# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ddb _database_code_depnum_ccdc_archive 'CCDC 907542' #TrackingRef '1.Mn+Nd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H51 Mn N2 Nd O12' _chemical_formula_weight 951.01 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.590(4) _cell_length_b 13.054(4) _cell_length_c 24.189(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3975(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.674 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6164 _exptl_absorpt_correction_T_max 0.8117 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21282 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7401 _reflns_number_gt 6586 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0321P)^2^+0.9457P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.037(14) _refine_ls_number_reflns 7401 _refine_ls_number_parameters 505 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.078 _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 Nd1 Nd 0.258729(19) 0.603625(18) 0.150059(10) 0.02333(8) Uani 1 1 d . . . Mn1 Mn 0.37776(7) 0.48223(6) 0.02339(4) 0.0311(2) Uani 1 1 d . . . O1 O -0.1029(4) 0.9944(4) 0.32416(18) 0.0651(15) Uani 1 1 d . . . O2 O -0.2056(4) 1.0342(5) 0.25720(18) 0.0821(19) Uani 1 1 d . . . O3 O 0.2257(4) 0.7622(4) 0.1998(2) 0.0821(15) Uani 1 1 d U . . O4 O 0.1186(4) 0.7325(4) 0.1361(2) 0.0731(16) Uani 1 1 d . . . O5 O 0.7077(3) 0.9530(3) -0.05970(14) 0.0316(9) Uani 1 1 d . . . O6 O 0.7290(3) 1.0162(3) 0.02260(15) 0.0467(10) Uani 1 1 d . . . O7 O 0.4132(3) 0.6361(3) 0.00519(17) 0.0415(10) Uani 1 1 d . . . O8 O 0.3888(3) 0.6805(3) 0.09178(16) 0.0418(10) Uani 1 1 d . . . O9 O 0.3504(3) 0.3420(3) 0.07019(15) 0.0386(10) Uani 1 1 d . . . O10 O 0.3604(3) 0.4501(3) 0.13861(18) 0.0456(11) Uani 1 1 d . . . O11 O 0.6255(4) 0.0765(3) 0.20135(16) 0.0574(13) Uani 1 1 d . . . H11A H 0.6818 0.0607 0.2162 0.086 Uiso 1 1 calc R . . O12 O 0.5889(3) 0.1284(3) 0.28628(15) 0.0372(10) Uani 1 1 d . . . C1 C -0.1164(5) 1.0068(4) 0.2742(2) 0.0401(14) Uani 1 1 d . . . C2 C -0.0272(5) 0.9944(5) 0.2331(3) 0.0463(16) Uani 1 1 d . . . H2A H -0.0389 1.0446 0.2036 0.056 Uiso 1 1 calc R . . C3 C 0.0825(6) 1.0161(7) 0.2579(4) 0.092(3) Uani 1 1 d U . . H3A H 0.1006 1.0879 0.2536 0.111 Uiso 1 1 calc R . . H3B H 0.0832 0.9995 0.2970 0.111 Uiso 1 1 calc R . . C4 C 0.1589(6) 0.9514(6) 0.2278(4) 0.076(3) Uani 1 1 d . . . H4A H 0.1918 0.9030 0.2529 0.091 Uiso 1 1 calc R . . H4B H 0.2142 0.9936 0.2117 0.091 Uiso 1 1 calc R . . C5 C 0.0996(4) 0.8937(5) 0.1821(2) 0.0407(13) Uani 1 1 d . . . C6 C -0.0163(4) 0.8878(5) 0.2054(2) 0.0335(12) Uani 1 1 d . . . C7 C 0.1483(6) 0.7879(6) 0.1731(3) 0.0725(16) Uani 1 1 d U . . C8 C 0.1082(7) 0.9515(5) 0.1277(3) 0.087(3) Uani 1 1 d . . . H8A H 0.1809 0.9520 0.1157 0.131 Uiso 1 1 calc R . . H8B H 0.0841 1.0206 0.1328 0.131 Uiso 1 1 calc R . . H8C H 0.0651 0.9183 0.1003 0.131 Uiso 1 1 calc R . . C9 C -0.1005(6) 0.8727(7) 0.1613(3) 0.080(3) Uani 1 1 d . . . H9A H -0.0931 0.8058 0.1453 0.119 Uiso 1 1 calc R . . H9B H -0.0922 0.9238 0.1331 0.119 Uiso 1 1 calc R . . H9C H -0.1697 0.8790 0.1777 0.119 Uiso 1 1 calc R . . C10 C -0.0276(6) 0.8024(5) 0.2461(3) 0.067(2) Uani 1 1 d . . . H10A H -0.0216 0.7380 0.2272 0.101 Uiso 1 1 calc R . . H10B H -0.0958 0.8068 0.2637 0.101 Uiso 1 1 calc R . . H10C H 0.0273 0.8076 0.2735 0.101 Uiso 1 1 calc R . . C11 C 0.6717(4) 0.9727(4) -0.0126(2) 0.0296(12) Uani 1 1 d . . . C12 C 0.5600(4) 0.9430(4) 0.0025(2) 0.0335(13) Uani 1 1 d . . . H12A H 0.5320 0.9975 0.0263 0.040 Uiso 1 1 calc R . . C13 C 0.4838(5) 0.9316(5) -0.0454(3) 0.0532(18) Uani 1 1 d . . . H13A H 0.5226 0.9221 -0.0797 0.064 Uiso 1 1 calc R . . H13B H 0.4398 0.9923 -0.0489 0.064 Uiso 1 1 calc R . . C14 C 0.4151(5) 0.8381(5) -0.0334(2) 0.0416(15) Uani 1 1 d . . . H14A H 0.4369 0.7805 -0.0560 0.050 Uiso 1 1 calc R . . H14B H 0.3409 0.8528 -0.0408 0.050 Uiso 1 1 calc R . . C15 C 0.4319(4) 0.8146(4) 0.0280(2) 0.0294(12) Uani 1 1 d . . . C16 C 0.5520(4) 0.8418(4) 0.0358(2) 0.0292(12) Uani 1 1 d . . . C17 C 0.4095(4) 0.7017(4) 0.0431(2) 0.0326(13) Uani 1 1 d . . . C18 C 0.3588(5) 0.8824(5) 0.0627(3) 0.0501(17) Uani 1 1 d . . . H18A H 0.2862 0.8630 0.0565 0.075 Uiso 1 1 calc R . . H18B H 0.3685 0.9528 0.0524 0.075 Uiso 1 1 calc R . . H18C H 0.3757 0.8741 0.1012 0.075 Uiso 1 1 calc R . . C19 C 0.6247(4) 0.7614(4) 0.0099(2) 0.0414(15) Uani 1 1 d . . . H19A H 0.6975 0.7807 0.0157 0.062 Uiso 1 1 calc R . . H19B H 0.6107 0.7571 -0.0291 0.062 Uiso 1 1 calc R . . H19C H 0.6117 0.6961 0.0268 0.062 Uiso 1 1 calc R . . C20 C 0.5843(5) 0.8551(5) 0.0967(2) 0.0516(17) Uani 1 1 d . . . H20A H 0.6585 0.8718 0.0988 0.077 Uiso 1 1 calc R . . H20B H 0.5713 0.7925 0.1164 0.077 Uiso 1 1 calc R . . H20C H 0.5434 0.9094 0.1129 0.077 Uiso 1 1 calc R . . C21 C 0.3549(4) 0.3600(4) 0.1199(2) 0.0307(13) Uani 1 1 d . . . C22 C 0.3562(4) 0.2726(4) 0.1616(2) 0.0328(13) Uani 1 1 d . . . H22A H 0.2990 0.2860 0.1881 0.039 Uiso 1 1 calc R . . C23 C 0.3354(6) 0.1683(5) 0.1370(3) 0.065(2) Uani 1 1 d . . . H23A H 0.3472 0.1690 0.0974 0.079 Uiso 1 1 calc R . . H23B H 0.2629 0.1467 0.1441 0.079 Uiso 1 1 calc R . . C24 C 0.4162(5) 0.0960(5) 0.1664(3) 0.0543(17) Uani 1 1 d . . . H24A H 0.3817 0.0327 0.1772 0.065 Uiso 1 1 calc R . . H24B H 0.4745 0.0796 0.1417 0.065 Uiso 1 1 calc R . . C25 C 0.4575(5) 0.1529(4) 0.2174(2) 0.0370(14) Uani 1 1 d . . . C26 C 0.4617(5) 0.2651(5) 0.1956(3) 0.0492(17) Uani 1 1 d . . . C27 C 0.5629(5) 0.1179(4) 0.2377(2) 0.0346(13) Uani 1 1 d . . . C28 C 0.3737(5) 0.1423(6) 0.2644(3) 0.066(2) Uani 1 1 d . . . H28A H 0.3717 0.0726 0.2770 0.099 Uiso 1 1 calc R . . H28B H 0.3050 0.1614 0.2506 0.099 Uiso 1 1 calc R . . H28C H 0.3926 0.1865 0.2946 0.099 Uiso 1 1 calc R . . C29 C 0.4620(8) 0.3441(6) 0.2433(3) 0.090(3) Uani 1 1 d . . . H29A H 0.5271 0.3384 0.2637 0.135 Uiso 1 1 calc R . . H29B H 0.4030 0.3311 0.2674 0.135 Uiso 1 1 calc R . . H29C H 0.4560 0.4120 0.2283 0.135 Uiso 1 1 calc R . . C30 C 0.5571(5) 0.2829(6) 0.1607(3) 0.072(3) Uani 1 1 d . . . H30A H 0.6199 0.2778 0.1831 0.109 Uiso 1 1 calc R . . H30B H 0.5534 0.3500 0.1446 0.109 Uiso 1 1 calc R . . H30C H 0.5598 0.2325 0.1319 0.109 Uiso 1 1 calc R . . N1 N 0.4486(5) 0.3814(4) -0.0414(3) 0.0611(17) Uani 1 1 d . . . N2 N 0.5512(4) 0.4612(4) 0.0441(3) 0.0558(16) Uani 1 1 d . . . C31 C 0.3931(8) 0.3441(6) -0.0840(3) 0.076(3) Uani 1 1 d . . . H31A H 0.3272 0.3730 -0.0916 0.092 Uiso 1 1 calc R . . C32 C 0.4277(9) 0.2659(7) -0.1169(4) 0.096(3) Uani 1 1 d U . . H32A H 0.3890 0.2439 -0.1474 0.116 Uiso 1 1 calc R . . C33 C 0.5197(10) 0.2229(8) -0.1029(5) 0.102(3) Uani 1 1 d U . . H33A H 0.5426 0.1668 -0.1234 0.122 Uiso 1 1 calc R . . C34 C 0.5811(8) 0.2548(7) -0.0616(4) 0.095(3) Uani 1 1 d U . . H34A H 0.6453 0.2227 -0.0537 0.114 Uiso 1 1 calc R . . C35 C 0.5446(8) 0.3413(5) -0.0293(4) 0.077(3) Uani 1 1 d . . . C36 C 0.6024(5) 0.3896(7) 0.0153(4) 0.072(2) Uani 1 1 d . . . C37 C 0.7081(7) 0.3649(8) 0.0269(5) 0.099(3) Uani 1 1 d U . . H37A H 0.7445 0.3152 0.0069 0.119 Uiso 1 1 calc R . . C38 C 0.7543(7) 0.4166(8) 0.0683(5) 0.102(3) Uani 1 1 d U . . H38A H 0.8242 0.4003 0.0770 0.123 Uiso 1 1 calc R . . C39 C 0.7057(7) 0.4919(7) 0.0987(4) 0.091(3) Uani 1 1 d U . . H39A H 0.7400 0.5270 0.1270 0.110 Uiso 1 1 calc R . . C40 C 0.6011(6) 0.5113(6) 0.0838(4) 0.072(2) Uani 1 1 d . . . H40A H 0.5642 0.5621 0.1027 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02575(13) 0.02192(12) 0.02232(12) 0.00044(11) 0.00172(12) 0.00109(12) Mn1 0.0334(5) 0.0240(4) 0.0359(5) 0.0023(4) 0.0044(4) 0.0049(4) O1 0.078(4) 0.083(4) 0.035(2) -0.008(2) 0.000(2) 0.045(3) O2 0.048(3) 0.158(6) 0.039(3) -0.019(3) -0.004(2) 0.053(3) O3 0.088(3) 0.069(3) 0.089(3) -0.041(2) -0.036(2) 0.044(2) O4 0.065(3) 0.067(3) 0.087(4) -0.034(3) -0.034(3) 0.042(3) O5 0.029(2) 0.037(2) 0.028(2) 0.0051(16) 0.0073(16) -0.0028(16) O6 0.050(3) 0.050(2) 0.040(2) -0.0089(19) 0.010(2) -0.016(2) O7 0.048(3) 0.023(2) 0.053(3) -0.0007(19) 0.010(2) -0.0018(17) O8 0.042(2) 0.048(2) 0.035(2) 0.014(2) 0.0007(19) -0.013(2) O9 0.049(3) 0.037(2) 0.030(2) 0.0070(18) -0.0015(19) 0.0002(19) O10 0.046(2) 0.029(2) 0.062(3) 0.004(2) -0.013(2) 0.0084(18) O11 0.065(3) 0.072(3) 0.035(2) -0.003(2) -0.005(2) 0.033(3) O12 0.041(2) 0.042(2) 0.029(2) -0.0031(18) -0.0094(17) 0.0051(18) C1 0.042(4) 0.039(3) 0.039(4) -0.009(3) 0.003(3) 0.014(3) C2 0.044(4) 0.032(4) 0.063(4) -0.003(3) 0.018(3) 0.009(3) C3 0.049(4) 0.095(6) 0.134(7) -0.059(5) 0.009(5) 0.001(4) C4 0.046(4) 0.070(5) 0.113(7) -0.056(5) 0.015(4) 0.002(4) C5 0.040(3) 0.029(3) 0.053(4) 0.002(3) 0.016(3) 0.009(3) C6 0.035(3) 0.035(3) 0.030(3) -0.005(3) 0.005(2) 0.007(3) C7 0.078(4) 0.061(3) 0.078(3) -0.039(3) -0.032(3) 0.041(3) C8 0.108(7) 0.049(5) 0.103(7) 0.025(4) 0.066(6) 0.039(5) C9 0.063(5) 0.115(7) 0.061(5) -0.037(5) -0.011(4) 0.023(5) C10 0.086(6) 0.037(4) 0.079(5) 0.002(4) 0.047(5) 0.003(4) C11 0.032(3) 0.026(3) 0.031(3) 0.000(2) 0.007(2) 0.002(2) C12 0.034(3) 0.027(3) 0.040(3) 0.000(2) 0.014(3) 0.002(2) C13 0.032(3) 0.060(4) 0.068(5) 0.035(4) -0.004(3) -0.004(3) C14 0.038(3) 0.044(4) 0.043(4) 0.013(3) 0.000(3) 0.001(3) C15 0.031(3) 0.026(3) 0.032(3) 0.003(2) 0.010(2) 0.001(2) C16 0.032(3) 0.024(3) 0.032(3) 0.002(2) 0.009(2) -0.001(2) C17 0.019(3) 0.037(3) 0.042(4) 0.010(3) 0.002(2) 0.002(2) C18 0.042(3) 0.037(4) 0.071(4) -0.008(3) 0.021(3) 0.001(3) C19 0.028(3) 0.040(3) 0.056(4) 0.018(3) 0.015(3) 0.005(3) C20 0.060(4) 0.061(4) 0.034(3) -0.005(3) -0.001(3) -0.013(3) C21 0.020(3) 0.027(3) 0.045(4) 0.008(3) 0.001(2) 0.005(2) C22 0.026(3) 0.034(3) 0.038(3) 0.005(2) -0.009(2) -0.003(2) C23 0.086(5) 0.038(4) 0.072(5) 0.012(3) -0.038(4) -0.012(4) C24 0.064(4) 0.038(4) 0.061(4) -0.003(3) -0.020(3) 0.002(3) C25 0.053(4) 0.025(3) 0.033(3) 0.004(3) -0.014(3) -0.005(3) C26 0.050(4) 0.032(3) 0.066(5) 0.019(3) -0.024(3) -0.009(3) C27 0.050(3) 0.024(3) 0.029(3) 0.003(3) 0.002(3) 0.004(3) C28 0.047(4) 0.094(6) 0.055(4) 0.012(4) -0.005(3) 0.009(4) C29 0.148(9) 0.044(5) 0.078(6) -0.010(4) -0.055(6) 0.010(5) C30 0.040(4) 0.080(5) 0.097(6) 0.055(5) -0.007(4) -0.005(3) N1 0.083(4) 0.039(3) 0.061(4) 0.011(3) 0.040(3) 0.015(3) N2 0.035(3) 0.044(3) 0.088(5) 0.031(3) 0.012(3) 0.005(3) C31 0.117(7) 0.047(4) 0.066(5) -0.006(4) 0.057(5) 0.003(4) C32 0.129(7) 0.083(6) 0.077(5) -0.004(5) 0.045(5) -0.011(5) C33 0.135(8) 0.071(6) 0.100(7) 0.005(5) 0.053(6) 0.020(6) C34 0.095(6) 0.079(6) 0.111(6) 0.029(5) 0.061(5) 0.036(5) C35 0.089(6) 0.040(4) 0.103(7) 0.033(5) 0.072(6) 0.024(4) C36 0.043(4) 0.060(5) 0.112(7) 0.047(5) 0.033(4) 0.011(4) C37 0.070(5) 0.092(6) 0.135(7) 0.043(6) 0.041(5) 0.027(4) C38 0.053(4) 0.101(6) 0.152(7) 0.059(6) 0.005(6) 0.001(5) C39 0.070(5) 0.086(6) 0.118(7) 0.041(5) -0.023(5) -0.029(4) C40 0.049(4) 0.060(5) 0.106(6) 0.054(5) -0.016(4) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O8 2.382(4) . ? Nd1 O10 2.395(4) . ? Nd1 O5 2.395(3) 4_465 ? Nd1 O3 2.431(4) . ? Nd1 O4 2.461(4) . ? Nd1 O12 2.481(4) 3_655 ? Nd1 O1 2.504(4) 3_545 ? Nd1 O2 2.510(4) 3_545 ? Nd1 C7 2.834(7) . ? Nd1 C1 2.858(6) 3_545 ? Mn1 O7 2.104(4) . ? Mn1 O6 2.179(4) 4_465 ? Mn1 O9 2.180(4) . ? Mn1 N1 2.233(6) . ? Mn1 N2 2.257(6) . ? Mn1 O5 2.464(4) 4_465 ? O1 C1 1.232(7) . ? O1 Nd1 2.504(4) 3 ? O2 C1 1.248(7) . ? O2 Nd1 2.510(4) 3 ? O3 C7 1.217(8) . ? O4 C7 1.210(8) . ? O5 C11 1.254(6) . ? O5 Nd1 2.395(3) 4_565 ? O5 Mn1 2.464(4) 4_565 ? O6 C11 1.251(6) . ? O6 Mn1 2.179(4) 4_565 ? O7 C17 1.255(7) . ? O8 C17 1.238(6) . ? O9 C21 1.227(6) . ? O10 C21 1.261(6) . ? O11 C27 1.298(7) . ? O11 H11A 0.8200 . ? O12 C27 1.228(6) . ? O12 Nd1 2.481(4) 3_645 ? C1 C2 1.507(8) . ? C1 Nd1 2.858(6) 3 ? C2 C3 1.532(10) . ? C2 C6 1.551(8) . ? C2 H2A 0.9800 . ? C3 C4 1.473(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.532(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C8 1.520(9) . ? C5 C7 1.526(8) . ? C5 C6 1.566(7) . ? C6 C10 1.493(9) . ? C6 C9 1.517(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.504(7) . ? C12 C13 1.513(8) . ? C12 C16 1.550(7) . ? C12 H12A 0.9800 . ? C13 C14 1.523(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.530(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C18 1.530(7) . ? C15 C17 1.544(7) . ? C15 C16 1.564(7) . ? C16 C19 1.526(7) . ? C16 C20 1.539(8) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.524(7) . ? C22 C23 1.509(8) . ? C22 C26 1.565(8) . ? C22 H22A 0.9800 . ? C23 C24 1.560(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.532(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C27 1.486(8) . ? C25 C26 1.558(8) . ? C25 C28 1.558(9) . ? C26 C30 1.486(9) . ? C26 C29 1.546(10) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1 C31 1.335(10) . ? N1 C35 1.350(10) . ? N2 C40 1.322(9) . ? N2 C36 1.332(10) . ? C31 C32 1.365(11) . ? C31 H31A 0.9300 . ? C32 C33 1.331(14) . ? C32 H32A 0.9300 . ? C33 C34 1.330(13) . ? C33 H33A 0.9300 . ? C34 C35 1.448(11) . ? C34 H34A 0.9300 . ? C35 C36 1.446(12) . ? C36 C37 1.397(11) . ? C37 C38 1.342(13) . ? C37 H37A 0.9300 . ? C38 C39 1.372(12) . ? C38 H38A 0.9300 . ? C39 C40 1.390(11) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Nd1 O10 85.23(14) . . ? O8 Nd1 O5 76.95(12) . 4_465 ? O10 Nd1 O5 77.26(13) . 4_465 ? O8 Nd1 O3 92.97(18) . . ? O10 Nd1 O3 149.51(15) . . ? O5 Nd1 O3 131.99(14) 4_465 . ? O8 Nd1 O4 97.09(17) . . ? O10 Nd1 O4 159.99(15) . . ? O5 Nd1 O4 83.88(14) 4_465 . ? O3 Nd1 O4 50.45(15) . . ? O8 Nd1 O12 77.35(13) . 3_655 ? O10 Nd1 O12 76.55(13) . 3_655 ? O5 Nd1 O12 144.48(12) 4_465 3_655 ? O3 Nd1 O12 73.38(15) . 3_655 ? O4 Nd1 O12 123.40(14) . 3_655 ? O8 Nd1 O1 157.77(14) . 3_545 ? O10 Nd1 O1 88.33(16) . 3_545 ? O5 Nd1 O1 80.88(13) 4_465 3_545 ? O3 Nd1 O1 103.2(2) . 3_545 ? O4 Nd1 O1 82.06(19) . 3_545 ? O12 Nd1 O1 121.69(14) 3_655 3_545 ? O8 Nd1 O2 149.77(13) . 3_545 ? O10 Nd1 O2 86.76(19) . 3_545 ? O5 Nd1 O2 129.26(14) 4_465 3_545 ? O3 Nd1 O2 79.6(2) . 3_545 ? O4 Nd1 O2 100.3(2) . 3_545 ? O12 Nd1 O2 72.44(13) 3_655 3_545 ? O1 Nd1 O2 50.44(14) 3_545 3_545 ? O8 Nd1 C7 95.5(2) . . ? O10 Nd1 C7 174.67(18) . . ? O5 Nd1 C7 108.05(17) 4_465 . ? O3 Nd1 C7 25.27(18) . . ? O4 Nd1 C7 25.18(17) . . ? O12 Nd1 C7 98.44(17) 3_655 . ? O1 Nd1 C7 92.9(2) 3_545 . ? O2 Nd1 C7 90.0(2) 3_545 . ? O8 Nd1 C1 175.36(16) . 3_545 ? O10 Nd1 C1 92.23(16) . 3_545 ? O5 Nd1 C1 106.31(15) 4_465 3_545 ? O3 Nd1 C1 87.24(19) . 3_545 ? O4 Nd1 C1 86.63(18) . 3_545 ? O12 Nd1 C1 98.29(15) 3_655 3_545 ? O1 Nd1 C1 25.48(15) 3_545 3_545 ? O2 Nd1 C1 25.86(15) 3_545 3_545 ? C7 Nd1 C1 86.7(2) . 3_545 ? O7 Mn1 O6 93.84(16) . 4_465 ? O7 Mn1 O9 160.71(16) . . ? O6 Mn1 O9 97.89(15) 4_465 . ? O7 Mn1 N1 109.32(18) . . ? O6 Mn1 N1 89.4(2) 4_465 . ? O9 Mn1 N1 86.15(17) . . ? O7 Mn1 N2 87.55(18) . . ? O6 Mn1 N2 161.1(2) 4_465 . ? O9 Mn1 N2 86.30(17) . . ? N1 Mn1 N2 72.4(3) . . ? O7 Mn1 O5 86.07(14) . 4_465 ? O6 Mn1 O5 55.37(13) 4_465 4_465 ? O9 Mn1 O5 88.05(14) . 4_465 ? N1 Mn1 O5 143.1(2) . 4_465 ? N2 Mn1 O5 143.48(19) . 4_465 ? C1 O1 Nd1 93.6(3) . 3 ? C1 O2 Nd1 92.8(4) . 3 ? C7 O3 Nd1 96.2(4) . . ? C7 O4 Nd1 94.9(4) . . ? C11 O5 Nd1 172.0(3) . 4_565 ? C11 O5 Mn1 85.4(3) . 4_565 ? Nd1 O5 Mn1 101.43(12) 4_565 4_565 ? C11 O6 Mn1 98.8(3) . 4_565 ? C17 O7 Mn1 119.4(4) . . ? C17 O8 Nd1 143.3(4) . . ? C21 O9 Mn1 109.9(3) . . ? C21 O10 Nd1 142.4(4) . . ? C27 O11 H11A 109.5 . . ? C27 O12 Nd1 141.8(4) . 3_645 ? O1 C1 O2 119.0(6) . . ? O1 C1 C2 122.0(6) . . ? O2 C1 C2 119.0(5) . . ? O1 C1 Nd1 61.0(3) . 3 ? O2 C1 Nd1 61.3(3) . 3 ? C2 C1 Nd1 159.5(4) . 3 ? C1 C2 C3 113.2(6) . . ? C1 C2 C6 116.5(5) . . ? C3 C2 C6 104.8(5) . . ? C1 C2 H2A 107.3 . . ? C3 C2 H2A 107.3 . . ? C6 C2 H2A 107.3 . . ? C4 C3 C2 106.8(6) . . ? C4 C3 H3A 110.4 . . ? C2 C3 H3A 110.4 . . ? C4 C3 H3B 110.4 . . ? C2 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C3 C4 C5 108.7(6) . . ? C3 C4 H4A 109.9 . . ? C5 C4 H4A 109.9 . . ? C3 C4 H4B 109.9 . . ? C5 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C8 C5 C7 107.3(5) . . ? C8 C5 C4 110.2(6) . . ? C7 C5 C4 110.6(6) . . ? C8 C5 C6 113.8(5) . . ? C7 C5 C6 112.4(6) . . ? C4 C5 C6 102.6(5) . . ? C10 C6 C9 107.4(6) . . ? C10 C6 C2 112.1(5) . . ? C9 C6 C2 111.0(5) . . ? C10 C6 C5 111.3(5) . . ? C9 C6 C5 113.8(5) . . ? C2 C6 C5 101.2(5) . . ? O4 C7 O3 118.4(6) . . ? O4 C7 C5 121.5(6) . . ? O3 C7 C5 119.7(6) . . ? O4 C7 Nd1 59.9(3) . . ? O3 C7 Nd1 58.5(3) . . ? C5 C7 Nd1 173.3(6) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 120.2(5) . . ? O6 C11 C12 119.4(5) . . ? O5 C11 C12 120.4(5) . . ? C11 C12 C13 115.6(5) . . ? C11 C12 C16 114.0(4) . . ? C13 C12 C16 105.8(5) . . ? C11 C12 H12A 107.0 . . ? C13 C12 H12A 107.0 . . ? C16 C12 H12A 107.0 . . ? C12 C13 C14 107.0(5) . . ? C12 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? C12 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? C13 C14 C15 105.5(5) . . ? C13 C14 H14A 110.6 . . ? C15 C14 H14A 110.6 . . ? C13 C14 H14B 110.6 . . ? C15 C14 H14B 110.6 . . ? H14A C14 H14B 108.8 . . ? C18 C15 C14 109.5(5) . . ? C18 C15 C17 108.2(4) . . ? C14 C15 C17 113.3(5) . . ? C18 C15 C16 112.6(5) . . ? C14 C15 C16 101.8(4) . . ? C17 C15 C16 111.4(4) . . ? C19 C16 C20 108.2(5) . . ? C19 C16 C12 109.5(4) . . ? C20 C16 C12 112.5(5) . . ? C19 C16 C15 112.0(4) . . ? C20 C16 C15 113.4(4) . . ? C12 C16 C15 101.2(4) . . ? O8 C17 O7 123.4(5) . . ? O8 C17 C15 118.5(5) . . ? O7 C17 C15 118.1(5) . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 122.2(5) . . ? O9 C21 C22 120.4(5) . . ? O10 C21 C22 117.4(5) . . ? C23 C22 C21 114.3(5) . . ? C23 C22 C26 107.4(5) . . ? C21 C22 C26 113.8(4) . . ? C23 C22 H22A 106.9 . . ? C21 C22 H22A 106.9 . . ? C26 C22 H22A 106.9 . . ? C22 C23 C24 104.6(5) . . ? C22 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? C22 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? C25 C24 C23 107.2(5) . . ? C25 C24 H24A 110.3 . . ? C23 C24 H24A 110.3 . . ? C25 C24 H24B 110.3 . . ? C23 C24 H24B 110.3 . . ? H24A C24 H24B 108.5 . . ? C27 C25 C24 114.8(5) . . ? C27 C25 C26 111.7(5) . . ? C24 C25 C26 101.3(5) . . ? C27 C25 C28 109.7(5) . . ? C24 C25 C28 108.4(5) . . ? C26 C25 C28 110.7(5) . . ? C30 C26 C29 108.5(6) . . ? C30 C26 C25 111.5(6) . . ? C29 C26 C25 112.0(6) . . ? C30 C26 C22 112.2(5) . . ? C29 C26 C22 110.6(6) . . ? C25 C26 C22 101.9(5) . . ? O12 C27 O11 122.2(5) . . ? O12 C27 C25 121.3(5) . . ? O11 C27 C25 116.6(5) . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 N1 C35 119.6(7) . . ? C31 N1 Mn1 123.2(5) . . ? C35 N1 Mn1 115.7(6) . . ? C40 N2 C36 119.8(7) . . ? C40 N2 Mn1 124.1(5) . . ? C36 N2 Mn1 116.0(6) . . ? N1 C31 C32 123.7(10) . . ? N1 C31 H31A 118.2 . . ? C32 C31 H31A 118.2 . . ? C33 C32 C31 116.4(11) . . ? C33 C32 H32A 121.8 . . ? C31 C32 H32A 121.8 . . ? C34 C33 C32 124.3(10) . . ? C34 C33 H33A 117.8 . . ? C32 C33 H33A 117.8 . . ? C33 C34 C35 117.7(10) . . ? C33 C34 H34A 121.2 . . ? C35 C34 H34A 121.2 . . ? N1 C35 C36 116.4(7) . . ? N1 C35 C34 118.0(10) . . ? C36 C35 C34 125.6(9) . . ? N2 C36 C37 121.2(10) . . ? N2 C36 C35 116.8(7) . . ? C37 C36 C35 121.9(9) . . ? C38 C37 C36 116.5(10) . . ? C38 C37 H37A 121.7 . . ? C36 C37 H37A 121.7 . . ? C37 C38 C39 124.6(9) . . ? C37 C38 H38A 117.7 . . ? C39 C38 H38A 117.7 . . ? C38 C39 C40 114.4(9) . . ? C38 C39 H39A 122.8 . . ? C40 C39 H39A 122.8 . . ? N2 C40 C39 123.3(9) . . ? N2 C40 H40A 118.3 . . ? C39 C40 H40A 118.3 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.993 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.078 data_ddb2 _database_code_depnum_ccdc_archive 'CCDC 907543' #TrackingRef '2 Mn+Dy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H51 Dy Mn N2 O12' _chemical_formula_weight 969.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.547(7) _cell_length_b 12.979(7) _cell_length_c 24.368(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3968(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 8.36 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 2.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8404 _exptl_absorpt_correction_T_max 0.8957 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20052 _diffrn_reflns_av_R_equivalents 0.1964 _diffrn_reflns_av_sigmaI/netI 0.2831 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6997 _reflns_number_gt 2778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(2) _refine_ls_number_reflns 6997 _refine_ls_number_parameters 505 _refine_ls_number_restraints 237 _refine_ls_R_factor_all 0.2223 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.970 _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 Dy1 Dy 0.75864(7) 0.39698(6) 0.84846(3) 0.0486(2) Uani 1 1 d . . . Mn1 Mn 0.8796(2) 0.51860(18) 0.97151(12) 0.0429(8) Uani 1 1 d . . . O1 O 0.8813(11) 0.3119(11) 0.9026(5) 0.076(5) Uani 1 1 d D . . O2 O 0.9115(9) 0.3614(9) 0.9841(7) 0.080(5) Uani 1 1 d . . . O3 O 1.2270(10) -0.0103(8) 0.9870(5) 0.070(4) Uani 1 1 d . . . O4 O 1.2000(7) 0.0521(7) 1.0661(4) 0.041(3) Uani 1 1 d . . . C1 C 0.9068(15) 0.2898(15) 0.9498(7) 0.071(8) Uani 1 1 d D . . C2 C 1.1691(13) 0.0300(13) 1.0210(8) 0.036(5) Uani 1 1 d U . . C3 C 0.9384(15) 0.1856(13) 0.9667(9) 0.058(6) Uani 1 1 d U . . C4 C 1.0559(17) 0.1578(14) 0.9677(7) 0.104(9) Uani 1 1 d DU . . C5 C 1.0582(16) 0.0600(14) 0.9992(8) 0.066(6) Uani 1 1 d DU . . H5A H 1.0346 0.0050 0.9745 0.079 Uiso 1 1 calc R . . C6 C 0.9832(15) 0.0629(18) 1.0461(8) 0.107(9) Uani 1 1 d U . . H6A H 1.0205 0.0735 1.0805 0.129 Uiso 1 1 calc R . . H6B H 0.9416 0.0001 1.0484 0.129 Uiso 1 1 calc R . . C7 C 0.9090(14) 0.1610(14) 1.0309(9) 0.079(7) Uani 1 1 d . . . H7A H 0.9255 0.2194 1.0542 0.095 Uiso 1 1 calc R . . H7B H 0.8341 0.1441 1.0348 0.095 Uiso 1 1 calc R . . C8 C 0.8695(14) 0.1123(17) 0.9369(9) 0.116(8) Uani 1 1 d . . . H8A H 0.8826 0.1180 0.8982 0.174 Uiso 1 1 calc R . . H8B H 0.7961 0.1278 0.9443 0.174 Uiso 1 1 calc R . . H8C H 0.8850 0.0434 0.9488 0.174 Uiso 1 1 calc R . . C9 C 1.1204(13) 0.2409(11) 0.9934(7) 0.067(6) Uani 1 1 d D . . H9A H 1.0980 0.2505 1.0307 0.101 Uiso 1 1 calc R . . H9B H 1.1105 0.3039 0.9734 0.101 Uiso 1 1 calc R . . H9C H 1.1944 0.2220 0.9927 0.101 Uiso 1 1 calc R . . C10 C 1.0875(14) 0.1470(16) 0.9089(7) 0.104(8) Uani 1 1 d DU . . H10A H 1.0454 0.0940 0.8920 0.156 Uiso 1 1 calc R . . H10B H 1.1616 0.1289 0.9067 0.156 Uiso 1 1 calc R . . H10C H 1.0758 0.2111 0.8902 0.156 Uiso 1 1 calc R . . O5 O 0.9059(9) 0.3694(10) 0.7872(5) 0.056(4) Uani 1 1 d . . . O6 O 0.8618(11) 0.4241(11) 0.7038(4) 0.092(5) Uani 1 1 d U . . O7 O 1.1463(8) 0.1612(9) 0.5747(4) 0.050(3) Uani 1 1 d . . . O8 O 1.1446(8) 0.0468(8) 0.6409(5) 0.051(4) Uani 1 1 d . . . C11 C 0.9281(16) 0.3816(17) 0.7425(10) 0.070(7) Uani 1 1 d . . . C12 C 1.1444(12) 0.1372(13) 0.6211(8) 0.035(5) Uani 1 1 d U . . C13 C 1.0356(17) 0.3442(14) 0.7205(8) 0.063(6) Uani 1 1 d . . . C14 C 1.038(2) 0.237(2) 0.6973(10) 0.108(8) Uani 1 1 d U . . C15 C 1.1450(12) 0.2220(12) 0.6669(8) 0.048(5) Uani 1 1 d U . . H15A H 1.2005 0.2053 0.6938 0.058 Uiso 1 1 calc R . . C16 C 1.1677(14) 0.3234(16) 0.6432(9) 0.120(9) Uani 1 1 d . . . H16A H 1.1558 0.3232 0.6039 0.144 Uiso 1 1 calc R . . H16B H 1.2406 0.3440 0.6504 0.144 Uiso 1 1 calc R . . C17 C 1.0828(15) 0.4005(15) 0.6745(9) 0.121(9) Uani 1 1 d . . . H17A H 1.1194 0.4614 0.6877 0.145 Uiso 1 1 calc R . . H17B H 1.0275 0.4221 0.6491 0.145 Uiso 1 1 calc R . . C18 C 1.1231(16) 0.3479(17) 0.7667(9) 0.136(9) Uani 1 1 d U . . H18A H 1.1897 0.3237 0.7521 0.204 Uiso 1 1 calc R . . H18B H 1.1018 0.3047 0.7967 0.204 Uiso 1 1 calc R . . H18C H 1.1312 0.4175 0.7794 0.204 Uiso 1 1 calc R . . C19 C 0.9423(15) 0.2181(16) 0.6606(10) 0.131(9) Uani 1 1 d U . . H19A H 0.9417 0.2677 0.6313 0.197 Uiso 1 1 calc R . . H19B H 0.8782 0.2246 0.6817 0.197 Uiso 1 1 calc R . . H19C H 0.9464 0.1499 0.6454 0.197 Uiso 1 1 calc R . . C20 C 1.032(2) 0.1494(18) 0.7461(11) 0.139(11) Uani 1 1 d U . . H20A H 1.0918 0.1579 0.7705 0.209 Uiso 1 1 calc R . . H20B H 1.0346 0.0820 0.7300 0.209 Uiso 1 1 calc R . . H20C H 0.9671 0.1575 0.7663 0.209 Uiso 1 1 calc R . . O9 O 0.3860(11) 0.7746(10) 0.6407(6) 0.107(5) Uani 1 1 d U . . O10 O 0.2809(11) 0.7468(11) 0.6982(6) 0.119(5) Uani 1 1 d U . . O11 O 0.6063(11) 0.5064(11) 0.8233(6) 0.093(5) Uani 1 1 d . . . O12 O 0.6973(10) 0.4620(12) 0.7589(7) 0.100(5) Uani 1 1 d U . . C21 C 0.3445(19) 0.7127(19) 0.6707(10) 0.102(5) Uani 1 1 d U . . C22 C 0.626(2) 0.497(2) 0.7721(12) 0.092(6) Uani 1 1 d U . . C23 C 0.5283(19) 0.5086(17) 0.7352(10) 0.104(6) Uani 1 1 d U . . H23A H 0.5339 0.4566 0.7062 0.124 Uiso 1 1 calc R . . C24 C 0.5172(14) 0.6172(17) 0.7064(8) 0.068(6) Uani 1 1 d U . . C25 C 0.4004(17) 0.6075(18) 0.6862(10) 0.099(5) Uani 1 1 d U . . C26 C 0.3381(15) 0.5582(14) 0.7329(8) 0.108(5) Uani 1 1 d U . . H26A H 0.3076 0.6107 0.7565 0.130 Uiso 1 1 calc R . . H26B H 0.2810 0.5156 0.7187 0.130 Uiso 1 1 calc R . . C27 C 0.4147(16) 0.4957(16) 0.7632(9) 0.113(5) Uani 1 1 d U . . H27A H 0.3933 0.4239 0.7625 0.136 Uiso 1 1 calc R . . H27B H 0.4178 0.5180 0.8012 0.136 Uiso 1 1 calc R . . C28 C 0.3971(17) 0.5500(15) 0.6310(10) 0.141(8) Uani 1 1 d U . . H28A H 0.3245 0.5432 0.6192 0.211 Uiso 1 1 calc R . . H28B H 0.4281 0.4829 0.6353 0.211 Uiso 1 1 calc R . . H28C H 0.4367 0.5881 0.6041 0.211 Uiso 1 1 calc R . . C29 C 0.6039(13) 0.6276(18) 0.6620(8) 0.135(9) Uani 1 1 d U . . H29A H 0.6723 0.6352 0.6792 0.203 Uiso 1 1 calc R . . H29B H 0.5895 0.6869 0.6397 0.203 Uiso 1 1 calc R . . H29C H 0.6041 0.5670 0.6394 0.203 Uiso 1 1 calc R . . C30 C 0.5352(17) 0.7051(14) 0.7468(9) 0.089(8) Uani 1 1 d . . . H30A H 0.4821 0.7024 0.7751 0.134 Uiso 1 1 calc R . . H30B H 0.5303 0.7697 0.7278 0.134 Uiso 1 1 calc R . . H30C H 0.6047 0.6985 0.7629 0.134 Uiso 1 1 calc R . . N1 N 1.0533(11) 0.5410(12) 0.9544(8) 0.075(6) Uani 1 1 d D . . N2 N 0.9472(16) 0.6176(16) 1.0418(8) 0.089(7) Uani 1 1 d . . . C31 C 1.1069(17) 0.4917(14) 0.9147(9) 0.084(7) Uani 1 1 d DU . . H31A H 1.0714 0.4418 0.8943 0.100 Uiso 1 1 calc R . . C32 C 1.2129(18) 0.5116(18) 0.9026(10) 0.130(10) Uani 1 1 d D . . H32A H 1.2483 0.4786 0.8741 0.156 Uiso 1 1 calc R . . C33 C 1.2618(15) 0.5821(18) 0.9350(10) 0.132(9) Uani 1 1 d DU . . H33A H 1.3334 0.5955 0.9283 0.159 Uiso 1 1 calc R . . C34 C 1.2126(15) 0.6361(15) 0.9777(9) 0.138(9) Uani 1 1 d DU . . H34A H 1.2488 0.6838 0.9992 0.166 Uiso 1 1 calc R . . C35 C 1.1043(14) 0.6130(18) 0.9856(9) 0.085(7) Uani 1 1 d DU . . C36 C 1.043(2) 0.6540(18) 1.0266(10) 0.080(7) Uani 1 1 d U . . C37 C 1.072(2) 0.739(2) 1.0639(12) 0.123(10) Uani 1 1 d U . . H37A H 1.1382 0.7709 1.0600 0.147 Uiso 1 1 calc R . . C38 C 1.005(3) 0.771(2) 1.1034(11) 0.128(12) Uani 1 1 d U . . H38A H 1.0212 0.8314 1.1227 0.154 Uiso 1 1 calc R . . C39 C 0.927(2) 0.725(2) 1.1142(12) 0.121(11) Uani 1 1 d U . . H39A H 0.8934 0.7394 1.1473 0.145 Uiso 1 1 calc R . . C40 C 0.882(2) 0.6516(18) 1.0810(10) 0.094(8) Uani 1 1 d . . . H40A H 0.8132 0.6277 1.0855 0.113 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0522(4) 0.0478(4) 0.0458(4) -0.0017(6) 0.0005(7) 0.0021(7) Mn1 0.0495(18) 0.0315(15) 0.0476(18) 0.0029(16) -0.0112(16) -0.0069(15) O1 0.093(11) 0.090(11) 0.046(9) 0.032(9) 0.008(8) 0.051(9) O2 0.047(8) 0.035(8) 0.157(16) 0.036(10) -0.013(9) 0.012(7) O3 0.063(10) 0.070(8) 0.077(9) -0.005(7) -0.045(8) 0.021(9) O4 0.033(7) 0.040(7) 0.049(7) 0.010(6) -0.020(6) -0.013(5) C1 0.027(12) 0.026(14) 0.16(3) 0.016(17) 0.010(16) -0.014(11) C2 0.029(10) 0.037(10) 0.043(11) -0.010(10) -0.024(9) 0.016(8) C3 0.063(12) 0.029(10) 0.084(13) -0.009(11) -0.034(11) -0.019(10) C4 0.086(18) 0.078(16) 0.15(2) -0.023(18) 0.055(17) -0.058(15) C5 0.078(13) 0.048(11) 0.072(13) 0.014(11) 0.027(11) 0.020(10) C6 0.073(15) 0.17(2) 0.077(16) 0.066(17) -0.007(13) -0.006(17) C7 0.072(15) 0.062(13) 0.104(19) 0.005(14) 0.010(14) -0.026(13) C8 0.097(16) 0.105(17) 0.15(2) 0.01(2) 0.001(16) 0.01(2) C9 0.059(13) 0.043(11) 0.100(17) 0.032(12) -0.016(13) 0.005(11) C10 0.105(14) 0.150(17) 0.057(12) 0.011(12) 0.040(11) 0.001(13) O5 0.058(8) 0.074(10) 0.037(8) 0.001(8) 0.028(6) 0.022(8) O6 0.120(10) 0.123(12) 0.035(7) 0.017(8) 0.002(7) 0.045(10) O7 0.047(7) 0.075(9) 0.030(7) -0.013(7) 0.019(6) 0.016(7) O8 0.041(7) 0.026(6) 0.087(11) 0.004(8) 0.019(8) -0.006(6) C11 0.077(16) 0.052(15) 0.082(18) -0.044(16) 0.038(14) 0.005(14) C12 0.025(8) 0.025(8) 0.055(10) -0.022(9) 0.017(8) 0.003(7) C13 0.101(18) 0.049(12) 0.038(13) -0.008(11) 0.004(13) 0.005(13) C14 0.109(15) 0.114(15) 0.102(15) -0.065(14) 0.030(13) -0.015(14) C15 0.023(9) 0.033(9) 0.089(14) 0.000(10) 0.016(9) -0.012(8) C16 0.089(16) 0.14(2) 0.13(2) -0.07(2) 0.015(17) -0.004(16) C17 0.141(19) 0.073(14) 0.15(2) 0.069(19) 0.062(17) 0.009(18) C18 0.104(14) 0.165(18) 0.139(16) -0.033(15) -0.005(14) 0.043(14) C19 0.082(13) 0.141(15) 0.170(17) -0.080(15) 0.013(15) 0.022(12) C20 0.168(19) 0.106(16) 0.144(17) 0.020(15) 0.056(15) 0.030(14) O9 0.102(9) 0.095(9) 0.123(10) 0.042(9) -0.003(9) 0.055(8) O10 0.109(10) 0.110(8) 0.139(9) 0.043(7) 0.005(8) 0.045(8) O11 0.073(10) 0.102(12) 0.104(13) 0.026(12) -0.012(9) 0.041(9) O12 0.072(12) 0.119(12) 0.111(11) 0.020(10) -0.029(10) 0.035(9) C21 0.099(8) 0.092(8) 0.116(8) 0.028(7) -0.005(7) 0.037(7) C22 0.074(15) 0.100(14) 0.101(13) 0.016(12) -0.024(13) 0.033(12) C23 0.103(13) 0.087(11) 0.121(13) 0.051(11) 0.012(11) 0.007(12) C24 0.056(12) 0.054(13) 0.093(15) 0.023(14) -0.039(11) 0.020(13) C25 0.113(11) 0.086(11) 0.098(11) 0.016(11) -0.001(10) 0.009(11) C26 0.107(10) 0.094(10) 0.124(11) 0.041(9) 0.005(9) 0.002(9) C27 0.110(11) 0.101(10) 0.130(11) 0.051(10) 0.001(9) 0.006(10) C28 0.161(15) 0.115(15) 0.145(17) -0.036(14) -0.013(15) 0.032(14) C29 0.111(15) 0.19(2) 0.102(17) 0.063(19) 0.076(15) 0.026(18) C30 0.081(17) 0.057(16) 0.13(2) 0.016(17) -0.025(16) 0.008(14) N1 0.043(11) 0.045(10) 0.136(18) 0.034(11) -0.004(11) -0.002(9) N2 0.072(14) 0.091(15) 0.104(17) 0.072(16) -0.041(12) -0.005(14) C31 0.061(12) 0.079(13) 0.111(15) 0.058(12) 0.004(12) 0.012(12) C32 0.08(2) 0.13(2) 0.18(3) 0.041(18) 0.063(19) 0.036(18) C33 0.088(13) 0.146(16) 0.163(17) 0.082(14) -0.002(12) -0.001(13) C34 0.096(14) 0.147(17) 0.173(18) 0.086(15) -0.008(13) -0.002(13) C35 0.044(11) 0.087(14) 0.125(15) 0.048(14) -0.006(12) -0.008(13) C36 0.085(13) 0.070(13) 0.086(14) 0.022(12) -0.052(12) 0.000(12) C37 0.134(17) 0.108(16) 0.126(18) 0.038(15) -0.061(15) -0.011(14) C38 0.19(3) 0.13(2) 0.065(19) -0.011(19) -0.05(2) -0.01(2) C39 0.147(19) 0.110(17) 0.106(17) -0.006(15) -0.042(16) -0.025(15) C40 0.10(2) 0.085(19) 0.10(2) 0.015(18) -0.037(17) -0.019(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 Dy1 O4 2.305(11) 4_457 ? Dy1 O8 2.307(10) 3_756 ? Dy1 O1 2.309(13) . ? Dy1 O10 2.311(13) 3_646 ? Dy1 O5 2.402(11) . ? Dy1 O9 2.426(12) 3_646 ? Dy1 O11 2.459(12) . ? Dy1 O12 2.464(16) . ? Dy1 C21 2.76(2) 3_646 ? Dy1 C22 2.82(3) . ? Mn1 O2 2.102(11) . ? Mn1 O3 2.167(11) 4_457 ? Mn1 O7 2.191(11) 3_756 ? Mn1 N1 2.238(14) . ? Mn1 N2 2.30(2) . ? O1 C1 1.227(10) . ? O2 C1 1.250(19) . ? O3 C2 1.222(16) . ? O3 Mn1 2.167(11) 4_557 ? O4 C2 1.199(17) . ? O4 Dy1 2.305(11) 4_557 ? C1 C3 1.47(2) . ? C2 C5 1.54(2) . ? C3 C8 1.48(2) . ? C3 C4 1.52(2) . ? C3 C7 1.64(2) . ? C4 C5 1.483(10) . ? C4 C9 1.485(10) . ? C4 C10 1.495(10) . ? C5 C6 1.48(2) . ? C5 H5A 0.9800 . ? C6 C7 1.62(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? O5 C11 1.14(2) . ? O6 C11 1.37(2) . ? O7 C12 1.172(18) . ? O7 Mn1 2.191(11) 3_746 ? O8 C12 1.269(17) . ? O8 Dy1 2.307(10) 3_746 ? C11 C13 1.53(2) . ? C12 C15 1.57(2) . ? C13 C17 1.46(2) . ? C13 C14 1.50(3) . ? C13 C18 1.57(2) . ? C14 C19 1.52(3) . ? C14 C15 1.54(2) . ? C14 C20 1.65(3) . ? C15 C16 1.46(2) . ? C15 H15A 0.9800 . ? C16 C17 1.65(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O9 C21 1.20(2) . ? O9 Dy1 2.426(12) 3_656 ? O10 C21 1.13(2) . ? O10 Dy1 2.311(13) 3_656 ? O11 C22 1.28(3) . ? O12 C22 1.06(2) . ? C21 C25 1.58(3) . ? C21 Dy1 2.76(2) 3_656 ? C22 C23 1.52(3) . ? C23 C24 1.58(2) . ? C23 C27 1.59(3) . ? C23 H23A 0.9800 . ? C24 C30 1.52(2) . ? C24 C29 1.54(2) . ? C24 C25 1.55(2) . ? C25 C26 1.52(2) . ? C25 C28 1.54(2) . ? C26 C27 1.46(2) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1 C31 1.34(2) . ? N1 C35 1.36(2) . ? N2 C40 1.33(2) . ? N2 C36 1.34(2) . ? C31 C32 1.39(2) . ? C31 H31A 0.9300 . ? C32 C33 1.35(3) . ? C32 H32A 0.9300 . ? C33 C34 1.398(10) . ? C33 H33A 0.9300 . ? C34 C35 1.405(10) . ? C34 H34A 0.9300 . ? C35 C36 1.37(3) . ? C36 C37 1.48(3) . ? C37 C38 1.34(3) . ? C37 H37A 0.9300 . ? C38 C39 1.18(3) . ? C38 H38A 0.9300 . ? C39 C40 1.37(3) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Dy1 O8 79.9(4) 4_457 3_756 ? O4 Dy1 O1 80.4(4) 4_457 . ? O8 Dy1 O1 89.3(5) 3_756 . ? O4 Dy1 O10 128.2(4) 4_457 3_646 ? O8 Dy1 O10 151.6(5) 3_756 3_646 ? O1 Dy1 O10 91.2(5) . 3_646 ? O4 Dy1 O5 148.1(4) 4_457 . ? O8 Dy1 O5 77.9(4) 3_756 . ? O1 Dy1 O5 76.8(4) . . ? O10 Dy1 O5 74.6(5) 3_646 . ? O4 Dy1 O9 81.4(4) 4_457 3_646 ? O8 Dy1 O9 158.9(5) 3_756 3_646 ? O1 Dy1 O9 97.1(5) . 3_646 ? O10 Dy1 O9 48.7(5) 3_646 3_646 ? O5 Dy1 O9 123.1(5) . 3_646 ? O4 Dy1 O11 79.2(4) 4_457 . ? O8 Dy1 O11 87.1(4) 3_756 . ? O1 Dy1 O11 159.6(5) . . ? O10 Dy1 O11 101.4(5) 3_646 . ? O5 Dy1 O11 122.0(5) . . ? O9 Dy1 O11 79.8(5) 3_646 . ? O4 Dy1 O12 127.0(4) 4_457 . ? O8 Dy1 O12 88.6(5) 3_756 . ? O1 Dy1 O12 151.5(5) . . ? O10 Dy1 O12 77.6(6) 3_646 . ? O5 Dy1 O12 75.0(4) . . ? O9 Dy1 O12 95.0(5) 3_646 . ? O11 Dy1 O12 48.6(4) . . ? O4 Dy1 C21 104.6(6) 4_457 3_646 ? O8 Dy1 C21 175.2(6) 3_756 3_646 ? O1 Dy1 C21 89.7(6) . 3_646 ? O10 Dy1 C21 23.8(6) 3_646 3_646 ? O5 Dy1 C21 97.3(6) . 3_646 ? O9 Dy1 C21 25.8(5) 3_646 3_646 ? O11 Dy1 C21 95.4(6) . 3_646 ? O12 Dy1 C21 90.0(6) . 3_646 ? O4 Dy1 C22 106.0(7) 4_457 . ? O8 Dy1 C22 89.8(6) 3_756 . ? O1 Dy1 C22 173.3(7) . . ? O10 Dy1 C22 86.4(7) 3_646 . ? O5 Dy1 C22 96.6(7) . . ? O9 Dy1 C22 86.0(7) 3_646 . ? O11 Dy1 C22 26.9(6) . . ? O12 Dy1 C22 21.8(6) . . ? C21 Dy1 C22 90.6(8) 3_646 . ? O2 Mn1 O3 93.0(5) . 4_457 ? O2 Mn1 O7 157.4(6) . 3_756 ? O3 Mn1 O7 98.7(4) 4_457 3_756 ? O2 Mn1 N1 88.2(5) . . ? O3 Mn1 N1 162.4(7) 4_457 . ? O7 Mn1 N1 86.5(5) 3_756 . ? O2 Mn1 N2 111.3(6) . . ? O3 Mn1 N2 90.3(7) 4_457 . ? O7 Mn1 N2 88.1(5) 3_756 . ? N1 Mn1 N2 73.0(8) . . ? C1 O1 Dy1 145.2(15) . . ? C1 O2 Mn1 128.0(12) . . ? C2 O3 Mn1 103.3(10) . 4_557 ? C2 O4 Dy1 177.2(12) . 4_557 ? O1 C1 O2 117.7(19) . . ? O1 C1 C3 123(2) . . ? O2 C1 C3 119.0(15) . . ? O4 C2 O3 122.1(15) . . ? O4 C2 C5 123.3(16) . . ? O3 C2 C5 114.3(16) . . ? C1 C3 C8 107.4(16) . . ? C1 C3 C4 119.1(17) . . ? C8 C3 C4 115.1(16) . . ? C1 C3 C7 112.7(17) . . ? C8 C3 C7 102.2(16) . . ? C4 C3 C7 99.0(14) . . ? C5 C4 C9 113.1(17) . . ? C5 C4 C10 114.2(16) . . ? C9 C4 C10 109.2(15) . . ? C5 C4 C3 103.3(15) . . ? C9 C4 C3 111.3(15) . . ? C10 C4 C3 105.3(17) . . ? C4 C5 C6 111.4(16) . . ? C4 C5 C2 114.3(19) . . ? C6 C5 C2 108.3(16) . . ? C4 C5 H5A 107.5 . . ? C6 C5 H5A 107.5 . . ? C2 C5 H5A 107.5 . . ? C5 C6 C7 102.0(15) . . ? C5 C6 H6A 111.4 . . ? C7 C6 H6A 111.4 . . ? C5 C6 H6B 111.4 . . ? C7 C6 H6B 111.4 . . ? H6A C6 H6B 109.2 . . ? C6 C7 C3 104.1(15) . . ? C6 C7 H7A 110.9 . . ? C3 C7 H7A 110.9 . . ? C6 C7 H7B 110.9 . . ? C3 C7 H7B 110.9 . . ? H7A C7 H7B 109.0 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 O5 Dy1 139.8(16) . . ? C12 O7 Mn1 105.6(11) . 3_746 ? C12 O8 Dy1 145.4(11) . 3_746 ? O5 C11 O6 125(2) . . ? O5 C11 C13 120(2) . . ? O6 C11 C13 115.0(18) . . ? O7 C12 O8 127.8(16) . . ? O7 C12 C15 120.0(16) . . ? O8 C12 C15 112.2(16) . . ? C17 C13 C14 99.4(18) . . ? C17 C13 C11 117.7(18) . . ? C14 C13 C11 116.4(19) . . ? C17 C13 C18 104.6(18) . . ? C14 C13 C18 106.4(19) . . ? C11 C13 C18 110.8(17) . . ? C13 C14 C19 111(2) . . ? C13 C14 C15 108.5(19) . . ? C19 C14 C15 112.7(18) . . ? C13 C14 C20 111.4(19) . . ? C19 C14 C20 106(2) . . ? C15 C14 C20 107(2) . . ? C16 C15 C14 104.1(16) . . ? C16 C15 C12 110.5(17) . . ? C14 C15 C12 115.2(15) . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? C12 C15 H15A 108.9 . . ? C15 C16 C17 103.8(15) . . ? C15 C16 H16A 111.0 . . ? C17 C16 H16A 111.0 . . ? C15 C16 H16B 111.0 . . ? C17 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? C13 C17 C16 108.2(16) . . ? C13 C17 H17A 110.1 . . ? C16 C17 H17A 110.1 . . ? C13 C17 H17B 110.1 . . ? C16 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O9 Dy1 92.7(15) . 3_656 ? C21 O10 Dy1 100.9(17) . 3_656 ? C22 O11 Dy1 92.4(14) . . ? C22 O12 Dy1 98(2) . . ? O10 C21 O9 114(2) . . ? O10 C21 C25 121(3) . . ? O9 C21 C25 122(2) . . ? O10 C21 Dy1 55.4(14) . 3_656 ? O9 C21 Dy1 61.5(13) . 3_656 ? C25 C21 Dy1 175.7(18) . 3_656 ? O12 C22 O11 120(3) . . ? O12 C22 C23 123(3) . . ? O11 C22 C23 115(2) . . ? O12 C22 Dy1 59.9(18) . . ? O11 C22 Dy1 60.7(13) . . ? C23 C22 Dy1 155.4(18) . . ? C22 C23 C24 115(2) . . ? C22 C23 C27 117(2) . . ? C24 C23 C27 101.9(17) . . ? C22 C23 H23A 107.5 . . ? C24 C23 H23A 107.5 . . ? C27 C23 H23A 107.5 . . ? C30 C24 C29 106.5(19) . . ? C30 C24 C25 114.0(18) . . ? C29 C24 C25 116.8(17) . . ? C30 C24 C23 111.6(16) . . ? C29 C24 C23 109.1(17) . . ? C25 C24 C23 98.7(18) . . ? C26 C25 C28 116(2) . . ? C26 C25 C24 106.3(18) . . ? C28 C25 C24 110.1(19) . . ? C26 C25 C21 108.3(19) . . ? C28 C25 C21 101.4(18) . . ? C24 C25 C21 115.1(19) . . ? C27 C26 C25 105.9(17) . . ? C27 C26 H26A 110.5 . . ? C25 C26 H26A 110.5 . . ? C27 C26 H26B 110.5 . . ? C25 C26 H26B 110.5 . . ? H26A C26 H26B 108.7 . . ? C26 C27 C23 108.3(18) . . ? C26 C27 H27A 110.0 . . ? C23 C27 H27A 110.0 . . ? C26 C27 H27B 110.0 . . ? C23 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C24 C30 H30A 109.5 . . ? C24 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C24 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 N1 C35 119.6(17) . . ? C31 N1 Mn1 124.1(15) . . ? C35 N1 Mn1 116.2(14) . . ? C40 N2 C36 129(3) . . ? C40 N2 Mn1 119.6(17) . . ? C36 N2 Mn1 108.7(18) . . ? N1 C31 C32 123(2) . . ? N1 C31 H31A 118.5 . . ? C32 C31 H31A 118.5 . . ? C31 C32 C33 116(2) . . ? C31 C32 H32A 122.0 . . ? C33 C32 H32A 122.0 . . ? C32 C33 C34 124.9(19) . . ? C32 C33 H33A 117.6 . . ? C34 C33 H33A 117.6 . . ? C33 C34 C35 114.9(19) . . ? C33 C34 H34A 122.5 . . ? C35 C34 H34A 122.5 . . ? N1 C35 C36 114(2) . . ? N1 C35 C34 122(2) . . ? C36 C35 C34 124(3) . . ? C35 C36 N2 125(3) . . ? C35 C36 C37 127(3) . . ? N2 C36 C37 109(2) . . ? C38 C37 C36 121(3) . . ? C38 C37 H37A 119.4 . . ? C36 C37 H37A 119.4 . . ? C39 C38 C37 121(4) . . ? C39 C38 H38A 119.4 . . ? C37 C38 H38A 119.4 . . ? C38 C39 C40 124(4) . . ? C38 C39 H39A 117.9 . . ? C40 C39 H39A 117.9 . . ? N2 C40 C39 114(3) . . ? N2 C40 H40A 123.0 . . ? C39 C40 H40A 123.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.095 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.135 data_ddb3 _database_code_depnum_ccdc_archive 'CCDC 907544' #TrackingRef '3 Mn+Eu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H51 Eu Mn N2 O12' _chemical_formula_weight 958.73 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.6092(13) _cell_length_b 13.0311(12) _cell_length_c 24.203(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3976.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 377 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 13.11 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 1.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8001 _exptl_absorpt_correction_T_max 0.8599 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20347 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7010 _reflns_number_gt 5926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(16) _refine_ls_number_reflns 7010 _refine_ls_number_parameters 505 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.062 _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 Eu1 Eu 0.74251(2) 0.89551(2) 0.150387(13) 0.02878(10) Uani 1 1 d . . . Mn1 Mn 0.62473(9) 1.01855(8) 0.02453(5) 0.0352(3) Uani 1 1 d . . . O1 O 1.0900(4) 0.6352(4) -0.0073(2) 0.0485(14) Uani 1 1 d . . . O2 O 1.1161(4) 0.6824(4) -0.0929(2) 0.0490(14) Uani 1 1 d . . . O3 O 0.7744(5) 1.0179(4) -0.0196(2) 0.0546(15) Uani 1 1 d . . . O4 O 0.7943(4) 0.9501(4) 0.0620(2) 0.0369(12) Uani 1 1 d . . . C1 C 1.0941(5) 0.7024(6) -0.0437(3) 0.0379(18) Uani 1 1 d . . . C2 C 0.8313(6) 0.9730(6) 0.0145(3) 0.0346(17) Uani 1 1 d . . . C3 C 1.0697(6) 0.8158(5) -0.0286(3) 0.0360(17) Uani 1 1 d . . . C4 C 0.9504(6) 0.8423(5) -0.0343(3) 0.0357(17) Uani 1 1 d . . . C5 C 0.9429(6) 0.9432(6) -0.0002(3) 0.0378(18) Uani 1 1 d . . . H5A H 0.9714 0.9981 -0.0236 0.045 Uiso 1 1 calc R . . C6 C 1.0190(6) 0.9303(7) 0.0478(4) 0.054(2) Uani 1 1 d . . . H6A H 0.9803 0.9186 0.0818 0.065 Uiso 1 1 calc R . . H6B H 1.0623 0.9913 0.0521 0.065 Uiso 1 1 calc R . . C7 C 1.0887(7) 0.8370(6) 0.0338(3) 0.047(2) Uani 1 1 d . . . H7A H 1.0682 0.7781 0.0559 0.057 Uiso 1 1 calc R . . H7B H 1.1629 0.8521 0.0408 0.057 Uiso 1 1 calc R . . C8 C 1.1435(6) 0.8849(6) -0.0626(4) 0.053(2) Uani 1 1 d . . . H8A H 1.1333 0.8712 -0.1013 0.080 Uiso 1 1 calc R . . H8B H 1.2158 0.8711 -0.0528 0.080 Uiso 1 1 calc R . . H8C H 1.1274 0.9555 -0.0552 0.080 Uiso 1 1 calc R . . C9 C 0.8775(6) 0.7606(6) -0.0095(3) 0.047(2) Uani 1 1 d . . . H9A H 0.8968 0.7489 0.0283 0.070 Uiso 1 1 calc R . . H9B H 0.8847 0.6979 -0.0300 0.070 Uiso 1 1 calc R . . H9C H 0.8053 0.7838 -0.0113 0.070 Uiso 1 1 calc R . . C10 C 0.9165(8) 0.8581(7) -0.0954(3) 0.061(3) Uani 1 1 d . . . H10A H 0.8424 0.8748 -0.0969 0.092 Uiso 1 1 calc R . . H10B H 0.9292 0.7962 -0.1158 0.092 Uiso 1 1 calc R . . H10C H 0.9569 0.9132 -0.1112 0.092 Uiso 1 1 calc R . . O5 O 0.8822(6) 0.7683(5) 0.1372(3) 0.085(2) Uani 1 1 d . . . O6 O 0.7710(6) 0.7368(5) 0.1982(3) 0.089(2) Uani 1 1 d U . . O7 O 1.1040(5) 0.5046(5) 0.3246(3) 0.072(2) Uani 1 1 d . . . O8 O 1.2014(5) 0.4582(7) 0.2574(3) 0.090(3) Uani 1 1 d . . . C11 C 0.8499(8) 0.7114(7) 0.1731(4) 0.064(2) Uani 1 1 d U . . C12 C 1.1143(7) 0.4909(6) 0.2749(3) 0.046(2) Uani 1 1 d . . . C13 C 0.8992(6) 0.6057(6) 0.1834(3) 0.0454(19) Uani 1 1 d . . . C14 C 1.0149(6) 0.6119(6) 0.2060(3) 0.0396(17) Uani 1 1 d . . . C15 C 1.0249(6) 0.5040(6) 0.2346(4) 0.048(2) Uani 1 1 d . . . H15A H 1.0354 0.4533 0.2052 0.058 Uiso 1 1 calc R . . C16 C 0.9180(8) 0.4837(10) 0.2595(5) 0.094(4) Uani 1 1 d U . . H16A H 0.9180 0.5017 0.2984 0.113 Uiso 1 1 calc R . . H16B H 0.8999 0.4116 0.2560 0.113 Uiso 1 1 calc R . . C17 C 0.8390(8) 0.5492(8) 0.2283(5) 0.087(4) Uani 1 1 d . . . H17A H 0.8055 0.5978 0.2531 0.104 Uiso 1 1 calc R . . H17B H 0.7843 0.5064 0.2120 0.104 Uiso 1 1 calc R . . C18 C 0.8905(9) 0.5471(8) 0.1293(5) 0.093(4) Uani 1 1 d . . . H18A H 0.8180 0.5465 0.1173 0.140 Uiso 1 1 calc R . . H18B H 0.9145 0.4779 0.1347 0.140 Uiso 1 1 calc R . . H18C H 0.9336 0.5799 0.1018 0.140 Uiso 1 1 calc R . . C19 C 1.0272(9) 0.6985(7) 0.2468(4) 0.071(3) Uani 1 1 d . . . H19A H 1.0216 0.7629 0.2278 0.106 Uiso 1 1 calc R . . H19B H 1.0953 0.6938 0.2644 0.106 Uiso 1 1 calc R . . H19C H 0.9724 0.6939 0.2743 0.106 Uiso 1 1 calc R . . C20 C 1.0997(8) 0.6270(8) 0.1620(4) 0.079(3) Uani 1 1 d . . . H20A H 1.0921 0.6938 0.1458 0.118 Uiso 1 1 calc R . . H20B H 1.0919 0.5756 0.1339 0.118 Uiso 1 1 calc R . . H20C H 1.1686 0.6211 0.1786 0.118 Uiso 1 1 calc R . . O9 O 0.6285(5) 0.9198(5) 0.2975(2) 0.0684(19) Uani 1 1 d . . . O10 O 0.5909(4) 0.8706(4) 0.2123(2) 0.0430(13) Uani 1 1 d . . . O11 O 0.3481(4) 0.6572(4) 0.4274(2) 0.0425(13) Uani 1 1 d . . . O12 O 0.3560(4) 0.5468(4) 0.3591(2) 0.0506(15) Uani 1 1 d . . . C21 C 0.5632(6) 0.8807(6) 0.2605(3) 0.0417(19) Uani 1 1 d . . . C22 C 0.3534(5) 0.6373(6) 0.3772(3) 0.0342(18) Uani 1 1 d . . . C23 C 0.4571(7) 0.8461(6) 0.2805(3) 0.043(2) Uani 1 1 d . . . C24 C 0.4608(7) 0.7333(7) 0.3024(4) 0.061(3) Uani 1 1 d . . . C25 C 0.3552(6) 0.7271(5) 0.3357(3) 0.0375(18) Uani 1 1 d . . . H25A H 0.2985 0.7144 0.3089 0.045 Uiso 1 1 calc R . . C26 C 0.3342(8) 0.8310(6) 0.3608(4) 0.074(3) Uani 1 1 d . . . H26A H 0.3473 0.8305 0.4003 0.089 Uiso 1 1 calc R . . H26B H 0.2618 0.8528 0.3541 0.089 Uiso 1 1 calc R . . C27 C 0.4159(7) 0.9026(7) 0.3298(4) 0.062(2) Uani 1 1 d . . . H27A H 0.3812 0.9655 0.3182 0.074 Uiso 1 1 calc R . . H27B H 0.4739 0.9204 0.3543 0.074 Uiso 1 1 calc R . . C28 C 0.3752(8) 0.8569(9) 0.2337(4) 0.076(3) Uani 1 1 d . . . H28A H 0.3737 0.9267 0.2212 0.114 Uiso 1 1 calc R . . H28B H 0.3063 0.8379 0.2472 0.114 Uiso 1 1 calc R . . H28C H 0.3946 0.8127 0.2036 0.114 Uiso 1 1 calc R . . C29 C 0.4588(10) 0.6537(9) 0.2532(5) 0.092(4) Uani 1 1 d U . . H29A H 0.5238 0.6584 0.2327 0.139 Uiso 1 1 calc R . . H29B H 0.4001 0.6688 0.2293 0.139 Uiso 1 1 calc R . . H29C H 0.4512 0.5855 0.2677 0.139 Uiso 1 1 calc R . . C30 C 0.5558(7) 0.7129(8) 0.3367(5) 0.092(4) Uani 1 1 d . . . H30A H 0.6182 0.7169 0.3140 0.138 Uiso 1 1 calc R . . H30B H 0.5507 0.6456 0.3526 0.138 Uiso 1 1 calc R . . H30C H 0.5602 0.7630 0.3657 0.138 Uiso 1 1 calc R . . N1 N 0.4508(6) 1.0398(6) 0.0443(4) 0.061(2) Uani 1 1 d . . . N2 N 0.5559(7) 1.1203(6) -0.0417(4) 0.069(2) Uani 1 1 d . . . C31 C 0.4009(8) 0.9909(8) 0.0835(5) 0.080(4) Uani 1 1 d . . . H31A H 0.4392 0.9415 0.1027 0.096 Uiso 1 1 calc R . . C32 C 0.2949(10) 1.0059(10) 0.0993(5) 0.100(4) Uani 1 1 d U . . H32A H 0.2602 0.9699 0.1271 0.120 Uiso 1 1 calc R . . C33 C 0.2500(12) 1.0821(11) 0.0673(6) 0.113(4) Uani 1 1 d U . . H33A H 0.1801 1.0989 0.0756 0.135 Uiso 1 1 calc R . . C34 C 0.2945(10) 1.1355(10) 0.0255(6) 0.100(4) Uani 1 1 d U . . H34A H 0.2574 1.1844 0.0052 0.120 Uiso 1 1 calc R . . C35 C 0.4004(7) 1.1115(9) 0.0151(5) 0.082(4) Uani 1 1 d . . . C36 C 0.4609(10) 1.1591(8) -0.0295(5) 0.078(3) Uani 1 1 d U . . C37 C 0.4230(11) 1.2471(9) -0.0637(5) 0.094(4) Uani 1 1 d U . . H37A H 0.3583 1.2792 -0.0573 0.113 Uiso 1 1 calc R . . C38 C 0.4866(14) 1.2761(11) -0.1033(6) 0.113(5) Uani 1 1 d U . . H38A H 0.4655 1.3334 -0.1234 0.136 Uiso 1 1 calc R . . C39 C 0.5763(13) 1.2343(10) -0.1180(5) 0.107(4) Uani 1 1 d U . . H39A H 0.6133 1.2553 -0.1492 0.129 Uiso 1 1 calc R . . C40 C 0.6128(12) 1.1564(8) -0.0839(5) 0.087(4) Uani 1 1 d . . . H40A H 0.6793 1.1283 -0.0908 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02785(16) 0.02798(16) 0.03051(17) -0.00005(15) -0.00169(17) 0.00014(16) Mn1 0.0350(6) 0.0288(6) 0.0419(7) -0.0029(5) -0.0048(5) 0.0055(5) O1 0.054(3) 0.029(3) 0.062(4) 0.001(3) 0.019(3) 0.000(2) O2 0.041(3) 0.056(3) 0.050(3) -0.020(3) -0.005(3) 0.019(3) O3 0.057(4) 0.056(3) 0.050(3) 0.016(3) 0.014(3) 0.020(3) O4 0.031(3) 0.040(3) 0.040(3) -0.003(2) 0.008(2) 0.001(2) C1 0.020(4) 0.045(5) 0.048(5) -0.014(4) 0.004(3) -0.002(3) C2 0.030(4) 0.030(4) 0.043(5) -0.007(4) 0.013(3) -0.005(3) C3 0.040(4) 0.029(4) 0.039(4) -0.001(3) 0.015(3) 0.000(3) C4 0.043(4) 0.027(4) 0.037(4) -0.006(3) 0.001(3) 0.004(3) C5 0.035(4) 0.035(4) 0.043(5) 0.005(3) 0.012(3) -0.005(3) C6 0.028(4) 0.069(6) 0.065(6) -0.031(5) 0.004(4) 0.002(4) C7 0.043(5) 0.055(5) 0.044(5) -0.012(4) -0.005(4) -0.002(4) C8 0.042(4) 0.041(5) 0.077(6) 0.006(5) 0.026(4) -0.003(4) C9 0.040(4) 0.043(4) 0.057(5) -0.015(4) 0.019(4) -0.014(4) C10 0.070(6) 0.077(7) 0.036(5) 0.001(4) 0.001(4) 0.026(5) O5 0.080(5) 0.076(5) 0.099(6) 0.039(4) 0.033(4) 0.049(4) O6 0.087(5) 0.079(4) 0.102(4) 0.045(3) 0.032(4) 0.042(4) O7 0.083(5) 0.087(5) 0.045(4) 0.009(3) -0.004(3) 0.051(4) O8 0.062(4) 0.158(7) 0.051(4) 0.015(4) -0.002(3) 0.054(5) C11 0.062(5) 0.057(4) 0.073(5) 0.028(4) 0.022(4) 0.030(4) C12 0.049(5) 0.044(5) 0.045(5) 0.016(4) -0.004(4) 0.014(4) C13 0.042(4) 0.040(4) 0.054(5) 0.004(4) -0.017(4) 0.009(4) C14 0.037(4) 0.040(4) 0.042(4) 0.008(4) -0.009(3) 0.008(4) C15 0.041(5) 0.039(5) 0.064(6) -0.001(4) -0.009(4) 0.008(4) C16 0.057(6) 0.104(7) 0.123(7) 0.053(6) -0.010(6) 0.004(5) C17 0.054(6) 0.075(7) 0.130(10) 0.057(7) -0.018(6) -0.003(5) C18 0.104(9) 0.070(7) 0.106(9) -0.025(7) -0.059(7) 0.037(7) C19 0.086(8) 0.049(6) 0.078(7) -0.008(5) -0.045(6) -0.001(5) C20 0.067(6) 0.102(8) 0.068(7) 0.028(6) 0.009(5) 0.017(6) O9 0.080(4) 0.086(5) 0.039(3) -0.001(3) 0.003(3) -0.034(4) O10 0.046(3) 0.049(3) 0.035(3) -0.001(2) 0.011(2) -0.006(3) O11 0.046(3) 0.045(3) 0.037(3) 0.013(2) 0.000(2) -0.002(2) O12 0.052(3) 0.028(3) 0.072(4) 0.000(3) 0.025(3) -0.008(2) C21 0.054(5) 0.035(5) 0.036(4) 0.001(4) 0.001(4) 0.003(4) C22 0.016(3) 0.037(4) 0.050(5) 0.013(4) 0.002(3) -0.007(3) C23 0.056(5) 0.035(4) 0.039(5) 0.005(4) 0.019(4) 0.005(4) C24 0.054(6) 0.051(5) 0.076(7) 0.027(5) 0.036(5) 0.009(4) C25 0.027(4) 0.036(4) 0.049(5) 0.011(3) 0.012(3) 0.006(3) C26 0.091(7) 0.045(5) 0.088(8) 0.015(5) 0.053(6) 0.011(5) C27 0.064(5) 0.047(5) 0.073(6) -0.011(5) 0.018(5) 0.008(5) C28 0.057(6) 0.097(8) 0.075(7) 0.002(6) 0.009(5) -0.009(6) C29 0.113(8) 0.068(6) 0.096(7) -0.007(6) 0.036(6) -0.009(6) C30 0.036(5) 0.095(8) 0.144(11) 0.068(8) 0.000(6) 0.004(5) N1 0.033(4) 0.057(5) 0.092(6) -0.036(5) -0.007(4) 0.004(4) N2 0.086(6) 0.047(5) 0.072(6) -0.013(4) -0.047(5) 0.019(4) C31 0.047(6) 0.078(7) 0.116(9) -0.067(7) 0.024(6) -0.024(5) C32 0.090(7) 0.095(7) 0.115(8) -0.038(6) 0.008(6) -0.033(6) C33 0.077(6) 0.120(8) 0.142(8) -0.057(7) -0.009(7) -0.010(7) C34 0.089(7) 0.087(7) 0.125(8) -0.034(6) -0.037(6) 0.031(6) C35 0.045(5) 0.074(7) 0.127(10) -0.065(8) -0.040(6) 0.021(6) C36 0.082(6) 0.059(5) 0.092(7) -0.024(5) -0.049(6) 0.012(5) C37 0.093(7) 0.084(7) 0.104(7) -0.032(6) -0.051(6) 0.030(6) C38 0.137(9) 0.092(8) 0.111(8) -0.007(7) -0.036(7) 0.006(7) C39 0.136(9) 0.104(8) 0.081(7) 0.002(6) -0.033(7) -0.013(7) C40 0.134(11) 0.054(6) 0.072(8) 0.004(6) -0.054(8) 0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O12 2.341(5) 3_655 ? Eu1 O2 2.346(5) 4_465 ? Eu1 O4 2.347(5) . ? Eu1 O6 2.396(6) . ? Eu1 O5 2.439(6) . ? Eu1 O10 2.450(5) . ? Eu1 O7 2.476(6) 3_755 ? Eu1 O8 2.479(6) 3_755 ? Eu1 C11 2.809(8) . ? Eu1 C12 2.842(8) 3_755 ? Eu1 Mn1 3.7491(12) . ? Mn1 O1 2.093(5) 4_465 ? Mn1 O3 2.170(5) . ? Mn1 O11 2.176(5) 3_655 ? Mn1 N2 2.253(8) . ? Mn1 N1 2.262(7) . ? Mn1 O4 2.488(5) . ? O1 C1 1.244(9) . ? O1 Mn1 2.093(5) 4_565 ? O2 C1 1.251(9) . ? O2 Eu1 2.346(5) 4_565 ? O3 C2 1.240(9) . ? O4 C2 1.275(8) . ? C1 C3 1.554(10) . ? C2 C5 1.504(10) . ? C3 C8 1.534(10) . ? C3 C4 1.550(10) . ? C3 C7 1.554(10) . ? C4 C9 1.528(10) . ? C4 C10 1.553(10) . ? C4 C5 1.555(10) . ? C5 C6 1.515(11) . ? C5 H5A 0.9800 . ? C6 C7 1.538(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? O5 C11 1.213(10) . ? O6 C11 1.211(10) . ? O7 C12 1.221(9) . ? O7 Eu1 2.476(6) 3_745 ? O8 C12 1.253(10) . ? O8 Eu1 2.479(6) 3_745 ? C11 C13 1.532(11) . ? C12 C15 1.501(11) . ? C12 Eu1 2.842(7) 3_745 ? C13 C17 1.516(13) . ? C13 C18 1.518(12) . ? C13 C14 1.561(10) . ? C14 C19 1.507(12) . ? C14 C20 1.521(11) . ? C14 C15 1.572(11) . ? C15 C16 1.500(13) . ? C15 H15A 0.9800 . ? C16 C17 1.514(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O9 C21 1.319(9) . ? O10 C21 1.227(8) . ? O11 C22 1.246(9) . ? O11 Mn1 2.176(5) 3_645 ? O12 C22 1.258(9) . ? O12 Eu1 2.341(5) 3_645 ? C21 C23 1.492(11) . ? C22 C25 1.542(9) . ? C23 C27 1.494(11) . ? C23 C28 1.539(12) . ? C23 C24 1.562(11) . ? C24 C30 1.481(13) . ? C24 C25 1.558(10) . ? C24 C29 1.580(15) . ? C25 C26 1.506(11) . ? C25 H25A 0.9800 . ? C26 C27 1.579(12) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1 C31 1.304(13) . ? N1 C35 1.333(13) . ? N2 C36 1.333(14) . ? N2 C40 1.336(14) . ? C31 C32 1.404(15) . ? C31 H31A 0.9300 . ? C32 C33 1.381(17) . ? C32 H32A 0.9300 . ? C33 C34 1.349(17) . ? C33 H33A 0.9300 . ? C34 C35 1.395(15) . ? C34 H34A 0.9300 . ? C35 C36 1.459(17) . ? C36 C37 1.493(15) . ? C37 C38 1.306(18) . ? C37 H37A 0.9300 . ? C38 C39 1.304(19) . ? C38 H38A 0.9300 . ? C39 C40 1.385(15) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Eu1 O2 86.9(2) 3_655 4_465 ? O12 Eu1 O4 78.64(18) 3_655 . ? O2 Eu1 O4 77.28(17) 4_465 . ? O12 Eu1 O6 148.6(2) 3_655 . ? O2 Eu1 O6 90.8(3) 4_465 . ? O4 Eu1 O6 131.3(2) . . ? O12 Eu1 O5 160.4(2) 3_655 . ? O2 Eu1 O5 96.8(2) 4_465 . ? O4 Eu1 O5 83.44(19) . . ? O6 Eu1 O5 50.9(2) . . ? O12 Eu1 O10 75.97(18) 3_655 . ? O2 Eu1 O10 77.00(17) 4_465 . ? O4 Eu1 O10 144.51(17) . . ? O6 Eu1 O10 73.0(2) . . ? O5 Eu1 O10 123.6(2) . . ? O12 Eu1 O7 87.4(2) 3_655 3_755 ? O2 Eu1 O7 157.6(2) 4_465 3_755 ? O4 Eu1 O7 80.33(19) . 3_755 ? O6 Eu1 O7 105.1(3) . 3_755 ? O5 Eu1 O7 81.8(3) . 3_755 ? O10 Eu1 O7 122.4(2) . 3_755 ? O12 Eu1 O8 87.8(3) 3_655 3_755 ? O2 Eu1 O8 150.44(19) 4_465 3_755 ? O4 Eu1 O8 129.89(19) . 3_755 ? O6 Eu1 O8 78.9(3) . 3_755 ? O5 Eu1 O8 97.8(3) . 3_755 ? O10 Eu1 O8 73.50(19) . 3_755 ? O7 Eu1 O8 50.8(2) 3_755 3_755 ? O12 Eu1 C11 173.7(2) 3_655 . ? O2 Eu1 C11 94.2(3) 4_465 . ? O4 Eu1 C11 107.7(2) . . ? O6 Eu1 C11 25.4(2) . . ? O5 Eu1 C11 25.5(2) . . ? O10 Eu1 C11 98.2(2) . . ? O7 Eu1 C11 93.8(3) 3_755 . ? O8 Eu1 C11 88.1(3) 3_755 . ? O12 Eu1 C12 91.8(2) 3_655 3_755 ? O2 Eu1 C12 176.5(2) 4_465 3_755 ? O4 Eu1 C12 105.7(2) . 3_755 ? O6 Eu1 C12 88.6(3) . 3_755 ? O5 Eu1 C12 85.5(3) . 3_755 ? O10 Eu1 C12 99.5(2) . 3_755 ? O7 Eu1 C12 25.4(2) 3_755 3_755 ? O8 Eu1 C12 26.1(2) 3_755 3_755 ? C11 Eu1 C12 86.7(3) . 3_755 ? O12 Eu1 Mn1 49.47(15) 3_655 . ? O2 Eu1 Mn1 55.57(14) 4_465 . ? O4 Eu1 Mn1 40.53(11) . . ? O6 Eu1 Mn1 145.2(2) . . ? O5 Eu1 Mn1 118.05(17) . . ? O10 Eu1 Mn1 104.14(13) . . ? O7 Eu1 Mn1 105.25(16) 3_755 . ? O8 Eu1 Mn1 134.7(2) 3_755 . ? C11 Eu1 Mn1 135.7(2) . . ? C12 Eu1 Mn1 125.55(17) 3_755 . ? O1 Mn1 O3 94.6(2) 4_465 . ? O1 Mn1 O11 159.2(2) 4_465 3_655 ? O3 Mn1 O11 97.4(2) . 3_655 ? O1 Mn1 N2 109.9(2) 4_465 . ? O3 Mn1 N2 89.3(3) . . ? O11 Mn1 N2 87.2(2) 3_655 . ? O1 Mn1 N1 87.5(2) 4_465 . ? O3 Mn1 N1 161.6(3) . . ? O11 Mn1 N1 86.4(2) 3_655 . ? N2 Mn1 N1 72.8(4) . . ? O1 Mn1 O4 84.81(19) 4_465 . ? O3 Mn1 O4 55.28(18) . . ? O11 Mn1 O4 88.14(18) 3_655 . ? N2 Mn1 O4 143.3(3) . . ? N1 Mn1 O4 143.1(3) . . ? O1 Mn1 Eu1 80.55(15) 4_465 . ? O3 Mn1 Eu1 93.09(15) . . ? O11 Mn1 Eu1 81.86(14) 3_655 . ? N2 Mn1 Eu1 169.07(19) . . ? N1 Mn1 Eu1 105.3(2) . . ? O4 Mn1 Eu1 37.81(11) . . ? C1 O1 Mn1 121.6(5) . 4_565 ? C1 O2 Eu1 143.7(5) . 4_565 ? C2 O3 Mn1 100.1(4) . . ? C2 O4 Eu1 173.6(5) . . ? C2 O4 Mn1 84.4(4) . . ? Eu1 O4 Mn1 101.66(17) . . ? O1 C1 O2 122.6(7) . . ? O1 C1 C3 119.7(7) . . ? O2 C1 C3 117.8(7) . . ? O3 C2 O4 120.0(7) . . ? O3 C2 C5 120.3(7) . . ? O4 C2 C5 119.7(7) . . ? C8 C3 C4 114.2(6) . . ? C8 C3 C1 108.2(6) . . ? C4 C3 C1 112.5(6) . . ? C8 C3 C7 109.0(7) . . ? C4 C3 C7 101.3(5) . . ? C1 C3 C7 111.6(6) . . ? C9 C4 C3 113.2(6) . . ? C9 C4 C10 107.5(7) . . ? C3 C4 C10 112.4(6) . . ? C9 C4 C5 110.1(6) . . ? C3 C4 C5 101.5(6) . . ? C10 C4 C5 112.1(6) . . ? C2 C5 C6 116.1(6) . . ? C2 C5 C4 113.7(6) . . ? C6 C5 C4 105.9(6) . . ? C2 C5 H5A 106.9 . . ? C6 C5 H5A 106.9 . . ? C4 C5 H5A 106.9 . . ? C5 C6 C7 106.3(6) . . ? C5 C6 H6A 110.5 . . ? C7 C6 H6A 110.5 . . ? C5 C6 H6B 110.5 . . ? C7 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C6 C7 C3 105.4(6) . . ? C6 C7 H7A 110.7 . . ? C3 C7 H7A 110.7 . . ? C6 C7 H7B 110.7 . . ? C3 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 O5 Eu1 94.5(5) . . ? C11 O6 Eu1 96.7(6) . . ? C12 O7 Eu1 94.3(5) . 3_745 ? C12 O8 Eu1 93.3(5) . 3_745 ? O6 C11 O5 117.9(8) . . ? O6 C11 C13 119.9(8) . . ? O5 C11 C13 122.0(8) . . ? O6 C11 Eu1 57.9(5) . . ? O5 C11 Eu1 60.0(4) . . ? C13 C11 Eu1 174.6(7) . . ? O7 C12 O8 118.3(8) . . ? O7 C12 C15 123.0(8) . . ? O8 C12 C15 118.5(8) . . ? O7 C12 Eu1 60.3(4) . 3_745 ? O8 C12 Eu1 60.6(4) . 3_745 ? C15 C12 Eu1 160.2(6) . 3_745 ? C17 C13 C18 109.7(9) . . ? C17 C13 C11 110.5(7) . . ? C18 C13 C11 106.4(7) . . ? C17 C13 C14 104.0(6) . . ? C18 C13 C14 113.3(7) . . ? C11 C13 C14 113.0(7) . . ? C19 C14 C20 106.9(8) . . ? C19 C14 C13 111.4(7) . . ? C20 C14 C13 114.7(7) . . ? C19 C14 C15 111.9(7) . . ? C20 C14 C15 111.5(7) . . ? C13 C14 C15 100.5(6) . . ? C16 C15 C12 113.1(8) . . ? C16 C15 C14 105.2(7) . . ? C12 C15 C14 116.6(7) . . ? C16 C15 H15A 107.1 . . ? C12 C15 H15A 107.1 . . ? C14 C15 H15A 107.1 . . ? C15 C16 C17 106.9(8) . . ? C15 C16 H16A 110.3 . . ? C17 C16 H16A 110.3 . . ? C15 C16 H16B 110.3 . . ? C17 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C16 C17 C13 107.6(8) . . ? C16 C17 H17A 110.2 . . ? C13 C17 H17A 110.2 . . ? C16 C17 H17B 110.2 . . ? C13 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O10 Eu1 142.2(5) . . ? C22 O11 Mn1 109.9(5) . 3_645 ? C22 O12 Eu1 144.0(5) . 3_645 ? O10 C21 O9 120.6(7) . . ? O10 C21 C23 122.1(7) . . ? O9 C21 C23 117.2(7) . . ? O11 C22 O12 122.4(7) . . ? O11 C22 C25 118.5(7) . . ? O12 C22 C25 119.0(7) . . ? C21 C23 C27 114.9(7) . . ? C21 C23 C28 109.5(7) . . ? C27 C23 C28 108.0(8) . . ? C21 C23 C24 111.5(7) . . ? C27 C23 C24 101.7(7) . . ? C28 C23 C24 110.9(8) . . ? C30 C24 C25 113.1(8) . . ? C30 C24 C23 112.6(8) . . ? C25 C24 C23 101.4(6) . . ? C30 C24 C29 108.5(9) . . ? C25 C24 C29 109.9(8) . . ? C23 C24 C29 111.2(8) . . ? C26 C25 C22 114.7(7) . . ? C26 C25 C24 108.2(7) . . ? C22 C25 C24 112.8(6) . . ? C26 C25 H25A 106.9 . . ? C22 C25 H25A 106.9 . . ? C24 C25 H25A 106.9 . . ? C25 C26 C27 103.0(6) . . ? C25 C26 H26A 111.2 . . ? C27 C26 H26A 111.2 . . ? C25 C26 H26B 111.2 . . ? C27 C26 H26B 111.2 . . ? H26A C26 H26B 109.1 . . ? C23 C27 C26 108.3(7) . . ? C23 C27 H27A 110.0 . . ? C26 C27 H27A 110.0 . . ? C23 C27 H27B 110.0 . . ? C26 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C24 C30 H30A 109.5 . . ? C24 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C24 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 N1 C35 119.9(9) . . ? C31 N1 Mn1 124.2(7) . . ? C35 N1 Mn1 115.8(7) . . ? C36 N2 C40 121.2(10) . . ? C36 N2 Mn1 114.4(8) . . ? C40 N2 Mn1 123.0(8) . . ? N1 C31 C32 126.1(13) . . ? N1 C31 H31A 116.9 . . ? C32 C31 H31A 116.9 . . ? C33 C32 C31 109.7(13) . . ? C33 C32 H32A 125.1 . . ? C31 C32 H32A 125.1 . . ? C34 C33 C32 128.4(14) . . ? C34 C33 H33A 115.8 . . ? C32 C33 H33A 115.8 . . ? C33 C34 C35 114.7(13) . . ? C33 C34 H34A 122.7 . . ? C35 C34 H34A 122.7 . . ? N1 C35 C34 121.2(14) . . ? N1 C35 C36 116.2(9) . . ? C34 C35 C36 122.6(13) . . ? N2 C36 C35 118.1(10) . . ? N2 C36 C37 117.1(12) . . ? C35 C36 C37 124.7(12) . . ? C38 C37 C36 115.6(13) . . ? C38 C37 H37A 122.2 . . ? C36 C37 H37A 122.2 . . ? C39 C38 C37 127.7(16) . . ? C39 C38 H38A 116.2 . . ? C37 C38 H38A 116.2 . . ? C38 C39 C40 115.6(15) . . ? C38 C39 H39A 122.2 . . ? C40 C39 H39A 122.2 . . ? N2 C40 C39 122.4(14) . . ? N2 C40 H40A 118.8 . . ? C39 C40 H40A 118.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.690 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.094 data_ddb4 _database_code_depnum_ccdc_archive 'CCDC 907545' #TrackingRef '4 Mn+La.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H51 La Mn N2 O12' _chemical_formula_weight 945.68 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.6554(15) _cell_length_b 13.1165(16) _cell_length_c 24.358(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4043.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 215 _cell_measurement_theta_min 2024 _cell_measurement_theta_max 12.71 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1932 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8261 _exptl_absorpt_correction_T_max 0.8482 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20762 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7097 _reflns_number_gt 6052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 7097 _refine_ls_number_parameters 505 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.23924(3) 1.10270(3) 0.350359(14) 0.02775(11) Uani 1 1 d . . . Mn1 Mn 0.12009(8) 0.98157(8) 0.47796(4) 0.0317(3) Uani 1 1 d . . . O1 O 0.5838(4) 1.3646(4) 0.5036(2) 0.0398(12) Uani 1 1 d . . . O2 O 0.6051(4) 1.3224(4) 0.59062(19) 0.0412(12) Uani 1 1 d . . . O3 O 0.2687(4) 0.9836(4) 0.52457(19) 0.0518(13) Uani 1 1 d . . . O4 O 0.2897(3) 1.0462(4) 0.44220(18) 0.0373(12) Uani 1 1 d . . . C1 C 0.5857(5) 1.3000(5) 0.5413(3) 0.0307(16) Uani 1 1 d . . . C2 C 0.3258(5) 1.0254(5) 0.4896(3) 0.0307(15) Uani 1 1 d . . . C3 C 0.5654(5) 1.1865(5) 0.5275(3) 0.0323(15) Uani 1 1 d . . . C4 C 0.4446(5) 1.1594(5) 0.5362(2) 0.0267(15) Uani 1 1 d . . . C5 C 0.4392(5) 1.0556(5) 0.5038(3) 0.0345(16) Uani 1 1 d . . . H5A H 0.4675 1.0026 0.5281 0.041 Uiso 1 1 calc R . . C6 C 0.5137(6) 1.0659(6) 0.4568(3) 0.049(2) Uani 1 1 d . . . H6A H 0.4748 1.0725 0.4227 0.059 Uiso 1 1 calc R . . H6B H 0.5586 1.0061 0.4543 0.059 Uiso 1 1 calc R . . C7 C 0.5815(6) 1.1619(6) 0.4667(3) 0.0403(18) Uani 1 1 d . . . H7A H 0.6553 1.1484 0.4589 0.048 Uiso 1 1 calc R . . H7B H 0.5578 1.2179 0.4438 0.048 Uiso 1 1 calc R . . C8 C 0.6383(6) 1.1207(6) 0.5632(3) 0.049(2) Uani 1 1 d . . . H8A H 0.7105 1.1391 0.5564 0.074 Uiso 1 1 calc R . . H8B H 0.6279 1.0501 0.5544 0.074 Uiso 1 1 calc R . . H8C H 0.6219 1.1318 0.6013 0.074 Uiso 1 1 calc R . . C9 C 0.3727(5) 1.2384(5) 0.5110(3) 0.0384(17) Uani 1 1 d . . . H9A H 0.3004 1.2198 0.5174 0.058 Uiso 1 1 calc R . . H9B H 0.3854 1.2419 0.4722 0.058 Uiso 1 1 calc R . . H9C H 0.3866 1.3036 0.5273 0.058 Uiso 1 1 calc R . . C10 C 0.4127(7) 1.1453(7) 0.5967(3) 0.056(2) Uani 1 1 d . . . H10A H 0.3388 1.1291 0.5988 0.084 Uiso 1 1 calc R . . H10B H 0.4261 1.2072 0.6165 0.084 Uiso 1 1 calc R . . H10C H 0.4532 1.0908 0.6125 0.084 Uiso 1 1 calc R . . O5 O -0.1247(4) 0.5717(4) 0.29928(19) 0.0596(17) Uani 1 1 d . . . O6 O -0.0887(4) 0.6279(4) 0.21598(18) 0.0389(12) Uani 1 1 d . . . O7 O 0.1475(4) 0.8381(4) 0.43217(18) 0.0398(12) Uani 1 1 d . . . O8 O 0.1351(4) 0.9480(4) 0.3646(2) 0.0465(14) Uani 1 1 d . . . C11 C -0.0616(6) 0.6166(5) 0.2635(3) 0.0362(16) Uani 1 1 d . . . C12 C 0.1409(5) 0.8573(6) 0.3824(3) 0.0329(16) Uani 1 1 d . . . C13 C 0.0441(5) 0.6507(5) 0.2851(3) 0.0344(17) Uani 1 1 d . . . C14 C 0.0375(7) 0.7634(6) 0.3058(3) 0.051(2) Uani 1 1 d . . . C15 C 0.1416(5) 0.7701(5) 0.3412(3) 0.0393(17) Uani 1 1 d . . . H15A H 0.1993 0.7842 0.3155 0.047 Uiso 1 1 calc R . . C16 C 0.1632(7) 0.6663(6) 0.3653(3) 0.066(3) Uani 1 1 d . . . H16A H 0.1502 0.6659 0.4045 0.079 Uiso 1 1 calc R . . H16B H 0.2356 0.6457 0.3585 0.079 Uiso 1 1 calc R . . C17 C 0.0838(7) 0.5942(6) 0.3347(3) 0.055(2) Uani 1 1 d . . . H17A H 0.1191 0.5318 0.3236 0.066 Uiso 1 1 calc R . . H17B H 0.0254 0.5766 0.3587 0.066 Uiso 1 1 calc R . . C18 C 0.1285(6) 0.6410(8) 0.2383(3) 0.068(3) Uani 1 1 d . . . H18A H 0.1321 0.5715 0.2261 0.102 Uiso 1 1 calc R . . H18B H 0.1963 0.6617 0.2520 0.102 Uiso 1 1 calc R . . H18C H 0.1087 0.6840 0.2081 0.102 Uiso 1 1 calc R . . C19 C 0.0407(10) 0.8411(8) 0.2587(4) 0.100(4) Uani 1 1 d . . . H19A H -0.0232 0.8364 0.2377 0.150 Uiso 1 1 calc R . . H19B H 0.1002 0.8269 0.2354 0.150 Uiso 1 1 calc R . . H19C H 0.0473 0.9086 0.2735 0.150 Uiso 1 1 calc R . . C20 C -0.0591(6) 0.7788(7) 0.3420(4) 0.079(3) Uani 1 1 d . . . H20A H -0.0589 0.7291 0.3709 0.118 Uiso 1 1 calc R . . H20B H -0.1220 0.7711 0.3203 0.118 Uiso 1 1 calc R . . H20C H -0.0574 0.8460 0.3576 0.118 Uiso 1 1 calc R . . O9 O 0.7197(7) 0.7611(6) 0.2014(3) 0.119(3) Uani 1 1 d . . . O10 O 0.6176(5) 0.7352(5) 0.1350(3) 0.076(2) Uani 1 1 d . . . O11 O 0.3965(5) 0.9923(5) 0.3227(2) 0.074(2) Uani 1 1 d . . . O12 O 0.2927(5) 1.0273(6) 0.2561(2) 0.085(2) Uani 1 1 d . . . C21 C 0.6476(6) 0.7882(6) 0.1720(3) 0.0417(18) Uani 1 1 d . . . C22 C 0.3805(7) 1.0029(6) 0.2719(3) 0.047(2) Uani 1 1 d . . . C23 C 0.5993(5) 0.8941(6) 0.1815(3) 0.0453(18) Uani 1 1 d . . . C24 C 0.4820(5) 0.8871(6) 0.2030(3) 0.0363(16) Uani 1 1 d . . . C25 C 0.4707(6) 0.9941(6) 0.2323(4) 0.050(2) Uani 1 1 d U . . H25A H 0.4584 1.0446 0.2033 0.060 Uiso 1 1 calc R . . C26 C 0.5775(7) 1.0160(9) 0.2558(5) 0.091(3) Uani 1 1 d U . . H26A H 0.5943 1.0877 0.2513 0.109 Uiso 1 1 calc R . . H26B H 0.5781 1.0002 0.2947 0.109 Uiso 1 1 calc R . . C27 C 0.6565(7) 0.9527(8) 0.2267(5) 0.082(3) Uani 1 1 d U . . H27A H 0.6895 0.9056 0.2522 0.098 Uiso 1 1 calc R . . H27B H 0.7110 0.9957 0.2110 0.098 Uiso 1 1 calc R . . C28 C 0.6055(9) 0.9516(7) 0.1266(4) 0.099(4) Uani 1 1 d . . . H28A H 0.6777 0.9544 0.1145 0.148 Uiso 1 1 calc R . . H28B H 0.5791 1.0196 0.1314 0.148 Uiso 1 1 calc R . . H28C H 0.5637 0.9167 0.0996 0.148 Uiso 1 1 calc R . . C29 C 0.3970(7) 0.8736(9) 0.1593(4) 0.084(3) Uani 1 1 d . . . H29A H 0.4043 0.8077 0.1426 0.126 Uiso 1 1 calc R . . H29B H 0.4047 0.9256 0.1319 0.126 Uiso 1 1 calc R . . H29C H 0.3285 0.8790 0.1760 0.126 Uiso 1 1 calc R . . C30 C 0.4708(8) 0.8027(7) 0.2436(4) 0.069(3) Uani 1 1 d . . . H30A H 0.4770 0.7384 0.2250 0.103 Uiso 1 1 calc R . . H30B H 0.4029 0.8071 0.2609 0.103 Uiso 1 1 calc R . . H30C H 0.5253 0.8082 0.2708 0.103 Uiso 1 1 calc R . . N1 N -0.0534(5) 0.9589(5) 0.4582(3) 0.0536(19) Uani 1 1 d . . . N2 N 0.0513(6) 0.8793(5) 0.5432(3) 0.061(2) Uani 1 1 d . . . C31 C -0.1041(7) 1.0078(7) 0.4189(4) 0.070(3) Uani 1 1 d . . . H31A H -0.0673 1.0584 0.4002 0.084 Uiso 1 1 calc R . . C32 C -0.2072(8) 0.9899(10) 0.4035(6) 0.115(5) Uani 1 1 d U . . H32A H -0.2404 1.0252 0.3752 0.138 Uiso 1 1 calc R . . C33 C -0.2573(8) 0.9137(10) 0.4342(6) 0.118(4) Uani 1 1 d U . . H33A H -0.3278 0.8988 0.4268 0.141 Uiso 1 1 calc R . . C34 C -0.2083(8) 0.8618(10) 0.4735(7) 0.117(5) Uani 1 1 d U . . H34A H -0.2429 0.8101 0.4924 0.140 Uiso 1 1 calc R . . C35 C -0.1028(6) 0.8867(8) 0.4860(5) 0.071(3) Uani 1 1 d . . . C36 C -0.0446(10) 0.8399(8) 0.5313(5) 0.086(3) Uani 1 1 d U . . C37 C -0.0794(11) 0.7546(8) 0.5631(5) 0.103(3) Uani 1 1 d U . . H37A H -0.1423 0.7221 0.5540 0.124 Uiso 1 1 calc R . . C38 C -0.0224(12) 0.7203(9) 0.6063(5) 0.111(4) Uani 1 1 d U . . H38A H -0.0466 0.6662 0.6276 0.133 Uiso 1 1 calc R . . C39 C 0.0716(12) 0.7669(8) 0.6181(5) 0.106(4) Uani 1 1 d U . . H39A H 0.1113 0.7462 0.6483 0.127 Uiso 1 1 calc R . . C40 C 0.1065(9) 0.8436(7) 0.5855(4) 0.073(3) Uani 1 1 d . . . H40A H 0.1719 0.8725 0.5931 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.03145(18) 0.02480(17) 0.02699(17) -0.00064(17) 0.00326(17) 0.00031(17) Mn1 0.0318(6) 0.0234(5) 0.0398(6) -0.0038(5) 0.0061(5) -0.0061(5) O1 0.041(3) 0.023(3) 0.055(3) -0.002(2) -0.010(2) 0.001(2) O2 0.038(3) 0.043(3) 0.042(3) -0.016(2) -0.001(2) -0.011(2) O3 0.053(3) 0.053(3) 0.050(3) 0.009(3) -0.006(3) -0.017(3) O4 0.033(3) 0.042(3) 0.037(3) -0.004(2) -0.009(2) 0.000(2) C1 0.018(3) 0.035(4) 0.040(4) -0.011(4) -0.003(3) 0.003(3) C2 0.031(4) 0.027(4) 0.034(4) -0.004(3) -0.009(3) 0.002(3) C3 0.043(4) 0.023(4) 0.031(3) -0.004(3) -0.017(3) 0.002(3) C4 0.028(3) 0.022(4) 0.030(4) 0.001(3) -0.002(3) -0.003(3) C5 0.031(4) 0.026(4) 0.047(4) 0.001(3) -0.013(3) 0.003(3) C6 0.044(4) 0.049(5) 0.055(5) -0.032(4) 0.002(4) -0.008(4) C7 0.037(4) 0.040(5) 0.043(4) -0.012(4) 0.006(3) -0.007(4) C8 0.042(4) 0.035(5) 0.071(5) 0.018(4) -0.021(4) 0.001(4) C9 0.030(4) 0.037(4) 0.048(4) -0.009(3) -0.012(3) 0.006(3) C10 0.056(5) 0.070(6) 0.040(4) 0.007(4) 0.001(4) -0.006(4) O5 0.072(4) 0.071(4) 0.036(3) 0.001(3) -0.007(3) -0.034(3) O6 0.041(3) 0.039(3) 0.036(3) 0.003(2) -0.012(2) -0.008(2) O7 0.048(3) 0.042(3) 0.029(3) -0.008(2) -0.003(2) 0.002(2) O8 0.046(3) 0.027(3) 0.066(4) 0.002(3) -0.012(3) -0.007(2) C11 0.051(4) 0.027(4) 0.031(4) -0.006(3) -0.003(3) -0.002(4) C12 0.020(3) 0.035(4) 0.043(4) -0.009(3) -0.006(3) -0.010(3) C13 0.037(4) 0.034(4) 0.032(4) -0.006(3) -0.015(3) -0.001(3) C14 0.060(5) 0.031(4) 0.062(5) -0.006(4) -0.022(4) -0.002(4) C15 0.035(4) 0.033(4) 0.049(5) -0.011(3) -0.009(3) 0.001(3) C16 0.083(6) 0.046(5) 0.068(6) -0.013(4) -0.044(5) 0.014(5) C17 0.074(5) 0.034(4) 0.058(5) -0.003(4) -0.022(4) -0.001(4) C18 0.051(5) 0.085(7) 0.068(6) -0.014(5) -0.016(5) -0.003(5) C19 0.161(12) 0.045(6) 0.093(8) 0.009(6) -0.076(8) -0.019(7) C20 0.047(5) 0.071(7) 0.118(8) -0.054(7) -0.006(6) -0.009(5) O9 0.136(7) 0.095(6) 0.127(6) -0.062(5) -0.073(5) 0.089(6) O10 0.083(4) 0.066(4) 0.079(4) -0.028(4) -0.025(4) 0.045(4) O11 0.087(5) 0.087(5) 0.047(3) -0.011(3) 0.001(3) 0.046(4) O12 0.057(4) 0.139(7) 0.058(4) -0.031(4) -0.006(3) 0.050(4) C21 0.043(4) 0.041(5) 0.041(4) -0.002(4) 0.011(4) 0.014(4) C22 0.060(5) 0.038(5) 0.043(5) -0.015(4) 0.012(4) 0.017(4) C23 0.044(4) 0.035(4) 0.057(4) 0.001(4) 0.020(3) 0.009(4) C24 0.043(4) 0.035(4) 0.031(3) -0.001(3) 0.009(3) 0.011(4) C25 0.041(4) 0.037(4) 0.073(5) -0.007(4) 0.018(4) 0.004(3) C26 0.061(5) 0.079(6) 0.133(6) -0.053(5) 0.007(5) -0.009(5) C27 0.044(4) 0.079(6) 0.123(7) -0.052(6) 0.008(5) 0.002(5) C28 0.123(9) 0.063(7) 0.110(8) 0.044(6) 0.084(7) 0.049(7) C29 0.076(6) 0.113(9) 0.065(6) -0.034(6) -0.017(5) 0.028(6) C30 0.081(7) 0.047(6) 0.078(6) 0.005(5) 0.038(5) 0.007(5) N1 0.033(4) 0.040(4) 0.088(5) -0.032(4) 0.002(4) 0.003(3) N2 0.075(5) 0.039(4) 0.070(5) -0.010(4) 0.041(4) -0.022(4) C31 0.047(5) 0.058(6) 0.104(7) -0.052(6) -0.009(5) 0.016(5) C32 0.046(6) 0.099(8) 0.200(12) -0.088(9) -0.026(6) 0.016(5) C33 0.034(5) 0.103(8) 0.217(11) -0.096(8) 0.007(6) 0.006(5) C34 0.049(6) 0.096(9) 0.206(12) -0.083(9) 0.031(6) -0.017(5) C35 0.043(5) 0.053(6) 0.118(8) -0.052(6) 0.044(5) -0.019(5) C36 0.106(7) 0.050(6) 0.103(7) -0.027(5) 0.082(6) -0.026(5) C37 0.134(8) 0.066(6) 0.109(7) -0.028(5) 0.082(6) -0.037(6) C38 0.165(9) 0.065(6) 0.102(7) 0.000(6) 0.082(7) -0.019(6) C39 0.171(10) 0.058(6) 0.088(6) 0.006(6) 0.068(7) -0.004(7) C40 0.105(8) 0.036(5) 0.078(7) 0.006(5) 0.040(6) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2 2.432(4) 4_476 ? La1 O4 2.441(4) . ? La1 O8 2.445(5) . ? La1 O9 2.485(6) 3_655 ? La1 O6 2.520(4) 3 ? La1 O10 2.537(5) 3_655 ? La1 O11 2.552(6) . ? La1 O12 2.590(6) . ? La1 C21 2.875(7) 3_655 ? La1 C22 2.926(7) . ? Mn1 O1 2.118(5) 4_476 ? Mn1 O3 2.197(5) . ? Mn1 O7 2.215(5) . ? Mn1 N2 2.255(7) . ? Mn1 N1 2.267(6) . ? Mn1 O4 2.467(5) . ? O1 C1 1.248(8) . ? O1 Mn1 2.118(5) 4_576 ? O2 C1 1.262(7) . ? O2 La1 2.432(4) 4_576 ? O3 C2 1.243(8) . ? O4 C2 1.272(7) . ? C1 C3 1.547(9) . ? C2 C5 1.528(9) . ? C3 C7 1.529(9) . ? C3 C8 1.533(9) . ? C3 C4 1.584(9) . ? C4 C9 1.510(9) . ? C4 C10 1.537(9) . ? C4 C5 1.575(9) . ? C5 C6 1.491(10) . ? C5 H5A 0.9800 . ? C6 C7 1.542(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? O5 C11 1.319(8) . ? O6 C11 1.217(7) . ? O6 La1 2.520(4) 3_545 ? O7 C12 1.241(8) . ? O8 C12 1.267(8) . ? C11 C13 1.505(10) . ? C12 C15 1.521(9) . ? C13 C17 1.505(10) . ? C13 C14 1.565(10) . ? C13 C18 1.566(11) . ? C14 C20 1.521(12) . ? C14 C19 1.535(13) . ? C14 C15 1.578(10) . ? C15 C16 1.508(10) . ? C15 H15A 0.9800 . ? C16 C17 1.567(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O9 C21 1.214(9) . ? O9 La1 2.485(6) 3_645 ? O10 C21 1.200(9) . ? O10 La1 2.537(5) 3_645 ? O11 C22 1.262(9) . ? O12 C22 1.218(9) . ? C21 C23 1.535(10) . ? C21 La1 2.875(7) 3_645 ? C22 C25 1.500(10) . ? C23 C27 1.526(12) . ? C23 C28 1.537(11) . ? C23 C24 1.577(9) . ? C24 C30 1.490(11) . ? C24 C29 1.524(10) . ? C24 C25 1.581(10) . ? C25 C26 1.495(12) . ? C25 H25A 0.9800 . ? C26 C27 1.480(12) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1 C31 1.318(11) . ? N1 C35 1.321(12) . ? N2 C40 1.331(12) . ? N2 C36 1.351(14) . ? C31 C32 1.378(13) . ? C31 H31A 0.9300 . ? C32 C33 1.401(18) . ? C32 H32A 0.9300 . ? C33 C34 1.328(18) . ? C33 H33A 0.9300 . ? C34 C35 1.408(13) . ? C34 H34A 0.9300 . ? C35 C36 1.463(15) . ? C36 C37 1.430(14) . ? C37 C38 1.353(18) . ? C37 H37A 0.9300 . ? C38 C39 1.368(18) . ? C38 H38A 0.9300 . ? C39 C40 1.355(13) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O4 76.32(15) 4_476 . ? O2 La1 O8 82.80(17) 4_476 . ? O4 La1 O8 76.04(16) . . ? O2 La1 O9 96.2(3) 4_476 3_655 ? O4 La1 O9 131.61(19) . 3_655 ? O8 La1 O9 151.49(19) . 3_655 ? O2 La1 O6 78.36(15) 4_476 3 ? O4 La1 O6 145.60(15) . 3 ? O8 La1 O6 78.02(16) . 3 ? O9 La1 O6 73.9(2) 3_655 3 ? O2 La1 O10 98.0(2) 4_476 3_655 ? O4 La1 O10 83.83(18) . 3_655 ? O8 La1 O10 159.10(19) . 3_655 ? O9 La1 O10 49.4(2) 3_655 3_655 ? O6 La1 O10 122.71(19) 3 3_655 ? O2 La1 O11 158.39(18) 4_476 . ? O4 La1 O11 82.27(17) . . ? O8 La1 O11 89.2(2) . . ? O9 La1 O11 100.2(3) 3_655 . ? O6 La1 O11 119.66(17) 3 . ? O10 La1 O11 82.5(2) 3_655 . ? O2 La1 O12 149.40(17) 4_476 . ? O4 La1 O12 128.89(18) . . ? O8 La1 O12 87.1(2) . . ? O9 La1 O12 79.3(3) 3_655 . ? O6 La1 O12 71.29(17) 3 . ? O10 La1 O12 101.5(2) 3_655 . ? O11 La1 O12 49.12(18) . . ? O2 La1 C21 96.79(19) 4_476 3_655 ? O4 La1 C21 107.5(2) . 3_655 ? O8 La1 C21 176.3(2) . 3_655 ? O9 La1 C21 24.8(2) 3_655 3_655 ? O6 La1 C21 98.3(2) 3 3_655 ? O10 La1 C21 24.60(19) 3_655 3_655 ? O11 La1 C21 92.4(2) . 3_655 ? O12 La1 C21 91.4(2) . 3_655 ? O2 La1 C22 173.4(2) 4_476 . ? O4 La1 C22 107.6(2) . . ? O8 La1 C22 92.9(2) . . ? O9 La1 C22 85.1(3) 3_655 . ? O6 La1 C22 95.8(2) 3 . ? O10 La1 C22 87.8(2) 3_655 . ? O11 La1 C22 25.5(2) . . ? O12 La1 C22 24.57(19) . . ? C21 La1 C22 87.2(2) 3_655 . ? O1 Mn1 O3 93.69(19) 4_476 . ? O1 Mn1 O7 161.87(19) 4_476 . ? O3 Mn1 O7 97.85(19) . . ? O1 Mn1 N2 109.5(2) 4_476 . ? O3 Mn1 N2 88.5(3) . . ? O7 Mn1 N2 84.8(2) . . ? O1 Mn1 N1 87.7(2) 4_476 . ? O3 Mn1 N1 160.1(3) . . ? O7 Mn1 N1 86.2(2) . . ? N2 Mn1 N1 72.4(3) . . ? O1 Mn1 O4 86.34(17) 4_476 . ? O3 Mn1 O4 55.48(17) . . ? O7 Mn1 O4 88.72(17) . . ? N2 Mn1 O4 142.1(3) . . ? N1 Mn1 O4 144.4(2) . . ? C1 O1 Mn1 119.1(4) . 4_576 ? C1 O2 La1 142.4(4) . 4_576 ? C2 O3 Mn1 98.6(4) . . ? C2 O4 La1 172.4(4) . . ? C2 O4 Mn1 85.3(4) . . ? La1 O4 Mn1 101.56(15) . . ? O1 C1 O2 123.1(6) . . ? O1 C1 C3 119.4(6) . . ? O2 C1 C3 117.6(6) . . ? O3 C2 O4 120.5(6) . . ? O3 C2 C5 120.3(6) . . ? O4 C2 C5 119.2(6) . . ? C7 C3 C8 110.6(6) . . ? C7 C3 C1 113.0(6) . . ? C8 C3 C1 108.6(5) . . ? C7 C3 C4 102.2(5) . . ? C8 C3 C4 112.2(6) . . ? C1 C3 C4 110.3(5) . . ? C9 C4 C10 108.3(6) . . ? C9 C4 C5 111.2(5) . . ? C10 C4 C5 111.4(6) . . ? C9 C4 C3 111.9(5) . . ? C10 C4 C3 114.2(5) . . ? C5 C4 C3 99.7(5) . . ? C6 C5 C2 116.4(6) . . ? C6 C5 C4 106.2(6) . . ? C2 C5 C4 112.3(5) . . ? C6 C5 H5A 107.2 . . ? C2 C5 H5A 107.2 . . ? C4 C5 H5A 107.2 . . ? C5 C6 C7 107.8(6) . . ? C5 C6 H6A 110.1 . . ? C7 C6 H6A 110.1 . . ? C5 C6 H6B 110.1 . . ? C7 C6 H6B 110.1 . . ? H6A C6 H6B 108.5 . . ? C3 C7 C6 104.5(6) . . ? C3 C7 H7A 110.9 . . ? C6 C7 H7A 110.9 . . ? C3 C7 H7B 110.9 . . ? C6 C7 H7B 110.9 . . ? H7A C7 H7B 108.9 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 O6 La1 143.8(5) . 3_545 ? C12 O7 Mn1 108.0(5) . . ? C12 O8 La1 142.7(5) . . ? O6 C11 O5 120.8(6) . . ? O6 C11 C13 123.1(6) . . ? O5 C11 C13 116.1(6) . . ? O7 C12 O8 121.9(6) . . ? O7 C12 C15 119.4(7) . . ? O8 C12 C15 118.7(6) . . ? C17 C13 C11 115.5(6) . . ? C17 C13 C14 103.0(6) . . ? C11 C13 C14 110.2(6) . . ? C17 C13 C18 108.5(6) . . ? C11 C13 C18 109.2(5) . . ? C14 C13 C18 110.3(7) . . ? C20 C14 C19 111.5(9) . . ? C20 C14 C13 110.8(7) . . ? C19 C14 C13 112.6(7) . . ? C20 C14 C15 110.3(6) . . ? C19 C14 C15 110.4(7) . . ? C13 C14 C15 100.6(6) . . ? C16 C15 C12 115.1(6) . . ? C16 C15 C14 108.3(6) . . ? C12 C15 C14 113.4(6) . . ? C16 C15 H15A 106.5 . . ? C12 C15 H15A 106.5 . . ? C14 C15 H15A 106.5 . . ? C15 C16 C17 104.2(6) . . ? C15 C16 H16A 110.9 . . ? C17 C16 H16A 110.9 . . ? C15 C16 H16B 110.9 . . ? C17 C16 H16B 110.9 . . ? H16A C16 H16B 108.9 . . ? C13 C17 C16 107.4(6) . . ? C13 C17 H17A 110.2 . . ? C16 C17 H17A 110.2 . . ? C13 C17 H17B 110.2 . . ? C16 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O9 La1 95.9(5) . 3_645 ? C21 O10 La1 93.7(5) . 3_645 ? C22 O11 La1 94.1(5) . . ? C22 O12 La1 93.3(5) . . ? O10 C21 O9 120.8(8) . . ? O10 C21 C23 120.7(7) . . ? O9 C21 C23 118.4(8) . . ? O10 C21 La1 61.7(4) . 3_645 ? O9 C21 La1 59.3(4) . 3_645 ? C23 C21 La1 173.0(5) . 3_645 ? O12 C22 O11 119.0(7) . . ? O12 C22 C25 120.7(7) . . ? O11 C22 C25 120.1(8) . . ? O12 C22 La1 62.1(4) . . ? O11 C22 La1 60.4(4) . . ? C25 C22 La1 156.9(5) . . ? C27 C23 C21 112.1(7) . . ? C27 C23 C28 110.9(8) . . ? C21 C23 C28 107.0(6) . . ? C27 C23 C24 103.6(6) . . ? C21 C23 C24 111.8(6) . . ? C28 C23 C24 111.5(7) . . ? C30 C24 C29 108.0(8) . . ? C30 C24 C23 110.7(6) . . ? C29 C24 C23 116.0(6) . . ? C30 C24 C25 110.7(6) . . ? C29 C24 C25 110.7(7) . . ? C23 C24 C25 100.5(6) . . ? C26 C25 C22 115.2(7) . . ? C26 C25 C24 105.2(6) . . ? C22 C25 C24 115.3(6) . . ? C26 C25 H25A 106.9 . . ? C22 C25 H25A 106.9 . . ? C24 C25 H25A 106.9 . . ? C27 C26 C25 108.6(8) . . ? C27 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? C27 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? C26 C27 C23 107.9(7) . . ? C26 C27 H27A 110.1 . . ? C23 C27 H27A 110.1 . . ? C26 C27 H27B 110.1 . . ? C23 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C24 C30 H30A 109.5 . . ? C24 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C24 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 N1 C35 119.3(8) . . ? C31 N1 Mn1 124.2(6) . . ? C35 N1 Mn1 116.3(7) . . ? C40 N2 C36 120.2(9) . . ? C40 N2 Mn1 123.6(6) . . ? C36 N2 Mn1 115.1(7) . . ? N1 C31 C32 125.2(12) . . ? N1 C31 H31A 117.4 . . ? C32 C31 H31A 117.4 . . ? C31 C32 C33 113.8(13) . . ? C31 C32 H32A 123.1 . . ? C33 C32 H32A 123.1 . . ? C34 C33 C32 122.6(11) . . ? C34 C33 H33A 118.7 . . ? C32 C33 H33A 118.7 . . ? C33 C34 C35 118.7(13) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? N1 C35 C34 120.3(13) . . ? N1 C35 C36 116.7(8) . . ? C34 C35 C36 122.9(12) . . ? N2 C36 C37 117.4(13) . . ? N2 C36 C35 116.9(8) . . ? C37 C36 C35 125.7(12) . . ? C38 C37 C36 121.2(13) . . ? C38 C37 H37A 119.4 . . ? C36 C37 H37A 119.4 . . ? C37 C38 C39 118.6(12) . . ? C37 C38 H38A 120.7 . . ? C39 C38 H38A 120.7 . . ? C40 C39 C38 119.4(14) . . ? C40 C39 H39A 120.3 . . ? C38 C39 H39A 120.3 . . ? N2 C40 C39 123.0(12) . . ? N2 C40 H40A 118.5 . . ? C39 C40 H40A 118.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.781 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.091