . . ? O4 Tb1 Tb2 83.14(8) . . ? O1 Tb1 Tb2 153.69(8) . . ? O2 Tb1 Tb2 36.76(8) . . ? O3 Tb1 Tb2 81.76(7) . . ? N5 Tb1 Tb2 126.18(9) . . ? N4 Tb1 Tb2 107.84(9) . . ? Mn1 Tb1 Tb2 53.207(13) . . ? Mn1 Tb1 Tb2 90.100(14) 2_776 . ? Tb2 Tb1 Tb2 118.925(7) 2_776 . ? O5 Tb2 O8 68.58(12) . . ? O5 Tb2 O1 69.95(11) . 2_776 ? O8 Tb2 O1 88.78(14) . 2_776 ? O5 Tb2 O2 68.51(11) . . ? O8 Tb2 O2 98.94(14) . . ? O1 Tb2 O2 131.14(11) 2_776 . ? O5 Tb2 O7 129.34(15) . . ? O8 Tb2 O7 82.57(17) . . ? O1 Tb2 O7 152.24(13) 2_776 . ? O2 Tb2 O7 76.43(13) . . ? O5 Tb2 O6 87.22(12) . . ? O8 Tb2 O6 155.68(13) . . ? O1 Tb2 O6 80.33(13) 2_776 . ? O2 Tb2 O6 73.14(13) . . ? O7 Tb2 O6 116.49(16) . . ? O5 Tb2 O9 153.18(15) . . ? O8 Tb2 O9 129.31(14) . . ? O1 Tb2 O9 88.99(14) 2_776 . ? O2 Tb2 O9 119.59(14) . . ? O7 Tb2 O9 76.59(18) . . ? O6 Tb2 O9 72.56(13) . . ? O5 Tb2 O10 134.95(12) . . ? O8 Tb2 O10 78.66(14) . . ? O1 Tb2 O10 79.56(13) 2_776 . ? O2 Tb2 O10 149.30(13) . . ? O7 Tb2 O10 72.90(15) . . ? O6 Tb2 O10 119.97(13) . . ? O9 Tb2 O10 51.21(14) . . ? O5 Tb2 N6 152.11(14) . . ? O8 Tb2 N6 103.90(15) . . ? O1 Tb2 N6 83.37(13) 2_776 . ? O2 Tb2 N6 138.95(14) . . ? O7 Tb2 N6 73.31(16) . . ? O6 Tb2 N6 96.41(14) . . ? O9 Tb2 N6 25.77(15) . . ? O10 Tb2 N6 25.44(14) . . ? O5 Tb2 Mn1 33.68(8) . . ? O8 Tb2 Mn1 35.80(9) . . ? O1 Tb2 Mn1 82.66(8) 2_776 . ? O2 Tb2 Mn1 76.90(8) . . ? O7 Tb2 Mn1 104.30(14) . . ? O6 Tb2 Mn1 120.51(9) . . ? O9 Tb2 Mn1 162.65(10) . . ? O10 Tb2 Mn1 112.02(10) . . ? N6 Tb2 Mn1 137.29(12) . . ? O5 Tb2 Tb1 34.43(8) . 2_776 ? O8 Tb2 Tb1 81.13(11) . 2_776 ? O1 Tb2 Tb1 36.21(7) 2_776 2_776 ? O2 Tb2 Tb1 97.18(8) . 2_776 ? O7 Tb2 Tb1 161.34(14) . 2_776 ? O6 Tb2 Tb1 77.24(10) . 2_776 ? O9 Tb2 Tb1 121.13(12) . 2_776 ? O10 Tb2 Tb1 112.43(10) . 2_776 ? N6 Tb2 Tb1 119.58(11) . 2_776 ? Mn1 Tb2 Tb1 57.039(15) . 2_776 ? O5 Tb2 Tb1 33.99(8) . . ? O8 Tb2 Tb1 89.53(9) . . ? O1 Tb2 Tb1 96.33(7) 2_776 . ? O2 Tb2 Tb1 36.27(8) . . ? O7 Tb2 Tb1 109.86(11) . . ? O6 Tb2 Tb1 70.35(9) . . ? O9 Tb2 Tb1 140.99(10) . . ? O10 Tb2 Tb1 167.52(10) . . ? N6 Tb2 Tb1 166.55(12) . . ? Mn1 Tb2 Tb1 55.573(13) . . ? Tb1 Tb2 Tb1 61.075(7) 2_776 . ? O1 C1 C2 121.7(4) . . ? O1 C1 C6 119.3(5) . . ? C2 C1 C6 118.9(4) . . ? C3 C2 C1 122.5(5) . . ? C3 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? C2 C3 C4 118.5(5) . . ? C2 C3 C7 119.7(6) . . ? C4 C3 C7 121.8(5) . . ? C5 C4 C3 118.6(5) . . ? C5 C4 C8 121.5(6) . . ? C3 C4 C8 119.9(6) . . ? C4 C5 C6 123.9(5) . . ? C4 C5 H5A 118.1 . . ? C6 C5 H5A 118.1 . . ? C1 C6 C5 117.5(5) . . ? C1 C6 C9 121.0(4) . . ? C5 C6 C9 121.5(5) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 C6 114.6(4) . . ? N5 C9 H9A 108.6 . . ? C6 C9 H9A 108.6 . . ? N5 C9 H9B 108.6 . . ? C6 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N5 C10 C11 112.0(4) . . ? N5 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? N5 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O3 C11 C10 110.9(4) . . ? O3 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N5 C12 C13 113.3(4) . . ? N5 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N5 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N4 C13 C12 112.7(4) . . ? N4 C13 H13A 109.0 . . ? C12 C13 H13A 109.0 . . ? N4 C13 H13B 109.0 . . ? C12 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N4 C14 C15 112.5(4) . . ? N4 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N4 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? O4 C15 C14 109.8(4) . . ? O4 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? O4 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 C16 N4 115.5(5) . . ? C17 C16 H16A 108.4 . . ? N4 C16 H16A 108.4 . . ? C17 C16 H16B 108.4 . . ? N4 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? C18 C17 C22 118.0(5) . . ? C18 C17 C16 121.3(6) . . ? C22 C17 C16 120.5(5) . . ? C19 C18 C17 122.8(6) . . ? C19 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C18 C19 C20 118.5(5) . . ? C18 C19 C23 120.8(8) . . ? C20 C19 C23 120.7(7) . . ? C21 C20 C19 119.4(6) . . ? C21 C20 C24 120.4(7) . . ? C19 C20 C24 120.3(6) . . ? C20 C21 C22 121.9(6) . . ? C20 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? O2 C22 C21 121.3(5) . . ? O2 C22 C17 119.4(5) . . ? C21 C22 C17 119.3(5) . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 C27 H27A 109.5 . . ? O8 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O8 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 N1 Mn1 126.3(4) . . ? N3 N2 N1 177.0(7) . . ? C14 N4 C13 107.7(4) . . ? C14 N4 C16 109.1(4) . . ? C13 N4 C16 111.3(4) . . ? C14 N4 Tb1 104.2(3) . . ? C13 N4 Tb1 113.3(3) . . ? C16 N4 Tb1 111.0(3) . . ? C12 N5 C9 110.8(4) . . ? C12 N5 C10 107.1(4) . . ? C9 N5 C10 110.4(4) . . ? C12 N5 Tb1 115.8(3) . . ? C9 N5 Tb1 107.0(3) . . ? C10 N5 Tb1 105.6(3) . . ? O11 N6 O10 123.1(6) . . ? O11 N6 O9 120.8(6) . . ? O10 N6 O9 116.0(5) . . ? O11 N6 Tb2 176.4(5) . . ? O10 N6 Tb2 59.0(3) . . ? O9 N6 Tb2 57.0(3) . . ? C1 O1 Tb1 127.1(3) . . ? C1 O1 Tb2 124.2(3) . 2_776 ? Tb1 O1 Tb2 106.73(12) . 2_776 ? C22 O2 Tb1 121.4(3) . . ? C22 O2 Tb2 129.6(3) . . ? Tb1 O2 Tb2 106.97(13) . . ? C11 O3 Mn1 118.3(3) . 2_776 ? C11 O3 Tb1 122.9(3) . . ? Mn1 O3 Tb1 98.70(12) 2_776 . ? C15 O4 Mn1 122.6(3) . . ? C15 O4 Tb1 124.8(3) . . ? Mn1 O4 Tb1 102.09(14) . . ? Mn1 O5 Tb2 104.12(14) . . ? Mn1 O5 Tb1 108.25(14) . 2_776 ? Tb2 O5 Tb1 112.50(13) . 2_776 ? Mn1 O5 Tb1 105.07(14) . . ? Tb2 O5 Tb1 113.52(13) . . ? Tb1 O5 Tb1 112.57(12) 2_776 . ? C26 O6 Tb2 133.7(4) . . ? C26 O6 H6 125.5 . . ? Tb2 O6 H6 99.6 . . ? C25 O7 Tb2 126.3(5) . . ? C27 O8 Mn1 126.6(4) . . ? C27 O8 Tb2 133.3(4) . . ? Mn1 O8 Tb2 99.90(15) . . ? N6 O9 Tb2 97.2(3) . . ? N6 O10 Tb2 95.5(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.242 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.145 #===End data_4 _database_code_depnum_ccdc_archive 'CCDC 876458' #TrackingRef '- C2DT30785E_ccdc_876455_876458_cif-rev.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H90 Dy4 Mn2 N12 O24' _chemical_formula_weight 2051.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mn Mn 0.3368 0.7283 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7766(10) _cell_length_b 12.0196(12) _cell_length_c 14.5690(14) _cell_angle_alpha 101.719(3) _cell_angle_beta 111.565(2) _cell_angle_gamma 93.299(3) _cell_volume 1858.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6026 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.46 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 4.377 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.496 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _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 R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13104 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7672 _reflns_number_gt 6026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0657P)^2^+11.7951P] 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 7672 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Mn1 Mn 1.13479(12) 0.86543(13) 0.41477(10) 0.0373(3) Uani 1 1 d . . . Dy1 Dy 0.87687(3) 0.86536(4) 0.46067(3) 0.03163(13) Uani 1 1 d . . . Dy2 Dy 0.94201(4) 0.99002(4) 0.25964(3) 0.03767(14) Uani 1 1 d . . . C1 C 0.8683(9) 0.7592(10) 0.6546(7) 0.044(2) Uani 1 1 d . . . C2 C 0.9340(9) 0.6873(10) 0.7118(8) 0.048(2) Uani 1 1 d . . . H2A H 1.0183 0.6917 0.7273 0.057 Uiso 1 1 calc R . . C3 C 0.8783(11) 0.6083(11) 0.7471(8) 0.058(3) Uani 1 1 d . . . C4 C 0.7512(11) 0.5989(10) 0.7203(8) 0.056(3) Uani 1 1 d . . . C5 C 0.6857(10) 0.6681(11) 0.6590(8) 0.057(3) Uani 1 1 d . . . H5A H 0.6003 0.6595 0.6388 0.068 Uiso 1 1 calc R . . C6 C 0.7411(9) 0.7493(10) 0.6266(7) 0.049(2) Uani 1 1 d . . . C7 C 0.9589(13) 0.5418(11) 0.8179(10) 0.071(3) Uani 1 1 d . . . H7A H 1.0435 0.5613 0.8279 0.107 Uiso 1 1 calc R . . H7B H 0.9334 0.4609 0.7884 0.107 Uiso 1 1 calc R . . H7C H 0.9506 0.5610 0.8822 0.107 Uiso 1 1 calc R . . C8 C 0.6842(14) 0.5180(14) 0.7579(12) 0.086(4) Uani 1 1 d . . . H8A H 0.5974 0.5224 0.7305 0.128 Uiso 1 1 calc R . . H8B H 0.7152 0.5398 0.8308 0.128 Uiso 1 1 calc R . . H8C H 0.6977 0.4408 0.7361 0.128 Uiso 1 1 calc R . . C9 C 0.6670(9) 0.8225(9) 0.5632(7) 0.045(2) Uani 1 1 d . . . H9A H 0.7040 0.9021 0.5945 0.055 Uiso 1 1 calc R . . H9B H 0.5847 0.8148 0.5636 0.055 Uiso 1 1 calc R . . C10 C 0.5721(8) 0.8690(10) 0.3972(8) 0.048(2) Uani 1 1 d . . . H10A H 0.4920 0.8560 0.4007 0.057 Uiso 1 1 calc R . . H10B H 0.5609 0.8462 0.3263 0.057 Uiso 1 1 calc R . . C11 C 0.6228(8) 0.9973(9) 0.4383(8) 0.045(2) Uani 1 1 d . . . H11A H 0.5765 1.0394 0.3901 0.054 Uiso 1 1 calc R . . H11B H 0.6129 1.0255 0.5018 0.054 Uiso 1 1 calc R . . C12 C 0.6036(8) 0.6694(9) 0.4033(7) 0.045(2) Uani 1 1 d . . . H12A H 0.5504 0.6424 0.4341 0.054 Uiso 1 1 calc R . . H12B H 0.5538 0.6625 0.3321 0.054 Uiso 1 1 calc R . . C13 C 0.7028(9) 0.5952(10) 0.4116(8) 0.051(2) Uani 1 1 d . . . H13A H 0.7381 0.5865 0.4808 0.061 Uiso 1 1 calc R . . H13B H 0.6658 0.5197 0.3673 0.061 Uiso 1 1 calc R . . C14 C 0.9159(8) 0.5896(9) 0.4360(8) 0.045(2) Uani 1 1 d . . . H14A H 0.9020 0.5079 0.4052 0.054 Uiso 1 1 calc R . . H14B H 0.9289 0.5992 0.5071 0.054 Uiso 1 1 calc R . . C15 C 1.0311(9) 0.6440(8) 0.4293(9) 0.046(2) Uani 1 1 d . . . H15A H 1.1033 0.6190 0.4741 0.055 Uiso 1 1 calc R . . H15B H 1.0271 0.6200 0.3603 0.055 Uiso 1 1 calc R . . C16 C 0.7717(9) 0.6102(9) 0.2737(7) 0.047(2) Uani 1 1 d . . . H16A H 0.7441 0.5282 0.2486 0.056 Uiso 1 1 calc R . . H16B H 0.8460 0.6262 0.2616 0.056 Uiso 1 1 calc R . . C17 C 0.6722(9) 0.6720(10) 0.2108(7) 0.047(2) Uani 1 1 d . . . C18 C 0.5557(11) 0.6085(11) 0.1458(8) 0.059(3) Uani 1 1 d . . . H18A H 0.5371 0.5312 0.1427 0.070 Uiso 1 1 calc R . . C19 C 0.4665(11) 0.6686(19) 0.0841(9) 0.090(6) Uani 1 1 d . . . C20 C 0.4957(11) 0.7817(13) 0.0885(9) 0.067(3) Uani 1 1 d . . . C21 C 0.6094(10) 0.8393(12) 0.1535(7) 0.057(3) Uani 1 1 d . . . H21A H 0.6277 0.9163 0.1554 0.069 Uiso 1 1 calc R . . C22 C 0.6986(8) 0.7889(9) 0.2167(7) 0.043(2) Uani 1 1 d . . . C23 C 0.3385(12) 0.5949(17) 0.0160(11) 0.097(6) Uani 1 1 d . . . H23A H 0.2838 0.6421 -0.0196 0.146 Uiso 1 1 calc R . . H23B H 0.3044 0.5646 0.0580 0.146 Uiso 1 1 calc R . . H23C H 0.3484 0.5328 -0.0321 0.146 Uiso 1 1 calc R . . C24 C 0.3979(14) 0.8380(18) 0.0212(13) 0.115(7) Uani 1 1 d . . . H24A H 0.3251 0.7828 -0.0179 0.173 Uiso 1 1 calc R . . H24B H 0.4280 0.8664 -0.0239 0.173 Uiso 1 1 calc R . . H24C H 0.3783 0.9006 0.0626 0.173 Uiso 1 1 calc R . . C25 C 0.869(2) 0.7239(17) 0.0816(15) 0.129(8) Uani 1 1 d . . . H25A H 0.8309 0.6902 0.0098 0.194 Uiso 1 1 calc R . . H25B H 0.8258 0.6895 0.1157 0.194 Uiso 1 1 calc R . . H25C H 0.9535 0.7108 0.1067 0.194 Uiso 1 1 calc R . . C26 C 0.7525(16) 1.1982(13) 0.2994(12) 0.084(4) Uani 1 1 d . . . H26A H 0.6875 1.2080 0.3239 0.125 Uiso 1 1 calc R . . H26B H 0.7235 1.2036 0.2299 0.125 Uiso 1 1 calc R . . H26C H 0.8216 1.2570 0.3402 0.125 Uiso 1 1 calc R . . C27 C 1.1854(14) 0.8663(15) 0.2262(10) 0.084(5) Uani 1 1 d . . . H27A H 1.2508 0.8282 0.2625 0.126 Uiso 1 1 calc R . . H27B H 1.2199 0.9339 0.2147 0.126 Uiso 1 1 calc R . . H27C H 1.1341 0.8155 0.1621 0.126 Uiso 1 1 calc R . . N1 N 1.2559(9) 0.7629(9) 0.4048(7) 0.056(2) Uani 1 1 d . . . N2 N 1.3071(8) 0.7125(10) 0.4653(8) 0.064(3) Uani 1 1 d . . . N3 N 1.3600(11) 0.6604(13) 0.5221(11) 0.094(4) Uani 1 1 d . . . N4 N 0.8043(7) 0.6402(7) 0.3847(6) 0.0412(17) Uani 1 1 d . . . N5 N 0.6559(7) 0.7955(7) 0.4553(6) 0.0393(16) Uani 1 1 d . . . N6 N 0.9406(10) 1.1104(10) 0.1050(7) 0.066(3) Uani 1 1 d . . . O1 O 0.9268(6) 0.8381(7) 0.6262(5) 0.0441(15) Uani 1 1 d . . . O2 O 0.8101(5) 0.8480(6) 0.2826(4) 0.0390(14) Uani 1 1 d . . . O3 O 0.7486(5) 1.0163(6) 0.4545(5) 0.0416(15) Uani 1 1 d . . . O4 O 1.0406(5) 0.7646(6) 0.4576(5) 0.0388(13) Uani 1 1 d . . . O5 O 1.0208(5) 0.9642(6) 0.4182(4) 0.0353(13) Uani 1 1 d . . . O6 O 0.7904(7) 1.0858(7) 0.3060(5) 0.0520(18) Uani 1 1 d . . . O7 O 0.8642(9) 0.8501(9) 0.1012(6) 0.072(2) Uani 1 1 d . . . O8 O 1.1121(7) 0.8984(8) 0.2855(5) 0.057(2) Uani 1 1 d . . . O9 O 0.8521(8) 1.1031(9) 0.1340(6) 0.067(2) Uani 1 1 d . . . O10 O 1.0322(8) 1.0611(8) 0.1470(6) 0.063(2) Uani 1 1 d . . . O11 O 0.9388(10) 1.1610(9) 0.0417(7) 0.081(3) Uani 1 1 d . . . O1W O 0.7778(14) 0.8949(18) -0.0788(9) 0.104(7) Uani 0.70(3) 1 d P . . O1W' O 0.664(3) 0.870(3) -0.140(2) 0.080(13) Uani 0.30(3) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0347(7) 0.0418(8) 0.0434(7) 0.0149(6) 0.0210(5) 0.0107(6) Dy1 0.0275(2) 0.0359(2) 0.0340(2) 0.01193(17) 0.01313(15) 0.00322(16) Dy2 0.0377(2) 0.0447(3) 0.0328(2) 0.01403(19) 0.01396(16) 0.00428(19) C1 0.043(5) 0.054(7) 0.037(4) 0.015(4) 0.018(4) -0.001(4) C2 0.046(5) 0.049(7) 0.052(5) 0.015(5) 0.021(4) 0.004(5) C3 0.067(7) 0.063(8) 0.046(5) 0.019(5) 0.024(5) 0.004(6) C4 0.079(7) 0.047(7) 0.044(5) 0.013(5) 0.029(5) -0.016(6) C5 0.050(6) 0.070(9) 0.052(6) 0.019(6) 0.021(5) -0.007(6) C6 0.046(5) 0.061(7) 0.042(5) 0.016(5) 0.020(4) -0.001(5) C7 0.096(9) 0.037(7) 0.081(8) 0.029(6) 0.029(7) -0.007(7) C8 0.095(10) 0.072(10) 0.092(10) 0.030(9) 0.041(8) -0.037(8) C9 0.044(5) 0.042(6) 0.058(6) 0.010(5) 0.030(4) 0.000(4) C10 0.023(4) 0.062(7) 0.058(6) 0.015(5) 0.016(4) 0.009(4) C11 0.028(4) 0.052(6) 0.063(6) 0.026(5) 0.019(4) 0.013(4) C12 0.037(5) 0.042(6) 0.051(5) 0.003(4) 0.016(4) -0.010(4) C13 0.046(5) 0.053(7) 0.055(6) 0.011(5) 0.022(4) 0.004(5) C14 0.040(5) 0.032(5) 0.068(6) 0.024(5) 0.020(4) -0.002(4) C15 0.047(5) 0.025(5) 0.074(6) 0.020(5) 0.029(5) 0.008(4) C16 0.046(5) 0.039(6) 0.050(5) 0.001(4) 0.020(4) -0.006(4) C17 0.042(5) 0.059(7) 0.036(4) 0.009(4) 0.015(4) -0.006(5) C18 0.061(6) 0.052(7) 0.048(6) 0.005(5) 0.012(5) -0.021(5) C19 0.041(6) 0.167(19) 0.043(6) 0.022(8) 0.000(5) 0.001(8) C20 0.053(6) 0.074(10) 0.066(7) 0.030(7) 0.010(5) -0.007(6) C21 0.046(6) 0.075(9) 0.044(5) 0.020(5) 0.007(4) 0.011(6) C22 0.039(5) 0.050(6) 0.037(4) 0.011(4) 0.012(4) 0.006(4) C23 0.057(7) 0.126(16) 0.075(9) 0.018(9) -0.001(6) -0.045(9) C24 0.067(9) 0.134(18) 0.109(12) 0.062(12) -0.020(8) -0.005(10) C25 0.23(3) 0.073(13) 0.134(16) 0.008(12) 0.130(18) 0.028(16) C26 0.113(12) 0.048(8) 0.096(10) 0.023(8) 0.043(9) 0.021(9) C27 0.090(10) 0.126(14) 0.078(8) 0.050(9) 0.062(8) 0.052(10) N1 0.059(5) 0.053(6) 0.074(6) 0.029(5) 0.039(5) 0.024(5) N2 0.039(5) 0.081(8) 0.085(7) 0.035(6) 0.029(5) 0.017(5) N3 0.055(6) 0.097(11) 0.131(11) 0.063(9) 0.019(7) 0.002(7) N4 0.041(4) 0.038(5) 0.046(4) 0.011(4) 0.018(3) 0.005(4) N5 0.035(4) 0.036(5) 0.046(4) 0.010(3) 0.016(3) -0.001(3) N6 0.077(7) 0.089(9) 0.045(5) 0.034(5) 0.027(5) 0.025(6) O1 0.037(3) 0.059(5) 0.038(3) 0.017(3) 0.014(3) 0.000(3) O2 0.035(3) 0.045(4) 0.035(3) 0.012(3) 0.010(2) -0.001(3) O3 0.029(3) 0.056(5) 0.044(3) 0.017(3) 0.017(2) 0.012(3) O4 0.036(3) 0.032(4) 0.052(3) 0.011(3) 0.021(3) 0.002(3) O5 0.025(3) 0.047(4) 0.035(3) 0.012(3) 0.012(2) 0.010(3) O6 0.053(4) 0.063(5) 0.054(4) 0.026(4) 0.029(3) 0.019(4) O7 0.089(6) 0.073(7) 0.048(4) -0.002(4) 0.029(4) -0.015(5) O8 0.067(5) 0.075(6) 0.050(4) 0.029(4) 0.037(4) 0.030(4) O9 0.070(5) 0.091(7) 0.055(4) 0.038(5) 0.028(4) 0.031(5) O10 0.064(5) 0.087(7) 0.055(4) 0.031(4) 0.033(4) 0.020(5) O11 0.112(8) 0.087(8) 0.060(5) 0.041(5) 0.039(5) 0.018(6) O1W 0.076(11) 0.20(2) 0.045(7) 0.039(9) 0.035(7) 0.014(11) O1W' 0.07(2) 0.10(3) 0.07(2) 0.006(18) 0.041(18) 0.015(19) _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 Mn1 O5 1.850(5) . ? Mn1 O8 1.930(6) . ? Mn1 O4 1.936(6) . ? Mn1 N1 1.964(8) . ? Mn1 O3 2.071(7) 2_776 ? Mn1 Dy2 3.2402(13) . ? Mn1 Dy1 3.3415(13) . ? Mn1 Dy1 3.4105(15) 2_776 ? Dy1 O5 2.334(7) 2_776 ? Dy1 O4 2.344(6) . ? Dy1 O5 2.347(6) . ? Dy1 O1 2.360(6) . ? Dy1 O2 2.378(5) . ? Dy1 O3 2.422(6) . ? Dy1 N5 2.656(7) . ? Dy1 N4 2.665(9) . ? Dy1 Mn1 3.4105(15) 2_776 ? Dy1 Dy2 3.8055(6) 2_776 ? Dy1 Dy2 3.8357(6) . ? Dy2 O5 2.245(5) . ? Dy2 O8 2.288(7) . ? Dy2 O7 2.385(8) . ? Dy2 O2 2.397(6) . ? Dy2 O1 2.402(7) 2_776 ? Dy2 O6 2.403(6) . ? Dy2 O9 2.464(7) . ? Dy2 O10 2.509(7) . ? Dy2 N6 2.911(9) . ? Dy2 Dy1 3.8055(6) 2_776 ? C1 O1 1.356(12) . ? C1 C6 1.391(13) . ? C1 C2 1.391(13) . ? C2 C3 1.403(15) . ? C2 H2A 0.9300 . ? C3 C4 1.393(16) . ? C3 C7 1.519(15) . ? C4 C5 1.398(15) . ? C4 C8 1.521(14) . ? C5 C6 1.394(15) . ? C5 H5A 0.9300 . ? C6 C9 1.488(14) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N5 1.494(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N5 1.503(11) . ? C10 C11 1.532(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O3 1.408(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.494(14) . ? C12 N5 1.528(13) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.493(13) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.487(11) . ? C14 C15 1.516(13) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O4 1.411(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.478(12) . ? C16 C17 1.533(14) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C22 1.399(15) . ? C17 C18 1.412(15) . ? C18 C19 1.445(19) . ? C18 H18A 0.9300 . ? C19 C20 1.37(2) . ? C19 C23 1.559(19) . ? C20 C21 1.366(17) . ? C20 C24 1.507(17) . ? C21 C22 1.381(13) . ? C21 H21A 0.9300 . ? C22 O2 1.356(12) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O7 1.49(2) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O6 1.457(14) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O8 1.446(11) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N1 N2 1.173(12) . ? N2 N3 1.158(14) . ? N6 O11 1.198(11) . ? N6 O9 1.266(12) . ? N6 O10 1.275(11) . ? O1 Dy2 2.402(7) 2_776 ? O3 Mn1 2.071(7) 2_776 ? O5 Dy1 2.334(7) 2_776 ? O1W O1W' 1.28(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 O8 85.0(3) . . ? O5 Mn1 O4 85.9(3) . . ? O8 Mn1 O4 133.6(3) . . ? O5 Mn1 N1 177.0(3) . . ? O8 Mn1 N1 92.0(3) . . ? O4 Mn1 N1 96.4(3) . . ? O5 Mn1 O3 84.1(3) . 2_776 ? O8 Mn1 O3 117.9(3) . 2_776 ? O4 Mn1 O3 106.2(3) . 2_776 ? N1 Mn1 O3 97.0(4) . 2_776 ? O5 Mn1 Dy2 42.21(17) . . ? O8 Mn1 Dy2 44.0(2) . . ? O4 Mn1 Dy2 107.79(18) . . ? N1 Mn1 Dy2 135.0(3) . . ? O3 Mn1 Dy2 111.17(18) 2_776 . ? O5 Mn1 Dy1 42.73(19) . . ? O8 Mn1 Dy1 112.5(2) . . ? O4 Mn1 Dy1 43.29(17) . . ? N1 Mn1 Dy1 139.5(3) . . ? O3 Mn1 Dy1 98.78(16) 2_776 . ? Dy2 Mn1 Dy1 71.28(3) . . ? O5 Mn1 Dy1 40.4(2) . 2_776 ? O8 Mn1 Dy1 97.6(2) . 2_776 ? O4 Mn1 Dy1 104.30(19) . 2_776 ? N1 Mn1 Dy1 140.0(3) . 2_776 ? O3 Mn1 Dy1 44.61(16) 2_776 2_776 ? Dy2 Mn1 Dy1 69.75(3) . 2_776 ? Dy1 Mn1 Dy1 70.45(3) . 2_776 ? O5 Dy1 O4 102.2(2) 2_776 . ? O5 Dy1 O5 67.4(2) 2_776 . ? O4 Dy1 O5 66.8(2) . . ? O5 Dy1 O1 69.7(2) 2_776 . ? O4 Dy1 O1 85.9(2) . . ? O5 Dy1 O1 121.4(2) . . ? O5 Dy1 O2 123.1(2) 2_776 . ? O4 Dy1 O2 89.9(2) . . ? O5 Dy1 O2 67.5(2) . . ? O1 Dy1 O2 167.1(3) . . ? O5 Dy1 O3 67.1(2) 2_776 . ? O4 Dy1 O3 161.4(2) . . ? O5 Dy1 O3 94.7(2) . . ? O1 Dy1 O3 103.4(2) . . ? O2 Dy1 O3 84.1(2) . . ? O5 Dy1 N5 114.5(2) 2_776 . ? O4 Dy1 N5 131.2(2) . . ? O5 Dy1 N5 156.8(2) . . ? O1 Dy1 N5 78.4(2) . . ? O2 Dy1 N5 95.4(2) . . ? O3 Dy1 N5 67.1(2) . . ? O5 Dy1 N4 157.9(2) 2_776 . ? O4 Dy1 N4 67.5(2) . . ? O5 Dy1 N4 121.2(2) . . ? O1 Dy1 N4 89.6(2) . . ? O2 Dy1 N4 77.5(2) . . ? O3 Dy1 N4 127.7(2) . . ? N5 Dy1 N4 66.5(2) . . ? O5 Dy1 Mn1 84.65(13) 2_776 . ? O4 Dy1 Mn1 34.49(15) . . ? O5 Dy1 Mn1 32.34(14) . . ? O1 Dy1 Mn1 107.43(15) . . ? O2 Dy1 Mn1 74.99(14) . . ? O3 Dy1 Mn1 127.00(15) . . ? N5 Dy1 Mn1 160.60(18) . . ? N4 Dy1 Mn1 94.70(16) . . ? O5 Dy1 Mn1 30.93(13) 2_776 2_776 ? O4 Dy1 Mn1 132.92(17) . 2_776 ? O5 Dy1 Mn1 82.90(15) . 2_776 ? O1 Dy1 Mn1 80.07(18) . 2_776 ? O2 Dy1 Mn1 111.37(16) . 2_776 ? O3 Dy1 Mn1 36.91(16) . 2_776 ? N5 Dy1 Mn1 89.56(18) . 2_776 ? N4 Dy1 Mn1 155.50(16) . 2_776 ? Mn1 Dy1 Mn1 109.55(3) . 2_776 ? O5 Dy1 Dy2 33.06(14) 2_776 2_776 ? O4 Dy1 Dy2 90.33(16) . 2_776 ? O5 Dy1 Dy2 89.84(14) . 2_776 ? O1 Dy1 Dy2 37.34(18) . 2_776 ? O2 Dy1 Dy2 155.08(16) . 2_776 ? O3 Dy1 Dy2 87.78(15) . 2_776 ? N5 Dy1 Dy2 103.07(17) . 2_776 ? N4 Dy1 Dy2 125.17(16) . 2_776 ? Mn1 Dy1 Dy2 91.52(3) . 2_776 ? Mn1 Dy1 Dy2 53.02(2) 2_776 2_776 ? O5 Dy1 Dy2 89.29(14) 2_776 . ? O4 Dy1 Dy2 83.20(14) . . ? O5 Dy1 Dy2 32.52(13) . . ? O1 Dy1 Dy2 153.70(16) . . ? O2 Dy1 Dy2 36.73(16) . . ? O3 Dy1 Dy2 81.48(14) . . ? N5 Dy1 Dy2 126.20(15) . . ? N4 Dy1 Dy2 108.00(16) . . ? Mn1 Dy1 Dy2 53.13(2) . . ? Mn1 Dy1 Dy2 89.96(2) 2_776 . ? Dy2 Dy1 Dy2 118.713(14) 2_776 . ? O5 Dy2 O8 68.6(2) . . ? O5 Dy2 O7 129.1(3) . . ? O8 Dy2 O7 82.4(3) . . ? O5 Dy2 O2 68.8(2) . . ? O8 Dy2 O2 98.8(3) . . ? O7 Dy2 O2 75.9(3) . . ? O5 Dy2 O1 70.4(2) . 2_776 ? O8 Dy2 O1 89.2(3) . 2_776 ? O7 Dy2 O1 152.1(3) . 2_776 ? O2 Dy2 O1 131.8(2) . 2_776 ? O5 Dy2 O6 87.5(2) . . ? O8 Dy2 O6 156.0(2) . . ? O7 Dy2 O6 115.7(3) . . ? O2 Dy2 O6 72.6(2) . . ? O1 Dy2 O6 81.1(2) 2_776 . ? O5 Dy2 O9 153.6(3) . . ? O8 Dy2 O9 129.0(2) . . ? O7 Dy2 O9 76.4(3) . . ? O2 Dy2 O9 119.5(3) . . ? O1 Dy2 O9 88.8(3) 2_776 . ? O6 Dy2 O9 73.0(2) . . ? O5 Dy2 O10 134.4(2) . . ? O8 Dy2 O10 78.3(2) . . ? O7 Dy2 O10 73.3(3) . . ? O2 Dy2 O10 149.3(3) . . ? O1 Dy2 O10 78.9(3) 2_776 . ? O6 Dy2 O10 120.7(2) . . ? O9 Dy2 O10 51.4(3) . . ? O5 Dy2 N6 152.3(3) . . ? O8 Dy2 N6 103.9(3) . . ? O7 Dy2 N6 73.3(3) . . ? O2 Dy2 N6 138.6(3) . . ? O1 Dy2 N6 83.1(3) 2_776 . ? O6 Dy2 N6 96.7(2) . . ? O9 Dy2 N6 25.5(3) . . ? O10 Dy2 N6 25.9(2) . . ? O5 Dy2 Mn1 33.61(14) . . ? O8 Dy2 Mn1 35.90(16) . . ? O7 Dy2 Mn1 104.1(2) . . ? O2 Dy2 Mn1 76.82(14) . . ? O1 Dy2 Mn1 83.20(15) 2_776 . ? O6 Dy2 Mn1 120.56(15) . . ? O9 Dy2 Mn1 162.6(2) . . ? O10 Dy2 Mn1 111.67(17) . . ? N6 Dy2 Mn1 137.4(2) . . ? O5 Dy2 Dy1 34.54(17) . 2_776 ? O8 Dy2 Dy1 81.35(19) . 2_776 ? O7 Dy2 Dy1 161.3(2) . 2_776 ? O2 Dy2 Dy1 97.52(14) . 2_776 ? O1 Dy2 Dy1 36.57(14) 2_776 2_776 ? O6 Dy2 Dy1 77.78(18) . 2_776 ? O9 Dy2 Dy1 121.3(2) . 2_776 ? O10 Dy2 Dy1 112.0(2) . 2_776 ? N6 Dy2 Dy1 119.7(2) . 2_776 ? Mn1 Dy2 Dy1 57.23(3) . 2_776 ? O5 Dy2 Dy1 34.19(15) . . ? O8 Dy2 Dy1 89.63(17) . . ? O7 Dy2 Dy1 109.5(2) . . ? O2 Dy2 Dy1 36.38(14) . . ? O1 Dy2 Dy1 96.87(14) 2_776 . ? O6 Dy2 Dy1 70.02(16) . . ? O9 Dy2 Dy1 141.13(18) . . ? O10 Dy2 Dy1 167.18(17) . . ? N6 Dy2 Dy1 166.5(2) . . ? Mn1 Dy2 Dy1 55.59(2) . . ? Dy1 Dy2 Dy1 61.287(14) 2_776 . ? O1 C1 C6 120.1(9) . . ? O1 C1 C2 120.8(8) . . ? C6 C1 C2 119.1(9) . . ? C1 C2 C3 122.8(9) . . ? C1 C2 H2A 118.6 . . ? C3 C2 H2A 118.6 . . ? C4 C3 C2 118.3(10) . . ? C4 C3 C7 122.3(10) . . ? C2 C3 C7 119.2(10) . . ? C3 C4 C5 118.2(10) . . ? C3 C4 C8 121.7(11) . . ? C5 C4 C8 120.1(11) . . ? C6 C5 C4 123.6(10) . . ? C6 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? C1 C6 C5 117.8(9) . . ? C1 C6 C9 120.8(9) . . ? C5 C6 C9 121.3(9) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 N5 115.1(8) . . ? C6 C9 H9A 108.5 . . ? N5 C9 H9A 108.5 . . ? C6 C9 H9B 108.5 . . ? N5 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N5 C10 C11 112.6(8) . . ? N5 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N5 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? O3 C11 C10 110.6(7) . . ? O3 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C13 C12 N5 112.2(8) . . ? C13 C12 H12A 109.2 . . ? N5 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? N5 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N4 C13 C12 114.4(9) . . ? N4 C13 H13A 108.6 . . ? C12 C13 H13A 108.6 . . ? N4 C13 H13B 108.6 . . ? C12 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? N4 C14 C15 112.8(7) . . ? N4 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? N4 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O4 C15 C14 109.5(7) . . ? O4 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? O4 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? N4 C16 C17 116.4(8) . . ? N4 C16 H16A 108.2 . . ? C17 C16 H16A 108.2 . . ? N4 C16 H16B 108.2 . . ? C17 C16 H16B 108.2 . . ? H16A C16 H16B 107.3 . . ? C22 C17 C18 121.1(10) . . ? C22 C17 C16 120.0(9) . . ? C18 C17 C16 118.9(10) . . ? C17 C18 C19 117.2(12) . . ? C17 C18 H18A 121.4 . . ? C19 C18 H18A 121.4 . . ? C20 C19 C18 120.7(12) . . ? C20 C19 C23 124.4(14) . . ? C18 C19 C23 114.9(17) . . ? C21 C20 C19 119.6(11) . . ? C21 C20 C24 122.9(14) . . ? C19 C20 C24 117.5(13) . . ? C20 C21 C22 123.2(13) . . ? C20 C21 H21A 118.4 . . ? C22 C21 H21A 118.4 . . ? O2 C22 C21 122.5(10) . . ? O2 C22 C17 119.4(8) . . ? C21 C22 C17 118.1(10) . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 C27 H27A 109.5 . . ? O8 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O8 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 N1 Mn1 125.6(8) . . ? N3 N2 N1 176.8(14) . . ? C16 N4 C14 109.6(7) . . ? C16 N4 C13 111.8(8) . . ? C14 N4 C13 107.9(7) . . ? C16 N4 Dy1 110.5(6) . . ? C14 N4 Dy1 103.3(6) . . ? C13 N4 Dy1 113.2(6) . . ? C9 N5 C10 110.2(7) . . ? C9 N5 C12 110.9(7) . . ? C10 N5 C12 108.7(7) . . ? C9 N5 Dy1 106.1(5) . . ? C10 N5 Dy1 104.6(5) . . ? C12 N5 Dy1 116.1(5) . . ? O11 N6 O9 122.1(10) . . ? O11 N6 O10 121.7(10) . . ? O9 N6 O10 116.2(8) . . ? O11 N6 Dy2 179.0(8) . . ? O9 N6 Dy2 57.1(5) . . ? O10 N6 Dy2 59.2(5) . . ? C1 O1 Dy1 127.2(6) . . ? C1 O1 Dy2 124.3(6) . 2_776 ? Dy1 O1 Dy2 106.1(3) . 2_776 ? C22 O2 Dy1 121.4(5) . . ? C22 O2 Dy2 129.5(5) . . ? Dy1 O2 Dy2 106.9(2) . . ? C11 O3 Mn1 117.7(6) . 2_776 ? C11 O3 Dy1 123.5(6) . . ? Mn1 O3 Dy1 98.5(2) 2_776 . ? C15 O4 Mn1 122.4(5) . . ? C15 O4 Dy1 124.8(5) . . ? Mn1 O4 Dy1 102.2(3) . . ? Mn1 O5 Dy2 104.2(2) . . ? Mn1 O5 Dy1 108.7(3) . 2_776 ? Dy2 O5 Dy1 112.4(3) . 2_776 ? Mn1 O5 Dy1 104.9(3) . . ? Dy2 O5 Dy1 113.3(2) . . ? Dy1 O5 Dy1 112.6(2) 2_776 . ? C26 O6 Dy2 132.0(8) . . ? C25 O7 Dy2 128.7(10) . . ? C27 O8 Mn1 126.3(7) . . ? C27 O8 Dy2 133.6(6) . . ? Mn1 O8 Dy2 100.1(3) . . ? N6 O9 Dy2 97.4(6) . . ? N6 O10 Dy2 95.0(6) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 1.081 _refine_diff_density_min -1.183 _refine_diff_density_rms 0.205