# Electronic Supplementary Material (ESI) for CrystEngComm # 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_Mn3DyNa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H83 Dy Mn3 N6 Na O22, H2 O ' _chemical_formula_sum 'C56 H85 Dy Mn3 N6 Na O23' _chemical_formula_weight 1560.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.439(5) _cell_length_b 14.807(5) _cell_length_c 19.751(5) _cell_angle_alpha 82.658(5) _cell_angle_beta 86.874(5) _cell_angle_gamma 76.935(5) _cell_volume 3231(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3690 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 22.28 _exptl_crystal_description block-shaped _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1598 _exptl_absorpt_coefficient_mu 1.804 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.611991 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _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 16912 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 25.02 _reflns_number_total 11172 _reflns_number_gt 8284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1261P)^2^+3.7395P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11172 _refine_ls_number_parameters 830 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2127 _refine_ls_wR_factor_gt 0.1915 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8823(11) -0.1420(7) 0.7718(7) 0.075(3) Uani 1 1 d . . . H1A H 0.9126 -0.1860 0.8103 0.112 Uiso 1 1 calc R . . H1B H 0.9482 -0.1300 0.7425 0.112 Uiso 1 1 calc R . . H1C H 0.8299 -0.1672 0.7470 0.112 Uiso 1 1 calc R . . C2 C 0.7102(9) -0.0573(6) 0.8294(4) 0.043(2) Uani 1 1 d . . . C3 C 0.6672(10) -0.1356(7) 0.8524(5) 0.058(3) Uani 1 1 d . . . H3 H 0.7117 -0.1934 0.8425 0.070 Uiso 1 1 calc R . . C4 C 0.5605(10) -0.1322(7) 0.8896(6) 0.059(3) Uani 1 1 d . . . H4 H 0.5341 -0.1862 0.9057 0.070 Uiso 1 1 calc R . . C5 C 0.4955(9) -0.0457(8) 0.9017(5) 0.055(3) Uani 1 1 d . . . H5 H 0.4237 -0.0418 0.9267 0.066 Uiso 1 1 calc R . . C6 C 0.5319(8) 0.0373(6) 0.8781(4) 0.042(2) Uani 1 1 d . . . C7 C 0.6427(8) 0.0309(6) 0.8437(4) 0.0352(18) Uani 1 1 d . . . C8 C 0.4485(8) 0.1265(6) 0.8846(4) 0.041(2) Uani 1 1 d . . . H8 H 0.3809 0.1254 0.9128 0.049 Uiso 1 1 calc R . . C9 C 0.3653(8) 0.2925(7) 0.8574(5) 0.047(2) Uani 1 1 d U . . C10 C 0.3667(15) 0.3260(13) 0.9251(9) 0.139(7) Uani 1 1 d U . . H10A H 0.3805 0.2735 0.9599 0.209 Uiso 1 1 calc R . . H10B H 0.2909 0.3668 0.9340 0.209 Uiso 1 1 calc R . . H10C H 0.4297 0.3592 0.9251 0.209 Uiso 1 1 calc R . . C11 C 0.2492(9) 0.2699(9) 0.8417(7) 0.078(4) Uani 1 1 d . . . H11A H 0.2589 0.2399 0.8003 0.094 Uiso 1 1 calc R . . H11B H 0.2263 0.2270 0.8787 0.094 Uiso 1 1 calc R . . C13 C 1.1679(10) 0.0869(9) 0.7556(6) 0.071(3) Uani 1 1 d . . . H13A H 1.2354 0.0891 0.7248 0.107 Uiso 1 1 calc R . . H13B H 1.1960 0.0611 0.8004 0.107 Uiso 1 1 calc R . . H13C H 1.1201 0.1489 0.7573 0.107 Uiso 1 1 calc R . . C14 C 1.0870(8) 0.0454(7) 0.6628(5) 0.046(2) Uani 1 1 d . . . C15 C 1.1645(9) -0.0130(7) 0.6216(6) 0.062(3) Uani 1 1 d . . . H15 H 1.2219 -0.0628 0.6415 0.075 Uiso 1 1 calc R . . C16 C 1.1563(9) 0.0031(8) 0.5509(6) 0.062(3) Uani 1 1 d . . . H16 H 1.2082 -0.0353 0.5233 0.074 Uiso 1 1 calc R . . C17 C 1.0697(9) 0.0770(7) 0.5222(5) 0.054(3) Uani 1 1 d . . . H17 H 1.0660 0.0893 0.4749 0.065 Uiso 1 1 calc R . . C18 C 0.9869(8) 0.1342(6) 0.5628(5) 0.046(2) Uani 1 1 d . . . C19 C 0.9985(8) 0.1176(6) 0.6343(5) 0.042(2) Uani 1 1 d . . . C20 C 0.8936(9) 0.2028(6) 0.5290(4) 0.046(2) Uani 1 1 d . . . H20 H 0.8973 0.2105 0.4815 0.055 Uiso 1 1 calc R . . C21 C 0.7090(9) 0.3227(6) 0.5184(4) 0.045(2) Uani 1 1 d . . . C22 C 0.6771(11) 0.2894(8) 0.4531(5) 0.064(3) Uani 1 1 d . . . H22A H 0.7450 0.2832 0.4218 0.097 Uiso 1 1 calc R . . H22B H 0.6105 0.3341 0.4323 0.097 Uiso 1 1 calc R . . H22C H 0.6557 0.2301 0.4639 0.097 Uiso 1 1 calc R . . C23 C 0.7527(9) 0.4140(6) 0.5037(5) 0.050(2) Uani 1 1 d . . . H23A H 0.7854 0.4264 0.5450 0.060 Uiso 1 1 calc R . . H23B H 0.8167 0.4067 0.4692 0.060 Uiso 1 1 calc R . . C24 C 0.5994(8) 0.3358(7) 0.5680(4) 0.047(2) Uani 1 1 d . . . H24A H 0.5413 0.3921 0.5522 0.056 Uiso 1 1 calc R . . H24B H 0.5614 0.2832 0.5696 0.056 Uiso 1 1 calc R . . C25 C 1.0896(9) -0.0726(7) 0.8869(6) 0.064(3) Uani 1 1 d . . . H25A H 1.1735 -0.0719 0.8829 0.096 Uiso 1 1 calc R . . H25B H 1.0692 -0.1043 0.8514 0.096 Uiso 1 1 calc R . . H25C H 1.0730 -0.1045 0.9306 0.096 Uiso 1 1 calc R . . C26 C 1.0503(8) 0.0778(7) 0.9216(5) 0.046(2) Uani 1 1 d . . . C27 C 1.1343(9) 0.0485(8) 0.9742(5) 0.057(3) Uani 1 1 d . . . H27 H 1.1746 -0.0137 0.9824 0.069 Uiso 1 1 calc R . . C28 C 1.1553(10) 0.1126(9) 1.0125(6) 0.066(3) Uani 1 1 d . . . H28 H 1.2138 0.0940 1.0455 0.080 Uiso 1 1 calc R . . C29 C 1.0938(9) 0.2031(9) 1.0046(5) 0.058(3) Uani 1 1 d . . . H29 H 1.1069 0.2440 1.0340 0.069 Uiso 1 1 calc R . . C30 C 1.0105(8) 0.2353(7) 0.9523(5) 0.047(2) Uani 1 1 d . . . C31 C 0.9919(8) 0.1717(7) 0.9083(4) 0.043(2) Uani 1 1 d . . . C32 C 0.9519(8) 0.3310(7) 0.9453(4) 0.043(2) Uani 1 1 d . . . H32 H 0.9686 0.3663 0.9778 0.052 Uiso 1 1 calc R . . C33 C 0.8226(8) 0.4757(7) 0.8957(5) 0.048(2) Uani 1 1 d . . . C34 C 0.8004(12) 0.5130(10) 0.9644(6) 0.087(4) Uani 1 1 d . . . H34A H 0.7586 0.4741 0.9946 0.131 Uiso 1 1 calc R . . H34B H 0.7528 0.5756 0.9585 0.131 Uiso 1 1 calc R . . H34C H 0.8758 0.5128 0.9836 0.131 Uiso 1 1 calc R . . C35 C 0.9053(10) 0.5288(8) 0.8470(7) 0.0730(18) Uani 1 1 d U . . H35A H 0.9208 0.5037 0.8035 0.088 Uiso 1 1 calc R . . H35B H 0.8703 0.5952 0.8390 0.088 Uiso 1 1 calc R . . C36 C 0.7072(9) 0.4858(7) 0.8590(5) 0.053(2) Uani 1 1 d . . . H36A H 0.6479 0.4659 0.8909 0.064 Uiso 1 1 calc R . . H36B H 0.6769 0.5510 0.8425 0.064 Uiso 1 1 calc R . . C37 C 0.6844(9) 0.6107(6) 0.6358(5) 0.049(2) Uani 1 1 d . . . C38 C 0.7129(11) 0.6993(8) 0.6030(6) 0.067(3) Uani 1 1 d U . . C39 C 0.736(3) 0.6940(13) 0.5289(8) 0.178(11) Uani 1 1 d . . . H39A H 0.7211 0.7560 0.5049 0.267 Uiso 1 1 calc R . . H39B H 0.6831 0.6598 0.5126 0.267 Uiso 1 1 calc R . . H39C H 0.8176 0.6629 0.5210 0.267 Uiso 1 1 calc R . . C40 C 0.812(3) 0.724(2) 0.6330(12) 0.29(2) Uani 1 1 d . . . H40A H 0.8594 0.6691 0.6577 0.429 Uiso 1 1 calc R . . H40B H 0.7810 0.7695 0.6637 0.429 Uiso 1 1 calc R . . H40C H 0.8599 0.7492 0.5976 0.429 Uiso 1 1 calc R . . C41 C 0.601(2) 0.7722(11) 0.6084(18) 0.27(2) Uani 1 1 d . . . H41A H 0.5976 0.7966 0.6514 0.406 Uiso 1 1 calc R . . H41B H 0.5326 0.7453 0.6054 0.406 Uiso 1 1 calc R . . H41C H 0.5998 0.8218 0.5718 0.406 Uiso 1 1 calc R . . C42 C 0.5892(8) 0.1337(6) 0.6716(4) 0.038(2) Uani 1 1 d . . . C43 C 0.5265(8) 0.0718(7) 0.6368(5) 0.050(2) Uani 1 1 d . . . C44 C 0.5061(10) -0.0088(7) 0.6891(5) 0.058(3) Uani 1 1 d . . . H44A H 0.4637 0.0157 0.7285 0.087 Uiso 1 1 calc R . . H44B H 0.5821 -0.0480 0.7025 0.087 Uiso 1 1 calc R . . H44C H 0.4596 -0.0446 0.6693 0.087 Uiso 1 1 calc R . . C45 C 0.4068(10) 0.1328(8) 0.6119(6) 0.069(3) Uani 1 1 d . . . H45A H 0.3631 0.1615 0.6494 0.104 Uiso 1 1 calc R . . H45B H 0.3607 0.0949 0.5941 0.104 Uiso 1 1 calc R . . H45C H 0.4213 0.1803 0.5768 0.104 Uiso 1 1 calc R . . C46 C 0.6034(12) 0.0342(9) 0.5765(6) 0.077(4) Uani 1 1 d . . . H46A H 0.5608 -0.0011 0.5533 0.115 Uiso 1 1 calc R . . H46B H 0.6774 -0.0054 0.5929 0.115 Uiso 1 1 calc R . . H46C H 0.6203 0.0854 0.5455 0.115 Uiso 1 1 calc R . . C47 C 0.3756(10) 0.6113(7) 0.7664(5) 0.054(2) Uani 1 1 d . . . C48 C 0.3352(10) 0.6762(8) 0.8221(6) 0.065(3) Uani 1 1 d . . . C49 C 0.4155(13) 0.6444(10) 0.8844(7) 0.096(5) Uani 1 1 d . . . H49A H 0.4936 0.6565 0.8730 0.145 Uiso 1 1 calc R . . H49B H 0.4225 0.5788 0.8976 0.145 Uiso 1 1 calc R . . H49C H 0.3804 0.6782 0.9216 0.145 Uiso 1 1 calc R . . C50 C 0.3492(14) 0.7715(9) 0.7917(8) 0.096(5) Uani 1 1 d . . . H50A H 0.4300 0.7679 0.7745 0.144 Uiso 1 1 calc R . . H50B H 0.3322 0.8132 0.8262 0.144 Uiso 1 1 calc R . . H50C H 0.2944 0.7943 0.7551 0.144 Uiso 1 1 calc R . . C51 C 0.2052(11) 0.6718(10) 0.8446(8) 0.096(4) Uani 1 1 d . . . H51A H 0.1792 0.7105 0.8804 0.143 Uiso 1 1 calc R . . H51B H 0.2019 0.6085 0.8609 0.143 Uiso 1 1 calc R . . H51C H 0.1536 0.6937 0.8064 0.143 Uiso 1 1 calc R . . C52 C 0.9425(8) 0.3795(6) 0.6938(4) 0.040(2) Uani 1 1 d . . . C53 C 1.0454(9) 0.4085(8) 0.6513(5) 0.056(3) Uani 1 1 d . . . C54 C 1.1544(10) 0.3278(9) 0.6530(6) 0.075(3) Uani 1 1 d . . . H54A H 1.1357 0.2776 0.6324 0.112 Uiso 1 1 calc R . . H54B H 1.1764 0.3065 0.6995 0.112 Uiso 1 1 calc R . . H54C H 1.2202 0.3482 0.6282 0.112 Uiso 1 1 calc R . . C55 C 1.0838(12) 0.4861(10) 0.6859(8) 0.094(4) Uani 1 1 d . . . H55A H 1.1387 0.5135 0.6561 0.141 Uiso 1 1 calc R . . H55B H 1.1222 0.4590 0.7281 0.141 Uiso 1 1 calc R . . H55C H 1.0141 0.5333 0.6950 0.141 Uiso 1 1 calc R . . C56 C 1.0140(12) 0.4440(11) 0.5802(6) 0.094(5) Uani 1 1 d . . . H56A H 0.9886 0.3968 0.5592 0.141 Uiso 1 1 calc R . . H56B H 1.0828 0.4596 0.5556 0.141 Uiso 1 1 calc R . . H56C H 0.9499 0.4986 0.5793 0.141 Uiso 1 1 calc R . . N1 N 0.4604(6) 0.2061(5) 0.8550(3) 0.0356(16) Uani 1 1 d . . . N2 N 0.8042(7) 0.2554(5) 0.5583(3) 0.0397(17) Uani 1 1 d . . . N3 N 0.8773(6) 0.3746(5) 0.8984(3) 0.0407(17) Uani 1 1 d . . . N4 N 0.6738(6) 0.2746(4) 0.8939(3) 0.0309(15) Uani 1 1 d . . . N5 N 0.6826(6) 0.2219(5) 0.9463(4) 0.0378(17) Uani 1 1 d . . . N6 N 0.6878(8) 0.1714(6) 0.9971(4) 0.053(2) Uani 1 1 d . . . O1 O 0.8170(6) -0.0563(4) 0.7954(3) 0.0518(16) Uani 1 1 d . . . O2 O 0.6915(5) 0.1037(4) 0.8226(3) 0.0393(13) Uani 1 1 d . . . O3 O 0.5094(5) 0.3520(4) 0.7793(3) 0.0361(13) Uani 1 1 d . . . O4 O 0.1597(8) 0.3513(7) 0.8334(6) 0.099(3) Uani 1 1 d . . . H4A H 0.1100 0.3452 0.8070 0.148 Uiso 1 1 calc R . . O5 O 1.0976(5) 0.0301(5) 0.7325(3) 0.0502(16) Uani 1 1 d . . . O6 O 0.9268(5) 0.1702(4) 0.6770(3) 0.0388(13) Uani 1 1 d . . . O7 O 0.6375(5) 0.3424(4) 0.6349(3) 0.0346(12) Uani 1 1 d . . . O8 O 0.6590(8) 0.4925(5) 0.4806(4) 0.072(2) Uani 1 1 d . . . H8A H 0.6745 0.5405 0.4906 0.107 Uiso 1 1 calc R . . O9 O 1.0212(5) 0.0196(5) 0.8811(3) 0.0526(16) Uani 1 1 d . . . O10 O 0.9229(5) 0.1956(4) 0.8551(3) 0.0411(14) Uani 1 1 d . . . O11 O 0.7228(5) 0.4331(4) 0.8039(3) 0.0356(13) Uani 1 1 d . . . O12 O 1.0222(7) 0.5085(6) 0.8894(4) 0.0730(18) Uani 1 1 d . . . H12 H 1.0058 0.4951 0.9299 0.109 Uiso 1 1 calc R . . O13 O 0.6320(6) 0.5596(4) 0.6075(3) 0.0467(15) Uani 1 1 d . . . O14 O 0.7094(6) 0.5849(4) 0.6986(3) 0.0524(16) Uani 1 1 d . . . O15 O 0.5280(5) 0.1806(4) 0.7157(3) 0.0384(13) Uani 1 1 d . . . O16 O 0.6981(5) 0.1355(4) 0.6558(3) 0.0411(14) Uani 1 1 d . . . O17 O 0.8435(5) 0.3898(4) 0.6660(3) 0.0397(13) Uani 1 1 d . . . O18 O 0.9648(5) 0.3447(4) 0.7544(3) 0.0368(13) Uani 1 1 d . . . O19 O 0.4817(5) 0.5600(4) 0.7680(3) 0.0462(15) Uani 1 1 d . . . O20 O 0.3043(7) 0.6146(5) 0.7191(4) 0.074(2) Uani 1 1 d . . . O21 O 0.7416(4) 0.2677(4) 0.7554(2) 0.0310(12) Uani 1 1 d . . . O22 O 0.4219(6) 0.4799(4) 0.6538(3) 0.0474(15) Uani 1 1 d . . . H22D H 0.4111 0.4289 0.6427 0.071 Uiso 1 1 d R . . H22E H 0.3657 0.5019 0.6811 0.071 Uiso 1 1 d R . . O23 O 0.1002(13) 0.7344(14) 0.6686(10) 0.171(6) Uani 1 1 d G . . H23C H 0.0705 0.7092 0.6394 0.256 Uiso 1 1 d G . . H23D H 0.0494 0.7463 0.7011 0.256 Uiso 1 1 d G . . Na1 Na 0.8909(3) 0.0868(2) 0.78616(17) 0.0431(8) Uani 1 1 d . . . Mn1 Mn 0.60371(10) 0.22906(8) 0.79858(6) 0.0304(3) Uani 1 1 d . . . Mn2 Mn 0.77668(11) 0.25253(8) 0.66033(6) 0.0322(3) Uani 1 1 d . . . Mn3 Mn 0.82071(11) 0.31290(8) 0.82479(6) 0.0325(3) Uani 1 1 d . . . Dy1 Dy 0.61199(4) 0.45198(3) 0.708910(19) 0.03641(17) Uani 1 1 d . . . C12 C 0.3887(9) 0.3547(7) 0.7868(5) 0.052(2) Uani 1 1 d U . . H12A H 0.3616 0.3302 0.7487 0.063 Uiso 1 1 calc R . . H12B H 0.3443 0.4187 0.7877 0.063 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 C1 0.079(8) 0.042(6) 0.095(9) -0.021(6) -0.003(7) 0.009(6) C2 0.058(6) 0.028(5) 0.044(5) 0.006(4) -0.016(4) -0.011(4) C3 0.081(8) 0.039(5) 0.056(6) -0.005(5) -0.017(6) -0.012(5) C4 0.063(7) 0.036(5) 0.073(7) 0.012(5) -0.006(6) -0.014(5) C5 0.055(6) 0.066(7) 0.046(5) 0.014(5) -0.008(5) -0.028(5) C6 0.047(5) 0.045(5) 0.038(5) 0.001(4) -0.005(4) -0.020(4) C7 0.043(5) 0.028(4) 0.032(4) 0.005(3) -0.010(4) -0.006(4) C8 0.036(5) 0.051(6) 0.040(5) -0.001(4) 0.006(4) -0.024(4) C9 0.030(4) 0.050(4) 0.056(5) -0.006(4) -0.001(4) 0.002(4) C10 0.108(11) 0.140(12) 0.150(12) -0.097(11) -0.031(9) 0.063(9) C11 0.043(6) 0.071(8) 0.107(10) 0.017(7) -0.016(6) 0.005(6) C13 0.058(7) 0.099(9) 0.063(7) 0.000(7) 0.007(5) -0.038(7) C14 0.041(5) 0.045(5) 0.051(6) -0.013(4) 0.007(4) -0.004(4) C15 0.051(6) 0.050(6) 0.086(8) -0.035(6) 0.011(6) 0.000(5) C16 0.045(6) 0.067(7) 0.079(8) -0.042(6) 0.019(5) -0.007(5) C17 0.059(6) 0.052(6) 0.057(6) -0.021(5) 0.018(5) -0.020(5) C18 0.046(5) 0.039(5) 0.049(5) -0.005(4) 0.007(4) -0.007(4) C19 0.038(5) 0.040(5) 0.050(5) -0.008(4) 0.016(4) -0.013(4) C20 0.062(6) 0.048(5) 0.032(4) -0.011(4) 0.018(4) -0.023(5) C21 0.059(6) 0.042(5) 0.032(4) 0.002(4) -0.004(4) -0.011(4) C22 0.094(9) 0.067(7) 0.036(5) -0.005(5) -0.009(5) -0.024(6) C23 0.057(6) 0.043(5) 0.041(5) -0.003(4) 0.007(4) 0.002(5) C24 0.051(6) 0.042(5) 0.042(5) 0.011(4) -0.019(4) -0.003(4) C25 0.040(6) 0.040(5) 0.091(8) 0.018(5) 0.001(5) 0.021(4) C26 0.033(5) 0.054(6) 0.042(5) 0.018(5) 0.000(4) -0.003(4) C27 0.043(6) 0.059(7) 0.059(6) 0.022(5) -0.007(5) -0.003(5) C28 0.049(6) 0.089(9) 0.050(6) 0.025(6) -0.011(5) -0.009(6) C29 0.042(6) 0.096(9) 0.033(5) 0.012(5) -0.019(4) -0.018(6) C30 0.031(5) 0.062(6) 0.045(5) 0.005(5) 0.002(4) -0.010(4) C31 0.038(5) 0.055(6) 0.030(4) 0.012(4) -0.007(4) -0.005(4) C32 0.039(5) 0.059(6) 0.036(5) -0.003(4) -0.010(4) -0.018(4) C33 0.048(6) 0.048(6) 0.052(6) -0.019(5) -0.003(4) -0.009(4) C34 0.081(9) 0.101(10) 0.077(8) -0.038(8) -0.012(7) 0.006(8) C35 0.068(4) 0.060(3) 0.100(4) -0.018(3) 0.006(3) -0.029(3) C36 0.051(6) 0.047(6) 0.058(6) -0.006(5) -0.011(5) -0.003(5) C37 0.061(6) 0.038(5) 0.042(5) 0.016(4) -0.001(5) -0.007(5) C38 0.079(6) 0.061(5) 0.065(5) -0.006(4) -0.008(5) -0.023(5) C39 0.37(4) 0.105(14) 0.083(12) -0.002(10) 0.038(16) -0.116(19) C40 0.45(5) 0.30(3) 0.20(2) 0.16(2) -0.20(3) -0.33(4) C41 0.18(2) 0.042(9) 0.52(5) 0.051(18) 0.16(3) 0.023(12) C42 0.052(6) 0.036(5) 0.028(4) -0.002(4) -0.009(4) -0.011(4) C43 0.046(6) 0.071(7) 0.040(5) -0.015(5) 0.008(4) -0.022(5) C44 0.073(7) 0.047(6) 0.059(6) -0.004(5) -0.014(5) -0.020(5) C45 0.079(8) 0.074(8) 0.066(7) -0.006(6) -0.028(6) -0.036(7) C46 0.102(10) 0.069(8) 0.074(8) -0.043(7) 0.013(7) -0.036(7) C47 0.056(6) 0.038(5) 0.062(6) -0.008(5) 0.004(5) 0.001(5) C48 0.048(6) 0.053(6) 0.085(8) -0.022(6) 0.012(6) 0.012(5) C49 0.096(10) 0.085(10) 0.107(11) -0.047(9) 0.006(9) 0.001(8) C50 0.108(11) 0.059(8) 0.123(12) -0.038(8) 0.018(9) -0.013(8) C51 0.063(8) 0.085(10) 0.128(12) -0.032(9) 0.016(8) 0.012(7) C52 0.050(6) 0.030(4) 0.041(5) -0.012(4) 0.004(4) -0.009(4) C53 0.045(6) 0.067(7) 0.052(6) 0.010(5) 0.007(5) -0.013(5) C54 0.062(7) 0.092(9) 0.064(7) 0.007(7) 0.007(6) -0.016(7) C55 0.074(9) 0.105(10) 0.121(11) -0.027(9) 0.023(8) -0.053(8) C56 0.072(8) 0.118(12) 0.078(9) 0.038(8) 0.005(7) -0.023(8) N1 0.022(3) 0.050(4) 0.034(4) -0.006(3) -0.003(3) -0.005(3) N2 0.056(5) 0.037(4) 0.027(3) -0.008(3) 0.009(3) -0.011(4) N3 0.036(4) 0.058(5) 0.031(4) -0.011(3) -0.007(3) -0.012(4) N4 0.035(4) 0.032(4) 0.020(3) 0.016(3) -0.009(3) -0.005(3) N5 0.024(4) 0.047(4) 0.043(4) -0.017(4) -0.001(3) -0.002(3) N6 0.064(5) 0.051(5) 0.033(4) 0.013(4) 0.001(4) 0.001(4) O1 0.052(4) 0.037(3) 0.059(4) -0.003(3) 0.003(3) 0.004(3) O2 0.041(3) 0.035(3) 0.039(3) -0.001(3) 0.003(3) -0.005(3) O3 0.030(3) 0.039(3) 0.037(3) -0.008(3) 0.000(2) 0.001(2) O4 0.072(6) 0.091(7) 0.127(9) -0.014(6) -0.009(6) -0.001(5) O5 0.037(3) 0.052(4) 0.057(4) -0.009(3) 0.000(3) 0.000(3) O6 0.032(3) 0.042(3) 0.038(3) -0.003(3) 0.007(2) -0.001(3) O7 0.034(3) 0.036(3) 0.031(3) -0.006(2) -0.005(2) -0.001(2) O8 0.097(6) 0.049(4) 0.063(5) 0.006(4) -0.034(4) -0.003(4) O9 0.037(3) 0.049(4) 0.065(4) 0.006(3) 0.001(3) -0.001(3) O10 0.040(3) 0.040(3) 0.041(3) 0.002(3) -0.005(3) -0.006(3) O11 0.039(3) 0.033(3) 0.031(3) 0.000(2) -0.010(2) 0.001(2) O12 0.068(4) 0.060(3) 0.100(4) -0.018(3) 0.006(3) -0.029(3) O13 0.050(4) 0.043(4) 0.050(4) -0.012(3) -0.001(3) -0.012(3) O14 0.059(4) 0.042(4) 0.056(4) -0.001(3) -0.007(3) -0.011(3) O15 0.035(3) 0.049(4) 0.031(3) -0.011(3) 0.000(2) -0.005(3) O16 0.035(3) 0.043(3) 0.046(3) -0.007(3) 0.006(3) -0.011(3) O17 0.044(4) 0.039(3) 0.036(3) 0.000(3) -0.009(3) -0.011(3) O18 0.030(3) 0.046(3) 0.031(3) 0.003(3) 0.001(2) -0.007(3) O19 0.043(4) 0.041(3) 0.049(4) -0.009(3) -0.001(3) 0.004(3) O20 0.057(5) 0.071(5) 0.084(5) -0.024(4) -0.022(4) 0.018(4) O21 0.028(3) 0.030(3) 0.028(3) 0.005(2) -0.002(2) 0.004(2) O22 0.049(4) 0.052(4) 0.037(3) 0.004(3) -0.015(3) -0.003(3) O23 0.136(12) 0.168(14) 0.189(16) -0.049(12) -0.011(11) 0.023(10) Na1 0.0365(18) 0.0406(19) 0.048(2) -0.0017(15) 0.0046(15) -0.0024(15) Mn1 0.0278(6) 0.0323(7) 0.0290(6) -0.0026(5) -0.0007(5) -0.0028(5) Mn2 0.0314(7) 0.0330(7) 0.0293(6) -0.0037(5) 0.0023(5) -0.0016(5) Mn3 0.0299(6) 0.0332(7) 0.0321(6) -0.0015(5) -0.0044(5) -0.0026(5) Dy1 0.0385(3) 0.0357(3) 0.0318(2) -0.00227(17) -0.00491(17) -0.00168(18) C12 0.050(5) 0.050(5) 0.050(5) 0.000(4) 0.000(4) 0.000(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 C1 O1 1.439(11) . ? C2 O1 1.363(11) . ? C2 C3 1.376(13) . ? C2 C7 1.413(12) . ? C3 C4 1.384(15) . ? C4 C5 1.370(15) . ? C5 C6 1.402(13) . ? C6 C7 1.394(12) . ? C6 C8 1.461(13) . ? C7 O2 1.334(10) . ? C8 N1 1.279(11) . ? C9 N1 1.485(11) . ? C9 C10 1.487(16) . ? C9 C11 1.498(14) . ? C9 C12 1.614(13) . ? C11 O4 1.392(13) . ? C13 O5 1.416(12) . ? C14 O5 1.373(11) . ? C14 C19 1.380(13) . ? C14 C15 1.398(13) . ? C15 C16 1.392(15) . ? C16 C17 1.382(15) . ? C17 C18 1.408(13) . ? C18 C19 1.410(13) . ? C18 C20 1.425(13) . ? C19 O6 1.340(10) . ? C20 N2 1.296(11) . ? C21 N2 1.484(12) . ? C21 C22 1.529(12) . ? C21 C23 1.533(13) . ? C21 C24 1.541(13) . ? C23 O8 1.436(11) . ? C24 O7 1.435(10) . ? C25 O9 1.406(11) . ? C26 O9 1.352(12) . ? C26 C31 1.399(13) . ? C26 C27 1.413(13) . ? C27 C28 1.356(16) . ? C28 C29 1.359(16) . ? C29 C30 1.407(12) . ? C30 C32 1.416(13) . ? C30 C31 1.417(13) . ? C31 O10 1.312(10) . ? C32 N3 1.299(11) . ? C33 N3 1.481(12) . ? C33 C36 1.509(13) . ? C33 C34 1.518(14) . ? C33 C35 1.575(14) . ? C35 O12 1.568(14) . ? C36 O11 1.398(11) . ? C37 O13 1.262(11) . ? C37 O14 1.279(11) . ? C37 C38 1.483(14) . ? C38 C40 1.44(2) . ? C38 C39 1.483(19) . ? C38 C41 1.49(2) . ? C42 O15 1.265(10) . ? C42 O16 1.272(10) . ? C42 C43 1.529(12) . ? C43 C44 1.527(13) . ? C43 C45 1.527(15) . ? C43 C46 1.527(13) . ? C47 O20 1.262(12) . ? C47 O19 1.278(11) . ? C47 C48 1.537(14) . ? C48 C50 1.500(17) . ? C48 C49 1.536(18) . ? C48 C51 1.542(16) . ? C52 O18 1.256(10) . ? C52 O17 1.257(10) . ? C52 C53 1.519(12) . ? C53 C56 1.469(15) . ? C53 C54 1.518(15) . ? C53 C55 1.563(16) . ? N1 Mn1 2.001(7) . ? N2 Mn2 2.019(6) . ? N3 Mn3 2.020(7) . ? N4 N5 1.208(9) . ? N4 Mn3 2.235(6) . ? N4 Mn1 2.318(6) . ? N5 N6 1.168(10) . ? O1 Na1 2.435(7) . ? O2 Mn1 1.914(6) . ? O2 Na1 2.322(7) . ? O3 C12 1.372(11) . ? O3 Mn1 1.898(6) . ? O3 Dy1 2.363(6) . ? O5 Na1 2.545(7) . ? O6 Mn2 1.886(6) . ? O6 Na1 2.407(6) . ? O7 Mn2 1.875(5) . ? O7 Dy1 2.281(5) . ? O9 Na1 2.425(7) . ? O10 Mn3 1.906(6) . ? O10 Na1 2.337(7) . ? O11 Mn3 1.886(5) . ? O11 Dy1 2.274(5) . ? O13 Dy1 2.430(6) . ? O14 Dy1 2.454(6) . ? O15 Mn1 2.164(5) . ? O16 Mn2 2.139(6) . ? O17 Mn2 2.344(6) . ? O17 Dy1 2.726(6) . ? O18 Mn3 2.192(5) . ? O19 Dy1 2.313(6) . ? O21 Mn1 1.919(5) . ? O21 Mn2 1.929(5) . ? O21 Mn3 1.946(5) . ? O21 Na1 2.844(6) . ? O21 Dy1 2.857(5) . ? O22 Dy1 2.413(6) . ? Na1 Mn2 3.354(4) . ? Na1 Mn3 3.436(4) . ? Na1 Mn1 3.493(4) . ? Mn1 Mn3 3.1094(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C2 C3 125.8(9) . . ? O1 C2 C7 115.2(7) . . ? C3 C2 C7 118.9(9) . . ? C2 C3 C4 122.9(10) . . ? C5 C4 C3 117.0(9) . . ? C4 C5 C6 123.2(10) . . ? C7 C6 C5 118.2(9) . . ? C7 C6 C8 122.5(8) . . ? C5 C6 C8 119.0(8) . . ? O2 C7 C6 124.3(8) . . ? O2 C7 C2 116.1(8) . . ? C6 C7 C2 119.6(8) . . ? N1 C8 C6 125.7(8) . . ? N1 C9 C10 108.6(9) . . ? N1 C9 C11 107.3(8) . . ? C10 C9 C11 114.6(11) . . ? N1 C9 C12 102.9(7) . . ? C10 C9 C12 122.3(12) . . ? C11 C9 C12 99.7(8) . . ? O4 C11 C9 109.9(10) . . ? O5 C14 C19 119.6(8) . . ? O5 C14 C15 119.8(9) . . ? C19 C14 C15 120.6(9) . . ? C16 C15 C14 120.2(10) . . ? C17 C16 C15 119.1(9) . . ? C16 C17 C18 121.7(10) . . ? C17 C18 C19 118.1(9) . . ? C17 C18 C20 117.7(9) . . ? C19 C18 C20 124.1(8) . . ? O6 C19 C14 117.3(8) . . ? O6 C19 C18 122.6(8) . . ? C14 C19 C18 120.1(8) . . ? N2 C20 C18 126.0(8) . . ? N2 C21 C22 114.5(8) . . ? N2 C21 C23 106.2(7) . . ? C22 C21 C23 112.0(8) . . ? N2 C21 C24 104.1(6) . . ? C22 C21 C24 109.9(8) . . ? C23 C21 C24 109.8(7) . . ? O8 C23 C21 112.8(8) . . ? O7 C24 C21 109.4(7) . . ? O9 C26 C31 115.6(8) . . ? O9 C26 C27 123.8(9) . . ? C31 C26 C27 120.5(10) . . ? C28 C27 C26 118.9(10) . . ? C27 C28 C29 122.4(10) . . ? C28 C29 C30 120.4(11) . . ? C29 C30 C32 117.8(9) . . ? C29 C30 C31 118.8(9) . . ? C32 C30 C31 123.4(8) . . ? O10 C31 C26 117.4(9) . . ? O10 C31 C30 123.9(8) . . ? C26 C31 C30 118.7(8) . . ? N3 C32 C30 126.9(8) . . ? N3 C33 C36 103.2(7) . . ? N3 C33 C34 115.2(9) . . ? C36 C33 C34 111.9(9) . . ? N3 C33 C35 107.1(8) . . ? C36 C33 C35 107.0(9) . . ? C34 C33 C35 111.8(9) . . ? O12 C35 C33 101.5(9) . . ? O11 C36 C33 112.3(8) . . ? O13 C37 O14 116.3(8) . . ? O13 C37 C38 125.2(9) . . ? O14 C37 C38 118.4(9) . . ? C40 C38 C39 110.7(18) . . ? C40 C38 C37 113.8(12) . . ? C39 C38 C37 109.3(10) . . ? C40 C38 C41 111(2) . . ? C39 C38 C41 105.5(19) . . ? C37 C38 C41 105.9(11) . . ? O15 C42 O16 123.4(7) . . ? O15 C42 C43 116.8(8) . . ? O16 C42 C43 119.8(7) . . ? C44 C43 C45 110.6(8) . . ? C44 C43 C46 110.2(9) . . ? C45 C43 C46 110.3(9) . . ? C44 C43 C42 108.6(7) . . ? C45 C43 C42 106.8(8) . . ? C46 C43 C42 110.2(8) . . ? O20 C47 O19 122.9(9) . . ? O20 C47 C48 118.3(9) . . ? O19 C47 C48 118.7(10) . . ? C50 C48 C49 108.7(12) . . ? C50 C48 C47 106.7(10) . . ? C49 C48 C47 110.7(9) . . ? C50 C48 C51 113.9(10) . . ? C49 C48 C51 108.6(11) . . ? C47 C48 C51 108.2(10) . . ? O18 C52 O17 125.1(8) . . ? O18 C52 C53 116.6(8) . . ? O17 C52 C53 118.3(8) . . ? C56 C53 C54 109.9(10) . . ? C56 C53 C52 113.2(9) . . ? C54 C53 C52 110.4(8) . . ? C56 C53 C55 109.5(11) . . ? C54 C53 C55 105.9(10) . . ? C52 C53 C55 107.7(8) . . ? C8 N1 C9 122.8(7) . . ? C8 N1 Mn1 125.0(6) . . ? C9 N1 Mn1 112.2(6) . . ? C20 N2 C21 121.9(7) . . ? C20 N2 Mn2 124.6(6) . . ? C21 N2 Mn2 113.5(5) . . ? C32 N3 C33 122.2(7) . . ? C32 N3 Mn3 124.3(6) . . ? C33 N3 Mn3 113.5(5) . . ? N5 N4 Mn3 128.2(5) . . ? N5 N4 Mn1 118.5(5) . . ? Mn3 N4 Mn1 86.1(2) . . ? N6 N5 N4 178.2(8) . . ? C2 O1 C1 117.5(8) . . ? C2 O1 Na1 117.8(5) . . ? C1 O1 Na1 124.5(7) . . ? C7 O2 Mn1 125.2(5) . . ? C7 O2 Na1 122.6(5) . . ? Mn1 O2 Na1 110.8(3) . . ? C12 O3 Mn1 112.1(5) . . ? C12 O3 Dy1 130.0(5) . . ? Mn1 O3 Dy1 112.8(2) . . ? C14 O5 C13 111.6(7) . . ? C14 O5 Na1 107.8(5) . . ? C13 O5 Na1 103.8(6) . . ? C19 O6 Mn2 128.9(6) . . ? C19 O6 Na1 114.2(5) . . ? Mn2 O6 Na1 102.1(2) . . ? C24 O7 Mn2 112.7(5) . . ? C24 O7 Dy1 137.8(5) . . ? Mn2 O7 Dy1 106.9(2) . . ? C26 O9 C25 117.0(8) . . ? C26 O9 Na1 118.4(5) . . ? C25 O9 Na1 122.9(7) . . ? C31 O10 Mn3 129.6(6) . . ? C31 O10 Na1 122.4(6) . . ? Mn3 O10 Na1 107.7(3) . . ? C36 O11 Mn3 112.6(5) . . ? C36 O11 Dy1 129.9(5) . . ? Mn3 O11 Dy1 115.0(3) . . ? C37 O13 Dy1 96.3(5) . . ? C37 O14 Dy1 94.8(6) . . ? C42 O15 Mn1 124.4(5) . . ? C42 O16 Mn2 124.8(5) . . ? C52 O17 Mn2 115.8(5) . . ? C52 O17 Dy1 132.8(5) . . ? Mn2 O17 Dy1 82.26(18) . . ? C52 O18 Mn3 120.5(5) . . ? C47 O19 Dy1 141.8(6) . . ? Mn1 O21 Mn2 118.8(3) . . ? Mn1 O21 Mn3 107.1(2) . . ? Mn2 O21 Mn3 134.0(3) . . ? Mn1 O21 Na1 92.3(2) . . ? Mn2 O21 Na1 87.06(19) . . ? Mn3 O21 Na1 89.62(19) . . ? Mn1 O21 Dy1 94.31(18) . . ? Mn2 O21 Dy1 86.45(17) . . ? Mn3 O21 Dy1 92.05(19) . . ? Na1 O21 Dy1 172.4(2) . . ? O2 Na1 O10 92.4(2) . . ? O2 Na1 O6 116.2(2) . . ? O10 Na1 O6 98.0(2) . . ? O2 Na1 O9 109.8(2) . . ? O10 Na1 O9 65.9(2) . . ? O6 Na1 O9 131.9(2) . . ? O2 Na1 O1 65.7(2) . . ? O10 Na1 O1 139.8(3) . . ? O6 Na1 O1 121.6(3) . . ? O9 Na1 O1 89.4(3) . . ? O2 Na1 O5 164.2(3) . . ? O10 Na1 O5 103.1(2) . . ? O6 Na1 O5 65.3(2) . . ? O9 Na1 O5 74.5(2) . . ? O1 Na1 O5 99.7(2) . . ? O2 Na1 O21 64.10(19) . . ? O10 Na1 O21 66.38(19) . . ? O6 Na1 O21 63.63(18) . . ? O9 Na1 O21 131.5(2) . . ? O1 Na1 O21 123.3(2) . . ? O5 Na1 O21 125.1(2) . . ? O2 Na1 Mn2 83.59(17) . . ? O10 Na1 Mn2 93.03(18) . . ? O6 Na1 Mn2 33.35(14) . . ? O9 Na1 Mn2 154.8(2) . . ? O1 Na1 Mn2 115.8(2) . . ? O5 Na1 Mn2 98.53(18) . . ? O21 Na1 Mn2 35.06(11) . . ? O2 Na1 Mn3 78.05(17) . . ? O10 Na1 Mn3 31.92(15) . . ? O6 Na1 Mn3 79.17(16) . . ? O9 Na1 Mn3 97.6(2) . . ? O1 Na1 Mn3 143.23(19) . . ? O5 Na1 Mn3 116.97(19) . . ? O21 Na1 Mn3 34.50(11) . . ? Mn2 Na1 Mn3 63.38(7) . . ? O2 Na1 Mn1 30.82(15) . . ? O10 Na1 Mn1 78.13(17) . . ? O6 Na1 Mn1 91.02(16) . . ? O9 Na1 Mn1 125.55(19) . . ? O1 Na1 Mn1 93.59(18) . . ? O5 Na1 Mn1 156.2(2) . . ? O21 Na1 Mn1 33.29(11) . . ? Mn2 Na1 Mn1 57.81(6) . . ? Mn3 Na1 Mn1 53.32(6) . . ? O3 Mn1 O2 176.3(2) . . ? O3 Mn1 O21 90.5(2) . . ? O2 Mn1 O21 92.9(2) . . ? O3 Mn1 N1 84.3(3) . . ? O2 Mn1 N1 92.1(3) . . ? O21 Mn1 N1 169.6(3) . . ? O3 Mn1 O15 92.2(2) . . ? O2 Mn1 O15 88.4(2) . . ? O21 Mn1 O15 102.4(2) . . ? N1 Mn1 O15 86.9(2) . . ? O3 Mn1 N4 88.9(2) . . ? O2 Mn1 N4 90.2(2) . . ? O21 Mn1 N4 82.5(2) . . ? N1 Mn1 N4 88.3(2) . . ? O15 Mn1 N4 174.9(2) . . ? O3 Mn1 Mn3 89.24(17) . . ? O2 Mn1 Mn3 92.69(18) . . ? O21 Mn1 Mn3 36.73(15) . . ? N1 Mn1 Mn3 133.84(19) . . ? O15 Mn1 Mn3 139.11(15) . . ? N4 Mn1 Mn3 45.81(16) . . ? O3 Mn1 Na1 144.95(18) . . ? O2 Mn1 Na1 38.42(18) . . ? O21 Mn1 Na1 54.45(16) . . ? N1 Mn1 Na1 129.9(2) . . ? O15 Mn1 Na1 96.62(16) . . ? N4 Mn1 Na1 85.26(17) . . ? Mn3 Mn1 Na1 62.39(7) . . ? O7 Mn2 O6 172.7(2) . . ? O7 Mn2 O21 90.9(2) . . ? O6 Mn2 O21 94.1(2) . . ? O7 Mn2 N2 82.9(3) . . ? O6 Mn2 N2 91.7(3) . . ? O21 Mn2 N2 172.2(3) . . ? O7 Mn2 O16 95.0(2) . . ? O6 Mn2 O16 89.6(2) . . ? O21 Mn2 O16 98.3(2) . . ? N2 Mn2 O16 86.9(3) . . ? O7 Mn2 O17 79.7(2) . . ? O6 Mn2 O17 96.0(2) . . ? O21 Mn2 O17 80.0(2) . . ? N2 Mn2 O17 94.2(2) . . ? O16 Mn2 O17 174.3(2) . . ? O7 Mn2 Na1 142.51(18) . . ? O6 Mn2 Na1 44.55(17) . . ? O21 Mn2 Na1 57.88(16) . . ? N2 Mn2 Na1 129.6(2) . . ? O16 Mn2 Na1 72.20(18) . . ? O17 Mn2 Na1 110.96(15) . . ? O11 Mn3 O10 173.8(2) . . ? O11 Mn3 O21 89.7(2) . . ? O10 Mn3 O21 96.2(2) . . ? O11 Mn3 N3 82.3(3) . . ? O10 Mn3 N3 91.7(3) . . ? O21 Mn3 N3 170.7(3) . . ? O11 Mn3 O18 92.6(2) . . ? O10 Mn3 O18 89.1(2) . . ? O21 Mn3 O18 93.5(2) . . ? N3 Mn3 O18 91.4(3) . . ? O11 Mn3 N4 89.0(2) . . ? O10 Mn3 N4 89.6(2) . . ? O21 Mn3 N4 84.2(2) . . ? N3 Mn3 N4 91.1(3) . . ? O18 Mn3 N4 177.2(2) . . ? O11 Mn3 Mn1 88.69(18) . . ? O10 Mn3 Mn1 94.86(18) . . ? O21 Mn3 Mn1 36.14(15) . . ? N3 Mn3 Mn1 138.4(2) . . ? O18 Mn3 Mn1 129.68(15) . . ? N4 Mn3 Mn1 48.06(16) . . ? O11 Mn3 Na1 145.56(18) . . ? O10 Mn3 Na1 40.40(19) . . ? O21 Mn3 Na1 55.88(16) . . ? N3 Mn3 Na1 132.1(2) . . ? O18 Mn3 Na1 89.50(17) . . ? N4 Mn3 Na1 87.92(18) . . ? Mn1 Mn3 Na1 64.29(7) . . ? O11 Dy1 O7 122.85(19) . . ? O11 Dy1 O19 82.6(2) . . ? O7 Dy1 O19 148.3(2) . . ? O11 Dy1 O3 81.94(19) . . ? O7 Dy1 O3 85.06(19) . . ? O19 Dy1 O3 80.0(2) . . ? O11 Dy1 O22 151.4(2) . . ? O7 Dy1 O22 75.1(2) . . ? O19 Dy1 O22 74.5(2) . . ? O3 Dy1 O22 77.55(19) . . ? O11 Dy1 O13 124.5(2) . . ? O7 Dy1 O13 84.82(19) . . ? O19 Dy1 O13 95.9(2) . . ? O3 Dy1 O13 152.7(2) . . ? O22 Dy1 O13 75.4(2) . . ? O11 Dy1 O14 73.8(2) . . ? O7 Dy1 O14 125.7(2) . . ? O19 Dy1 O14 76.5(2) . . ? O3 Dy1 O14 148.0(2) . . ? O22 Dy1 O14 115.8(2) . . ? O13 Dy1 O14 52.5(2) . . ? O11 Dy1 O17 74.93(18) . . ? O7 Dy1 O17 65.28(18) . . ? O19 Dy1 O17 145.8(2) . . ? O3 Dy1 O17 120.95(17) . . ? O22 Dy1 O17 133.03(19) . . ? O13 Dy1 O17 76.84(19) . . ? O14 Dy1 O17 72.7(2) . . ? O11 Dy1 O21 62.34(17) . . ? O7 Dy1 O21 62.51(17) . . ? O19 Dy1 O21 129.99(18) . . ? O3 Dy1 O21 61.74(17) . . ? O22 Dy1 O21 121.90(19) . . ? O13 Dy1 O21 132.81(18) . . ? O14 Dy1 O21 120.78(19) . . ? O17 Dy1 O21 59.34(15) . . ? O3 C12 C9 108.6(7) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.687 _refine_diff_density_min -3.353 _refine_diff_density_rms 0.155 _database_code_depnum_ccdc_archive 'CCDC 947811' ####################################################################### # # 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_Mn3TbNa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H83 Mn3 N6 Na O22 Tb, H2 O ' _chemical_formula_sum 'C56 H85 Mn3 N6 Na O23 Tb' _chemical_formula_weight 1557.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.455(5) _cell_length_b 14.841(5) _cell_length_c 19.776(5) _cell_angle_alpha 82.715(5) _cell_angle_beta 87.032(5) _cell_angle_gamma 76.958(5) _cell_volume 3248(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5467 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.06 _exptl_crystal_description block-shaped _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 1.733 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.795078 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _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 16620 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11176 _reflns_number_gt 9130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0965P)^2^+8.8860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11176 _refine_ls_number_parameters 830 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 C1 C 0.5899(7) -0.0734(5) 0.8886(5) 0.051(2) Uani 1 1 d . . . H1A H 0.6731 -0.0730 0.8805 0.077 Uiso 1 1 calc R . . H1B H 0.5643 -0.1072 0.8559 0.077 Uiso 1 1 calc R . . H1C H 0.5786 -0.1029 0.9338 0.077 Uiso 1 1 calc R . . C2 C 0.5507(6) 0.0775(5) 0.9235(4) 0.0400(17) Uani 1 1 d . . . C3 C 0.6344(6) 0.0489(6) 0.9735(4) 0.046(2) Uani 1 1 d . . . H3 H 0.6769 -0.0127 0.9799 0.055 Uiso 1 1 calc R . . C4 C 0.6550(7) 0.1135(7) 1.0144(4) 0.055(2) Uani 1 1 d . . . H4 H 0.7110 0.0941 1.0487 0.066 Uiso 1 1 calc R . . C5 C 0.5949(7) 0.2040(6) 1.0053(4) 0.047(2) Uani 1 1 d . . . H5 H 0.6093 0.2455 1.0337 0.057 Uiso 1 1 calc R . . C6 C 0.5105(6) 0.2358(5) 0.9529(3) 0.0363(16) Uani 1 1 d . . . C7 C 0.4911(6) 0.1724(5) 0.9093(3) 0.0324(15) Uani 1 1 d . . . C8 C 0.4504(6) 0.3325(5) 0.9460(3) 0.0322(15) Uani 1 1 d . . . H8 H 0.4666 0.3684 0.9781 0.039 Uiso 1 1 calc R . . C9 C 0.3213(7) 0.4751(5) 0.8965(4) 0.0380(17) Uani 1 1 d . . . C10 C 0.2985(9) 0.5115(8) 0.9655(5) 0.069(3) Uani 1 1 d . . . H10A H 0.2587 0.4713 0.9956 0.104 Uiso 1 1 calc R . . H10B H 0.2489 0.5733 0.9600 0.104 Uiso 1 1 calc R . . H10C H 0.3735 0.5128 0.9844 0.104 Uiso 1 1 calc R . . C11 C 0.4053(8) 0.5268(7) 0.8499(6) 0.0623(14) Uani 1 1 d . . . H11A H 0.4178 0.5038 0.8057 0.075 Uiso 1 1 calc R . . H11B H 0.3718 0.5933 0.8434 0.075 Uiso 1 1 calc R . . C12 C 0.2029(7) 0.4857(5) 0.8606(4) 0.0415(18) Uani 1 1 d . . . H12A H 0.1445 0.4644 0.8922 0.050 Uiso 1 1 calc R . . H12B H 0.1713 0.5508 0.8444 0.050 Uiso 1 1 calc R . . C13 C 0.3817(9) -0.1402(6) 0.7710(5) 0.064(3) Uani 1 1 d . . . H13A H 0.4077 -0.1864 0.8090 0.097 Uiso 1 1 calc R . . H13B H 0.4503 -0.1288 0.7441 0.097 Uiso 1 1 calc R . . H13C H 0.3300 -0.1623 0.7435 0.097 Uiso 1 1 calc R . . C14 C 0.2111(7) -0.0573(5) 0.8301(4) 0.0383(17) Uani 1 1 d . . . C15 C 0.1696(8) -0.1367(5) 0.8512(4) 0.048(2) Uani 1 1 d . . . H15 H 0.2134 -0.1942 0.8406 0.058 Uiso 1 1 calc R . . C16 C 0.0613(8) -0.1313(5) 0.8889(4) 0.050(2) Uani 1 1 d . . . H16 H 0.0357 -0.1852 0.9055 0.060 Uiso 1 1 calc R . . C17 C -0.0058(7) -0.0465(6) 0.9009(4) 0.0458(19) Uani 1 1 d . . . H17 H -0.0782 -0.0432 0.9250 0.055 Uiso 1 1 calc R . . C18 C 0.0321(6) 0.0371(5) 0.8776(3) 0.0341(15) Uani 1 1 d . . . C19 C 0.1443(6) 0.0309(5) 0.8431(3) 0.0306(14) Uani 1 1 d . . . C20 C -0.0509(6) 0.1251(5) 0.8844(3) 0.0364(16) Uani 1 1 d . . . H20 H -0.1182 0.1238 0.9126 0.044 Uiso 1 1 calc R . . C21 C -0.1348(6) 0.2904(5) 0.8568(4) 0.0375(16) Uani 1 1 d . . . C22 C -0.1310(11) 0.3320(10) 0.9218(7) 0.122(6) Uani 1 1 d . . . H22A H -0.1217 0.2838 0.9596 0.183 Uiso 1 1 calc R . . H22B H -0.2042 0.3771 0.9277 0.183 Uiso 1 1 calc R . . H22C H -0.0645 0.3619 0.9195 0.183 Uiso 1 1 calc R . . C23 C -0.1109(7) 0.3545(6) 0.7886(5) 0.055(2) Uani 1 1 d . . . H23A H -0.1401 0.3330 0.7497 0.066 Uiso 1 1 calc R . . H23B H -0.1536 0.4183 0.7914 0.066 Uiso 1 1 calc R . . C24 C -0.2527(7) 0.2696(6) 0.8444(5) 0.060(2) Uani 1 1 d . . . H24A H -0.2456 0.2375 0.8041 0.072 Uiso 1 1 calc R . . H24B H -0.2738 0.2282 0.8828 0.072 Uiso 1 1 calc R . . C25 C 0.6678(8) 0.0851(8) 0.7567(5) 0.066(3) Uani 1 1 d . . . H25A H 0.7360 0.0866 0.7266 0.099 Uiso 1 1 calc R . . H25B H 0.6945 0.0588 0.8016 0.099 Uiso 1 1 calc R . . H25C H 0.6211 0.1473 0.7583 0.099 Uiso 1 1 calc R . . C26 C 0.5871(6) 0.0446(5) 0.6632(4) 0.0382(17) Uani 1 1 d . . . C27 C 0.6624(7) -0.0118(5) 0.6222(5) 0.047(2) Uani 1 1 d . . . H27 H 0.7191 -0.0621 0.6418 0.056 Uiso 1 1 calc R . . C28 C 0.6550(7) 0.0055(6) 0.5512(4) 0.046(2) Uani 1 1 d . . . H28 H 0.7078 -0.0320 0.5237 0.055 Uiso 1 1 calc R . . C29 C 0.5701(7) 0.0775(6) 0.5231(4) 0.0456(19) Uani 1 1 d . . . H29 H 0.5668 0.0893 0.4758 0.055 Uiso 1 1 calc R . . C30 C 0.4864(6) 0.1352(5) 0.5630(4) 0.0340(15) Uani 1 1 d . . . C31 C 0.4965(6) 0.1192(5) 0.6345(4) 0.0327(15) Uani 1 1 d . . . C32 C 0.3919(7) 0.2026(5) 0.5290(4) 0.0376(17) Uani 1 1 d . . . H32 H 0.3938 0.2092 0.4816 0.045 Uiso 1 1 calc R . . C33 C 0.2067(7) 0.3229(5) 0.5197(3) 0.0348(16) Uani 1 1 d . . . C34 C 0.1752(9) 0.2906(6) 0.4542(4) 0.052(2) Uani 1 1 d . . . H34A H 0.2425 0.2860 0.4228 0.078 Uiso 1 1 calc R . . H34B H 0.1077 0.3347 0.4340 0.078 Uiso 1 1 calc R . . H34C H 0.1554 0.2308 0.4644 0.078 Uiso 1 1 calc R . . C35 C 0.2512(7) 0.4144(5) 0.5046(3) 0.0368(16) Uani 1 1 d . . . H35A H 0.2836 0.4271 0.5458 0.044 Uiso 1 1 calc R . . H35B H 0.3155 0.4063 0.4705 0.044 Uiso 1 1 calc R . . C36 C 0.0992(7) 0.3359(5) 0.5688(3) 0.0349(16) Uani 1 1 d . . . H36A H 0.0410 0.3920 0.5529 0.042 Uiso 1 1 calc R . . H36B H 0.0612 0.2834 0.5705 0.042 Uiso 1 1 calc R . . C37 C 0.1842(7) 0.6085(5) 0.6376(4) 0.0380(17) Uani 1 1 d . . . C38 C 0.2112(8) 0.6989(5) 0.6030(4) 0.0433(18) Uani 1 1 d . . . C39 C 0.312(2) 0.7218(15) 0.6335(9) 0.240(16) Uani 1 1 d . . . H39A H 0.2834 0.7714 0.6612 0.360 Uiso 1 1 calc R . . H39B H 0.3650 0.7412 0.5982 0.360 Uiso 1 1 calc R . . H39C H 0.3549 0.6679 0.6614 0.360 Uiso 1 1 calc R . . C40 C 0.2326(19) 0.6956(10) 0.5294(7) 0.134(7) Uani 1 1 d . . . H40A H 0.2582 0.7506 0.5096 0.201 Uiso 1 1 calc R . . H40B H 0.1600 0.6924 0.5087 0.201 Uiso 1 1 calc R . . H40C H 0.2938 0.6416 0.5219 0.201 Uiso 1 1 calc R . . C41 C 0.1041(15) 0.7714(8) 0.6086(14) 0.215(14) Uani 1 1 d . . . H41A H 0.0931 0.7856 0.6548 0.323 Uiso 1 1 calc R . . H41B H 0.0360 0.7504 0.5957 0.323 Uiso 1 1 calc R . . H41C H 0.1122 0.8262 0.5790 0.323 Uiso 1 1 calc R . . C42 C 0.4433(6) 0.3795(4) 0.6943(3) 0.0288(14) Uani 1 1 d . . . C43 C 0.5478(7) 0.4094(5) 0.6526(4) 0.0412(18) Uani 1 1 d . . . C44 C 0.6546(7) 0.3272(6) 0.6536(4) 0.048(2) Uani 1 1 d . . . H44A H 0.6335 0.2780 0.6330 0.073 Uiso 1 1 calc R . . H44B H 0.6771 0.3052 0.6999 0.073 Uiso 1 1 calc R . . H44C H 0.7206 0.3463 0.6286 0.073 Uiso 1 1 calc R . . C45 C 0.5819(8) 0.4870(6) 0.6870(5) 0.056(2) Uani 1 1 d . . . H45A H 0.6392 0.5133 0.6585 0.084 Uiso 1 1 calc R . . H45B H 0.6164 0.4614 0.7304 0.084 Uiso 1 1 calc R . . H45C H 0.5116 0.5346 0.6934 0.084 Uiso 1 1 calc R . . C46 C 0.5132(8) 0.4446(7) 0.5808(4) 0.058(2) Uani 1 1 d . . . H46A H 0.5796 0.4636 0.5560 0.088 Uiso 1 1 calc R . . H46B H 0.4461 0.4969 0.5804 0.088 Uiso 1 1 calc R . . H46C H 0.4915 0.3961 0.5597 0.088 Uiso 1 1 calc R . . C47 C 0.0895(6) 0.1339(5) 0.6727(3) 0.0294(14) Uani 1 1 d . . . C48 C 0.0293(7) 0.0714(5) 0.6371(4) 0.0379(17) Uani 1 1 d . . . C49 C 0.0077(7) -0.0083(5) 0.6895(4) 0.0447(18) Uani 1 1 d . . . H49A H -0.0409 -0.0429 0.6700 0.067 Uiso 1 1 calc R . . H49B H -0.0328 0.0165 0.7291 0.067 Uiso 1 1 calc R . . H49C H 0.0831 -0.0488 0.7024 0.067 Uiso 1 1 calc R . . C50 C 0.1044(9) 0.0351(7) 0.5775(5) 0.062(3) Uani 1 1 d . . . H50A H 0.1148 0.0865 0.5448 0.093 Uiso 1 1 calc R . . H50B H 0.0649 -0.0045 0.5565 0.093 Uiso 1 1 calc R . . H50C H 0.1813 0.0002 0.5931 0.093 Uiso 1 1 calc R . . C51 C -0.0933(8) 0.1310(6) 0.6119(4) 0.051(2) Uani 1 1 d . . . H51A H -0.0806 0.1822 0.5796 0.076 Uiso 1 1 calc R . . H51B H -0.1405 0.1546 0.6500 0.076 Uiso 1 1 calc R . . H51C H -0.1348 0.0933 0.5904 0.076 Uiso 1 1 calc R . . C52 C -0.1240(7) 0.6120(5) 0.7670(4) 0.0435(18) Uani 1 1 d . . . C53 C -0.1642(7) 0.6747(6) 0.8234(5) 0.051(2) Uani 1 1 d . . . C54 C -0.1515(11) 0.7703(7) 0.7943(6) 0.079(3) Uani 1 1 d . . . H54A H -0.0717 0.7673 0.7759 0.119 Uiso 1 1 calc R . . H54B H -0.1666 0.8107 0.8295 0.119 Uiso 1 1 calc R . . H54C H -0.2081 0.7941 0.7587 0.119 Uiso 1 1 calc R . . C55 C -0.2935(9) 0.6716(8) 0.8475(6) 0.076(3) Uani 1 1 d . . . H55A H -0.3154 0.7073 0.8852 0.114 Uiso 1 1 calc R . . H55B H -0.2985 0.6083 0.8614 0.114 Uiso 1 1 calc R . . H55C H -0.3471 0.6975 0.8107 0.114 Uiso 1 1 calc R . . C56 C -0.0844(9) 0.6427(8) 0.8850(5) 0.074(3) Uani 1 1 d . . . H56A H -0.0051 0.6514 0.8729 0.112 Uiso 1 1 calc R . . H56B H -0.0811 0.5779 0.8995 0.112 Uiso 1 1 calc R . . H56C H -0.1166 0.6785 0.9215 0.112 Uiso 1 1 calc R . . N1 N 0.3766(5) 0.3735(4) 0.8997(3) 0.0301(12) Uani 1 1 d . . . N2 N -0.0391(5) 0.2053(4) 0.8545(3) 0.0294(12) Uani 1 1 d . . . N3 N 0.3033(5) 0.2554(4) 0.5589(3) 0.0292(12) Uani 1 1 d . . . N4 N 0.1732(5) 0.2734(4) 0.8957(3) 0.0270(11) Uani 1 1 d . . . N5 N 0.1826(4) 0.2205(4) 0.9471(3) 0.0271(12) Uani 1 1 d . . . N6 N 0.1878(6) 0.1712(5) 0.9973(3) 0.0467(16) Uani 1 1 d . . . O1 O 0.5207(4) 0.0201(3) 0.8819(3) 0.0398(12) Uani 1 1 d . . . O2 O 0.4211(4) 0.1959(3) 0.8558(2) 0.0306(10) Uani 1 1 d . . . O3 O 0.2233(4) 0.4327(3) 0.8053(2) 0.0282(10) Uani 1 1 d . . . O4 O 0.5246(5) 0.5047(4) 0.8890(4) 0.0623(14) Uani 1 1 d . . . H4A H 0.5102 0.4985 0.9301 0.094 Uiso 1 1 calc R . . O5 O 0.3180(5) -0.0556(3) 0.7956(3) 0.0404(12) Uani 1 1 d . . . O6 O 0.1914(4) 0.1044(3) 0.8232(2) 0.0288(10) Uani 1 1 d . . . O7 O 0.0102(4) 0.3506(3) 0.7801(2) 0.0264(9) Uani 1 1 d . . . O8 O -0.3423(7) 0.3483(6) 0.8356(4) 0.082(2) Uani 1 1 d . . . H8A H -0.3575 0.3613 0.7950 0.123 Uiso 1 1 calc R . . O9 O 0.5962(4) 0.0296(4) 0.7324(3) 0.0402(12) Uani 1 1 d . . . O10 O 0.4269(4) 0.1708(3) 0.6781(2) 0.0292(10) Uani 1 1 d . . . O11 O 0.1371(4) 0.3427(3) 0.6350(2) 0.0260(9) Uani 1 1 d . . . O12 O 0.1602(6) 0.4917(4) 0.4810(3) 0.0515(14) Uani 1 1 d . . . H12 H 0.1484 0.5298 0.5086 0.077 Uiso 1 1 calc R . . O13 O 0.1330(4) 0.5593(3) 0.6065(2) 0.0346(11) Uani 1 1 d . . . O14 O 0.2077(5) 0.5846(3) 0.7001(2) 0.0388(12) Uani 1 1 d . . . O15 O 0.1972(4) 0.1359(3) 0.6566(2) 0.0331(10) Uani 1 1 d . . . O16 O 0.0285(4) 0.1795(3) 0.7171(2) 0.0300(10) Uani 1 1 d . . . O17 O 0.3442(4) 0.3896(3) 0.6669(2) 0.0290(10) Uani 1 1 d . . . O18 O 0.4644(4) 0.3446(3) 0.7557(2) 0.0281(10) Uani 1 1 d . . . O19 O -0.0200(4) 0.5602(3) 0.7691(3) 0.0374(11) Uani 1 1 d . . . O20 O -0.1972(5) 0.6149(4) 0.7207(3) 0.0612(17) Uani 1 1 d . . . O21 O 0.2408(3) 0.2669(3) 0.7561(2) 0.0227(9) Uani 1 1 d . . . O22 O -0.0781(4) 0.4814(4) 0.6536(2) 0.0368(11) Uani 1 1 d . . . H22D H -0.1107 0.4337 0.6628 0.055 Uiso 1 1 d R . . H22E H -0.1266 0.5297 0.6676 0.055 Uiso 1 1 d R . . O23 O 0.6004(9) 0.7380(8) 0.6670(6) 0.117(3) Uani 1 1 d G . . H23C H 0.5327 0.7711 0.6543 0.176 Uiso 1 1 d G . . H23D H 0.5902 0.6933 0.6964 0.176 Uiso 1 1 d G . . Na1 Na 0.3903(2) 0.08670(18) 0.78679(14) 0.0336(6) Uani 1 1 d . . . Mn1 Mn 0.10353(8) 0.22888(6) 0.79896(4) 0.0223(2) Uani 1 1 d . . . Mn2 Mn 0.27632(8) 0.25270(6) 0.66121(5) 0.0236(2) Uani 1 1 d . . . Mn3 Mn 0.32022(8) 0.31271(6) 0.82572(5) 0.0238(2) Uani 1 1 d . . . Tb1 Tb 0.11083(3) 0.45253(2) 0.709397(15) 0.02607(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(4) 0.036(4) 0.065(6) 0.016(4) 0.004(4) 0.005(3) C2 0.028(4) 0.046(4) 0.039(4) 0.011(3) 0.003(3) -0.005(3) C3 0.030(4) 0.053(5) 0.044(5) 0.024(4) -0.006(3) -0.002(3) C4 0.042(5) 0.078(6) 0.040(5) 0.021(4) -0.017(4) -0.014(4) C5 0.037(4) 0.071(6) 0.032(4) 0.016(4) -0.011(3) -0.019(4) C6 0.025(3) 0.054(5) 0.029(4) 0.012(3) -0.003(3) -0.015(3) C7 0.021(3) 0.041(4) 0.031(4) 0.013(3) 0.002(3) -0.010(3) C8 0.028(3) 0.047(4) 0.023(3) 0.001(3) -0.005(3) -0.015(3) C9 0.045(4) 0.039(4) 0.035(4) -0.013(3) -0.006(3) -0.011(3) C10 0.071(6) 0.085(7) 0.050(6) -0.033(5) -0.018(5) 0.004(5) C11 0.050(3) 0.050(3) 0.096(4) -0.013(3) 0.004(3) -0.028(2) C12 0.050(4) 0.039(4) 0.039(4) -0.009(3) -0.011(3) -0.012(3) C13 0.067(6) 0.035(5) 0.085(7) -0.014(5) 0.003(5) 0.003(4) C14 0.051(5) 0.026(4) 0.038(4) 0.001(3) -0.012(3) -0.010(3) C15 0.066(6) 0.028(4) 0.049(5) 0.004(3) -0.011(4) -0.011(4) C16 0.060(5) 0.034(4) 0.059(5) 0.009(4) -0.013(4) -0.024(4) C17 0.046(4) 0.052(5) 0.042(4) 0.009(4) -0.001(3) -0.023(4) C18 0.042(4) 0.032(4) 0.030(4) 0.003(3) 0.000(3) -0.016(3) C19 0.038(4) 0.032(4) 0.022(3) 0.001(3) -0.007(3) -0.009(3) C20 0.031(4) 0.052(5) 0.029(4) -0.001(3) 0.007(3) -0.019(3) C21 0.028(4) 0.043(4) 0.040(4) -0.006(3) 0.003(3) -0.004(3) C22 0.087(8) 0.124(11) 0.139(12) -0.099(10) -0.038(8) 0.062(8) C23 0.044(5) 0.049(5) 0.066(6) 0.006(4) 0.010(4) -0.006(4) C24 0.029(4) 0.058(5) 0.081(7) 0.016(5) -0.013(4) 0.004(4) C25 0.047(5) 0.106(8) 0.054(6) -0.002(5) 0.002(4) -0.041(5) C26 0.030(4) 0.037(4) 0.049(5) -0.008(3) 0.006(3) -0.010(3) C27 0.033(4) 0.036(4) 0.069(6) -0.014(4) 0.006(4) 0.000(3) C28 0.036(4) 0.044(5) 0.059(5) -0.022(4) 0.018(4) -0.006(4) C29 0.046(4) 0.046(5) 0.049(5) -0.019(4) 0.018(4) -0.017(4) C30 0.035(4) 0.032(4) 0.037(4) -0.007(3) 0.007(3) -0.012(3) C31 0.029(3) 0.027(3) 0.044(4) -0.009(3) 0.010(3) -0.009(3) C32 0.055(5) 0.036(4) 0.029(4) -0.008(3) 0.011(3) -0.025(4) C33 0.053(4) 0.030(4) 0.022(3) -0.002(3) -0.002(3) -0.010(3) C34 0.085(6) 0.047(5) 0.027(4) -0.009(3) -0.013(4) -0.013(4) C35 0.050(4) 0.032(4) 0.024(3) 0.006(3) 0.000(3) -0.005(3) C36 0.045(4) 0.031(4) 0.029(4) 0.000(3) -0.011(3) -0.009(3) C37 0.041(4) 0.031(4) 0.038(4) -0.002(3) 0.000(3) -0.002(3) C38 0.059(5) 0.031(4) 0.044(4) -0.003(3) -0.004(4) -0.017(4) C39 0.40(3) 0.26(2) 0.149(15) 0.143(16) -0.174(19) -0.30(3) C40 0.27(2) 0.078(9) 0.074(9) 0.009(7) 0.025(11) -0.090(11) C41 0.123(13) 0.034(7) 0.44(4) 0.048(12) 0.130(18) 0.004(7) C42 0.032(4) 0.022(3) 0.030(4) 0.001(3) -0.002(3) -0.004(3) C43 0.038(4) 0.048(4) 0.035(4) 0.012(3) 0.003(3) -0.014(3) C44 0.036(4) 0.059(5) 0.044(5) 0.000(4) 0.001(3) -0.003(4) C45 0.052(5) 0.048(5) 0.074(6) -0.003(4) 0.011(4) -0.029(4) C46 0.053(5) 0.069(6) 0.048(5) 0.015(4) 0.013(4) -0.020(5) C47 0.035(4) 0.031(4) 0.023(3) 0.003(3) -0.005(3) -0.012(3) C48 0.046(4) 0.045(4) 0.031(4) -0.016(3) 0.003(3) -0.022(3) C49 0.054(5) 0.042(4) 0.044(4) -0.010(3) -0.005(4) -0.021(4) C50 0.082(7) 0.062(6) 0.056(6) -0.030(5) 0.016(5) -0.037(5) C51 0.058(5) 0.050(5) 0.050(5) 0.002(4) -0.022(4) -0.026(4) C52 0.045(5) 0.030(4) 0.054(5) -0.003(3) -0.004(4) -0.005(3) C53 0.042(4) 0.041(5) 0.066(6) -0.018(4) 0.005(4) 0.002(4) C54 0.090(8) 0.053(6) 0.098(9) -0.036(6) 0.014(6) -0.014(5) C55 0.057(6) 0.071(7) 0.093(8) -0.026(6) 0.007(6) 0.006(5) C56 0.069(6) 0.081(7) 0.073(7) -0.048(6) 0.001(5) 0.005(5) N1 0.029(3) 0.037(3) 0.026(3) -0.001(2) -0.003(2) -0.012(2) N2 0.026(3) 0.036(3) 0.028(3) -0.005(2) 0.002(2) -0.010(2) N3 0.038(3) 0.029(3) 0.023(3) -0.003(2) 0.002(2) -0.010(2) N4 0.027(3) 0.029(3) 0.025(3) 0.002(2) -0.003(2) -0.010(2) N5 0.022(3) 0.032(3) 0.024(3) 0.002(3) -0.005(2) -0.002(2) N6 0.057(4) 0.043(4) 0.033(4) 0.014(3) -0.002(3) -0.005(3) O1 0.030(3) 0.034(3) 0.045(3) 0.013(2) 0.003(2) 0.004(2) O2 0.027(2) 0.032(2) 0.028(2) 0.0054(19) -0.0040(19) -0.0019(19) O3 0.029(2) 0.028(2) 0.026(2) -0.0034(18) -0.0040(18) -0.0018(19) O4 0.050(3) 0.050(3) 0.096(4) -0.013(3) 0.004(3) -0.028(2) O5 0.046(3) 0.027(3) 0.044(3) -0.003(2) 0.005(2) -0.003(2) O6 0.029(2) 0.023(2) 0.033(2) 0.0014(18) 0.0012(19) -0.0070(19) O7 0.026(2) 0.027(2) 0.022(2) 0.0018(18) -0.0017(17) 0.0005(18) O8 0.071(5) 0.085(5) 0.086(5) -0.004(4) 0.000(4) -0.011(4) O9 0.029(3) 0.042(3) 0.046(3) -0.003(2) 0.001(2) -0.003(2) O10 0.028(2) 0.031(2) 0.028(2) -0.0046(19) 0.0019(19) -0.0051(19) O11 0.030(2) 0.027(2) 0.020(2) 0.0013(17) -0.0072(18) -0.0049(18) O12 0.078(4) 0.040(3) 0.035(3) 0.000(2) -0.014(3) -0.010(3) O13 0.045(3) 0.028(2) 0.031(3) 0.000(2) -0.006(2) -0.010(2) O14 0.055(3) 0.033(3) 0.029(3) 0.002(2) -0.004(2) -0.014(2) O15 0.035(3) 0.026(2) 0.038(3) -0.003(2) 0.004(2) -0.007(2) O16 0.029(2) 0.035(3) 0.025(2) -0.0054(19) -0.0009(19) -0.005(2) O17 0.030(2) 0.029(2) 0.027(2) 0.0035(19) -0.0008(19) -0.0092(19) O18 0.028(2) 0.029(2) 0.026(2) 0.0041(18) -0.0017(18) -0.0072(19) O19 0.035(3) 0.031(3) 0.043(3) -0.005(2) -0.003(2) 0.000(2) O20 0.052(4) 0.060(4) 0.066(4) -0.022(3) -0.020(3) 0.011(3) O21 0.022(2) 0.028(2) 0.020(2) -0.0017(17) 0.0020(17) -0.0082(18) O22 0.037(3) 0.040(3) 0.031(3) 0.000(2) -0.008(2) -0.005(2) O23 0.101(7) 0.100(8) 0.137(10) -0.006(6) -0.008(6) 0.005(6) Na1 0.0303(14) 0.0288(14) 0.0373(15) 0.0036(11) 0.0039(11) -0.0022(11) Mn1 0.0222(5) 0.0228(5) 0.0207(5) 0.0008(4) 0.0006(4) -0.0048(4) Mn2 0.0253(5) 0.0241(5) 0.0202(5) 0.0001(4) 0.0014(4) -0.0046(4) Mn3 0.0236(5) 0.0258(5) 0.0208(5) 0.0021(4) -0.0037(4) -0.0050(4) Tb1 0.0307(2) 0.02495(19) 0.02149(18) 0.00013(12) -0.00368(12) -0.00476(13) _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 C1 O1 1.428(9) . ? C2 O1 1.364(9) . ? C2 C3 1.373(10) . ? C2 C7 1.420(10) . ? C3 C4 1.396(13) . ? C4 C5 1.359(12) . ? C5 C6 1.416(10) . ? C6 C7 1.413(10) . ? C6 C8 1.437(10) . ? C7 O2 1.324(8) . ? C8 N1 1.276(8) . ? C9 N1 1.493(9) . ? C9 C10 1.517(10) . ? C9 C12 1.532(10) . ? C9 C11 1.558(12) . ? C11 O4 1.554(11) . ? C12 O3 1.406(8) . ? C13 O5 1.433(9) . ? C14 O5 1.374(9) . ? C14 C15 1.377(10) . ? C14 C19 1.406(10) . ? C15 C16 1.405(12) . ? C16 C17 1.361(12) . ? C17 C18 1.420(10) . ? C18 C19 1.414(10) . ? C18 C20 1.449(10) . ? C19 O6 1.331(8) . ? C20 N2 1.292(9) . ? C21 N2 1.477(9) . ? C21 C24 1.490(11) . ? C21 C22 1.502(13) . ? C21 C23 1.598(11) . ? C23 O7 1.378(9) . ? C24 O8 1.369(10) . ? C25 O9 1.424(10) . ? C26 O9 1.364(9) . ? C26 C27 1.369(10) . ? C26 C31 1.417(10) . ? C27 C28 1.397(12) . ? C28 C29 1.353(12) . ? C29 C30 1.414(10) . ? C30 C31 1.411(10) . ? C30 C32 1.429(11) . ? C31 O10 1.336(8) . ? C32 N3 1.300(9) . ? C33 N3 1.490(9) . ? C33 C36 1.520(10) . ? C33 C34 1.525(9) . ? C33 C35 1.544(10) . ? C35 O12 1.413(9) . ? C36 O11 1.424(8) . ? C37 O13 1.265(9) . ? C37 O14 1.267(9) . ? C37 C38 1.515(10) . ? C38 C41 1.447(15) . ? C38 C39 1.457(15) . ? C38 C40 1.469(15) . ? C42 O17 1.253(8) . ? C42 O18 1.270(8) . ? C42 C43 1.534(9) . ? C43 C46 1.491(11) . ? C43 C44 1.519(11) . ? C43 C45 1.540(11) . ? C47 O16 1.262(8) . ? C47 O15 1.263(8) . ? C47 C48 1.528(9) . ? C48 C50 1.506(11) . ? C48 C49 1.527(11) . ? C48 C51 1.550(11) . ? C52 O20 1.263(9) . ? C52 O19 1.263(9) . ? C52 C53 1.531(11) . ? C53 C54 1.498(14) . ? C53 C56 1.523(13) . ? C53 C55 1.540(13) . ? N1 Mn3 2.017(5) . ? N2 Mn1 1.993(5) . ? N3 Mn2 2.027(5) . ? N4 N5 1.197(7) . ? N4 Mn3 2.256(5) . ? N4 Mn1 2.334(5) . ? N5 N6 1.152(8) . ? O1 Na1 2.428(6) . ? O2 Mn3 1.897(4) . ? O2 Na1 2.341(5) . ? O3 Mn3 1.881(4) . ? O3 Tb1 2.298(4) . ? O5 Na1 2.420(6) . ? O6 Mn1 1.908(4) . ? O6 Na1 2.321(5) . ? O7 Mn1 1.882(4) . ? O7 Tb1 2.379(4) . ? O9 Na1 2.550(5) . ? O10 Mn2 1.891(4) . ? O10 Na1 2.412(5) . ? O11 Mn2 1.882(4) . ? O11 Tb1 2.291(4) . ? O13 Tb1 2.455(5) . ? O14 Tb1 2.445(5) . ? O15 Mn2 2.143(5) . ? O16 Mn1 2.151(4) . ? O17 Mn2 2.350(4) . ? O17 Tb1 2.750(4) . ? O18 Mn3 2.195(4) . ? O19 Tb1 2.326(5) . ? O21 Mn1 1.911(4) . ? O21 Mn2 1.927(4) . ? O21 Mn3 1.957(4) . ? O21 Na1 2.843(5) . ? O21 Tb1 2.882(4) . ? O22 Tb1 2.407(5) . ? Na1 Mn2 3.358(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C2 C3 124.3(7) . . ? O1 C2 C7 114.2(6) . . ? C3 C2 C7 121.5(8) . . ? C2 C3 C4 119.2(8) . . ? C5 C4 C3 121.3(7) . . ? C4 C5 C6 120.6(8) . . ? C7 C6 C5 119.1(7) . . ? C7 C6 C8 123.3(6) . . ? C5 C6 C8 117.7(7) . . ? O2 C7 C6 124.2(6) . . ? O2 C7 C2 117.8(7) . . ? C6 C7 C2 118.1(6) . . ? N1 C8 C6 125.8(6) . . ? N1 C9 C10 114.5(7) . . ? N1 C9 C12 103.9(5) . . ? C10 C9 C12 110.5(7) . . ? N1 C9 C11 106.6(6) . . ? C10 C9 C11 111.7(7) . . ? C12 C9 C11 109.3(7) . . ? O4 C11 C9 104.4(7) . . ? O3 C12 C9 109.0(6) . . ? O5 C14 C15 124.8(7) . . ? O5 C14 C19 114.1(6) . . ? C15 C14 C19 121.1(7) . . ? C14 C15 C16 120.2(7) . . ? C17 C16 C15 119.5(7) . . ? C16 C17 C18 121.6(7) . . ? C19 C18 C17 118.6(7) . . ? C19 C18 C20 122.8(6) . . ? C17 C18 C20 118.4(7) . . ? O6 C19 C14 118.0(6) . . ? O6 C19 C18 123.3(6) . . ? C14 C19 C18 118.7(6) . . ? N2 C20 C18 125.3(6) . . ? N2 C21 C24 109.7(6) . . ? N2 C21 C22 110.7(7) . . ? C24 C21 C22 114.2(8) . . ? N2 C21 C23 103.5(6) . . ? C24 C21 C23 102.8(7) . . ? C22 C21 C23 115.2(10) . . ? O7 C23 C21 109.5(6) . . ? O8 C24 C21 112.4(8) . . ? O9 C26 C27 121.0(7) . . ? O9 C26 C31 118.4(6) . . ? C27 C26 C31 120.6(7) . . ? C26 C27 C28 120.8(7) . . ? C29 C28 C27 119.3(7) . . ? C28 C29 C30 122.3(8) . . ? C31 C30 C29 118.1(7) . . ? C31 C30 C32 123.5(6) . . ? C29 C30 C32 118.2(7) . . ? O10 C31 C30 124.4(6) . . ? O10 C31 C26 116.8(6) . . ? C30 C31 C26 118.8(6) . . ? N3 C32 C30 125.3(6) . . ? N3 C33 C36 104.7(5) . . ? N3 C33 C34 114.3(6) . . ? C36 C33 C34 110.5(6) . . ? N3 C33 C35 105.9(6) . . ? C36 C33 C35 110.1(6) . . ? C34 C33 C35 111.0(6) . . ? O12 C35 C33 113.2(6) . . ? O11 C36 C33 109.7(5) . . ? O13 C37 O14 119.5(7) . . ? O13 C37 C38 121.4(7) . . ? O14 C37 C38 119.0(7) . . ? C41 C38 C39 110.7(16) . . ? C41 C38 C40 104.9(14) . . ? C39 C38 C40 110.5(13) . . ? C41 C38 C37 107.6(8) . . ? C39 C38 C37 111.7(8) . . ? C40 C38 C37 111.1(7) . . ? O17 C42 O18 123.9(6) . . ? O17 C42 C43 119.6(6) . . ? O18 C42 C43 116.5(6) . . ? C46 C43 C44 109.8(7) . . ? C46 C43 C42 111.1(6) . . ? C44 C43 C42 109.5(6) . . ? C46 C43 C45 109.8(7) . . ? C44 C43 C45 109.0(7) . . ? C42 C43 C45 107.5(6) . . ? O16 C47 O15 124.1(6) . . ? O16 C47 C48 117.5(6) . . ? O15 C47 C48 118.4(6) . . ? C50 C48 C49 111.2(7) . . ? C50 C48 C47 111.3(6) . . ? C49 C48 C47 108.3(6) . . ? C50 C48 C51 109.8(7) . . ? C49 C48 C51 108.9(6) . . ? C47 C48 C51 107.3(6) . . ? O20 C52 O19 123.7(7) . . ? O20 C52 C53 117.9(7) . . ? O19 C52 C53 118.5(7) . . ? C54 C53 C56 108.7(9) . . ? C54 C53 C52 106.4(8) . . ? C56 C53 C52 111.1(7) . . ? C54 C53 C55 112.8(8) . . ? C56 C53 C55 107.7(8) . . ? C52 C53 C55 110.3(7) . . ? C8 N1 C9 121.3(6) . . ? C8 N1 Mn3 125.8(5) . . ? C9 N1 Mn3 112.9(4) . . ? C20 N2 C21 122.2(6) . . ? C20 N2 Mn1 125.2(5) . . ? C21 N2 Mn1 112.5(4) . . ? C32 N3 C33 122.1(6) . . ? C32 N3 Mn2 125.1(5) . . ? C33 N3 Mn2 112.8(4) . . ? N5 N4 Mn3 128.3(4) . . ? N5 N4 Mn1 118.6(4) . . ? Mn3 N4 Mn1 85.35(18) . . ? N6 N5 N4 177.7(7) . . ? C2 O1 C1 115.9(6) . . ? C2 O1 Na1 119.4(4) . . ? C1 O1 Na1 123.2(5) . . ? C7 O2 Mn3 129.1(4) . . ? C7 O2 Na1 122.4(4) . . ? Mn3 O2 Na1 108.3(2) . . ? C12 O3 Mn3 114.0(4) . . ? C12 O3 Tb1 127.8(4) . . ? Mn3 O3 Tb1 114.9(2) . . ? C14 O5 C13 117.2(6) . . ? C14 O5 Na1 117.8(4) . . ? C13 O5 Na1 124.8(5) . . ? C19 O6 Mn1 125.8(4) . . ? C19 O6 Na1 121.2(4) . . ? Mn1 O6 Na1 111.1(2) . . ? C23 O7 Mn1 112.6(4) . . ? C23 O7 Tb1 129.2(4) . . ? Mn1 O7 Tb1 113.58(19) . . ? C26 O9 C25 112.0(6) . . ? C26 O9 Na1 109.0(4) . . ? C25 O9 Na1 103.5(5) . . ? C31 O10 Mn2 127.5(4) . . ? C31 O10 Na1 114.7(4) . . ? Mn2 O10 Na1 101.93(19) . . ? C36 O11 Mn2 113.0(4) . . ? C36 O11 Tb1 137.8(4) . . ? Mn2 O11 Tb1 106.82(18) . . ? C37 O13 Tb1 93.4(4) . . ? C37 O14 Tb1 93.9(4) . . ? C47 O15 Mn2 124.9(4) . . ? C47 O16 Mn1 124.4(4) . . ? C42 O17 Mn2 116.2(4) . . ? C42 O17 Tb1 133.4(4) . . ? Mn2 O17 Tb1 82.00(13) . . ? C42 O18 Mn3 121.2(4) . . ? C52 O19 Tb1 141.8(5) . . ? Mn1 O21 Mn2 119.4(2) . . ? Mn1 O21 Mn3 107.13(19) . . ? Mn2 O21 Mn3 133.5(2) . . ? Mn1 O21 Na1 92.57(16) . . ? Mn2 O21 Na1 87.28(15) . . ? Mn3 O21 Na1 89.75(16) . . ? Mn1 O21 Tb1 94.28(15) . . ? Mn2 O21 Tb1 86.23(14) . . ? Mn3 O21 Tb1 91.67(15) . . ? Na1 O21 Tb1 172.26(16) . . ? O6 Na1 O2 91.71(18) . . ? O6 Na1 O10 116.27(18) . . ? O2 Na1 O10 97.59(18) . . ? O6 Na1 O5 66.31(17) . . ? O2 Na1 O5 139.9(2) . . ? O10 Na1 O5 122.0(2) . . ? O6 Na1 O1 109.79(19) . . ? O2 Na1 O1 66.00(18) . . ? O10 Na1 O1 131.51(19) . . ? O5 Na1 O1 89.44(19) . . ? O6 Na1 O9 164.1(2) . . ? O2 Na1 O9 103.92(19) . . ? O10 Na1 O9 64.97(17) . . ? O5 Na1 O9 99.15(19) . . ? O1 Na1 O9 74.98(18) . . ? O6 Na1 O21 63.70(14) . . ? O2 Na1 O21 66.11(15) . . ? O10 Na1 O21 63.60(14) . . ? O5 Na1 O21 123.38(18) . . ? O1 Na1 O21 131.33(18) . . ? O9 Na1 O21 125.20(17) . . ? O6 Na1 Mn2 83.52(13) . . ? O2 Na1 Mn2 92.62(13) . . ? O10 Na1 Mn2 33.43(11) . . ? O5 Na1 Mn2 116.11(16) . . ? O1 Na1 Mn2 154.42(16) . . ? O9 Na1 Mn2 98.29(14) . . ? O21 Na1 Mn2 34.98(8) . . ? O7 Mn1 O6 176.23(19) . . ? O7 Mn1 O21 90.72(18) . . ? O6 Mn1 O21 92.58(18) . . ? O7 Mn1 N2 84.4(2) . . ? O6 Mn1 N2 92.0(2) . . ? O21 Mn1 N2 170.2(2) . . ? O7 Mn1 O16 92.93(18) . . ? O6 Mn1 O16 88.11(18) . . ? O21 Mn1 O16 102.56(17) . . ? N2 Mn1 O16 86.3(2) . . ? O7 Mn1 N4 88.96(19) . . ? O6 Mn1 N4 89.64(19) . . ? O21 Mn1 N4 83.20(18) . . ? N2 Mn1 N4 88.1(2) . . ? O16 Mn1 N4 173.90(18) . . ? O11 Mn2 O10 172.31(19) . . ? O11 Mn2 O21 91.27(18) . . ? O10 Mn2 O21 94.04(18) . . ? O11 Mn2 N3 82.5(2) . . ? O10 Mn2 N3 91.8(2) . . ? O21 Mn2 N3 172.6(2) . . ? O11 Mn2 O15 94.86(18) . . ? O10 Mn2 O15 89.94(19) . . ? O21 Mn2 O15 97.71(17) . . ? N3 Mn2 O15 86.8(2) . . ? O11 Mn2 O17 79.92(17) . . ? O10 Mn2 O17 95.44(18) . . ? O21 Mn2 O17 80.67(16) . . ? N3 Mn2 O17 94.29(19) . . ? O15 Mn2 O17 174.46(17) . . ? O11 Mn2 Na1 142.82(14) . . ? O10 Mn2 Na1 44.64(14) . . ? O21 Mn2 Na1 57.74(13) . . ? N3 Mn2 Na1 129.53(17) . . ? O15 Mn2 Na1 72.10(14) . . ? O17 Mn2 Na1 111.01(12) . . ? O3 Mn3 O2 173.61(19) . . ? O3 Mn3 O21 90.28(18) . . ? O2 Mn3 O21 95.72(19) . . ? O3 Mn3 N1 82.1(2) . . ? O2 Mn3 N1 91.7(2) . . ? O21 Mn3 N1 170.9(2) . . ? O3 Mn3 O18 92.44(18) . . ? O2 Mn3 O18 89.34(18) . . ? O21 Mn3 O18 93.78(16) . . ? N1 Mn3 O18 91.53(19) . . ? O3 Mn3 N4 89.5(2) . . ? O2 Mn3 N4 88.9(2) . . ? O21 Mn3 N4 84.29(18) . . ? N1 Mn3 N4 90.6(2) . . ? O18 Mn3 N4 177.28(18) . . ? O11 Tb1 O3 122.38(15) . . ? O11 Tb1 O19 148.49(16) . . ? O3 Tb1 O19 82.75(16) . . ? O11 Tb1 O7 84.89(15) . . ? O3 Tb1 O7 81.44(15) . . ? O19 Tb1 O7 80.29(16) . . ? O11 Tb1 O22 75.36(16) . . ? O3 Tb1 O22 151.90(16) . . ? O19 Tb1 O22 74.54(17) . . ? O7 Tb1 O22 78.64(16) . . ? O11 Tb1 O14 125.82(16) . . ? O3 Tb1 O14 73.72(16) . . ? O19 Tb1 O14 76.49(17) . . ? O7 Tb1 O14 147.73(15) . . ? O22 Tb1 O14 115.54(17) . . ? O11 Tb1 O13 84.13(15) . . ? O3 Tb1 O13 124.65(16) . . ? O19 Tb1 O13 97.01(17) . . ? O7 Tb1 O13 153.46(15) . . ? O22 Tb1 O13 75.23(16) . . ? O14 Tb1 O13 53.03(15) . . ? O11 Tb1 O17 65.16(14) . . ? O3 Tb1 O17 74.48(14) . . ? O19 Tb1 O17 145.82(15) . . ? O7 Tb1 O17 120.01(13) . . ? O22 Tb1 O17 133.04(15) . . ? O14 Tb1 O17 72.88(15) . . ? O13 Tb1 O17 76.39(14) . . ? O11 Tb1 O21 62.30(13) . . ? O3 Tb1 O21 62.18(13) . . ? O19 Tb1 O21 129.70(15) . . ? O7 Tb1 O21 60.85(13) . . ? O22 Tb1 O21 122.08(14) . . ? O14 Tb1 O21 120.87(14) . . ? O13 Tb1 O21 132.07(14) . . ? O17 Tb1 O21 59.27(12) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 3.158 _refine_diff_density_min -3.852 _refine_diff_density_rms 0.145 _database_code_depnum_ccdc_archive 'CCDC 947812' ####################################################################### # # 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_Mn3GdNa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H83 Gd Mn3 N6 Na O22, H2 O ' _chemical_formula_sum 'C56 H85 Gd Mn3 N6 Na O23' _chemical_formula_weight 1555.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.405(5) _cell_length_b 14.776(5) _cell_length_c 19.775(5) _cell_angle_alpha 82.630(5) _cell_angle_beta 86.886(5) _cell_angle_gamma 76.901(5) _cell_volume 3218(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1740 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 19.45 _exptl_crystal_description block-shaped _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1594 _exptl_absorpt_coefficient_mu 1.681 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.712835 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _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 16931 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.1315 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 25.02 _reflns_number_total 11163 _reflns_number_gt 6754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1507P)^2^+6.9533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11163 _refine_ls_number_parameters 800 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1473 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.2829 _refine_ls_wR_factor_gt 0.2420 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.066 _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 C1 C -0.0886(15) 0.5742(11) 0.6116(10) 0.072(5) Uani 1 1 d . . . H1A H -0.0777 0.6027 0.5659 0.108 Uiso 1 1 calc R . . H1B H -0.0599 0.6078 0.6433 0.108 Uiso 1 1 calc R . . H1C H -0.1726 0.5761 0.6207 0.108 Uiso 1 1 calc R . . C2 C -0.0500(13) 0.4214(11) 0.5771(8) 0.051(4) Uani 1 1 d . . . C3 C -0.1361(14) 0.4503(12) 0.5254(8) 0.057(4) Uani 1 1 d . . . H3 H -0.1793 0.5120 0.5184 0.068 Uiso 1 1 calc R . . C4 C -0.1543(14) 0.3866(14) 0.4864(8) 0.065(5) Uani 1 1 d . . . H4 H -0.2106 0.4062 0.4523 0.078 Uiso 1 1 calc R . . C5 C -0.0948(15) 0.2951(12) 0.4942(7) 0.056(4) Uani 1 1 d . . . H5 H -0.1098 0.2540 0.4655 0.067 Uiso 1 1 calc R . . C6 C -0.0095(12) 0.2632(11) 0.5465(6) 0.045(4) Uani 1 1 d . . . C7 C 0.0087(11) 0.3262(9) 0.5903(7) 0.040(3) Uani 1 1 d . . . C8 C 0.0485(12) 0.1659(10) 0.5553(7) 0.042(3) Uani 1 1 d . . . H8 H 0.0288 0.1290 0.5248 0.050 Uiso 1 1 calc R . . C9 C 0.1780(12) 0.0222(10) 0.6026(7) 0.0499(12) Uani 1 1 d D . . C10 C 0.2956(16) 0.0099(11) 0.6397(8) 0.061(4) Uani 1 1 d . . . H10A H 0.3238 -0.0554 0.6575 0.073 Uiso 1 1 calc R . . H10B H 0.3566 0.0278 0.6080 0.073 Uiso 1 1 calc R . . C11 C 0.197(2) -0.0171(16) 0.5361(11) 0.114(9) Uani 1 1 d . . . H11A H 0.2271 0.0256 0.5026 0.172 Uiso 1 1 calc R . . H11B H 0.1219 -0.0261 0.5216 0.172 Uiso 1 1 calc R . . H11C H 0.2542 -0.0760 0.5413 0.172 Uiso 1 1 calc R . . C12 C 0.0652(12) -0.0155(10) 0.6377(7) 0.0499(12) Uani 1 1 d DU . . H12A H 0.0171 0.0260 0.6680 0.060 Uiso 1 1 calc R . . H12B H 0.0147 -0.0315 0.6053 0.060 Uiso 1 1 calc R . . C13 C 0.1152(17) 0.6411(12) 0.7282(10) 0.078(5) Uani 1 1 d . . . H13A H 0.1637 0.6617 0.7586 0.117 Uiso 1 1 calc R . . H13B H 0.0431 0.6301 0.7519 0.117 Uiso 1 1 calc R . . H13C H 0.0943 0.6884 0.6901 0.117 Uiso 1 1 calc R . . C14 C 0.2900(14) 0.5570(10) 0.6696(7) 0.047(4) Uani 1 1 d . . . C15 C 0.3302(17) 0.6386(10) 0.6479(7) 0.059(4) Uani 1 1 d . . . H15 H 0.2851 0.6968 0.6570 0.071 Uiso 1 1 calc R . . C16 C 0.4397(16) 0.6301(12) 0.6125(8) 0.062(4) Uani 1 1 d . . . H16 H 0.4690 0.6834 0.5979 0.074 Uiso 1 1 calc R . . C17 C 0.5032(14) 0.5471(11) 0.5989(8) 0.053(4) Uani 1 1 d . . . H17 H 0.5733 0.5442 0.5722 0.064 Uiso 1 1 calc R . . C18 C 0.4679(13) 0.4635(10) 0.6236(7) 0.043(3) Uani 1 1 d . . . C19 C 0.3554(13) 0.4687(10) 0.6573(6) 0.042(3) Uani 1 1 d . . . C20 C 0.5491(13) 0.3752(9) 0.6151(7) 0.043(3) Uani 1 1 d . . . H20 H 0.6148 0.3768 0.5854 0.052 Uiso 1 1 calc R . . C21 C 0.6356(13) 0.2084(10) 0.6416(7) 0.0499(12) Uani 1 1 d . . . C22 C 0.6332(13) 0.1772(10) 0.5680(7) 0.0499(12) Uani 1 1 d U . . H22A H 0.5775 0.1372 0.5684 0.075 Uiso 1 1 calc R . . H22B H 0.7122 0.1439 0.5554 0.075 Uiso 1 1 calc R . . H22C H 0.6085 0.2316 0.5355 0.075 Uiso 1 1 calc R . . C23 C 0.6134(13) 0.1391(10) 0.7117(7) 0.052(4) Uani 1 1 d U . . H23A H 0.6528 0.0747 0.7069 0.063 Uiso 1 1 calc R . . H23B H 0.6461 0.1577 0.7507 0.063 Uiso 1 1 calc R . . C24 C 0.7491(13) 0.2302(10) 0.6595(7) 0.0499(12) Uani 1 1 d . . . H24A H 0.7726 0.2744 0.6237 0.060 Uiso 1 1 calc R . . H24B H 0.7364 0.2596 0.7013 0.060 Uiso 1 1 calc R . . C25 C -0.1737(15) 0.4141(13) 0.7428(9) 0.070(5) Uani 1 1 d . . . H25A H -0.1268 0.3520 0.7398 0.104 Uiso 1 1 calc R . . H25B H -0.2035 0.4416 0.6986 0.104 Uiso 1 1 calc R . . H25C H -0.2403 0.4116 0.7743 0.104 Uiso 1 1 calc R . . C26 C -0.0890(12) 0.4554(10) 0.8356(7) 0.044(3) Uani 1 1 d . . . C27 C -0.1653(15) 0.5122(12) 0.8761(9) 0.063(4) Uani 1 1 d . . . H27 H -0.2227 0.5618 0.8556 0.076 Uiso 1 1 calc R . . C28 C -0.1599(15) 0.4984(11) 0.9471(9) 0.062(4) Uani 1 1 d . . . H28 H -0.2128 0.5374 0.9739 0.074 Uiso 1 1 calc R . . C29 C -0.0730(15) 0.4243(11) 0.9761(8) 0.057(4) Uani 1 1 d . . . H29 H -0.0699 0.4118 1.0233 0.068 Uiso 1 1 calc R . . C30 C 0.0102(12) 0.3680(9) 0.9358(7) 0.038(3) Uani 1 1 d . . . C31 C 0.0013(11) 0.3816(8) 0.8644(7) 0.035(3) Uani 1 1 d . . . C32 C 0.1012(14) 0.2994(10) 0.9697(7) 0.049(4) Uani 1 1 d . . . H32 H 0.0960 0.2910 1.0171 0.058 Uiso 1 1 calc R . . C33 C 0.2890(14) 0.1771(9) 0.9814(7) 0.046(3) Uani 1 1 d . . . C34 C 0.3196(18) 0.2102(11) 1.0475(7) 0.070(5) Uani 1 1 d . . . H34A H 0.3834 0.1638 1.0697 0.104 Uiso 1 1 calc R . . H34B H 0.2497 0.2191 1.0773 0.104 Uiso 1 1 calc R . . H34C H 0.3449 0.2682 1.0369 0.104 Uiso 1 1 calc R . . C35 C 0.2455(13) 0.0856(9) 0.9949(7) 0.051(4) Uani 1 1 d . . . H35A H 0.1805 0.0925 1.0288 0.061 Uiso 1 1 calc R . . H35B H 0.2138 0.0736 0.9532 0.061 Uiso 1 1 calc R . . C36 C 0.3975(13) 0.1668(10) 0.9327(7) 0.047(3) Uani 1 1 d . . . H36A H 0.4328 0.2210 0.9313 0.056 Uiso 1 1 calc R . . H36B H 0.4577 0.1117 0.9489 0.056 Uiso 1 1 calc R . . C37 C 0.3167(13) -0.1112(10) 0.8642(7) 0.047(3) Uani 1 1 d . . . C38 C 0.197(4) -0.231(2) 0.8635(15) 0.242(12) Uani 1 1 d U . . H38A H 0.2055 -0.2977 0.8746 0.363 Uiso 1 1 calc R . . H38B H 0.2096 -0.2171 0.8152 0.363 Uiso 1 1 calc R . . H38C H 0.1177 -0.1997 0.8766 0.363 Uiso 1 1 calc R . . C39 C 0.2847(16) -0.2011(10) 0.8994(9) 0.062(4) Uani 1 1 d . . . C40 C 0.252(3) -0.1929(17) 0.9723(11) 0.151(13) Uani 1 1 d . . . H40A H 0.1735 -0.1532 0.9761 0.227 Uiso 1 1 calc R . . H40B H 0.3100 -0.1664 0.9920 0.227 Uiso 1 1 calc R . . H40C H 0.2524 -0.2538 0.9961 0.227 Uiso 1 1 calc R . . C41 C 0.401(3) -0.2714(15) 0.9010(17) 0.156(10) Uani 1 1 d U . . H41A H 0.3859 -0.3330 0.9120 0.234 Uiso 1 1 calc R . . H41B H 0.4508 -0.2597 0.9350 0.234 Uiso 1 1 calc R . . H41C H 0.4410 -0.2669 0.8572 0.234 Uiso 1 1 calc R . . C42 C 0.0574(12) 0.1189(8) 0.8062(7) 0.035(3) Uani 1 1 d . . . C43 C -0.0480(12) 0.0910(10) 0.8475(7) 0.047(4) Uani 1 1 d . . . C44 C -0.1556(16) 0.1685(13) 0.8462(9) 0.075(5) Uani 1 1 d . . . H44A H -0.1377 0.2192 0.8666 0.113 Uiso 1 1 calc R . . H44B H -0.2206 0.1471 0.8713 0.113 Uiso 1 1 calc R . . H44C H -0.1784 0.1896 0.7999 0.113 Uiso 1 1 calc R . . C45 C -0.0790(19) 0.0104(15) 0.8149(10) 0.089(6) Uani 1 1 d . . . H45A H -0.1365 -0.0159 0.8436 0.134 Uiso 1 1 calc R . . H45B H -0.0072 -0.0371 0.8097 0.134 Uiso 1 1 calc R . . H45C H -0.1126 0.0340 0.7709 0.134 Uiso 1 1 calc R . . C46 C -0.0117(19) 0.0552(16) 0.9205(9) 0.094(7) Uani 1 1 d . . . H46A H 0.0043 0.1054 0.9423 0.142 Uiso 1 1 calc R . . H46B H 0.0594 0.0058 0.9206 0.142 Uiso 1 1 calc R . . H46C H -0.0759 0.0317 0.9448 0.142 Uiso 1 1 calc R . . C47 C 0.4098(13) 0.3678(9) 0.8288(6) 0.040(3) Uani 1 1 d . . . C48 C 0.4703(13) 0.4276(11) 0.8623(7) 0.048(4) Uani 1 1 d . . . C49 C 0.3974(18) 0.4620(13) 0.9248(9) 0.077(6) Uani 1 1 d . . . H49A H 0.3220 0.5020 0.9107 0.115 Uiso 1 1 calc R . . H49B H 0.4418 0.4962 0.9480 0.115 Uiso 1 1 calc R . . H49C H 0.3828 0.4093 0.9551 0.115 Uiso 1 1 calc R . . C50 C 0.4878(15) 0.5095(10) 0.8119(8) 0.058(4) Uani 1 1 d . . . H50A H 0.5264 0.4870 0.7710 0.087 Uiso 1 1 calc R . . H50B H 0.5372 0.5435 0.8314 0.087 Uiso 1 1 calc R . . H50C H 0.4109 0.5500 0.8011 0.087 Uiso 1 1 calc R . . C51 C 0.5921(15) 0.3688(12) 0.8872(8) 0.068(5) Uani 1 1 d . . . H51A H 0.5801 0.3142 0.9162 0.102 Uiso 1 1 calc R . . H51B H 0.6301 0.4053 0.9123 0.102 Uiso 1 1 calc R . . H51C H 0.6425 0.3501 0.8487 0.102 Uiso 1 1 calc R . . C52 C 0.6226(15) -0.1126(10) 0.7340(9) 0.055(4) Uani 1 1 d . . . C53 C 0.6665(15) -0.1760(12) 0.6782(10) 0.068(5) Uani 1 1 d . . . C54 C 0.653(3) -0.2720(14) 0.7089(13) 0.117(9) Uani 1 1 d . . . H54A H 0.5724 -0.2687 0.7262 0.175 Uiso 1 1 calc R . . H54B H 0.7085 -0.2944 0.7454 0.175 Uiso 1 1 calc R . . H54C H 0.6708 -0.3139 0.6745 0.175 Uiso 1 1 calc R . . C55 C 0.7983(18) -0.1729(15) 0.6556(12) 0.101(7) Uani 1 1 d . . . H55A H 0.8491 -0.1913 0.6944 0.151 Uiso 1 1 calc R . . H55B H 0.8016 -0.1104 0.6364 0.151 Uiso 1 1 calc R . . H55C H 0.8255 -0.2150 0.6220 0.151 Uiso 1 1 calc R . . C56 C 0.585(2) -0.1471(16) 0.6177(11) 0.104(8) Uani 1 1 d . . . H56A H 0.6169 -0.1850 0.5821 0.156 Uiso 1 1 calc R . . H56B H 0.5818 -0.0825 0.6014 0.156 Uiso 1 1 calc R . . H56C H 0.5061 -0.1554 0.6312 0.156 Uiso 1 1 calc R . . N1 N 0.1235(10) 0.1250(8) 0.6001(5) 0.042(3) Uani 1 1 d . . . N2 N 0.5391(9) 0.2943(8) 0.6449(5) 0.039(3) Uani 1 1 d . . . N3 N 0.1926(11) 0.2464(7) 0.9405(5) 0.041(3) Uani 1 1 d . . . N4 N 0.3273(9) 0.2256(7) 0.6043(5) 0.035(2) Uani 1 1 d . . . N5 N 0.3186(9) 0.2784(7) 0.5526(5) 0.035(2) Uani 1 1 d . . . N6 N 0.3145(11) 0.3275(9) 0.5032(6) 0.053(3) Uani 1 1 d . . . O1 O -0.0225(8) 0.4789(7) 0.6187(5) 0.049(2) Uani 1 1 d . . . O2 O 0.0774(8) 0.3039(6) 0.6439(4) 0.040(2) Uani 1 1 d . . . O3 O 0.2770(8) 0.0662(6) 0.6942(4) 0.039(2) Uani 1 1 d . . . O4 O 0.1404(9) -0.0925(7) 0.6717(5) 0.0499(12) Uani 1 1 d . . . H4A H 0.1098 -0.1379 0.6738 0.075 Uiso 1 1 calc R . . O5 O 0.1814(9) 0.5564(6) 0.7043(5) 0.047(2) Uani 1 1 d . . . O6 O 0.3094(8) 0.3949(6) 0.6764(4) 0.039(2) Uani 1 1 d . . . O7 O 0.4923(7) 0.1475(6) 0.7206(4) 0.036(2) Uani 1 1 d . . . O8 O 0.8416(9) 0.1502(7) 0.6685(5) 0.0499(12) Uani 1 1 d . . . H8A H 0.8429 0.1193 0.6368 0.075 Uiso 1 1 calc R . . O9 O -0.0994(8) 0.4702(6) 0.7663(5) 0.049(2) Uani 1 1 d . . . O10 O 0.0713(7) 0.3294(6) 0.8216(4) 0.037(2) Uani 1 1 d . . . O11 O 0.3627(8) 0.1586(6) 0.8659(4) 0.037(2) Uani 1 1 d . . . O12 O 0.3386(13) 0.0073(8) 1.0182(6) 0.080(4) Uani 1 1 d . . . H12 H 0.3456 -0.0331 0.9925 0.120 Uiso 1 1 calc R . . O13 O 0.3681(9) -0.0634(6) 0.8945(4) 0.044(2) Uani 1 1 d . . . O14 O 0.2884(9) -0.0871(6) 0.8018(5) 0.049(2) Uani 1 1 d . . . O15 O 0.1579(8) 0.1082(6) 0.8339(4) 0.038(2) Uani 1 1 d . . . O16 O 0.0359(7) 0.1530(6) 0.7449(4) 0.038(2) Uani 1 1 d . . . O17 O 0.4708(8) 0.3209(6) 0.7839(4) 0.039(2) Uani 1 1 d . . . O18 O 0.3013(8) 0.3648(6) 0.8431(5) 0.044(2) Uani 1 1 d . . . O19 O 0.6999(11) -0.1130(8) 0.7804(7) 0.077(4) Uani 1 1 d . . . O20 O 0.5197(9) -0.0620(7) 0.7333(5) 0.051(2) Uani 1 1 d . . . O21 O 0.2604(7) 0.2305(5) 0.7447(4) 0.0322(19) Uani 1 1 d . . . O22 O 0.5803(8) 0.0194(7) 0.8474(4) 0.047(2) Uani 1 1 d . . . H22D H 0.6064 -0.0391 0.8582 0.071 Uiso 1 1 d R . . H22E H 0.6306 0.0407 0.8202 0.071 Uiso 1 1 d R . . O23 O 0.905(3) 0.7640(17) 0.8318(15) 0.191(10) Uani 1 1 d G . . H23C H 0.8849 0.7228 0.8615 0.287 Uiso 1 1 d G . . H23D H 0.9453 0.7375 0.7995 0.287 Uiso 1 1 d G . . Na1 Na 0.1075(4) 0.4129(4) 0.7127(3) 0.0420(12) Uani 1 1 d . . . Gd1 Gd 0.38721(6) 0.04662(4) 0.79175(3) 0.0356(2) Uani 1 1 d . . . Mn1 Mn 0.17940(17) 0.18593(13) 0.67404(9) 0.0326(5) Uani 1 1 d . . . Mn2 Mn 0.39664(17) 0.27028(13) 0.70135(9) 0.0316(5) Uani 1 1 d . . . Mn3 Mn 0.22255(17) 0.24769(13) 0.83924(9) 0.0337(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.056(11) 0.047(9) 0.098(14) 0.016(9) 0.013(9) 0.003(8) C2 0.038(8) 0.052(9) 0.053(9) 0.019(7) -0.003(7) -0.004(7) C3 0.044(9) 0.062(10) 0.054(10) 0.024(8) -0.012(7) -0.007(8) C4 0.041(9) 0.113(15) 0.039(9) 0.022(10) -0.021(7) -0.024(10) C5 0.065(11) 0.062(10) 0.040(8) 0.007(7) -0.009(7) -0.015(9) C6 0.034(8) 0.074(10) 0.029(7) 0.011(7) -0.004(6) -0.027(7) C7 0.030(7) 0.042(8) 0.042(8) 0.009(6) -0.002(6) -0.005(6) C8 0.035(8) 0.058(9) 0.035(7) -0.003(6) -0.012(6) -0.016(7) C9 0.0516(19) 0.0554(19) 0.0376(18) -0.0176(15) -0.0050(15) 0.0063(15) C10 0.082(12) 0.053(9) 0.049(9) -0.012(8) -0.022(8) -0.009(9) C11 0.13(2) 0.098(16) 0.095(16) -0.059(14) -0.039(15) 0.043(15) C12 0.0516(19) 0.0554(19) 0.0376(18) -0.0176(15) -0.0050(15) 0.0063(15) C13 0.082(13) 0.054(10) 0.092(14) -0.017(10) -0.005(11) 0.001(10) C14 0.057(10) 0.041(8) 0.042(8) 0.007(6) -0.007(7) -0.016(7) C15 0.090(13) 0.040(8) 0.043(9) 0.003(7) -0.014(9) -0.007(8) C16 0.074(12) 0.055(10) 0.064(11) 0.005(8) -0.006(9) -0.035(10) C17 0.043(9) 0.054(10) 0.063(10) 0.012(8) -0.001(7) -0.022(8) C18 0.047(9) 0.049(8) 0.037(8) 0.003(6) -0.010(6) -0.024(7) C19 0.051(9) 0.048(8) 0.029(7) 0.007(6) -0.011(6) -0.019(7) C20 0.048(9) 0.047(8) 0.038(8) 0.007(6) -0.002(6) -0.022(7) C21 0.0516(19) 0.0554(19) 0.0376(18) -0.0176(15) -0.0050(15) 0.0063(15) C22 0.0516(19) 0.0554(19) 0.0376(18) -0.0176(15) -0.0050(15) 0.0063(15) C23 0.050(4) 0.050(4) 0.050(4) 0.000(2) 0.000(2) 0.000(2) C24 0.0516(19) 0.0554(19) 0.0376(18) -0.0176(15) -0.0050(15) 0.0063(15) C25 0.060(11) 0.098(14) 0.061(11) -0.005(10) -0.005(9) -0.041(10) C26 0.030(7) 0.046(8) 0.055(9) -0.009(7) -0.010(6) -0.004(6) C27 0.058(10) 0.059(10) 0.071(12) -0.017(9) 0.006(9) -0.008(8) C28 0.058(10) 0.058(10) 0.067(11) -0.020(9) 0.014(8) -0.004(9) C29 0.064(11) 0.057(10) 0.055(9) -0.021(8) 0.018(8) -0.021(9) C30 0.040(8) 0.035(7) 0.042(8) -0.009(6) 0.006(6) -0.011(6) C31 0.033(7) 0.030(7) 0.044(8) 0.004(6) 0.006(6) -0.014(6) C32 0.063(10) 0.049(9) 0.040(8) -0.011(7) 0.022(7) -0.026(8) C33 0.066(10) 0.039(8) 0.033(7) -0.004(6) -0.005(7) -0.010(7) C34 0.123(16) 0.056(10) 0.027(8) 0.000(7) -0.014(9) -0.014(10) C35 0.054(9) 0.044(8) 0.042(8) 0.013(7) -0.006(7) 0.006(7) C36 0.051(9) 0.046(8) 0.041(8) -0.008(6) -0.008(7) -0.002(7) C37 0.045(9) 0.048(8) 0.046(9) 0.003(7) -0.001(7) -0.010(7) C38 0.38(2) 0.236(18) 0.176(17) 0.156(13) -0.192(15) -0.273(17) C39 0.077(12) 0.039(8) 0.065(11) 0.007(7) -0.011(9) -0.010(8) C40 0.29(4) 0.087(16) 0.078(16) 0.009(13) 0.05(2) -0.07(2) C41 0.142(17) 0.063(12) 0.24(2) 0.036(13) 0.053(16) -0.012(13) C42 0.036(8) 0.027(6) 0.039(8) -0.001(5) -0.002(6) -0.007(6) C43 0.031(7) 0.061(9) 0.042(8) 0.015(7) 0.001(6) -0.010(7) C44 0.070(12) 0.082(13) 0.065(12) -0.002(10) 0.014(9) -0.007(10) C45 0.082(14) 0.110(16) 0.093(15) -0.005(12) 0.002(11) -0.058(13) C46 0.088(15) 0.137(19) 0.056(11) 0.030(12) 0.007(10) -0.045(14) C47 0.045(9) 0.046(8) 0.027(7) -0.008(6) -0.003(6) -0.004(7) C48 0.050(9) 0.063(10) 0.040(8) -0.016(7) 0.003(7) -0.025(8) C49 0.111(16) 0.074(12) 0.064(11) -0.042(10) 0.032(11) -0.050(12) C50 0.072(11) 0.053(9) 0.059(10) -0.007(8) -0.016(8) -0.031(9) C51 0.071(12) 0.081(12) 0.062(11) 0.015(9) -0.025(9) -0.046(10) C52 0.059(11) 0.034(8) 0.069(11) 0.004(7) 0.003(9) -0.013(8) C53 0.048(10) 0.062(11) 0.093(14) -0.018(10) 0.007(9) -0.004(8) C54 0.17(2) 0.060(13) 0.12(2) -0.029(13) 0.032(18) -0.024(15) C55 0.081(15) 0.085(14) 0.127(19) -0.036(14) 0.033(13) 0.007(12) C56 0.124(19) 0.109(17) 0.078(15) -0.051(13) 0.002(14) -0.002(15) N1 0.045(7) 0.045(6) 0.034(6) -0.002(5) -0.003(5) -0.009(6) N2 0.028(6) 0.051(7) 0.041(6) -0.003(5) -0.003(5) -0.016(5) N3 0.062(8) 0.033(6) 0.028(6) 0.002(5) 0.002(5) -0.013(6) N4 0.040(6) 0.034(6) 0.028(6) 0.001(5) -0.001(5) -0.008(5) N5 0.033(6) 0.042(6) 0.029(6) 0.003(5) -0.001(5) -0.008(5) N6 0.045(7) 0.061(8) 0.042(7) 0.022(6) -0.007(6) -0.004(6) O1 0.039(5) 0.044(6) 0.054(6) 0.016(5) -0.003(5) 0.000(5) O2 0.042(5) 0.040(5) 0.034(5) 0.000(4) -0.003(4) -0.004(4) O3 0.038(5) 0.041(5) 0.034(5) 0.000(4) -0.004(4) -0.002(4) O4 0.0516(19) 0.0554(19) 0.0376(18) -0.0176(15) -0.0050(15) 0.0063(15) O5 0.055(6) 0.031(5) 0.054(6) -0.005(4) -0.003(5) -0.003(5) O6 0.043(5) 0.039(5) 0.034(5) 0.004(4) 0.000(4) -0.009(4) O7 0.034(5) 0.038(5) 0.032(5) 0.000(4) 0.002(4) 0.001(4) O8 0.0516(19) 0.0554(19) 0.0376(18) -0.0176(15) -0.0050(15) 0.0063(15) O9 0.043(6) 0.043(5) 0.053(6) 0.004(5) 0.000(5) 0.001(5) O10 0.031(5) 0.037(5) 0.041(5) -0.005(4) 0.007(4) -0.003(4) O11 0.039(5) 0.040(5) 0.028(4) 0.005(4) -0.014(4) -0.003(4) O12 0.128(11) 0.062(7) 0.047(7) -0.003(6) -0.018(7) -0.013(8) O13 0.060(6) 0.034(5) 0.038(5) -0.003(4) -0.009(5) -0.009(5) O14 0.066(7) 0.040(5) 0.043(6) -0.005(4) -0.009(5) -0.011(5) O15 0.033(5) 0.048(5) 0.030(5) 0.000(4) -0.004(4) -0.007(4) O16 0.027(5) 0.043(5) 0.042(5) -0.001(4) -0.006(4) -0.007(4) O17 0.036(5) 0.042(5) 0.040(5) 0.001(4) -0.010(4) -0.010(4) O18 0.039(6) 0.043(5) 0.050(6) -0.010(4) 0.012(4) -0.011(4) O19 0.070(8) 0.070(8) 0.088(9) -0.018(7) -0.023(7) 0.005(7) O20 0.046(6) 0.043(5) 0.058(6) -0.005(5) -0.002(5) 0.002(5) O21 0.034(5) 0.035(5) 0.027(4) 0.000(4) -0.003(4) -0.008(4) O22 0.046(6) 0.050(6) 0.041(6) 0.006(4) -0.010(4) -0.002(5) O23 0.19(3) 0.19(2) 0.18(2) -0.047(19) -0.03(2) 0.00(2) Na1 0.033(3) 0.040(3) 0.047(3) 0.001(2) 0.002(2) 0.000(2) Gd1 0.0389(4) 0.0354(4) 0.0302(4) 0.0012(3) -0.0060(3) -0.0048(3) Mn1 0.0321(11) 0.0338(10) 0.0295(10) 0.0020(8) -0.0064(8) -0.0046(8) Mn2 0.0298(10) 0.0346(10) 0.0284(10) 0.0011(8) -0.0025(8) -0.0056(8) Mn3 0.0343(11) 0.0347(10) 0.0294(10) 0.0008(8) -0.0019(8) -0.0046(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.432(17) . ? C2 O1 1.351(18) . ? C2 C7 1.411(19) . ? C2 C3 1.42(2) . ? C3 C4 1.35(2) . ? C4 C5 1.36(2) . ? C5 C6 1.420(19) . ? C6 C7 1.40(2) . ? C6 C8 1.43(2) . ? C7 O2 1.315(15) . ? C8 N1 1.262(16) . ? C9 C11 1.49(2) . ? C9 N1 1.500(18) . ? C9 C10 1.53(2) . ? C9 C12 1.605(15) . ? C10 O3 1.423(16) . ? C12 O4 1.380(16) . ? C13 O5 1.430(18) . ? C14 O5 1.384(17) . ? C14 C19 1.39(2) . ? C14 C15 1.40(2) . ? C15 C16 1.39(2) . ? C16 C17 1.33(2) . ? C17 C18 1.406(19) . ? C18 C19 1.404(19) . ? C18 C20 1.44(2) . ? C19 O6 1.319(15) . ? C20 N2 1.289(16) . ? C21 C24 1.48(2) . ? C21 N2 1.486(17) . ? C21 C22 1.585(18) . ? C21 C23 1.66(2) . ? C23 O7 1.362(16) . ? C24 O8 1.394(16) . ? C25 O9 1.443(18) . ? C26 C27 1.37(2) . ? C26 O9 1.367(16) . ? C26 C31 1.404(18) . ? C27 C28 1.39(2) . ? C28 C29 1.38(2) . ? C29 C30 1.399(19) . ? C30 C32 1.41(2) . ? C30 C31 1.406(18) . ? C31 O10 1.328(15) . ? C32 N3 1.309(17) . ? C33 N3 1.512(17) . ? C33 C36 1.52(2) . ? C33 C35 1.531(19) . ? C33 C34 1.537(19) . ? C35 O12 1.427(17) . ? C36 O11 1.429(15) . ? C37 O13 1.239(16) . ? C37 O14 1.278(16) . ? C37 C39 1.53(2) . ? C37 Gd1 2.829(14) . ? C38 C39 1.44(3) . ? C39 C40 1.48(3) . ? C39 C41 1.49(3) . ? C42 O15 1.265(15) . ? C42 O16 1.266(14) . ? C42 C43 1.521(17) . ? C43 C44 1.48(2) . ? C43 C46 1.52(2) . ? C43 C45 1.54(2) . ? C47 O18 1.264(15) . ? C47 O17 1.274(15) . ? C47 C48 1.475(19) . ? C48 C50 1.51(2) . ? C48 C49 1.53(2) . ? C48 C51 1.53(2) . ? C52 O20 1.240(18) . ? C52 O19 1.306(19) . ? C52 C53 1.53(2) . ? C53 C54 1.51(3) . ? C53 C56 1.51(3) . ? C53 C55 1.55(3) . ? N1 Mn1 2.014(11) . ? N2 Mn2 1.994(10) . ? N3 Mn3 2.011(10) . ? N4 N5 1.196(13) . ? N4 Mn1 2.254(10) . ? N4 Mn2 2.340(10) . ? N5 N6 1.137(14) . ? O1 Na1 2.404(10) . ? O2 Mn1 1.907(9) . ? O2 Na1 2.328(10) . ? O3 Mn1 1.872(8) . ? O3 Gd1 2.311(8) . ? O5 Na1 2.437(10) . ? O6 Mn2 1.901(9) . ? O6 Na1 2.341(10) . ? O7 Mn2 1.896(8) . ? O7 Gd1 2.393(8) . ? O9 Na1 2.543(11) . ? O10 Mn3 1.889(9) . ? O10 Na1 2.405(10) . ? O11 Mn3 1.878(8) . ? O11 Gd1 2.309(8) . ? O13 Gd1 2.467(9) . ? O14 Gd1 2.470(9) . ? O15 Mn3 2.357(9) . ? O15 Gd1 2.691(9) . ? O16 Mn1 2.194(9) . ? O17 Mn2 2.166(8) . ? O18 Mn3 2.133(9) . ? O20 Gd1 2.320(10) . ? O21 Mn2 1.907(8) . ? O21 Mn3 1.931(8) . ? O21 Mn1 1.973(8) . ? O21 Gd1 2.838(8) . ? O21 Na1 2.873(9) . ? O22 Gd1 2.444(9) . ? Na1 Mn3 3.359(5) . ? Na1 Mn1 3.441(6) . ? Na1 Mn2 3.501(5) . ? Gd1 Mn3 3.351(2) . ? Gd1 Mn1 3.526(2) . ? Mn1 Mn2 3.115(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C2 C7 115.8(12) . . ? O1 C2 C3 124.1(14) . . ? C7 C2 C3 120.0(15) . . ? C4 C3 C2 118.6(15) . . ? C3 C4 C5 123.7(14) . . ? C4 C5 C6 119.2(15) . . ? C7 C6 C5 119.1(14) . . ? C7 C6 C8 122.6(12) . . ? C5 C6 C8 118.1(13) . . ? O2 C7 C6 125.1(12) . . ? O2 C7 C2 116.0(13) . . ? C6 C7 C2 119.0(13) . . ? N1 C8 C6 126.8(13) . . ? C11 C9 N1 116.6(13) . . ? C11 C9 C10 112.3(14) . . ? N1 C9 C10 103.8(11) . . ? C11 C9 C12 104.1(15) . . ? N1 C9 C12 97.8(10) . . ? C10 C9 C12 122.1(12) . . ? O3 C10 C9 109.8(13) . . ? O4 C12 C9 91.4(10) . . ? O5 C14 C19 114.1(12) . . ? O5 C14 C15 123.3(14) . . ? C19 C14 C15 122.6(15) . . ? C16 C15 C14 117.8(15) . . ? C17 C16 C15 121.0(15) . . ? C16 C17 C18 122.2(15) . . ? C19 C18 C17 118.7(14) . . ? C19 C18 C20 122.0(12) . . ? C17 C18 C20 119.2(13) . . ? O6 C19 C14 119.4(13) . . ? O6 C19 C18 123.2(13) . . ? C14 C19 C18 117.4(13) . . ? N2 C20 C18 126.1(13) . . ? C24 C21 N2 107.4(11) . . ? C24 C21 C22 115.9(12) . . ? N2 C21 C22 107.2(11) . . ? C24 C21 C23 98.9(11) . . ? N2 C21 C23 104.4(11) . . ? C22 C21 C23 121.7(12) . . ? O7 C23 C21 107.3(11) . . ? O8 C24 C21 111.8(12) . . ? C27 C26 O9 120.2(13) . . ? C27 C26 C31 120.7(14) . . ? O9 C26 C31 119.1(12) . . ? C26 C27 C28 122.2(16) . . ? C29 C28 C27 117.6(15) . . ? C28 C29 C30 121.4(15) . . ? C29 C30 C32 117.3(13) . . ? C29 C30 C31 120.1(13) . . ? C32 C30 C31 122.6(12) . . ? O10 C31 C26 116.9(12) . . ? O10 C31 C30 125.2(11) . . ? C26 C31 C30 117.9(12) . . ? N3 C32 C30 125.9(13) . . ? N3 C33 C36 103.1(10) . . ? N3 C33 C35 106.4(11) . . ? C36 C33 C35 110.7(12) . . ? N3 C33 C34 114.3(12) . . ? C36 C33 C34 109.8(13) . . ? C35 C33 C34 112.1(12) . . ? O12 C35 C33 112.9(13) . . ? O11 C36 C33 110.3(11) . . ? O13 C37 O14 121.1(13) . . ? O13 C37 C39 121.8(13) . . ? O14 C37 C39 117.1(13) . . ? O13 C37 Gd1 60.5(7) . . ? O14 C37 Gd1 60.7(7) . . ? C39 C37 Gd1 175.5(11) . . ? C38 C39 C40 114(2) . . ? C38 C39 C41 110(2) . . ? C40 C39 C41 104(2) . . ? C38 C39 C37 113.1(15) . . ? C40 C39 C37 110.7(15) . . ? C41 C39 C37 104.2(15) . . ? O15 C42 O16 124.5(11) . . ? O15 C42 C43 119.9(11) . . ? O16 C42 C43 115.6(11) . . ? C44 C43 C46 110.4(15) . . ? C44 C43 C42 112.3(12) . . ? C46 C43 C42 110.2(12) . . ? C44 C43 C45 108.5(14) . . ? C46 C43 C45 108.4(15) . . ? C42 C43 C45 106.9(12) . . ? O18 C47 O17 121.6(12) . . ? O18 C47 C48 121.2(12) . . ? O17 C47 C48 117.2(12) . . ? C47 C48 C50 109.3(11) . . ? C47 C48 C49 111.0(12) . . ? C50 C48 C49 110.5(13) . . ? C47 C48 C51 108.3(12) . . ? C50 C48 C51 110.4(12) . . ? C49 C48 C51 107.4(14) . . ? O20 C52 O19 122.6(15) . . ? O20 C52 C53 120.9(15) . . ? O19 C52 C53 116.5(15) . . ? C54 C53 C56 107.4(19) . . ? C54 C53 C52 105.3(16) . . ? C56 C53 C52 110.5(15) . . ? C54 C53 C55 112.8(17) . . ? C56 C53 C55 110.1(18) . . ? C52 C53 C55 110.6(15) . . ? C8 N1 C9 120.9(12) . . ? C8 N1 Mn1 125.4(10) . . ? C9 N1 Mn1 113.8(8) . . ? C20 N2 C21 122.8(12) . . ? C20 N2 Mn2 124.6(10) . . ? C21 N2 Mn2 112.6(9) . . ? C32 N3 C33 122.0(11) . . ? C32 N3 Mn3 125.2(10) . . ? C33 N3 Mn3 112.8(8) . . ? N5 N4 Mn1 128.6(9) . . ? N5 N4 Mn2 118.8(8) . . ? Mn1 N4 Mn2 85.4(3) . . ? N6 N5 N4 177.7(13) . . ? C2 O1 C1 117.6(12) . . ? C2 O1 Na1 119.0(8) . . ? C1 O1 Na1 122.5(10) . . ? C7 O2 Mn1 128.2(8) . . ? C7 O2 Na1 123.2(8) . . ? Mn1 O2 Na1 108.3(4) . . ? C10 O3 Mn1 115.0(8) . . ? C10 O3 Gd1 128.3(8) . . ? Mn1 O3 Gd1 114.5(4) . . ? C14 O5 C13 118.6(12) . . ? C14 O5 Na1 117.2(8) . . ? C13 O5 Na1 124.0(10) . . ? C19 O6 Mn2 126.6(9) . . ? C19 O6 Na1 120.6(9) . . ? Mn2 O6 Na1 110.8(4) . . ? C23 O7 Mn2 115.7(8) . . ? C23 O7 Gd1 128.3(8) . . ? Mn2 O7 Gd1 112.2(4) . . ? C26 O9 C25 111.9(11) . . ? C26 O9 Na1 108.1(8) . . ? C25 O9 Na1 104.7(9) . . ? C31 O10 Mn3 127.4(8) . . ? C31 O10 Na1 114.4(7) . . ? Mn3 O10 Na1 102.2(4) . . ? C36 O11 Mn3 112.1(8) . . ? C36 O11 Gd1 138.9(7) . . ? Mn3 O11 Gd1 105.9(3) . . ? C37 O13 Gd1 93.6(8) . . ? C37 O14 Gd1 92.4(8) . . ? C42 O15 Mn3 114.9(8) . . ? C42 O15 Gd1 133.3(8) . . ? Mn3 O15 Gd1 82.9(3) . . ? C42 O16 Mn1 121.4(8) . . ? C47 O17 Mn2 125.5(8) . . ? C47 O18 Mn3 126.1(9) . . ? C52 O20 Gd1 143.4(11) . . ? Mn2 O21 Mn3 119.3(4) . . ? Mn2 O21 Mn1 106.8(4) . . ? Mn3 O21 Mn1 133.8(4) . . ? Mn2 O21 Gd1 95.6(3) . . ? Mn3 O21 Gd1 87.1(3) . . ? Mn1 O21 Gd1 92.5(3) . . ? Mn2 O21 Na1 91.9(3) . . ? Mn3 O21 Na1 86.4(3) . . ? Mn1 O21 Na1 88.5(3) . . ? Gd1 O21 Na1 171.8(3) . . ? O2 Na1 O6 91.8(4) . . ? O2 Na1 O1 65.9(3) . . ? O6 Na1 O1 110.2(4) . . ? O2 Na1 O10 98.1(3) . . ? O6 Na1 O10 115.9(3) . . ? O1 Na1 O10 131.6(4) . . ? O2 Na1 O5 140.0(4) . . ? O6 Na1 O5 66.1(3) . . ? O1 Na1 O5 89.9(4) . . ? O10 Na1 O5 121.3(4) . . ? O2 Na1 O9 103.8(4) . . ? O6 Na1 O9 164.1(4) . . ? O1 Na1 O9 74.5(3) . . ? O10 Na1 O9 65.2(3) . . ? O5 Na1 O9 99.3(4) . . ? O2 Na1 O21 66.7(3) . . ? O6 Na1 O21 63.5(3) . . ? O1 Na1 O21 131.8(4) . . ? O10 Na1 O21 63.5(3) . . ? O5 Na1 O21 122.7(3) . . ? O9 Na1 O21 125.4(3) . . ? O2 Na1 Mn3 93.3(3) . . ? O6 Na1 Mn3 83.3(2) . . ? O1 Na1 Mn3 154.8(3) . . ? O10 Na1 Mn3 33.4(2) . . ? O5 Na1 Mn3 115.2(3) . . ? O9 Na1 Mn3 98.5(3) . . ? O21 Na1 Mn3 35.01(16) . . ? O2 Na1 Mn1 31.7(2) . . ? O6 Na1 Mn1 77.6(3) . . ? O1 Na1 Mn1 97.5(3) . . ? O10 Na1 Mn1 79.2(2) . . ? O5 Na1 Mn1 143.2(3) . . ? O9 Na1 Mn1 117.4(3) . . ? O21 Na1 Mn1 34.97(17) . . ? Mn3 Na1 Mn1 63.73(10) . . ? O2 Na1 Mn2 78.0(3) . . ? O6 Na1 Mn2 30.5(2) . . ? O1 Na1 Mn2 125.9(3) . . ? O10 Na1 Mn2 90.9(2) . . ? O5 Na1 Mn2 93.5(3) . . ? O9 Na1 Mn2 156.1(3) . . ? O21 Na1 Mn2 32.99(17) . . ? Mn3 Na1 Mn2 57.70(9) . . ? Mn1 Na1 Mn2 53.31(9) . . ? O11 Gd1 O3 123.1(3) . . ? O11 Gd1 O20 147.4(3) . . ? O3 Gd1 O20 82.5(3) . . ? O11 Gd1 O7 84.6(3) . . ? O3 Gd1 O7 81.2(3) . . ? O20 Gd1 O7 79.6(3) . . ? O11 Gd1 O22 74.6(3) . . ? O3 Gd1 O22 150.5(3) . . ? O20 Gd1 O22 74.2(3) . . ? O7 Gd1 O22 77.1(3) . . ? O11 Gd1 O13 85.5(3) . . ? O3 Gd1 O13 125.4(3) . . ? O20 Gd1 O13 95.5(3) . . ? O7 Gd1 O13 152.3(3) . . ? O22 Gd1 O13 75.4(3) . . ? O11 Gd1 O14 126.4(3) . . ? O3 Gd1 O14 74.2(3) . . ? O20 Gd1 O14 76.8(3) . . ? O7 Gd1 O14 147.8(3) . . ? O22 Gd1 O14 116.4(3) . . ? O13 Gd1 O14 52.7(3) . . ? O11 Gd1 O15 65.8(3) . . ? O3 Gd1 O15 75.7(3) . . ? O20 Gd1 O15 146.2(3) . . ? O7 Gd1 O15 121.2(3) . . ? O22 Gd1 O15 133.0(3) . . ? O13 Gd1 O15 77.2(3) . . ? O14 Gd1 O15 72.6(3) . . ? O11 Gd1 C37 107.0(4) . . ? O3 Gd1 C37 100.6(4) . . ? O20 Gd1 C37 84.9(4) . . ? O7 Gd1 C37 164.1(4) . . ? O22 Gd1 C37 95.2(4) . . ? O13 Gd1 C37 25.9(3) . . ? O14 Gd1 C37 26.8(4) . . ? O15 Gd1 C37 74.2(4) . . ? O11 Gd1 O21 62.4(2) . . ? O3 Gd1 O21 62.4(3) . . ? O20 Gd1 O21 129.8(3) . . ? O7 Gd1 O21 61.3(3) . . ? O22 Gd1 O21 121.1(3) . . ? O13 Gd1 O21 133.7(3) . . ? O14 Gd1 O21 121.1(3) . . ? O15 Gd1 O21 60.0(2) . . ? C37 Gd1 O21 133.5(3) . . ? O11 Gd1 Mn3 32.6(2) . . ? O3 Gd1 Mn3 91.0(2) . . ? O20 Gd1 Mn3 162.9(2) . . ? O7 Gd1 Mn3 83.7(2) . . ? O22 Gd1 Mn3 106.1(2) . . ? O13 Gd1 Mn3 101.2(2) . . ? O14 Gd1 Mn3 116.8(2) . . ? O15 Gd1 Mn3 44.27(19) . . ? C37 Gd1 Mn3 111.9(3) . . ? O21 Gd1 Mn3 35.13(16) . . ? O11 Gd1 Mn1 94.39(19) . . ? O3 Gd1 Mn1 28.9(2) . . ? O20 Gd1 Mn1 107.7(2) . . ? O7 Gd1 Mn1 72.9(2) . . ? O22 Gd1 Mn1 148.9(2) . . ? O13 Gd1 Mn1 133.6(2) . . ? O14 Gd1 Mn1 93.7(2) . . ? O15 Gd1 Mn1 61.02(17) . . ? C37 Gd1 Mn1 115.9(3) . . ? O21 Gd1 Mn1 33.99(16) . . ? Mn3 Gd1 Mn1 62.88(5) . . ? O3 Mn1 O2 173.6(4) . . ? O3 Mn1 O21 89.4(4) . . ? O2 Mn1 O21 96.5(4) . . ? O3 Mn1 N1 82.2(4) . . ? O2 Mn1 N1 91.7(4) . . ? O21 Mn1 N1 170.3(4) . . ? O3 Mn1 O16 92.3(4) . . ? O2 Mn1 O16 89.8(3) . . ? O21 Mn1 O16 93.2(3) . . ? N1 Mn1 O16 92.0(4) . . ? O3 Mn1 N4 89.2(4) . . ? O2 Mn1 N4 89.0(4) . . ? O21 Mn1 N4 84.4(3) . . ? N1 Mn1 N4 90.6(4) . . ? O16 Mn1 N4 177.2(4) . . ? O3 Mn1 Mn2 88.9(3) . . ? O2 Mn1 Mn2 94.5(3) . . ? O21 Mn1 Mn2 35.9(2) . . ? N1 Mn1 Mn2 138.4(3) . . ? O16 Mn1 Mn2 129.1(2) . . ? N4 Mn1 Mn2 48.5(3) . . ? O3 Mn1 Na1 146.0(3) . . ? O2 Mn1 Na1 40.0(3) . . ? O21 Mn1 Na1 56.6(2) . . ? N1 Mn1 Na1 131.7(3) . . ? O16 Mn1 Na1 89.6(2) . . ? N4 Mn1 Na1 87.8(3) . . ? Mn2 Mn1 Na1 64.32(10) . . ? O3 Mn1 Gd1 36.6(3) . . ? O2 Mn1 Gd1 149.6(3) . . ? O21 Mn1 Gd1 53.5(2) . . ? N1 Mn1 Gd1 118.6(3) . . ? O16 Mn1 Gd1 87.4(2) . . ? N4 Mn1 Gd1 92.3(3) . . ? Mn2 Mn1 Gd1 64.72(5) . . ? Na1 Mn1 Gd1 109.70(10) . . ? O7 Mn2 O6 175.5(4) . . ? O7 Mn2 O21 90.3(4) . . ? O6 Mn2 O21 93.8(4) . . ? O7 Mn2 N2 84.4(4) . . ? O6 Mn2 N2 91.3(4) . . ? O21 Mn2 N2 169.6(4) . . ? O7 Mn2 O17 92.9(4) . . ? O6 Mn2 O17 88.0(4) . . ? O21 Mn2 O17 102.1(3) . . ? N2 Mn2 O17 87.1(4) . . ? O7 Mn2 N4 89.3(4) . . ? O6 Mn2 N4 89.4(4) . . ? O21 Mn2 N4 83.5(3) . . ? N2 Mn2 N4 87.5(4) . . ? O17 Mn2 N4 173.9(3) . . ? O7 Mn2 Mn1 89.6(3) . . ? O6 Mn2 Mn1 92.6(3) . . ? O21 Mn2 Mn1 37.3(2) . . ? N2 Mn2 Mn1 133.4(3) . . ? O17 Mn2 Mn1 139.4(2) . . ? N4 Mn2 Mn1 46.2(3) . . ? O7 Mn2 Na1 145.3(3) . . ? O6 Mn2 Na1 38.7(3) . . ? O21 Mn2 Na1 55.1(3) . . ? N2 Mn2 Na1 129.3(3) . . ? O17 Mn2 Na1 96.2(3) . . ? N4 Mn2 Na1 85.1(3) . . ? Mn1 Mn2 Na1 62.37(10) . . ? O7 Mn2 Gd1 38.3(3) . . ? O6 Mn2 Gd1 145.9(3) . . ? O21 Mn2 Gd1 52.3(2) . . ? N2 Mn2 Gd1 122.7(3) . . ? O17 Mn2 Gd1 95.5(2) . . ? N4 Mn2 Gd1 89.7(2) . . ? Mn1 Mn2 Gd1 63.22(5) . . ? Na1 Mn2 Gd1 107.32(10) . . ? O11 Mn3 O10 172.7(4) . . ? O11 Mn3 O21 90.5(4) . . ? O10 Mn3 O21 94.6(4) . . ? O11 Mn3 N3 83.1(4) . . ? O10 Mn3 N3 91.3(4) . . ? O21 Mn3 N3 172.0(4) . . ? O11 Mn3 O18 94.4(4) . . ? O10 Mn3 O18 90.1(4) . . ? O21 Mn3 O18 98.1(3) . . ? N3 Mn3 O18 87.1(4) . . ? O11 Mn3 O15 79.6(3) . . ? O10 Mn3 O15 96.1(3) . . ? O21 Mn3 O15 79.7(3) . . ? N3 Mn3 O15 94.4(4) . . ? O18 Mn3 O15 173.5(3) . . ? O11 Mn3 Gd1 41.5(3) . . ? O10 Mn3 Gd1 139.1(3) . . ? O21 Mn3 Gd1 57.8(2) . . ? N3 Mn3 Gd1 114.4(3) . . ? O18 Mn3 Gd1 120.9(3) . . ? O15 Mn3 Gd1 52.8(2) . . ? O11 Mn3 Na1 142.7(3) . . ? O10 Mn3 Na1 44.4(3) . . ? O21 Mn3 Na1 58.6(3) . . ? N3 Mn3 Na1 129.1(3) . . ? O18 Mn3 Na1 72.3(3) . . ? O15 Mn3 Na1 111.1(2) . . ? Gd1 Mn3 Na1 116.21(10) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.606 _refine_diff_density_min -5.756 _refine_diff_density_rms 0.195 _database_code_depnum_ccdc_archive 'CCDC 947813' ####################################################################### # # 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_Mn3NdNa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H83 Mn3 N6 Na Nd O22, H2 O ' _chemical_formula_sum 'C56 H85 Mn3 N6 Na Nd O23' _chemical_formula_weight 1542.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.450(5) _cell_length_b 14.850(5) _cell_length_c 19.884(5) _cell_angle_alpha 82.488(5) _cell_angle_beta 86.821(5) _cell_angle_gamma 76.780(5) _cell_volume 3262(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7659 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.10 _exptl_crystal_description block-shaped _exptl_crystal_colour brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1586 _exptl_absorpt_coefficient_mu 1.437 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38289 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11371 _reflns_number_gt 6825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11371 _refine_ls_number_parameters 812 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2757 _refine_ls_wR_factor_gt 0.2346 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 C1 C 1.0898(11) 0.4261(8) 0.3891(7) 0.070(4) Uani 1 1 d . . . H1A H 1.1740 0.4251 0.3851 0.104 Uiso 1 1 calc R . . H1B H 1.0684 0.3943 0.3542 0.104 Uiso 1 1 calc R . . H1C H 1.0721 0.3955 0.4328 0.104 Uiso 1 1 calc R . . C2 C 1.0507(10) 0.5777(8) 0.4236(5) 0.053(3) Uani 1 1 d . . . C3 C 1.1360(10) 0.5473(10) 0.4736(6) 0.060(3) Uani 1 1 d . . . H3 H 1.1799 0.4859 0.4795 0.072 Uiso 1 1 calc R . . C4 C 1.1527(11) 0.6114(11) 0.5138(6) 0.070(4) Uani 1 1 d . . . H4 H 1.2068 0.5916 0.5488 0.084 Uiso 1 1 calc R . . C5 C 1.0940(11) 0.7026(10) 0.5048(5) 0.061(3) Uani 1 1 d . . . H5 H 1.1090 0.7433 0.5333 0.073 Uiso 1 1 calc R . . C6 C 1.0111(9) 0.7356(8) 0.4530(5) 0.041(2) Uani 1 1 d . . . C7 C 0.9909(9) 0.6736(7) 0.4096(5) 0.045(3) Uani 1 1 d . . . C8 C 0.9509(10) 0.8321(8) 0.4453(5) 0.050(3) Uani 1 1 d . . . H8 H 0.9664 0.8680 0.4773 0.060 Uiso 1 1 calc R . . C9 C 0.8208(10) 0.9753(8) 0.3979(6) 0.0541(12) Uani 1 1 d D . . C10 C 0.810(2) 1.0138(15) 0.4627(10) 0.162(11) Uani 1 1 d . . . H10A H 0.7739 0.9750 0.4964 0.242 Uiso 1 1 calc R . . H10B H 0.7598 1.0756 0.4575 0.242 Uiso 1 1 calc R . . H10C H 0.8876 1.0158 0.4769 0.242 Uiso 1 1 calc R . . O23 O 0.1063(19) 0.249(2) 0.1692(14) 0.253(12) Uani 1 1 d G . . H23A H 0.0771 0.2294 0.1372 0.380 Uiso 1 1 d G . . H23B H 0.0532 0.2607 0.2004 0.380 Uiso 1 1 d G . . C11 C 0.8983(9) 1.0251(8) 0.3438(6) 0.0541(12) Uani 1 1 d D . . H11A H 0.8631 1.0910 0.3329 0.065 Uiso 1 1 calc R . . H11B H 0.9140 0.9953 0.3026 0.065 Uiso 1 1 calc R . . C12 C 0.7077(13) 0.9871(9) 0.3595(7) 0.077(4) Uani 1 1 d . . . H12A H 0.6460 0.9689 0.3901 0.092 Uiso 1 1 calc R . . H12B H 0.6797 1.0523 0.3422 0.092 Uiso 1 1 calc R . . C13 C 0.8862(14) 0.3614(10) 0.2696(8) 0.095(5) Uani 1 1 d . . . H13A H 0.9241 0.3184 0.3066 0.142 Uiso 1 1 calc R . . H13B H 0.9461 0.3757 0.2369 0.142 Uiso 1 1 calc R . . H13C H 0.8317 0.3339 0.2485 0.142 Uiso 1 1 calc R . . C14 C 0.7136(11) 0.4438(7) 0.3294(5) 0.051(3) Uani 1 1 d . . . C15 C 0.6721(13) 0.3655(8) 0.3514(6) 0.061(3) Uani 1 1 d . . . H15 H 0.7160 0.3078 0.3411 0.073 Uiso 1 1 calc R . . C16 C 0.5660(13) 0.3706(9) 0.3886(6) 0.069(4) Uani 1 1 d . . . H16 H 0.5411 0.3165 0.4056 0.082 Uiso 1 1 calc R . . C17 C 0.4980(11) 0.4553(9) 0.4002(6) 0.059(3) Uani 1 1 d . . . H17 H 0.4250 0.4585 0.4237 0.071 Uiso 1 1 calc R . . C18 C 0.5349(11) 0.5365(7) 0.3779(5) 0.048(3) Uani 1 1 d . . . C19 C 0.6471(9) 0.5322(7) 0.3430(5) 0.039(2) Uani 1 1 d . . . C20 C 0.4524(9) 0.6241(8) 0.3850(5) 0.048(3) Uani 1 1 d . . . H20 H 0.3850 0.6220 0.4130 0.058 Uiso 1 1 calc R . . C21 C 0.3674(10) 0.7897(8) 0.3598(6) 0.0541(12) Uani 1 1 d . . . C22 C 0.3600(10) 0.8169(8) 0.4341(5) 0.0541(12) Uani 1 1 d . . . H22C H 0.4141 0.7699 0.4621 0.081 Uiso 1 1 calc R . . H22D H 0.2796 0.8217 0.4521 0.081 Uiso 1 1 calc R . . H22E H 0.3819 0.8757 0.4333 0.081 Uiso 1 1 calc R . . C23 C 0.3865(10) 0.8582(8) 0.2880(5) 0.052(3) Uani 1 1 d . . . H23C H 0.3555 0.8376 0.2497 0.063 Uiso 1 1 calc R . . H23D H 0.3460 0.9224 0.2915 0.063 Uiso 1 1 calc R . . C24 C 0.2521(13) 0.7684(10) 0.3426(9) 0.090(5) Uani 1 1 d . . . H24A H 0.2631 0.7396 0.3009 0.108 Uiso 1 1 calc R . . H24B H 0.2287 0.7246 0.3785 0.108 Uiso 1 1 calc R . . C25 C 1.1722(14) 0.5855(12) 0.2571(7) 0.088(5) Uani 1 1 d . . . H25A H 1.2362 0.5901 0.2244 0.132 Uiso 1 1 calc R . . H25B H 1.2053 0.5566 0.3000 0.132 Uiso 1 1 calc R . . H25C H 1.1249 0.6467 0.2620 0.132 Uiso 1 1 calc R . . C26 C 1.0917(9) 0.5449(7) 0.1652(5) 0.046(3) Uani 1 1 d . . . C27 C 1.1681(11) 0.4869(8) 0.1256(6) 0.061(3) Uani 1 1 d . . . H27 H 1.2259 0.4372 0.1452 0.073 Uiso 1 1 calc R . . C28 C 1.1573(11) 0.5042(9) 0.0554(7) 0.069(4) Uani 1 1 d . . . H28 H 1.2100 0.4659 0.0283 0.083 Uiso 1 1 calc R . . C29 C 1.0733(11) 0.5744(8) 0.0255(6) 0.061(3) Uani 1 1 d . . . H29 H 1.0701 0.5851 -0.0216 0.073 Uiso 1 1 calc R . . C30 C 0.9897(9) 0.6320(7) 0.0658(5) 0.043(2) Uani 1 1 d . . . C31 C 0.9996(9) 0.6187(7) 0.1360(5) 0.043(2) Uani 1 1 d . . . C32 C 0.8953(10) 0.7006(7) 0.0313(5) 0.046(3) Uani 1 1 d . . . H32 H 0.8985 0.7070 -0.0158 0.055 Uiso 1 1 calc R . . C33 C 0.7134(10) 0.8206(7) 0.0190(5) 0.046(3) Uani 1 1 d . . . C34 C 0.6860(12) 0.7891(9) -0.0464(5) 0.063(3) Uani 1 1 d . . . H34A H 0.7524 0.7899 -0.0780 0.095 Uiso 1 1 calc R . . H34B H 0.6151 0.8304 -0.0653 0.095 Uiso 1 1 calc R . . H34C H 0.6730 0.7270 -0.0375 0.095 Uiso 1 1 calc R . . C35 C 0.7575(11) 0.9117(7) 0.0057(5) 0.058(3) Uani 1 1 d . . . H35A H 0.7900 0.9227 0.0471 0.070 Uiso 1 1 calc R . . H35B H 0.8219 0.9047 -0.0283 0.070 Uiso 1 1 calc R . . C36 C 0.6033(10) 0.8337(8) 0.0666(5) 0.049(3) Uani 1 1 d . . . H36A H 0.5457 0.8900 0.0503 0.058 Uiso 1 1 calc R . . H36B H 0.5655 0.7814 0.0677 0.058 Uiso 1 1 calc R . . C37 C 0.6849(11) 1.1142(8) 0.1346(6) 0.052(3) Uani 1 1 d . . . C38 C 0.7126(13) 1.2040(9) 0.0981(6) 0.066(3) Uani 1 1 d . . . C39 C 0.798(3) 1.2384(19) 0.1362(13) 0.27(2) Uani 1 1 d . . . H39A H 0.8783 1.2071 0.1255 0.398 Uiso 1 1 calc R . . H39B H 0.7816 1.2259 0.1840 0.398 Uiso 1 1 calc R . . H39C H 0.7881 1.3043 0.1238 0.398 Uiso 1 1 calc R . . C40 C 0.749(3) 1.1937(14) 0.0280(9) 0.173(12) Uani 1 1 d . . . H40A H 0.7669 1.2508 0.0061 0.260 Uiso 1 1 calc R . . H40B H 0.6853 1.1794 0.0050 0.260 Uiso 1 1 calc R . . H40C H 0.8193 1.1441 0.0265 0.260 Uiso 1 1 calc R . . C41 C 0.597(2) 1.2708(13) 0.0928(18) 0.231(18) Uani 1 1 d . . . H41A H 0.6081 1.3296 0.0702 0.347 Uiso 1 1 calc R . . H41B H 0.5627 1.2789 0.1374 0.347 Uiso 1 1 calc R . . H41C H 0.5436 1.2478 0.0671 0.347 Uiso 1 1 calc R . . C42 C 0.9435(9) 0.8805(7) 0.1949(5) 0.039(2) Uani 1 1 d . . . C43 C 1.0472(11) 0.9096(9) 0.1539(6) 0.059(3) Uani 1 1 d . . . C44 C 1.0141(14) 0.9454(14) 0.0803(7) 0.108(6) Uani 1 1 d . . . H44A H 1.0749 0.9749 0.0585 0.162 Uiso 1 1 calc R . . H44B H 0.9384 0.9897 0.0792 0.162 Uiso 1 1 calc R . . H44C H 1.0081 0.8941 0.0569 0.162 Uiso 1 1 calc R . . C45 C 1.0760(14) 0.9902(12) 0.1870(9) 0.102(5) Uani 1 1 d . . . H45A H 1.1138 0.9660 0.2295 0.153 Uiso 1 1 calc R . . H45B H 1.0030 1.0350 0.1945 0.153 Uiso 1 1 calc R . . H45C H 1.1291 1.0196 0.1574 0.153 Uiso 1 1 calc R . . C46 C 1.1554(13) 0.8298(11) 0.1549(7) 0.085(4) Uani 1 1 d . . . H46A H 1.1757 0.8060 0.2010 0.128 Uiso 1 1 calc R . . H46B H 1.2219 0.8512 0.1320 0.128 Uiso 1 1 calc R . . H46C H 1.1378 0.7813 0.1323 0.128 Uiso 1 1 calc R . . C47 C 0.5921(10) 0.6337(7) 0.1735(5) 0.041(2) Uani 1 1 d . . . C48 C 0.5337(11) 0.5713(8) 0.1375(5) 0.054(3) Uani 1 1 d . . . C49 C 0.5141(12) 0.4910(8) 0.1871(6) 0.062(3) Uani 1 1 d . . . H49A H 0.4754 0.4523 0.1651 0.093 Uiso 1 1 calc R . . H49B H 0.4643 0.5140 0.2244 0.093 Uiso 1 1 calc R . . H49C H 0.5900 0.4552 0.2037 0.093 Uiso 1 1 calc R . . C50 C 0.4100(12) 0.6330(10) 0.1131(6) 0.074(4) Uani 1 1 d . . . H50A H 0.4226 0.6875 0.0845 0.111 Uiso 1 1 calc R . . H50B H 0.3607 0.6515 0.1518 0.111 Uiso 1 1 calc R . . H50C H 0.3707 0.5980 0.0880 0.111 Uiso 1 1 calc R . . C51 C 0.6040(14) 0.5396(10) 0.0776(7) 0.085(4) Uani 1 1 d . . . H51A H 0.6781 0.4979 0.0918 0.127 Uiso 1 1 calc R . . H51B H 0.6209 0.5923 0.0487 0.127 Uiso 1 1 calc R . . H51C H 0.5591 0.5077 0.0533 0.127 Uiso 1 1 calc R . . C52 C 0.3728(13) 1.1149(8) 0.2661(7) 0.062(3) Uani 1 1 d . . . C53 C 0.3299(13) 1.1774(10) 0.3193(8) 0.083(4) Uani 1 1 d . . . C54 C 0.4117(19) 1.1477(15) 0.3798(10) 0.140(8) Uani 1 1 d . . . H54A H 0.4934 1.1450 0.3647 0.209 Uiso 1 1 calc R . . H54B H 0.4040 1.0873 0.4010 0.209 Uiso 1 1 calc R . . H54C H 0.3892 1.1920 0.4119 0.209 Uiso 1 1 calc R . . C55 C 0.2056(18) 1.1755(14) 0.3459(12) 0.140(8) Uani 1 1 d . . . H55A H 0.1860 1.2134 0.3823 0.210 Uiso 1 1 calc R . . H55B H 0.2014 1.1126 0.3623 0.210 Uiso 1 1 calc R . . H55C H 0.1496 1.1994 0.3102 0.210 Uiso 1 1 calc R . . C56 C 0.344(2) 1.2710(11) 0.2922(12) 0.148(9) Uani 1 1 d . . . H56A H 0.4225 1.2671 0.2717 0.222 Uiso 1 1 calc R . . H56B H 0.3339 1.3092 0.3284 0.222 Uiso 1 1 calc R . . H56C H 0.2845 1.2979 0.2588 0.222 Uiso 1 1 calc R . . N1 N 0.8787(7) 0.8734(6) 0.3993(4) 0.042(2) Uani 1 1 d . . . N2 N 0.4627(7) 0.7054(6) 0.3562(4) 0.041(2) Uani 1 1 d . . . N3 N 0.8067(8) 0.7539(5) 0.0598(4) 0.043(2) Uani 1 1 d . . . N4 N 0.6734(7) 0.7744(5) 0.3951(4) 0.0350(18) Uani 1 1 d . . . N5 N 0.6826(7) 0.7225(6) 0.4464(4) 0.0385(19) Uani 1 1 d . . . N6 N 0.6864(10) 0.6736(7) 0.4966(4) 0.067(3) Uani 1 1 d . . . O1 O 1.0219(6) 0.5215(5) 0.3819(4) 0.0509(19) Uani 1 1 d . . . O2 O 0.9224(6) 0.6975(4) 0.3556(3) 0.0392(16) Uani 1 1 d . . . O3 O 0.7253(6) 0.9341(4) 0.3057(3) 0.0404(16) Uani 1 1 d . . . O4 O 1.0130(6) 1.0066(5) 0.3884(4) 0.0541(12) Uani 1 1 d . . . H4A H 1.0227 0.9546 0.4100 0.081 Uiso 1 1 calc R . . O5 O 0.8209(7) 0.4457(5) 0.2950(4) 0.056(2) Uani 1 1 d . . . O6 O 0.6924(6) 0.6058(4) 0.3233(3) 0.0395(16) Uani 1 1 d . . . O7 O 0.5076(6) 0.8494(4) 0.2810(3) 0.0386(16) Uani 1 1 d . . . O8 O 0.1621(12) 0.8492(9) 0.3346(7) 0.121(4) Uani 1 1 d . . . H8A H 0.1295 0.8529 0.2983 0.181 Uiso 1 1 calc R . . O9 O 1.0993(7) 0.5312(5) 0.2348(4) 0.0540(19) Uani 1 1 d . . . O10 O 0.9279(6) 0.6708(4) 0.1786(3) 0.0386(15) Uani 1 1 d . . . O11 O 0.6386(6) 0.8402(4) 0.1337(3) 0.0366(15) Uani 1 1 d . . . O12 O 0.6654(9) 0.9910(6) -0.0169(4) 0.075(3) Uani 1 1 d . . . H12 H 0.6434 0.9852 -0.0544 0.112 Uiso 1 1 calc R . . O13 O 0.9650(6) 0.8462(4) 0.2553(3) 0.0436(17) Uani 1 1 d . . . O14 O 0.8452(6) 0.8898(4) 0.1663(3) 0.0397(16) Uani 1 1 d . . . O15 O 0.6992(7) 0.6352(5) 0.1581(3) 0.0443(17) Uani 1 1 d . . . O16 O 0.5291(6) 0.6802(5) 0.2173(3) 0.0440(17) Uani 1 1 d . . . O17 O 0.7098(7) 1.0913(5) 0.1961(3) 0.056(2) Uani 1 1 d . . . O18 O 0.6336(7) 1.0652(5) 0.1032(3) 0.0528(19) Uani 1 1 d . . . O19 O 0.4756(7) 1.0645(5) 0.2676(4) 0.060(2) Uani 1 1 d . . . O20 O 0.2971(10) 1.1168(7) 0.2205(6) 0.097(3) Uani 1 1 d . . . O21 O 0.7405(5) 0.7692(4) 0.2558(3) 0.0311(14) Uani 1 1 d . . . O22 O 0.4152(6) 0.9833(5) 0.1509(3) 0.0536(19) Uani 1 1 d . . . H22A H 0.4049 0.9323 0.1400 0.080 Uiso 1 1 d R . . H22B H 0.3587 1.0053 0.1778 0.080 Uiso 1 1 d R . . Na1 Na 0.8916(4) 0.5885(3) 0.28748(19) 0.0450(10) Uani 1 1 d . . . Mn1 Mn 0.60381(13) 0.72951(9) 0.29922(6) 0.0324(4) Uani 1 1 d . . . Mn2 Mn 0.77792(13) 0.75244(9) 0.16122(6) 0.0342(4) Uani 1 1 d . . . Mn3 Mn 0.82110(13) 0.81400(9) 0.32585(6) 0.0339(4) Uani 1 1 d . . . Nd1 Nd 0.61133(5) 0.95495(3) 0.20804(2) 0.0382(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(7) 0.056(8) 0.095(9) 0.010(7) 0.004(7) 0.009(6) C2 0.043(7) 0.068(8) 0.042(6) 0.009(5) -0.001(5) -0.009(6) C3 0.042(7) 0.079(9) 0.048(7) 0.019(6) -0.008(5) -0.004(6) C4 0.052(8) 0.097(11) 0.053(7) 0.023(7) -0.015(6) -0.016(7) C5 0.055(8) 0.085(9) 0.040(6) 0.011(6) -0.008(5) -0.021(7) C6 0.032(6) 0.059(7) 0.032(5) 0.008(5) -0.010(4) -0.016(5) C7 0.036(6) 0.056(7) 0.037(5) 0.012(5) 0.001(5) -0.012(5) C8 0.050(7) 0.062(7) 0.042(6) -0.004(5) -0.012(5) -0.019(6) C9 0.039(3) 0.052(3) 0.067(3) -0.015(2) 0.008(2) 0.002(2) C10 0.20(2) 0.135(17) 0.136(16) -0.098(14) -0.079(16) 0.056(16) O23 0.19(2) 0.28(3) 0.24(3) -0.01(2) 0.048(19) 0.04(2) C11 0.039(3) 0.052(3) 0.067(3) -0.015(2) 0.008(2) 0.002(2) C12 0.094(11) 0.061(8) 0.073(8) -0.020(7) -0.041(8) 0.006(7) C13 0.098(12) 0.064(9) 0.112(12) -0.041(9) -0.017(9) 0.023(8) C14 0.067(8) 0.040(6) 0.047(6) 0.000(5) -0.021(6) -0.013(5) C15 0.083(10) 0.032(6) 0.063(7) 0.004(5) -0.010(7) -0.007(6) C16 0.076(10) 0.055(8) 0.078(9) 0.020(6) -0.019(8) -0.034(7) C17 0.056(8) 0.065(8) 0.058(7) 0.010(6) 0.002(6) -0.026(7) C18 0.065(8) 0.043(6) 0.040(5) 0.004(4) -0.013(5) -0.021(6) C19 0.039(6) 0.037(6) 0.040(5) 0.001(4) -0.011(5) -0.009(5) C20 0.034(6) 0.070(8) 0.044(6) -0.002(5) 0.007(5) -0.024(6) C21 0.039(3) 0.052(3) 0.067(3) -0.015(2) 0.008(2) 0.002(2) C22 0.039(3) 0.052(3) 0.067(3) -0.015(2) 0.008(2) 0.002(2) C23 0.050(8) 0.050(7) 0.050(6) 0.000(5) 0.000(5) 0.000(5) C24 0.066(10) 0.057(9) 0.135(13) 0.020(8) -0.019(9) 0.000(7) C25 0.077(11) 0.141(14) 0.059(8) -0.003(9) 0.003(7) -0.059(11) C26 0.035(6) 0.045(6) 0.057(7) 0.000(5) 0.006(5) -0.007(5) C27 0.059(8) 0.051(7) 0.068(8) -0.019(6) 0.006(6) 0.003(6) C28 0.046(8) 0.063(8) 0.093(10) -0.030(7) 0.026(7) 0.003(6) C29 0.067(9) 0.058(8) 0.062(7) -0.027(6) 0.019(6) -0.016(7) C30 0.046(7) 0.044(6) 0.040(5) -0.010(4) 0.005(5) -0.013(5) C31 0.043(7) 0.037(6) 0.050(6) -0.007(5) 0.006(5) -0.010(5) C32 0.056(7) 0.047(6) 0.035(5) -0.009(5) 0.011(5) -0.015(5) C33 0.064(8) 0.037(6) 0.031(5) -0.003(4) -0.008(5) 0.000(5) C34 0.083(10) 0.073(8) 0.031(6) -0.012(5) -0.011(6) -0.005(7) C35 0.078(9) 0.044(6) 0.042(6) 0.011(5) -0.006(6) 0.000(6) C36 0.063(8) 0.052(6) 0.031(5) 0.000(4) -0.011(5) -0.014(5) C37 0.059(8) 0.041(6) 0.049(7) -0.005(5) -0.002(6) 0.001(5) C38 0.086(10) 0.055(8) 0.059(7) 0.005(6) -0.005(7) -0.027(7) C39 0.45(5) 0.24(3) 0.19(2) 0.14(2) -0.21(3) -0.30(4) C40 0.33(4) 0.113(16) 0.091(13) 0.026(11) 0.021(17) -0.11(2) C41 0.17(3) 0.059(13) 0.41(5) 0.06(2) 0.08(3) 0.000(14) C42 0.039(6) 0.034(5) 0.042(6) -0.002(4) 0.003(5) -0.006(4) C43 0.061(8) 0.069(8) 0.052(7) 0.011(6) -0.007(6) -0.032(7) C44 0.074(11) 0.162(17) 0.085(10) 0.038(10) 0.002(8) -0.052(11) C45 0.071(11) 0.105(12) 0.138(14) 0.000(11) 0.000(10) -0.043(10) C46 0.075(10) 0.092(11) 0.071(9) 0.007(8) 0.006(8) 0.008(8) C47 0.042(7) 0.054(6) 0.030(5) -0.003(4) 0.002(5) -0.022(5) C48 0.067(8) 0.070(8) 0.036(5) -0.013(5) 0.006(5) -0.036(7) C49 0.074(9) 0.053(7) 0.064(7) -0.004(6) -0.020(6) -0.022(6) C50 0.087(11) 0.084(10) 0.058(7) 0.008(7) -0.026(7) -0.039(8) C51 0.092(12) 0.081(10) 0.095(11) -0.043(8) 0.005(9) -0.030(9) C52 0.066(9) 0.039(6) 0.070(8) -0.004(6) -0.004(7) 0.008(6) C53 0.065(10) 0.067(9) 0.115(12) -0.040(9) 0.026(9) -0.005(7) C54 0.145(18) 0.144(18) 0.121(15) -0.087(14) -0.012(14) 0.030(14) C55 0.118(17) 0.104(15) 0.18(2) -0.040(14) 0.052(15) 0.002(12) C56 0.20(2) 0.056(11) 0.19(2) -0.048(12) 0.065(18) -0.029(12) N1 0.036(5) 0.055(5) 0.035(4) -0.006(4) -0.010(4) -0.006(4) N2 0.032(5) 0.052(5) 0.038(4) -0.004(4) 0.001(4) -0.012(4) N3 0.062(6) 0.035(5) 0.029(4) -0.004(3) 0.004(4) -0.006(4) N4 0.033(5) 0.041(5) 0.030(4) 0.004(3) -0.002(3) -0.010(4) N5 0.036(5) 0.045(5) 0.034(4) -0.002(4) -0.003(4) -0.007(4) N6 0.081(8) 0.074(7) 0.041(5) 0.015(5) -0.005(5) -0.016(6) O1 0.049(5) 0.038(4) 0.056(4) 0.012(3) -0.006(4) 0.001(3) O2 0.041(4) 0.036(4) 0.038(3) -0.001(3) -0.007(3) -0.004(3) O3 0.052(5) 0.035(4) 0.033(3) -0.008(3) 0.002(3) -0.006(3) O4 0.039(3) 0.052(3) 0.067(3) -0.015(2) 0.008(2) 0.002(2) O5 0.059(5) 0.046(4) 0.057(4) -0.008(3) 0.005(4) 0.002(4) O6 0.045(4) 0.032(4) 0.039(4) 0.006(3) -0.003(3) -0.010(3) O7 0.038(4) 0.041(4) 0.032(3) -0.001(3) 0.004(3) -0.003(3) O8 0.106(10) 0.120(10) 0.139(11) -0.024(9) 0.005(8) -0.028(8) O9 0.045(5) 0.060(5) 0.053(5) 0.002(4) 0.000(4) -0.008(4) O10 0.036(4) 0.038(4) 0.037(3) -0.005(3) 0.000(3) -0.001(3) O11 0.039(4) 0.036(4) 0.031(3) 0.001(3) -0.014(3) -0.002(3) O12 0.113(8) 0.060(5) 0.048(5) 0.005(4) -0.026(5) -0.012(5) O13 0.048(5) 0.043(4) 0.040(4) 0.003(3) -0.005(3) -0.013(3) O14 0.039(4) 0.044(4) 0.038(4) 0.001(3) -0.004(3) -0.016(3) O15 0.048(5) 0.042(4) 0.044(4) -0.008(3) 0.004(3) -0.011(3) O16 0.035(4) 0.060(5) 0.037(4) -0.013(3) 0.000(3) -0.007(3) O17 0.079(6) 0.048(4) 0.043(4) -0.003(3) -0.001(4) -0.023(4) O18 0.079(6) 0.042(4) 0.037(4) -0.001(3) -0.004(4) -0.015(4) O19 0.056(5) 0.049(5) 0.071(5) -0.017(4) 0.001(4) 0.003(4) O20 0.089(8) 0.087(8) 0.105(8) -0.032(6) -0.018(7) 0.017(6) O21 0.034(4) 0.032(3) 0.027(3) -0.004(2) 0.001(3) -0.007(3) O22 0.047(5) 0.065(5) 0.042(4) 0.001(3) -0.014(3) 0.000(4) Na1 0.045(3) 0.040(2) 0.044(2) 0.0027(16) 0.0034(18) -0.0046(18) Mn1 0.0328(9) 0.0331(8) 0.0295(7) -0.0007(6) -0.0002(6) -0.0054(6) Mn2 0.0376(9) 0.0343(8) 0.0277(7) -0.0013(6) 0.0005(6) -0.0037(6) Mn3 0.0356(9) 0.0355(8) 0.0292(7) -0.0002(6) -0.0059(6) -0.0060(6) Nd1 0.0469(4) 0.0347(3) 0.0314(3) -0.0006(2) -0.0066(2) -0.0061(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.445(13) . ? C2 O1 1.353(13) . ? C2 C3 1.391(15) . ? C2 C7 1.431(15) . ? C3 C4 1.371(18) . ? C4 C5 1.361(18) . ? C5 C6 1.403(14) . ? C6 C7 1.405(14) . ? C6 C8 1.433(15) . ? C7 O2 1.327(11) . ? C8 N1 1.266(12) . ? C9 C10 1.464(18) . ? C9 C12 1.504(16) . ? C9 N1 1.505(13) . ? C9 C11 1.575(12) . ? C11 O4 1.577(13) . ? C12 O3 1.387(13) . ? C13 O5 1.441(13) . ? C14 C15 1.367(15) . ? C14 O5 1.376(14) . ? C14 C19 1.409(14) . ? C15 C16 1.378(17) . ? C16 C17 1.360(17) . ? C17 C18 1.378(15) . ? C18 C19 1.419(15) . ? C18 C20 1.440(15) . ? C19 O6 1.321(11) . ? C20 N2 1.295(13) . ? C21 N2 1.468(13) . ? C21 C24 1.493(18) . ? C21 C22 1.573(15) . ? C21 C23 1.676(15) . ? C23 O7 1.363(13) . ? C24 O8 1.389(16) . ? C25 O9 1.409(15) . ? C26 C27 1.372(15) . ? C26 O9 1.376(12) . ? C26 C31 1.422(14) . ? C27 C28 1.394(17) . ? C28 C29 1.345(17) . ? C29 C30 1.418(14) . ? C30 C31 1.392(13) . ? C30 C32 1.439(14) . ? C31 O10 1.338(11) . ? C32 N3 1.290(12) . ? C33 N3 1.477(13) . ? C33 C34 1.510(13) . ? C33 C36 1.525(15) . ? C33 C35 1.535(15) . ? C35 O12 1.431(13) . ? C36 O11 1.437(11) . ? C37 O17 1.256(12) . ? C37 O18 1.272(13) . ? C37 C38 1.523(16) . ? C37 Nd1 2.882(12) . ? C38 C40 1.45(2) . ? C38 C41 1.46(3) . ? C38 C39 1.48(2) . ? C42 O13 1.257(11) . ? C42 O14 1.261(12) . ? C42 C43 1.515(15) . ? C43 C46 1.506(17) . ? C43 C44 1.529(17) . ? C43 C45 1.543(19) . ? C47 O15 1.253(11) . ? C47 O16 1.270(12) . ? C47 C48 1.525(14) . ? C48 C51 1.467(16) . ? C48 C49 1.496(15) . ? C48 C50 1.565(18) . ? C52 O19 1.241(14) . ? C52 O20 1.281(15) . ? C52 C53 1.488(17) . ? C53 C56 1.46(2) . ? C53 C55 1.50(2) . ? C53 C54 1.52(2) . ? N1 Mn3 2.013(8) . ? N2 Mn1 1.995(8) . ? N3 Mn2 2.024(7) . ? N4 N5 1.190(10) . ? N4 Mn3 2.256(7) . ? N4 Mn1 2.337(8) . ? N5 N6 1.151(11) . ? O1 Na1 2.425(8) . ? O2 Mn3 1.892(6) . ? O2 Na1 2.337(8) . ? O3 Mn3 1.874(6) . ? O3 Nd1 2.348(6) . ? O5 Na1 2.422(9) . ? O6 Mn1 1.898(6) . ? O6 Na1 2.319(8) . ? O7 Mn1 1.870(6) . ? O7 Nd1 2.457(6) . ? O9 Na1 2.551(8) . ? O10 Mn2 1.882(6) . ? O10 Na1 2.406(7) . ? O11 Mn2 1.871(6) . ? O11 Nd1 2.356(6) . ? O13 Mn3 2.200(7) . ? O14 Mn2 2.355(7) . ? O14 Nd1 2.752(7) . ? O15 Mn2 2.144(7) . ? O16 Mn1 2.163(7) . ? O17 Nd1 2.513(7) . ? O18 Nd1 2.516(6) . ? O19 Nd1 2.368(7) . ? O21 Mn1 1.919(6) . ? O21 Mn2 1.941(5) . ? O21 Mn3 1.974(6) . ? O21 Na1 2.854(7) . ? O21 Nd1 2.881(6) . ? O22 Nd1 2.498(7) . ? Na1 Mn2 3.352(4) . ? Na1 Mn3 3.436(4) . ? Na1 Mn1 3.491(4) . ? Mn1 Mn3 3.129(2) . ? Mn1 Nd1 3.6097(17) . ? Mn2 Nd1 3.3853(17) . ? Mn3 Nd1 3.5609(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C2 C3 123.7(11) . . ? O1 C2 C7 114.3(9) . . ? C3 C2 C7 121.9(12) . . ? C4 C3 C2 117.3(12) . . ? C5 C4 C3 123.1(12) . . ? C4 C5 C6 120.6(13) . . ? C5 C6 C7 119.1(11) . . ? C5 C6 C8 118.9(10) . . ? C7 C6 C8 122.0(9) . . ? O2 C7 C6 125.0(9) . . ? O2 C7 C2 117.3(10) . . ? C6 C7 C2 117.8(9) . . ? N1 C8 C6 126.4(10) . . ? C10 C9 C12 117.2(12) . . ? C10 C9 N1 116.7(11) . . ? C12 C9 N1 104.0(9) . . ? C10 C9 C11 112.1(14) . . ? C12 C9 C11 100.7(10) . . ? N1 C9 C11 104.1(8) . . ? C9 C11 O4 96.1(8) . . ? O3 C12 C9 112.0(10) . . ? C15 C14 O5 125.5(11) . . ? C15 C14 C19 120.5(12) . . ? O5 C14 C19 114.0(9) . . ? C14 C15 C16 121.0(11) . . ? C17 C16 C15 119.6(11) . . ? C16 C17 C18 121.6(12) . . ? C17 C18 C19 119.6(11) . . ? C17 C18 C20 118.5(11) . . ? C19 C18 C20 121.6(9) . . ? O6 C19 C14 118.7(10) . . ? O6 C19 C18 123.7(9) . . ? C14 C19 C18 117.6(9) . . ? N2 C20 C18 126.5(10) . . ? N2 C21 C24 108.0(10) . . ? N2 C21 C22 108.5(9) . . ? C24 C21 C22 110.5(11) . . ? N2 C21 C23 104.2(8) . . ? C24 C21 C23 97.6(10) . . ? C22 C21 C23 126.6(9) . . ? O7 C23 C21 104.7(8) . . ? O8 C24 C21 110.6(12) . . ? C27 C26 O9 120.8(10) . . ? C27 C26 C31 121.3(10) . . ? O9 C26 C31 117.9(9) . . ? C26 C27 C28 118.6(11) . . ? C29 C28 C27 122.2(11) . . ? C28 C29 C30 119.9(11) . . ? C31 C30 C29 119.6(10) . . ? C31 C30 C32 122.9(9) . . ? C29 C30 C32 117.5(9) . . ? O10 C31 C30 124.5(9) . . ? O10 C31 C26 117.2(9) . . ? C30 C31 C26 118.3(9) . . ? N3 C32 C30 126.1(9) . . ? N3 C33 C34 115.0(8) . . ? N3 C33 C36 103.9(7) . . ? C34 C33 C36 110.9(10) . . ? N3 C33 C35 105.7(9) . . ? C34 C33 C35 111.3(9) . . ? C36 C33 C35 109.6(9) . . ? O12 C35 C33 113.4(10) . . ? O11 C36 C33 109.7(8) . . ? O17 C37 O18 121.0(10) . . ? O17 C37 C38 119.1(11) . . ? O18 C37 C38 119.8(10) . . ? O17 C37 Nd1 60.5(6) . . ? O18 C37 Nd1 60.6(5) . . ? C38 C37 Nd1 174.5(9) . . ? C40 C38 C41 103.5(19) . . ? C40 C38 C39 114.2(19) . . ? C41 C38 C39 111(2) . . ? C40 C38 C37 110.8(12) . . ? C41 C38 C37 105.3(13) . . ? C39 C38 C37 111.7(11) . . ? O13 C42 O14 125.3(9) . . ? O13 C42 C43 115.9(9) . . ? O14 C42 C43 118.8(9) . . ? C46 C43 C42 111.0(10) . . ? C46 C43 C44 109.0(12) . . ? C42 C43 C44 111.8(10) . . ? C46 C43 C45 110.1(12) . . ? C42 C43 C45 106.6(10) . . ? C44 C43 C45 108.3(12) . . ? O15 C47 O16 124.4(9) . . ? O15 C47 C48 117.6(9) . . ? O16 C47 C48 117.9(9) . . ? C51 C48 C49 111.5(11) . . ? C51 C48 C47 112.4(10) . . ? C49 C48 C47 108.9(8) . . ? C51 C48 C50 108.2(10) . . ? C49 C48 C50 109.7(10) . . ? C47 C48 C50 105.9(10) . . ? O19 C52 O20 123.8(12) . . ? O19 C52 C53 120.6(13) . . ? O20 C52 C53 115.7(12) . . ? C56 C53 C52 108.0(14) . . ? C56 C53 C55 113.1(15) . . ? C52 C53 C55 113.8(14) . . ? C56 C53 C54 105.5(18) . . ? C52 C53 C54 109.6(12) . . ? C55 C53 C54 106.5(16) . . ? C8 N1 C9 120.7(9) . . ? C8 N1 Mn3 126.2(8) . . ? C9 N1 Mn3 113.0(6) . . ? C20 N2 C21 122.8(9) . . ? C20 N2 Mn1 124.5(7) . . ? C21 N2 Mn1 112.7(7) . . ? C32 N3 C33 121.2(8) . . ? C32 N3 Mn2 124.7(7) . . ? C33 N3 Mn2 114.0(6) . . ? N5 N4 Mn3 128.2(6) . . ? N5 N4 Mn1 118.9(6) . . ? Mn3 N4 Mn1 85.9(2) . . ? N6 N5 N4 177.2(11) . . ? C2 O1 C1 116.3(9) . . ? C2 O1 Na1 119.7(6) . . ? C1 O1 Na1 122.9(7) . . ? C7 O2 Mn3 128.9(7) . . ? C7 O2 Na1 122.4(6) . . ? Mn3 O2 Na1 108.2(3) . . ? C12 O3 Mn3 114.2(6) . . ? C12 O3 Nd1 128.6(6) . . ? Mn3 O3 Nd1 114.6(3) . . ? C14 O5 C13 117.9(10) . . ? C14 O5 Na1 117.2(6) . . ? C13 O5 Na1 124.7(9) . . ? C19 O6 Mn1 126.2(6) . . ? C19 O6 Na1 120.7(6) . . ? Mn1 O6 Na1 111.4(3) . . ? C23 O7 Mn1 117.0(6) . . ? C23 O7 Nd1 126.3(6) . . ? Mn1 O7 Nd1 112.4(3) . . ? C26 O9 C25 111.1(9) . . ? C26 O9 Na1 109.0(6) . . ? C25 O9 Na1 105.5(8) . . ? C31 O10 Mn2 128.2(6) . . ? C31 O10 Na1 114.8(5) . . ? Mn2 O10 Na1 102.1(3) . . ? C36 O11 Mn2 113.5(6) . . ? C36 O11 Nd1 137.3(6) . . ? Mn2 O11 Nd1 105.9(3) . . ? C42 O13 Mn3 121.1(6) . . ? C42 O14 Mn2 116.5(6) . . ? C42 O14 Nd1 131.9(6) . . ? Mn2 O14 Nd1 82.6(2) . . ? C47 O15 Mn2 125.0(6) . . ? C47 O16 Mn1 123.8(6) . . ? C37 O17 Nd1 93.8(7) . . ? C37 O18 Nd1 93.2(6) . . ? C52 O19 Nd1 142.8(8) . . ? Mn1 O21 Mn2 119.1(3) . . ? Mn1 O21 Mn3 107.0(3) . . ? Mn2 O21 Mn3 133.7(3) . . ? Mn1 O21 Na1 91.9(2) . . ? Mn2 O21 Na1 86.5(2) . . ? Mn3 O21 Na1 88.8(2) . . ? Mn1 O21 Nd1 95.4(2) . . ? Mn2 O21 Nd1 86.88(19) . . ? Mn3 O21 Nd1 92.4(2) . . ? Na1 O21 Nd1 171.9(2) . . ? O6 Na1 O2 92.2(3) . . ? O6 Na1 O10 116.1(3) . . ? O2 Na1 O10 98.3(3) . . ? O6 Na1 O5 66.7(3) . . ? O2 Na1 O5 140.8(3) . . ? O10 Na1 O5 120.4(3) . . ? O6 Na1 O1 110.0(3) . . ? O2 Na1 O1 66.1(3) . . ? O10 Na1 O1 131.8(3) . . ? O5 Na1 O1 89.7(3) . . ? O6 Na1 O9 164.2(3) . . ? O2 Na1 O9 103.2(3) . . ? O10 Na1 O9 65.3(2) . . ? O5 Na1 O9 98.7(3) . . ? O1 Na1 O9 74.2(3) . . ? O6 Na1 O21 63.8(2) . . ? O2 Na1 O21 66.5(2) . . ? O10 Na1 O21 63.9(2) . . ? O5 Na1 O21 123.3(3) . . ? O1 Na1 O21 131.8(3) . . ? O9 Na1 O21 125.5(2) . . ? O6 Na1 Mn2 83.57(18) . . ? O2 Na1 Mn2 93.32(19) . . ? O10 Na1 Mn2 33.29(16) . . ? O5 Na1 Mn2 115.2(2) . . ? O1 Na1 Mn2 155.0(2) . . ? O9 Na1 Mn2 98.55(19) . . ? O21 Na1 Mn2 35.31(12) . . ? O6 Na1 Mn3 77.97(19) . . ? O2 Na1 Mn3 31.53(16) . . ? O10 Na1 Mn3 79.66(18) . . ? O5 Na1 Mn3 144.2(2) . . ? O1 Na1 Mn3 97.4(2) . . ? O9 Na1 Mn3 117.1(2) . . ? O21 Na1 Mn3 35.06(12) . . ? Mn2 Na1 Mn3 64.05(8) . . ? O6 Na1 Mn1 30.42(16) . . ? O2 Na1 Mn1 78.19(19) . . ? O10 Na1 Mn1 91.31(18) . . ? O5 Na1 Mn1 94.0(2) . . ? O1 Na1 Mn1 125.7(2) . . ? O9 Na1 Mn1 156.6(2) . . ? O21 Na1 Mn1 33.33(13) . . ? Mn2 Na1 Mn1 58.17(7) . . ? Mn3 Na1 Mn1 53.71(7) . . ? O7 Mn1 O6 175.4(3) . . ? O7 Mn1 O21 91.3(3) . . ? O6 Mn1 O21 93.0(3) . . ? O7 Mn1 N2 83.7(3) . . ? O6 Mn1 N2 91.8(3) . . ? O21 Mn1 N2 169.3(3) . . ? O7 Mn1 O16 92.3(3) . . ? O6 Mn1 O16 88.4(3) . . ? O21 Mn1 O16 102.3(2) . . ? N2 Mn1 O16 87.4(3) . . ? O7 Mn1 N4 89.3(3) . . ? O6 Mn1 N4 89.6(3) . . ? O21 Mn1 N4 83.1(2) . . ? N2 Mn1 N4 87.4(3) . . ? O16 Mn1 N4 174.3(3) . . ? O7 Mn1 Mn3 90.2(2) . . ? O6 Mn1 Mn3 92.3(2) . . ? O21 Mn1 Mn3 37.11(17) . . ? N2 Mn1 Mn3 133.1(2) . . ? O16 Mn1 Mn3 139.43(18) . . ? N4 Mn1 Mn3 45.97(18) . . ? O7 Mn1 Na1 146.0(2) . . ? O6 Mn1 Na1 38.2(2) . . ? O21 Mn1 Na1 54.81(18) . . ? N2 Mn1 Na1 129.3(3) . . ? O16 Mn1 Na1 96.59(19) . . ? N4 Mn1 Na1 85.1(2) . . ? Mn3 Mn1 Na1 62.26(8) . . ? O7 Mn1 Nd1 39.0(2) . . ? O6 Mn1 Nd1 145.4(2) . . ? O21 Mn1 Nd1 52.62(17) . . ? N2 Mn1 Nd1 122.7(2) . . ? O16 Mn1 Nd1 95.16(19) . . ? N4 Mn1 Nd1 89.50(18) . . ? Mn3 Mn1 Nd1 63.33(4) . . ? Na1 Mn1 Nd1 107.35(7) . . ? O11 Mn2 O10 172.5(3) . . ? O11 Mn2 O21 91.4(3) . . ? O10 Mn2 O21 94.5(3) . . ? O11 Mn2 N3 82.1(3) . . ? O10 Mn2 N3 91.6(3) . . ? O21 Mn2 N3 172.1(3) . . ? O11 Mn2 O15 94.0(3) . . ? O10 Mn2 O15 89.8(3) . . ? O21 Mn2 O15 97.8(2) . . ? N3 Mn2 O15 87.2(3) . . ? O11 Mn2 O14 80.9(3) . . ? O10 Mn2 O14 95.5(3) . . ? O21 Mn2 O14 80.0(2) . . ? N3 Mn2 O14 94.4(3) . . ? O15 Mn2 O14 174.4(3) . . ? O11 Mn2 Na1 142.9(2) . . ? O10 Mn2 Na1 44.6(2) . . ? O21 Mn2 Na1 58.19(18) . . ? N3 Mn2 Na1 129.5(2) . . ? O15 Mn2 Na1 72.1(2) . . ? O14 Mn2 Na1 110.62(17) . . ? O11 Mn2 Nd1 42.01(19) . . ? O10 Mn2 Nd1 139.6(2) . . ? O21 Mn2 Nd1 58.19(17) . . ? N3 Mn2 Nd1 114.0(2) . . ? O15 Mn2 Nd1 120.7(2) . . ? O14 Mn2 Nd1 53.73(17) . . ? Na1 Mn2 Nd1 116.23(8) . . ? O3 Mn3 O2 173.3(3) . . ? O3 Mn3 O21 90.2(3) . . ? O2 Mn3 O21 96.3(3) . . ? O3 Mn3 N1 82.3(3) . . ? O2 Mn3 N1 91.1(3) . . ? O21 Mn3 N1 171.1(3) . . ? O3 Mn3 O13 92.0(3) . . ? O2 Mn3 O13 89.4(3) . . ? O21 Mn3 O13 93.4(2) . . ? N1 Mn3 O13 91.6(3) . . ? O3 Mn3 N4 89.7(3) . . ? O2 Mn3 N4 89.2(3) . . ? O21 Mn3 N4 84.1(3) . . ? N1 Mn3 N4 91.2(3) . . ? O13 Mn3 N4 176.9(3) . . ? O3 Mn3 Mn1 89.7(2) . . ? O2 Mn3 Mn1 94.5(2) . . ? O21 Mn3 Mn1 35.91(17) . . ? N1 Mn3 Mn1 138.7(2) . . ? O13 Mn3 Mn1 129.30(18) . . ? N4 Mn3 Mn1 48.15(19) . . ? O3 Mn3 Na1 146.3(2) . . ? O2 Mn3 Na1 40.2(2) . . ? O21 Mn3 Na1 56.15(18) . . ? N1 Mn3 Na1 131.3(3) . . ? O13 Mn3 Na1 89.55(19) . . ? N4 Mn3 Na1 87.6(2) . . ? Mn1 Mn3 Na1 64.04(8) . . ? O3 Mn3 Nd1 36.84(19) . . ? O2 Mn3 Nd1 149.8(2) . . ? O21 Mn3 Nd1 53.94(17) . . ? N1 Mn3 Nd1 119.0(2) . . ? O13 Mn3 Nd1 87.82(17) . . ? N4 Mn3 Nd1 92.05(19) . . ? Mn1 Mn3 Nd1 64.93(4) . . ? Na1 Mn3 Nd1 109.68(8) . . ? O3 Nd1 O11 121.8(2) . . ? O3 Nd1 O19 83.3(2) . . ? O11 Nd1 O19 147.7(3) . . ? O3 Nd1 O7 81.1(2) . . ? O11 Nd1 O7 83.9(2) . . ? O19 Nd1 O7 80.2(2) . . ? O3 Nd1 O22 151.5(2) . . ? O11 Nd1 O22 75.2(2) . . ? O19 Nd1 O22 74.1(3) . . ? O7 Nd1 O22 78.2(2) . . ? O3 Nd1 O17 74.9(2) . . ? O11 Nd1 O17 126.0(2) . . ? O19 Nd1 O17 77.2(3) . . ? O7 Nd1 O17 148.7(2) . . ? O22 Nd1 O17 115.4(3) . . ? O3 Nd1 O18 124.9(2) . . ? O11 Nd1 O18 85.4(2) . . ? O19 Nd1 O18 96.5(3) . . ? O7 Nd1 O18 153.5(2) . . ? O22 Nd1 O18 75.7(3) . . ? O17 Nd1 O18 51.9(2) . . ? O3 Nd1 O14 74.6(2) . . ? O11 Nd1 O14 65.0(2) . . ? O19 Nd1 O14 146.9(2) . . ? O7 Nd1 O14 119.3(2) . . ? O22 Nd1 O14 133.0(2) . . ? O17 Nd1 O14 73.4(2) . . ? O18 Nd1 O14 77.1(2) . . ? O3 Nd1 O21 61.85(19) . . ? O11 Nd1 O21 61.85(17) . . ? O19 Nd1 O21 129.5(2) . . ? O7 Nd1 O21 60.37(19) . . ? O22 Nd1 O21 121.5(2) . . ? O17 Nd1 O21 121.6(2) . . ? O18 Nd1 O21 132.8(2) . . ? O14 Nd1 O21 59.07(17) . . ? O3 Nd1 C37 100.0(3) . . ? O11 Nd1 C37 107.1(3) . . ? O19 Nd1 C37 85.6(3) . . ? O7 Nd1 C37 165.6(3) . . ? O22 Nd1 C37 95.4(3) . . ? O17 Nd1 C37 25.8(3) . . ? O18 Nd1 C37 26.1(3) . . ? O14 Nd1 C37 74.5(3) . . ? O21 Nd1 C37 132.9(3) . . ? O3 Nd1 Mn2 90.07(15) . . ? O11 Nd1 Mn2 32.11(14) . . ? O19 Nd1 Mn2 162.4(2) . . ? O7 Nd1 Mn2 82.64(15) . . ? O22 Nd1 Mn2 106.31(18) . . ? O17 Nd1 Mn2 116.86(19) . . ? O18 Nd1 Mn2 100.63(17) . . ? O14 Nd1 Mn2 43.62(14) . . ? O21 Nd1 Mn2 34.93(11) . . ? C37 Nd1 Mn2 111.7(2) . . ? O3 Nd1 Mn3 28.60(15) . . ? O11 Nd1 Mn3 93.44(14) . . ? O19 Nd1 Mn3 107.95(19) . . ? O7 Nd1 Mn3 72.07(16) . . ? O22 Nd1 Mn3 149.15(17) . . ? O17 Nd1 Mn3 94.58(18) . . ? O18 Nd1 Mn3 132.84(19) . . ? O14 Nd1 Mn3 60.23(13) . . ? O21 Nd1 Mn3 33.64(12) . . ? C37 Nd1 Mn3 115.5(2) . . ? Mn2 Nd1 Mn3 62.38(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.381 _refine_diff_density_min -5.164 _refine_diff_density_rms 0.191 #===END _database_code_depnum_ccdc_archive 'CCDC 947814'