# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ghosh, Ashutosh' _publ_contact_author_email 'ghosh 59@yahoo.com' _publ_section_title ; Structure and magnetic properties of an unprecedented syn-anti u-nitrito-1kO:2kO' bridged Mn(III)-salen complex and its isoelectronic and isostructural formate analogue ; _publ_author_name 'Ashutosh Ghosh' data_1 _database_code_depnum_ccdc_archive 'CCDC 799078' #TrackingRef '- all 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 Mn3 N6 O12' _chemical_formula_weight 1098.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Mn Mn 0.3368 0.7283 '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 13.8053(16) _cell_length_b 13.8932(18) _cell_length_c 14.0281(16) _cell_angle_alpha 103.698(10) _cell_angle_beta 106.301(10) _cell_angle_gamma 104.191(11) _cell_volume 2364.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16595 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 30.00 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number n/a _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 16595 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13129 _reflns_number_gt 8315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.1389P)^2^+3.9567P] 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 13129 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.2672 _refine_ls_wR_factor_gt 0.2593 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.76180(6) 0.13113(6) 0.99389(6) 0.02935(19) Uani 1 1 d . . . Mn2 Mn 0.51427(6) -0.23384(6) 0.66784(6) 0.02835(19) Uani 1 1 d . . . Mn3 Mn 1.12963(6) 0.51624(6) 1.28752(6) 0.02788(18) Uani 1 1 d . . . O50 O 0.6069(3) -0.2043(3) 0.5930(3) 0.0360(8) Uani 1 1 d . . . C49 C 0.6490(4) -0.1144(4) 0.5802(4) 0.0364(11) Uani 1 1 d . . . C48 C 0.7288(5) -0.1063(5) 0.5344(5) 0.0435(13) Uani 1 1 d . . . H48 H 0.7524 -0.1630 0.5175 0.052 Uiso 1 1 calc R . . C47 C 0.7722(5) -0.0158(5) 0.5141(5) 0.0517(16) Uani 1 1 d . . . H47 H 0.8225 -0.0138 0.4816 0.062 Uiso 1 1 calc R . . C12 C 0.8303(4) 0.0237(4) 1.1419(4) 0.0331(11) Uani 1 1 d . . . C13 C 0.8033(5) -0.0423(4) 1.2003(4) 0.0392(12) Uani 1 1 d . . . H13 H 0.7332 -0.0648 1.1979 0.047 Uiso 1 1 calc R . . C14 C 0.8792(5) -0.0737(5) 1.2607(5) 0.0444(14) Uani 1 1 d . . . H14 H 0.8595 -0.1163 1.2989 0.053 Uiso 1 1 calc R . . C15 C 0.9846(5) -0.0428(5) 1.2654(5) 0.0469(14) Uani 1 1 d . . . H15 H 1.0350 -0.0636 1.3074 0.056 Uiso 1 1 calc R . . C16 C 1.0140(5) 0.0185(5) 1.2080(5) 0.0418(13) Uani 1 1 d . . . H16 H 1.0846 0.0385 1.2113 0.050 Uiso 1 1 calc R . . C17 C 0.9378(4) 0.0528(4) 1.1423(4) 0.0353(11) Uani 1 1 d . . . C18 C 0.9747(4) 0.1132(4) 1.0827(4) 0.0349(11) Uani 1 1 d . . . H18 H 1.0469 0.1302 1.0915 0.042 Uiso 1 1 calc R . . C20 C 0.9623(4) 0.2112(4) 0.9632(5) 0.0367(11) Uani 1 1 d . . . H20A H 1.0180 0.1886 0.9456 0.044 Uiso 1 1 calc R . . H20B H 0.9940 0.2840 1.0085 0.044 Uiso 1 1 calc R . . C21 C 0.8741(4) 0.2011(5) 0.8628(4) 0.0364(11) Uani 1 1 d . . . H21A H 0.8969 0.2575 0.8359 0.044 Uiso 1 1 calc R . . H21B H 0.8556 0.1343 0.8089 0.044 Uiso 1 1 calc R . . C23 C 0.7254(4) 0.2643(4) 0.8633(4) 0.0347(11) Uani 1 1 d . . . H23 H 0.7444 0.3004 0.8197 0.042 Uiso 1 1 calc R . . C24 C 0.6354(4) 0.2739(4) 0.8922(4) 0.0360(11) Uani 1 1 d . . . C26 C 0.5191(6) 0.3763(6) 0.9079(6) 0.0576(18) Uani 1 1 d . . . H26 H 0.4990 0.4341 0.9007 0.069 Uiso 1 1 calc R . . C27 C 0.4688(6) 0.3109(8) 0.9519(6) 0.069(2) Uani 1 1 d . . . H27 H 0.4137 0.3242 0.9725 0.082 Uiso 1 1 calc R . . C28 C 0.4997(5) 0.2224(7) 0.9665(5) 0.0568(19) Uani 1 1 d . . . H28 H 0.4626 0.1765 0.9930 0.068 Uiso 1 1 calc R . . C29 C 0.5867(4) 0.2064(5) 0.9403(4) 0.0376(12) Uani 1 1 d . . . C32 C 0.4529(4) -0.4471(4) 0.6716(4) 0.0322(10) Uani 1 1 d . . . C33 C 0.4534(4) -0.5511(4) 0.6353(4) 0.0361(11) Uani 1 1 d . . . H33 H 0.4980 -0.5642 0.5986 0.043 Uiso 1 1 calc R . . C34 C 0.3905(5) -0.6329(5) 0.6526(5) 0.0434(13) Uani 1 1 d . . . H34 H 0.3931 -0.7001 0.6281 0.052 Uiso 1 1 calc R . . C35 C 0.3221(5) -0.6159(5) 0.7070(5) 0.0473(15) Uani 1 1 d . . . H35 H 0.2786 -0.6720 0.7176 0.057 Uiso 1 1 calc R . . C36 C 0.3191(5) -0.5178(5) 0.7443(5) 0.0410(13) Uani 1 1 d . . . H36 H 0.2744 -0.5072 0.7815 0.049 Uiso 1 1 calc R . . C37 C 0.3830(4) -0.4304(4) 0.7278(4) 0.0341(11) Uani 1 1 d . . . C38 C 0.3762(4) -0.3285(5) 0.7707(4) 0.0353(11) Uani 1 1 d . . . H38 H 0.3343 -0.3233 0.8119 0.042 Uiso 1 1 calc R . . C40 C 0.4164(5) -0.1415(5) 0.8077(5) 0.0403(12) Uani 1 1 d . . . H40A H 0.4793 -0.1020 0.8706 0.048 Uiso 1 1 calc R . . H40B H 0.3536 -0.1516 0.8274 0.048 Uiso 1 1 calc R . . C41 C 0.4088(5) -0.0833(5) 0.7294(5) 0.0411(13) Uani 1 1 d . . . H41A H 0.3381 -0.1128 0.6751 0.049 Uiso 1 1 calc R . . H41B H 0.4219 -0.0096 0.7641 0.049 Uiso 1 1 calc R . . N42 N 0.4913(3) -0.0948(3) 0.6828(4) 0.0336(9) Uani 1 1 d . . . C72 C 0.7165(4) -0.1002(4) 0.8728(4) 0.0354(11) Uani 1 1 d . . . H72 H 0.7706 -0.0978 0.9314 0.042 Uiso 1 1 calc R . . C75 C 0.3577(4) -0.3009(4) 0.4371(4) 0.0316(10) Uani 1 1 d . . . H75 H 0.4206 -0.2637 0.4315 0.038 Uiso 1 1 calc R . . C78 C 0.8952(4) 0.3585(4) 1.1861(4) 0.0321(10) Uani 1 1 d . . . H78 H 0.8843 0.4167 1.2243 0.039 Uiso 1 1 calc R . . C52 C 1.0434(4) 0.6597(4) 1.3941(4) 0.0315(10) Uani 1 1 d . . . C53 C 0.9967(4) 0.7394(4) 1.3911(4) 0.0358(11) Uani 1 1 d . . . H53 H 0.9648 0.7471 1.3268 0.043 Uiso 1 1 calc R . . C54 C 0.9975(5) 0.8062(4) 1.4825(5) 0.0405(12) Uani 1 1 d . . . H54 H 0.9652 0.8572 1.4786 0.049 Uiso 1 1 calc R . . C55 C 1.0473(5) 0.7973(5) 1.5816(5) 0.0401(12) Uani 1 1 d . . . H55 H 1.0492 0.8428 1.6431 0.048 Uiso 1 1 calc R . . C56 C 1.0922(4) 0.7206(5) 1.5848(4) 0.0375(12) Uani 1 1 d . . . H56 H 1.1249 0.7147 1.6497 0.045 Uiso 1 1 calc R . . C57 C 1.0912(4) 0.6496(4) 1.4934(4) 0.0331(10) Uani 1 1 d . . . C58 C 1.1332(4) 0.5657(4) 1.5026(4) 0.0339(11) Uani 1 1 d . . . H58 H 1.1550 0.5583 1.5687 0.041 Uiso 1 1 calc R . . C60 C 1.1852(4) 0.4145(4) 1.4435(5) 0.0348(11) Uani 1 1 d . . . H60A H 1.1283 0.3470 1.4096 0.042 Uiso 1 1 calc R . . H60B H 1.2153 0.4248 1.5179 0.042 Uiso 1 1 calc R . . C61 C 1.2701(4) 0.4183(4) 1.3957(4) 0.0333(11) Uani 1 1 d . . . H61A H 1.3342 0.4779 1.4396 0.040 Uiso 1 1 calc R . . H61B H 1.2885 0.3546 1.3887 0.040 Uiso 1 1 calc R . . N62 N 1.2251(3) 0.4287(3) 1.2907(3) 0.0287(8) Uani 1 1 d . . . C63 C 1.2504(4) 0.3868(4) 1.2126(4) 0.0311(10) Uani 1 1 d . . . H63 H 1.2954 0.3473 1.2235 0.037 Uiso 1 1 calc R . . C64 C 1.2138(4) 0.3971(4) 1.1100(4) 0.0298(10) Uani 1 1 d . . . C65 C 1.2409(4) 0.3387(4) 1.0315(4) 0.0347(11) Uani 1 1 d . . . H66 H 1.2814 0.2965 1.0483 0.042 Uiso 1 1 calc R . . C66 C 1.2094(4) 0.3419(5) 0.9296(5) 0.0379(12) Uani 1 1 d . . . H67 H 1.2276 0.3019 0.8785 0.045 Uiso 1 1 calc R . . C67 C 1.1494(4) 0.4070(4) 0.9055(4) 0.0342(11) Uani 1 1 d . . . H68 H 1.1272 0.4096 0.8374 0.041 Uiso 1 1 calc R . . C68 C 1.1229(4) 0.4674(4) 0.9812(4) 0.0335(11) Uani 1 1 d . . . H69 H 1.0846 0.5111 0.9636 0.040 Uiso 1 1 calc R . . C69 C 1.1533(4) 0.4636(4) 1.0858(4) 0.0296(10) Uani 1 1 d . . . O11 O 0.7558(3) 0.0531(3) 1.0880(3) 0.0366(8) Uani 1 1 d . . . O30 O 0.6181(3) 0.1281(3) 0.9606(3) 0.0384(9) Uani 1 1 d . . . O31 O 0.5154(3) -0.3732(3) 0.6513(3) 0.0329(8) Uani 1 1 d . . . O71 O 0.6535(3) -0.1889(3) 0.8161(3) 0.0401(9) Uani 1 1 d . . . O73 O 0.7171(3) -0.0150(3) 0.8620(3) 0.0440(10) Uani 1 1 d . . . O74 O 0.3632(3) -0.3040(3) 0.5272(3) 0.0404(9) Uani 1 1 d . . . O76 O 0.2779(3) -0.3418(3) 0.3546(3) 0.0403(9) Uani 1 1 d . . . O77 O 0.8119(3) 0.2840(3) 1.1253(3) 0.0364(8) Uani 1 1 d . . . O79 O 0.9898(3) 0.3656(3) 1.2025(3) 0.0368(8) Uani 1 1 d . . . O51 O 1.0410(3) 0.5996(3) 1.3039(3) 0.0349(8) Uani 1 1 d . . . O70 O 1.1260(3) 0.5234(3) 1.1549(3) 0.0307(7) Uani 1 1 d . . . N19 N 0.9161(3) 0.1463(3) 1.0174(3) 0.0306(9) Uani 1 1 d . . . N22 N 0.7812(3) 0.2079(3) 0.8950(3) 0.0306(9) Uani 1 1 d . . . N39 N 0.4235(3) -0.2441(4) 0.7565(4) 0.0344(9) Uani 1 1 d . . . N59 N 1.1432(3) 0.5002(3) 1.4272(3) 0.0303(9) Uani 1 1 d . . . C25 C 0.5985(5) 0.3570(5) 0.8747(6) 0.0483(15) Uani 1 1 d . . . H25 H 0.6285 0.3986 0.8404 0.058 Uiso 1 1 calc R . . C44 C 0.6199(4) -0.0238(4) 0.6095(5) 0.0387(12) Uani 1 1 d . . . C45 C 0.6663(5) 0.0678(5) 0.5886(5) 0.0479(15) Uani 1 1 d . . . H45 H 0.6453 0.1261 0.6070 0.057 Uiso 1 1 calc R . . C43 C 0.5408(5) -0.0207(5) 0.6580(5) 0.0409(13) Uani 1 1 d . . . H43 H 0.5248 0.0411 0.6724 0.049 Uiso 1 1 calc R . . C46 C 0.7417(5) 0.0729(6) 0.5418(6) 0.0531(17) Uani 1 1 d . . . H46 H 0.7717 0.1338 0.5288 0.064 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 Mn1 0.0229(3) 0.0301(4) 0.0312(4) 0.0125(3) 0.0061(3) 0.0042(3) Mn2 0.0246(3) 0.0265(4) 0.0293(4) 0.0092(3) 0.0056(3) 0.0054(3) Mn3 0.0275(3) 0.0282(4) 0.0240(4) 0.0102(3) 0.0028(3) 0.0087(3) O50 0.0314(18) 0.0312(19) 0.042(2) 0.0118(16) 0.0142(16) 0.0047(14) C49 0.026(2) 0.037(3) 0.033(3) 0.010(2) 0.001(2) 0.000(2) C48 0.037(3) 0.040(3) 0.044(3) 0.011(3) 0.014(2) 0.001(2) C47 0.043(3) 0.048(4) 0.051(4) 0.020(3) 0.012(3) -0.004(3) C12 0.036(3) 0.031(3) 0.023(2) 0.0048(19) 0.0026(19) 0.009(2) C13 0.045(3) 0.035(3) 0.031(3) 0.012(2) 0.006(2) 0.009(2) C14 0.060(4) 0.036(3) 0.035(3) 0.011(2) 0.009(3) 0.021(3) C15 0.054(4) 0.045(3) 0.038(3) 0.013(3) 0.006(3) 0.023(3) C16 0.040(3) 0.050(3) 0.032(3) 0.012(2) 0.004(2) 0.022(3) C17 0.036(3) 0.037(3) 0.026(2) 0.007(2) 0.002(2) 0.015(2) C18 0.027(2) 0.034(3) 0.034(3) 0.003(2) 0.006(2) 0.007(2) C20 0.025(2) 0.036(3) 0.042(3) 0.009(2) 0.011(2) 0.003(2) C21 0.034(3) 0.037(3) 0.037(3) 0.011(2) 0.015(2) 0.008(2) C23 0.032(2) 0.031(3) 0.034(3) 0.013(2) 0.007(2) 0.003(2) C24 0.033(2) 0.038(3) 0.030(3) 0.011(2) 0.002(2) 0.010(2) C26 0.046(3) 0.072(5) 0.055(4) 0.019(4) 0.007(3) 0.035(3) C27 0.046(4) 0.117(7) 0.060(5) 0.037(5) 0.016(3) 0.051(4) C28 0.037(3) 0.103(6) 0.045(4) 0.038(4) 0.014(3) 0.035(4) C29 0.029(2) 0.052(3) 0.027(3) 0.013(2) 0.004(2) 0.013(2) C32 0.026(2) 0.033(3) 0.029(2) 0.011(2) 0.0018(19) 0.0034(19) C33 0.037(3) 0.033(3) 0.034(3) 0.013(2) 0.007(2) 0.007(2) C34 0.043(3) 0.032(3) 0.045(3) 0.016(3) 0.004(3) 0.006(2) C35 0.038(3) 0.044(3) 0.050(4) 0.022(3) 0.007(3) 0.000(2) C36 0.036(3) 0.044(3) 0.040(3) 0.021(3) 0.011(2) 0.004(2) C37 0.032(2) 0.039(3) 0.027(2) 0.013(2) 0.006(2) 0.007(2) C38 0.032(2) 0.043(3) 0.029(3) 0.014(2) 0.008(2) 0.009(2) C40 0.044(3) 0.039(3) 0.038(3) 0.011(2) 0.014(2) 0.017(2) C41 0.037(3) 0.038(3) 0.052(4) 0.016(3) 0.018(3) 0.017(2) N42 0.030(2) 0.030(2) 0.036(2) 0.0103(18) 0.0068(18) 0.0084(17) C72 0.033(2) 0.031(3) 0.030(3) 0.007(2) -0.001(2) 0.008(2) C75 0.028(2) 0.027(2) 0.036(3) 0.015(2) 0.007(2) 0.0046(18) C78 0.033(2) 0.027(2) 0.033(3) 0.009(2) 0.010(2) 0.0091(19) C52 0.026(2) 0.029(2) 0.033(3) 0.008(2) 0.0070(19) 0.0033(18) C53 0.033(2) 0.033(3) 0.035(3) 0.009(2) 0.006(2) 0.011(2) C54 0.037(3) 0.032(3) 0.048(3) 0.007(2) 0.017(3) 0.008(2) C55 0.044(3) 0.034(3) 0.038(3) 0.008(2) 0.018(2) 0.008(2) C56 0.037(3) 0.040(3) 0.029(3) 0.008(2) 0.010(2) 0.006(2) C57 0.029(2) 0.035(3) 0.032(3) 0.011(2) 0.010(2) 0.005(2) C58 0.026(2) 0.039(3) 0.031(3) 0.015(2) 0.0046(19) 0.005(2) C60 0.033(2) 0.033(3) 0.038(3) 0.018(2) 0.008(2) 0.010(2) C61 0.036(2) 0.037(3) 0.023(2) 0.017(2) 0.0003(19) 0.011(2) N62 0.0251(18) 0.028(2) 0.030(2) 0.0143(17) 0.0046(16) 0.0051(15) C63 0.024(2) 0.031(2) 0.033(3) 0.011(2) 0.0028(19) 0.0087(18) C64 0.025(2) 0.029(2) 0.032(2) 0.012(2) 0.0050(19) 0.0061(18) C65 0.030(2) 0.039(3) 0.035(3) 0.014(2) 0.009(2) 0.012(2) C66 0.033(3) 0.040(3) 0.037(3) 0.011(2) 0.011(2) 0.009(2) C67 0.029(2) 0.042(3) 0.027(2) 0.014(2) 0.0063(19) 0.006(2) C68 0.032(2) 0.035(3) 0.027(2) 0.012(2) 0.0022(19) 0.010(2) C69 0.024(2) 0.026(2) 0.031(2) 0.0095(19) 0.0032(18) 0.0022(17) O11 0.0307(17) 0.040(2) 0.038(2) 0.0177(17) 0.0091(15) 0.0095(15) O30 0.0216(16) 0.045(2) 0.048(2) 0.0252(19) 0.0091(15) 0.0047(15) O31 0.0290(17) 0.0264(17) 0.040(2) 0.0104(15) 0.0118(15) 0.0053(14) O71 0.0368(19) 0.0302(19) 0.038(2) 0.0076(16) -0.0036(16) 0.0081(15) O73 0.047(2) 0.033(2) 0.033(2) 0.0089(17) -0.0008(17) 0.0003(17) O74 0.0275(17) 0.051(2) 0.032(2) 0.0118(18) 0.0037(15) 0.0049(16) O76 0.041(2) 0.035(2) 0.0297(19) 0.0157(16) -0.0012(16) -0.0020(16) O77 0.0304(17) 0.034(2) 0.036(2) 0.0068(16) 0.0080(15) 0.0044(15) O79 0.0295(17) 0.0291(18) 0.043(2) 0.0078(16) 0.0071(16) 0.0050(14) O51 0.0360(18) 0.037(2) 0.0244(17) 0.0058(15) 0.0020(14) 0.0143(16) O70 0.0338(17) 0.0313(18) 0.0239(17) 0.0104(14) 0.0027(14) 0.0131(14) N19 0.0275(19) 0.026(2) 0.031(2) 0.0037(17) 0.0069(17) 0.0047(16) N22 0.030(2) 0.030(2) 0.030(2) 0.0124(17) 0.0079(17) 0.0061(16) N39 0.031(2) 0.039(2) 0.030(2) 0.0086(19) 0.0069(17) 0.0119(18) N59 0.0267(19) 0.029(2) 0.029(2) 0.0135(17) 0.0025(16) 0.0037(16) C25 0.037(3) 0.042(3) 0.054(4) 0.015(3) 0.001(3) 0.012(2) C44 0.034(3) 0.033(3) 0.037(3) 0.013(2) 0.001(2) 0.004(2) C45 0.046(3) 0.041(3) 0.049(4) 0.024(3) 0.006(3) 0.005(3) C43 0.039(3) 0.034(3) 0.040(3) 0.013(2) 0.001(2) 0.012(2) C46 0.043(3) 0.053(4) 0.053(4) 0.027(3) 0.008(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O30 1.894(4) . ? Mn1 O11 1.902(4) . ? Mn1 N22 1.975(4) . ? Mn1 N19 2.010(4) . ? Mn1 O73 2.212(4) . ? Mn1 O77 2.257(4) . ? Mn2 O50 1.899(4) . ? Mn2 O31 1.900(4) . ? Mn2 N39 2.001(5) . ? Mn2 N42 2.005(4) . ? Mn2 O71 2.228(4) . ? Mn2 O74 2.230(4) . ? Mn3 O70 1.874(4) . ? Mn3 O51 1.901(4) . ? Mn3 N59 1.987(4) . ? Mn3 N62 2.000(4) . ? Mn3 O76 2.242(4) 1_666 ? Mn3 O79 2.252(4) . ? O50 C49 1.319(7) . ? C49 C44 1.417(8) . ? C49 C48 1.419(8) . ? C48 C47 1.384(9) . ? C48 H48 0.9300 . ? C47 C46 1.403(10) . ? C47 H47 0.9300 . ? C12 O11 1.309(6) . ? C12 C13 1.417(8) . ? C12 C17 1.437(8) . ? C13 C14 1.382(8) . ? C13 H13 0.9300 . ? C14 C15 1.389(10) . ? C14 H14 0.9300 . ? C15 C16 1.370(9) . ? C15 H15 0.9300 . ? C16 C17 1.446(7) . ? C16 H16 0.9300 . ? C17 C18 1.423(8) . ? C18 N19 1.293(7) . ? C18 H18 0.9300 . ? C20 N19 1.455(7) . ? C20 C21 1.532(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N22 1.491(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C23 N22 1.294(7) . ? C23 C24 1.436(8) . ? C23 H23 0.9300 . ? C24 C25 1.416(8) . ? C24 C29 1.426(8) . ? C26 C25 1.365(10) . ? C26 C27 1.372(12) . ? C26 H26 0.9300 . ? C27 C28 1.437(11) . ? C27 H27 0.9300 . ? C28 C29 1.402(8) . ? C28 H28 0.9300 . ? C29 O30 1.327(7) . ? C32 O31 1.312(6) . ? C32 C33 1.417(8) . ? C32 C37 1.434(8) . ? C33 C34 1.367(8) . ? C33 H33 0.9300 . ? C34 C35 1.399(9) . ? C34 H34 0.9300 . ? C35 C36 1.354(9) . ? C35 H35 0.9300 . ? C36 C37 1.423(8) . ? C36 H36 0.9300 . ? C37 C38 1.438(8) . ? C38 N39 1.285(7) . ? C38 H38 0.9300 . ? C40 N39 1.477(7) . ? C40 C41 1.506(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N42 1.486(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? N42 C43 1.267(7) . ? C72 O73 1.226(7) . ? C72 O71 1.237(6) . ? C72 H72 0.9300 . ? C75 O76 1.241(6) . ? C75 O74 1.257(7) . ? C75 H75 0.9300 . ? C78 O79 1.235(6) . ? C78 O77 1.253(6) . ? C78 H78 0.9300 . ? C52 O51 1.328(6) . ? C52 C53 1.413(7) . ? C52 C57 1.420(8) . ? C53 C54 1.389(8) . ? C53 H53 0.9300 . ? C54 C55 1.417(9) . ? C54 H54 0.9300 . ? C55 C56 1.360(8) . ? C55 H55 0.9300 . ? C56 C57 1.414(8) . ? C56 H56 0.9300 . ? C57 C58 1.440(8) . ? C58 N59 1.287(7) . ? C58 H58 0.9300 . ? C60 N59 1.482(6) . ? C60 C61 1.501(8) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 N62 1.486(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? N62 C63 1.294(7) . ? C63 C64 1.439(7) . ? C63 H63 0.9300 . ? C64 C65 1.403(7) . ? C64 C69 1.426(7) . ? C65 C66 1.386(8) . ? C65 H66 0.9300 . ? C66 C67 1.406(8) . ? C66 H67 0.9300 . ? C67 C68 1.382(8) . ? C67 H68 0.9300 . ? C68 C69 1.427(7) . ? C68 H69 0.9300 . ? C69 O70 1.323(6) . ? O76 Mn3 2.242(4) 1_444 ? C25 H25 0.9300 . ? C44 C45 1.413(8) . ? C44 C43 1.443(9) . ? C45 C46 1.374(10) . ? C45 H45 0.9300 . ? C43 H43 0.9300 . ? C46 H46 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O30 Mn1 O11 95.04(16) . . ? O30 Mn1 N22 90.61(17) . . ? O11 Mn1 N22 173.99(17) . . ? O30 Mn1 N19 172.53(18) . . ? O11 Mn1 N19 92.41(17) . . ? N22 Mn1 N19 81.96(18) . . ? O30 Mn1 O73 92.37(18) . . ? O11 Mn1 O73 90.68(17) . . ? N22 Mn1 O73 87.02(17) . . ? N19 Mn1 O73 88.02(17) . . ? O30 Mn1 O77 88.84(16) . . ? O11 Mn1 O77 91.37(16) . . ? N22 Mn1 O77 90.80(17) . . ? N19 Mn1 O77 90.49(15) . . ? O73 Mn1 O77 177.52(16) . . ? O50 Mn2 O31 94.71(16) . . ? O50 Mn2 N39 172.27(18) . . ? O31 Mn2 N39 92.30(18) . . ? O50 Mn2 N42 91.72(18) . . ? O31 Mn2 N42 171.93(17) . . ? N39 Mn2 N42 81.59(19) . . ? O50 Mn2 O71 91.14(17) . . ? O31 Mn2 O71 85.22(15) . . ? N39 Mn2 O71 86.22(17) . . ? N42 Mn2 O71 99.55(16) . . ? O50 Mn2 O74 95.94(16) . . ? O31 Mn2 O74 86.75(16) . . ? N39 Mn2 O74 87.68(16) . . ? N42 Mn2 O74 87.74(17) . . ? O71 Mn2 O74 169.70(15) . . ? O70 Mn3 O51 95.45(16) . . ? O70 Mn3 N59 174.21(17) . . ? O51 Mn3 N59 90.33(17) . . ? O70 Mn3 N62 92.51(16) . . ? O51 Mn3 N62 172.02(17) . . ? N59 Mn3 N62 81.71(18) . . ? O70 Mn3 O76 86.63(15) . 1_666 ? O51 Mn3 O76 92.28(17) . 1_666 ? N59 Mn3 O76 92.98(16) . 1_666 ? N62 Mn3 O76 87.54(16) . 1_666 ? O70 Mn3 O79 87.16(16) . . ? O51 Mn3 O79 93.48(15) . . ? N59 Mn3 O79 92.68(16) . . ? N62 Mn3 O79 87.55(15) . . ? O76 Mn3 O79 171.90(15) 1_666 . ? C49 O50 Mn2 128.5(4) . . ? O50 C49 C44 124.3(5) . . ? O50 C49 C48 118.7(5) . . ? C44 C49 C48 117.0(5) . . ? C47 C48 C49 121.5(6) . . ? C47 C48 H48 119.3 . . ? C49 C48 H48 119.3 . . ? C48 C47 C46 121.1(6) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? O11 C12 C13 118.7(5) . . ? O11 C12 C17 123.0(5) . . ? C13 C12 C17 118.3(5) . . ? C14 C13 C12 121.2(6) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 121.2(6) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 119.8(6) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.5(6) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C12 124.6(5) . . ? C18 C17 C16 117.6(5) . . ? C12 C17 C16 117.8(5) . . ? N19 C18 C17 125.2(5) . . ? N19 C18 H18 117.4 . . ? C17 C18 H18 117.4 . . ? N19 C20 C21 109.0(4) . . ? N19 C20 H20A 109.9 . . ? C21 C20 H20A 109.9 . . ? N19 C20 H20B 109.9 . . ? C21 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? N22 C21 C20 105.0(4) . . ? N22 C21 H21A 110.8 . . ? C20 C21 H21A 110.8 . . ? N22 C21 H21B 110.8 . . ? C20 C21 H21B 110.8 . . ? H21A C21 H21B 108.8 . . ? N22 C23 C24 123.1(5) . . ? N22 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? C25 C24 C29 120.4(5) . . ? C25 C24 C23 117.0(5) . . ? C29 C24 C23 122.6(5) . . ? C25 C26 C27 120.4(7) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C28 121.2(6) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 118.9(7) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? O30 C29 C28 117.9(6) . . ? O30 C29 C24 123.7(5) . . ? C28 C29 C24 118.4(6) . . ? O31 C32 C33 118.2(5) . . ? O31 C32 C37 124.7(5) . . ? C33 C32 C37 117.1(5) . . ? C34 C33 C32 122.0(6) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 120.4(6) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C36 C35 C34 120.0(6) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 121.5(6) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C36 C37 C32 118.9(5) . . ? C36 C37 C38 118.2(5) . . ? C32 C37 C38 122.8(5) . . ? N39 C38 C37 125.2(5) . . ? N39 C38 H38 117.4 . . ? C37 C38 H38 117.4 . . ? N39 C40 C41 107.1(5) . . ? N39 C40 H40A 110.3 . . ? C41 C40 H40A 110.3 . . ? N39 C40 H40B 110.3 . . ? C41 C40 H40B 110.3 . . ? H40A C40 H40B 108.6 . . ? N42 C41 C40 107.1(4) . . ? N42 C41 H41A 110.3 . . ? C40 C41 H41A 110.3 . . ? N42 C41 H41B 110.3 . . ? C40 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C43 N42 C41 120.8(5) . . ? C43 N42 Mn2 126.0(4) . . ? C41 N42 Mn2 113.3(3) . . ? O73 C72 O71 128.7(5) . . ? O73 C72 H72 115.7 . . ? O71 C72 H72 115.7 . . ? O76 C75 O74 127.4(5) . . ? O76 C75 H75 116.3 . . ? O74 C75 H75 116.3 . . ? O79 C78 O77 129.2(5) . . ? O79 C78 H78 115.4 . . ? O77 C78 H78 115.4 . . ? O51 C52 C53 118.0(5) . . ? O51 C52 C57 123.9(5) . . ? C53 C52 C57 118.1(5) . . ? C54 C53 C52 121.1(5) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C53 C54 C55 120.5(5) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C56 C55 C54 118.5(5) . . ? C56 C55 H55 120.8 . . ? C54 C55 H55 120.8 . . ? C55 C56 C57 122.8(5) . . ? C55 C56 H56 118.6 . . ? C57 C56 H56 118.6 . . ? C56 C57 C52 118.9(5) . . ? C56 C57 C58 119.3(5) . . ? C52 C57 C58 121.7(5) . . ? N59 C58 C57 125.6(5) . . ? N59 C58 H58 117.2 . . ? C57 C58 H58 117.2 . . ? N59 C60 C61 106.7(4) . . ? N59 C60 H60A 110.4 . . ? C61 C60 H60A 110.4 . . ? N59 C60 H60B 110.4 . . ? C61 C60 H60B 110.4 . . ? H60A C60 H60B 108.6 . . ? N62 C61 C60 106.7(4) . . ? N62 C61 H61A 110.4 . . ? C60 C61 H61A 110.4 . . ? N62 C61 H61B 110.4 . . ? C60 C61 H61B 110.4 . . ? H61A C61 H61B 108.6 . . ? C63 N62 C61 121.4(4) . . ? C63 N62 Mn3 125.5(3) . . ? C61 N62 Mn3 113.0(3) . . ? N62 C63 C64 124.6(5) . . ? N62 C63 H63 117.7 . . ? C64 C63 H63 117.7 . . ? C65 C64 C69 119.5(5) . . ? C65 C64 C63 117.2(5) . . ? C69 C64 C63 123.3(5) . . ? C66 C65 C64 122.3(5) . . ? C66 C65 H66 118.8 . . ? C64 C65 H66 118.8 . . ? C65 C66 C67 118.3(5) . . ? C65 C66 H67 120.9 . . ? C67 C66 H67 120.9 . . ? C68 C67 C66 121.2(5) . . ? C68 C67 H68 119.4 . . ? C66 C67 H68 119.4 . . ? C67 C68 C69 121.0(5) . . ? C67 C68 H69 119.5 . . ? C69 C68 H69 119.5 . . ? O70 C69 C64 124.0(5) . . ? O70 C69 C68 118.3(4) . . ? C64 C69 C68 117.7(5) . . ? C12 O11 Mn1 129.4(4) . . ? C29 O30 Mn1 123.1(3) . . ? C32 O31 Mn2 127.5(3) . . ? C72 O71 Mn2 128.6(4) . . ? C72 O73 Mn1 124.1(4) . . ? C75 O74 Mn2 123.8(3) . . ? C75 O76 Mn3 136.7(3) . 1_444 ? C78 O77 Mn1 139.5(4) . . ? C78 O79 Mn3 124.7(3) . . ? C52 O51 Mn3 126.5(3) . . ? C69 O70 Mn3 127.9(3) . . ? C18 N19 C20 121.1(4) . . ? C18 N19 Mn1 125.1(4) . . ? C20 N19 Mn1 113.3(3) . . ? C23 N22 C21 120.8(5) . . ? C23 N22 Mn1 125.9(4) . . ? C21 N22 Mn1 113.1(3) . . ? C38 N39 C40 121.6(5) . . ? C38 N39 Mn2 125.7(4) . . ? C40 N39 Mn2 112.7(4) . . ? C58 N59 C60 121.9(4) . . ? C58 N59 Mn3 124.5(4) . . ? C60 N59 Mn3 112.8(3) . . ? C26 C25 C24 120.4(7) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C45 C44 C49 120.2(6) . . ? C45 C44 C43 117.0(6) . . ? C49 C44 C43 122.8(5) . . ? C46 C45 C44 121.7(7) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? N42 C43 C44 125.8(5) . . ? N42 C43 H43 117.1 . . ? C44 C43 H43 117.1 . . ? C45 C46 C47 118.5(6) . . ? C45 C46 H46 120.8 . . ? C47 C46 H46 120.8 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.222 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.133 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 799079' #TrackingRef '- all 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42 Mn3 N9 O12' _chemical_formula_weight 1101.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Mn Mn 0.3368 0.7283 '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 13.767(4) _cell_length_b 14.3539(16) _cell_length_c 13.870(2) _cell_angle_alpha 108.718(13) _cell_angle_beta 107.147(18) _cell_angle_gamma 103.931(15) _cell_volume 2303.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16382 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 30.00 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.886 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number n/a _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 16382 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.1362 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12876 _reflns_number_gt 6567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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. isor restraints have been applied to atoms C25, C26 and C27 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0288P)^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 12876 _refine_ls_number_parameters 671 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 0.757 _refine_ls_restrained_S_all 0.768 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.77819(3) 0.14942(4) 1.01709(3) 0.03357(13) Uani 1 1 d . A . Mn2 Mn 0.54099(3) -0.21048(3) 0.66736(3) 0.02202(10) Uani 1 1 d . . . Mn3 Mn 1.12856(3) 0.52672(3) 1.27700(3) 0.02213(10) Uani 1 1 d . . . O50 O 0.62959(14) -0.18663(14) 0.59099(13) 0.0256(4) Uani 1 1 d . A . C49 C 0.6646(2) -0.1027(2) 0.5727(2) 0.0266(6) Uani 1 1 d . . . C48 C 0.7387(2) -0.0996(2) 0.5213(2) 0.0342(7) Uani 1 1 d . A . H48 H 0.7599 -0.1571 0.4996 0.041 Uiso 1 1 calc R . . C47 C 0.7807(3) -0.0128(3) 0.5024(2) 0.0445(9) Uani 1 1 d . . . H47 H 0.8305 -0.0124 0.4694 0.053 Uiso 1 1 calc R A . C12 C 0.8533(2) 0.0489(3) 1.1579(2) 0.0356(8) Uani 1 1 d . . . C13 C 0.8272(3) -0.0120(3) 1.2143(3) 0.0508(10) Uani 1 1 d . . . H13 H 0.7612 -0.0230 1.2224 0.061 Uiso 1 1 calc R . . C14 C 0.8974(3) -0.0558(3) 1.2578(2) 0.0440(9) Uani 1 1 d . . . H14 H 0.8774 -0.0972 1.2935 0.053 Uiso 1 1 calc R . . C15 C 0.9976(3) -0.0394(2) 1.2496(2) 0.0390(8) Uani 1 1 d . . . H15 H 1.0451 -0.0685 1.2804 0.047 Uiso 1 1 calc R . . C16 C 1.0256(2) 0.0203(2) 1.1952(2) 0.0332(7) Uani 1 1 d . . . H16 H 1.0929 0.0320 1.1899 0.040 Uiso 1 1 calc R . . C17 C 0.9545(2) 0.0642(2) 1.1471(2) 0.0273(7) Uani 1 1 d . . . C18 C 0.9890(2) 0.1246(2) 1.0895(2) 0.0279(7) Uani 1 1 d . A . H18 H 1.0582 0.1343 1.0895 0.033 Uiso 1 1 calc R . . C20 C 0.9760(2) 0.2298(2) 0.9859(2) 0.0320(7) Uani 1 1 d . A . H20A H 1.0310 0.2077 0.9653 0.038 Uiso 1 1 calc R . . H20B H 1.0101 0.3040 1.0378 0.038 Uiso 1 1 calc R . . C21 C 0.8833(2) 0.2144(2) 0.8832(2) 0.0322(7) Uani 1 1 d . A . H21A H 0.9040 0.2715 0.8615 0.039 Uiso 1 1 calc R . . H21B H 0.8656 0.1479 0.8217 0.039 Uiso 1 1 calc R . . C23 C 0.7191(3) 0.2498(2) 0.8689(2) 0.0311(7) Uani 1 1 d . A . H23 H 0.7351 0.2827 0.8245 0.037 Uiso 1 1 calc R . . C24 C 0.6189(3) 0.2437(2) 0.8828(2) 0.0314(7) Uani 1 1 d . . . C26 C 0.4609(4) 0.2899(4) 0.8458(4) 0.0915(15) Uani 1 1 d U . . H26 H 0.4215 0.3256 0.8161 0.110 Uiso 1 1 calc R . . C27 C 0.4199(3) 0.2316(3) 0.8986(3) 0.0545(10) Uani 1 1 d U . . H27 H 0.3530 0.2277 0.9029 0.065 Uiso 1 1 calc R . . C28 C 0.4783(2) 0.1807(2) 0.9435(2) 0.0286(7) Uani 1 1 d . . . H28 H 0.4508 0.1422 0.9786 0.034 Uiso 1 1 calc R . . C29 C 0.5786(2) 0.1852(2) 0.9378(2) 0.0254(6) Uani 1 1 d . . . C32 C 0.4847(2) -0.4168(2) 0.66872(19) 0.0213(6) Uani 1 1 d . . . C33 C 0.4838(2) -0.5191(2) 0.6257(2) 0.0249(6) Uani 1 1 d . A . H33 H 0.5304 -0.5325 0.5909 0.030 Uiso 1 1 calc R . . C34 C 0.4149(2) -0.6009(2) 0.6339(2) 0.0310(7) Uani 1 1 d . . . H34 H 0.4151 -0.6688 0.6038 0.037 Uiso 1 1 calc R A . C35 C 0.3449(2) -0.5830(3) 0.6869(2) 0.0371(8) Uani 1 1 d . A . H35 H 0.2977 -0.6387 0.6910 0.045 Uiso 1 1 calc R . . C36 C 0.3466(2) -0.4839(3) 0.7320(2) 0.0340(7) Uani 1 1 d . . . H36 H 0.3016 -0.4718 0.7693 0.041 Uiso 1 1 calc R A . C37 C 0.4146(2) -0.3979(2) 0.72441(19) 0.0242(6) Uani 1 1 d . A . C38 C 0.4067(2) -0.2965(2) 0.7691(2) 0.0283(7) Uani 1 1 d . . . H38 H 0.3643 -0.2896 0.8103 0.034 Uiso 1 1 calc R A . C40 C 0.4375(2) -0.1149(2) 0.8057(2) 0.0326(7) Uani 1 1 d . . . H40A H 0.5015 -0.0646 0.8727 0.039 Uiso 1 1 calc R A . H40B H 0.3742 -0.1272 0.8240 0.039 Uiso 1 1 calc R . . C41 C 0.4205(2) -0.0741(2) 0.7163(2) 0.0380(8) Uani 1 1 d . A . H41A H 0.3485 -0.1160 0.6566 0.046 Uiso 1 1 calc R . . H41B H 0.4267 -0.0009 0.7472 0.046 Uiso 1 1 calc R . . N42 N 0.50579(19) -0.08286(18) 0.67424(16) 0.0286(6) Uani 1 1 d . A . N75 N 0.38033(19) -0.28531(19) 0.42805(19) 0.0314(6) Uani 1 1 d . . . N78 N 0.8875(2) 0.3892(2) 1.21805(19) 0.0356(6) Uani 1 1 d . A . C52 C 1.0358(2) 0.6695(2) 1.3806(2) 0.0215(6) Uani 1 1 d . A . C53 C 0.9796(2) 0.7379(2) 1.3720(2) 0.0246(6) Uani 1 1 d . . . H53 H 0.9586 0.7479 1.3071 0.030 Uiso 1 1 calc R . . C54 C 0.9550(2) 0.7901(2) 1.4577(2) 0.0315(7) Uani 1 1 d . . . H54 H 0.9188 0.8361 1.4509 0.038 Uiso 1 1 calc R . . C55 C 0.9836(3) 0.7748(2) 1.5547(2) 0.0413(8) Uani 1 1 d . . . H55 H 0.9662 0.8102 1.6123 0.050 Uiso 1 1 calc R . . C56 C 1.0371(3) 0.7080(2) 1.5651(2) 0.0359(8) Uani 1 1 d . . . H56 H 1.0564 0.6987 1.6305 0.043 Uiso 1 1 calc R . . C57 C 1.0641(2) 0.6523(2) 1.4787(2) 0.0221(6) Uani 1 1 d . . . C58 C 1.1195(2) 0.5828(2) 1.4949(2) 0.0235(6) Uani 1 1 d . A . H58 H 1.1352 0.5771 1.5622 0.028 Uiso 1 1 calc R . . C60 C 1.2140(2) 0.4643(2) 1.4536(2) 0.0280(7) Uani 1 1 d . A . H60A H 1.1903 0.4345 1.5001 0.034 Uiso 1 1 calc R . . H60B H 1.2909 0.5091 1.4946 0.034 Uiso 1 1 calc R . . C61 C 1.1976(2) 0.3766(2) 1.3476(2) 0.0269(6) Uani 1 1 d . . . H61A H 1.2557 0.3492 1.3613 0.032 Uiso 1 1 calc R . . H61B H 1.1282 0.3190 1.3194 0.032 Uiso 1 1 calc R . . N62 N 1.19902(16) 0.42165(17) 1.26653(16) 0.0213(5) Uani 1 1 d . . . C63 C 1.2459(2) 0.3955(2) 1.2000(2) 0.0243(6) Uani 1 1 d . . . H63 H 1.2860 0.3531 1.2100 0.029 Uiso 1 1 calc R . . C64 C 1.2402(2) 0.4277(2) 1.1110(2) 0.0249(6) Uani 1 1 d . . . C65 C 1.2986(3) 0.3971(3) 1.0471(3) 0.0549(10) Uani 1 1 d . . . H66 H 1.3462 0.3642 1.0684 0.066 Uiso 1 1 calc R . . C66 C 1.2865(4) 0.4150(3) 0.9530(3) 0.0771(14) Uani 1 1 d . . . H67 H 1.3283 0.3977 0.9133 0.092 Uiso 1 1 calc R . . C67 C 1.2113(3) 0.4592(3) 0.9183(3) 0.0537(10) Uani 1 1 d . . . H68 H 1.1998 0.4673 0.8525 0.064 Uiso 1 1 calc R . . C68 C 1.1538(2) 0.4909(2) 0.9788(2) 0.0304(7) Uani 1 1 d . . . H69 H 1.1042 0.5208 0.9541 0.037 Uiso 1 1 calc R . . C69 C 1.1689(2) 0.4788(2) 1.07802(19) 0.0201(6) Uani 1 1 d . A . O11 O 0.78272(15) 0.08992(19) 1.11906(17) 0.0481(6) Uani 1 1 d . . . O30 O 0.63088(14) 0.13350(17) 0.98151(16) 0.0415(6) Uani 1 1 d . . . O31 O 0.55111(14) -0.34146(14) 0.65661(13) 0.0232(4) Uani 1 1 d . A . N72A N 0.7579(5) -0.0673(6) 0.8954(5) 0.034(2) Uani 0.585(12) 1 d P A 1 O71A O 0.7052(5) -0.1605(5) 0.8224(6) 0.0397(17) Uani 0.585(12) 1 d P A 1 N72B N 0.6935(8) -0.1126(8) 0.8335(7) 0.023(2) Uani 0.415(12) 1 d P A 2 O71B O 0.7459(6) -0.1435(7) 0.8951(7) 0.047(3) Uani 0.415(12) 1 d P A 2 O73 O 0.72056(19) -0.00709(18) 0.87130(19) 0.0591(7) Uani 1 1 d . . . O74 O 0.38131(14) -0.30728(15) 0.50786(14) 0.0319(5) Uani 1 1 d . A . O76 O 0.29614(15) -0.34276(15) 0.33790(14) 0.0296(5) Uani 1 1 d . . . O77 O 0.80212(16) 0.30869(18) 1.15504(16) 0.0432(6) Uani 1 1 d . . . O79 O 0.97024(15) 0.38424(15) 1.20050(14) 0.0316(5) Uani 1 1 d . . . O51 O 1.06073(15) 0.62525(15) 1.29681(13) 0.0278(5) Uani 1 1 d . . . O70 O 1.11277(13) 0.51311(15) 1.13402(13) 0.0259(4) Uani 1 1 d . . . N19 N 0.93132(17) 0.16595(18) 1.03817(17) 0.0276(6) Uani 1 1 d . . . N22 N 0.78850(19) 0.21385(17) 0.91236(17) 0.0276(6) Uani 1 1 d . . . N39 N 0.45304(18) -0.21454(19) 0.75741(16) 0.0258(5) Uani 1 1 d . A . N59 N 1.14940(17) 0.52757(17) 1.42486(16) 0.0220(5) Uani 1 1 d . . . C25 C 0.5577(3) 0.2947(3) 0.8380(3) 0.0701(12) Uani 1 1 d U . . H25 H 0.5834 0.3329 0.8018 0.084 Uiso 1 1 calc R . . C44 C 0.6313(2) -0.0154(2) 0.5998(2) 0.0298(7) Uani 1 1 d . A . C45 C 0.6754(3) 0.0717(2) 0.5793(2) 0.0447(9) Uani 1 1 d . . . H45 H 0.6537 0.1292 0.5983 0.054 Uiso 1 1 calc R A . C43 C 0.5507(2) -0.0125(2) 0.6462(2) 0.0326(7) Uani 1 1 d . . . H43 H 0.5294 0.0455 0.6569 0.039 Uiso 1 1 calc R A . C46 C 0.7497(3) 0.0736(3) 0.5319(3) 0.0491(10) Uani 1 1 d . A . H46 H 0.7789 0.1321 0.5197 0.059 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 Mn1 0.0165(2) 0.0522(3) 0.0351(2) 0.0305(2) 0.0072(2) 0.0051(2) Mn2 0.0234(2) 0.0258(2) 0.0205(2) 0.00936(19) 0.01054(18) 0.0136(2) Mn3 0.0206(2) 0.0333(3) 0.01653(19) 0.01142(19) 0.00821(17) 0.0144(2) O50 0.0326(11) 0.0231(11) 0.0290(10) 0.0132(9) 0.0187(9) 0.0124(9) C49 0.0299(16) 0.0234(16) 0.0188(13) 0.0081(13) 0.0029(12) 0.0072(13) C48 0.0341(18) 0.0339(18) 0.0348(16) 0.0183(15) 0.0127(14) 0.0093(15) C47 0.0334(19) 0.047(2) 0.0433(19) 0.0281(18) 0.0061(15) -0.0027(17) C12 0.0205(16) 0.062(2) 0.0348(16) 0.0312(17) 0.0116(14) 0.0164(16) C13 0.0325(18) 0.096(3) 0.057(2) 0.058(2) 0.0257(17) 0.034(2) C14 0.045(2) 0.070(3) 0.0438(18) 0.0403(19) 0.0250(17) 0.0318(19) C15 0.042(2) 0.054(2) 0.0257(15) 0.0172(16) 0.0120(15) 0.0264(18) C16 0.0245(16) 0.045(2) 0.0253(15) 0.0061(15) 0.0103(13) 0.0164(15) C17 0.0175(14) 0.0411(19) 0.0192(13) 0.0104(14) 0.0054(12) 0.0100(14) C18 0.0145(14) 0.0330(18) 0.0218(14) 0.0013(13) 0.0050(12) 0.0023(13) C20 0.0284(16) 0.0298(17) 0.0262(14) 0.0052(14) 0.0130(13) -0.0013(14) C21 0.0350(18) 0.0308(18) 0.0301(15) 0.0136(14) 0.0185(14) 0.0034(14) C23 0.049(2) 0.0206(16) 0.0246(15) 0.0094(13) 0.0208(15) 0.0084(15) C24 0.048(2) 0.0296(17) 0.0295(15) 0.0173(14) 0.0210(15) 0.0214(16) C26 0.129(4) 0.136(4) 0.142(4) 0.120(3) 0.108(3) 0.117(3) C27 0.076(3) 0.071(3) 0.068(2) 0.046(2) 0.053(2) 0.059(2) C28 0.0328(17) 0.0286(17) 0.0260(14) 0.0121(13) 0.0112(13) 0.0142(14) C29 0.0289(16) 0.0218(16) 0.0188(13) 0.0097(12) 0.0024(12) 0.0061(13) C32 0.0168(14) 0.0281(16) 0.0160(12) 0.0104(12) 0.0036(11) 0.0056(12) C33 0.0232(15) 0.0275(16) 0.0234(14) 0.0105(13) 0.0103(12) 0.0077(13) C34 0.0319(17) 0.0265(17) 0.0310(15) 0.0148(14) 0.0082(14) 0.0071(14) C35 0.0303(18) 0.041(2) 0.0336(16) 0.0205(16) 0.0104(14) 0.0006(16) C36 0.0248(16) 0.052(2) 0.0246(15) 0.0185(16) 0.0121(13) 0.0087(16) C37 0.0186(14) 0.0322(17) 0.0163(12) 0.0077(13) 0.0060(11) 0.0054(13) C38 0.0170(14) 0.045(2) 0.0169(13) 0.0064(14) 0.0070(12) 0.0098(14) C40 0.0267(16) 0.0399(19) 0.0256(15) 0.0031(14) 0.0109(13) 0.0178(15) C41 0.0383(19) 0.040(2) 0.0312(16) 0.0049(15) 0.0090(15) 0.0272(16) N42 0.0323(14) 0.0276(14) 0.0193(11) 0.0047(11) 0.0031(11) 0.0167(12) N75 0.0334(15) 0.0319(15) 0.0295(13) 0.0161(12) 0.0086(12) 0.0139(12) N78 0.0299(15) 0.0577(19) 0.0325(14) 0.0257(14) 0.0180(12) 0.0223(14) C52 0.0183(14) 0.0207(15) 0.0207(13) 0.0044(12) 0.0095(11) 0.0034(12) C53 0.0243(15) 0.0267(16) 0.0252(14) 0.0112(13) 0.0120(12) 0.0104(13) C54 0.0425(19) 0.0255(17) 0.0374(16) 0.0158(14) 0.0227(15) 0.0187(15) C55 0.068(2) 0.039(2) 0.0370(17) 0.0167(16) 0.0367(18) 0.0309(19) C56 0.056(2) 0.0367(19) 0.0236(15) 0.0163(15) 0.0214(15) 0.0203(17) C57 0.0229(15) 0.0214(15) 0.0216(13) 0.0085(12) 0.0113(12) 0.0057(12) C58 0.0229(15) 0.0245(16) 0.0183(13) 0.0100(12) 0.0061(12) 0.0024(13) C60 0.0249(15) 0.0389(18) 0.0211(14) 0.0149(14) 0.0054(12) 0.0152(14) C61 0.0225(15) 0.0344(18) 0.0275(14) 0.0162(14) 0.0094(12) 0.0130(14) N62 0.0164(11) 0.0260(13) 0.0187(11) 0.0096(10) 0.0047(9) 0.0058(10) C63 0.0208(15) 0.0195(15) 0.0310(15) 0.0098(13) 0.0085(12) 0.0085(12) C64 0.0287(16) 0.0252(16) 0.0323(15) 0.0155(13) 0.0208(13) 0.0137(13) C65 0.083(3) 0.072(3) 0.078(2) 0.055(2) 0.066(2) 0.064(2) C66 0.140(4) 0.107(3) 0.097(3) 0.082(3) 0.106(3) 0.101(3) C67 0.100(3) 0.059(2) 0.058(2) 0.045(2) 0.062(2) 0.055(2) C68 0.0402(18) 0.0296(17) 0.0286(15) 0.0146(14) 0.0192(14) 0.0149(15) C69 0.0178(14) 0.0184(14) 0.0207(13) 0.0056(12) 0.0094(11) 0.0032(12) O11 0.0221(11) 0.0947(19) 0.0619(14) 0.0631(15) 0.0225(11) 0.0294(12) O30 0.0179(10) 0.0574(15) 0.0599(14) 0.0469(13) 0.0092(10) 0.0093(10) O31 0.0199(10) 0.0233(11) 0.0300(10) 0.0120(9) 0.0137(8) 0.0082(8) N72A 0.024(3) 0.038(4) 0.027(3) 0.006(3) 0.004(3) 0.006(3) O71A 0.035(3) 0.034(3) 0.033(3) 0.003(3) 0.004(2) 0.013(3) N72B 0.024(4) 0.027(5) 0.016(4) 0.010(4) 0.008(4) 0.009(4) O71B 0.049(4) 0.044(6) 0.042(5) 0.025(4) 0.003(4) 0.016(4) O73 0.0439(15) 0.0344(15) 0.0659(16) 0.0272(14) -0.0151(12) -0.0008(13) O74 0.0267(11) 0.0410(13) 0.0235(10) 0.0141(10) 0.0072(9) 0.0084(10) O76 0.0272(11) 0.0299(12) 0.0210(9) 0.0096(9) 0.0024(9) 0.0037(9) O77 0.0179(11) 0.0635(16) 0.0410(12) 0.0184(12) 0.0129(10) 0.0071(11) O79 0.0198(10) 0.0433(13) 0.0333(11) 0.0135(10) 0.0149(9) 0.0127(10) O51 0.0331(11) 0.0440(13) 0.0208(9) 0.0166(9) 0.0165(9) 0.0267(10) O70 0.0187(10) 0.0442(13) 0.0181(9) 0.0142(9) 0.0078(8) 0.0152(9) N19 0.0175(12) 0.0315(15) 0.0207(11) 0.0062(11) 0.0058(10) -0.0032(11) N22 0.0287(14) 0.0235(14) 0.0217(12) 0.0080(11) 0.0082(11) 0.0002(11) N39 0.0215(13) 0.0348(15) 0.0170(11) 0.0060(11) 0.0061(10) 0.0126(12) N59 0.0180(12) 0.0283(14) 0.0202(11) 0.0113(11) 0.0069(10) 0.0092(11) C25 0.104(3) 0.094(3) 0.104(3) 0.081(3) 0.084(3) 0.078(3) C44 0.0279(16) 0.0220(16) 0.0238(14) 0.0075(13) -0.0031(13) 0.0039(14) C45 0.040(2) 0.0241(18) 0.0441(19) 0.0129(16) -0.0072(16) 0.0031(16) C43 0.0354(18) 0.0202(16) 0.0240(14) -0.0011(13) -0.0040(13) 0.0149(14) C46 0.0324(19) 0.044(2) 0.054(2) 0.0358(19) -0.0059(17) -0.0046(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O11 1.8661(19) . ? Mn1 O30 1.8769(19) . ? Mn1 N22 1.976(2) . ? Mn1 N19 1.984(2) . ? Mn1 O73 2.246(3) . ? Mn1 O77 2.335(2) . ? Mn2 O50 1.8763(17) . ? Mn2 O31 1.8800(18) . ? Mn2 N39 1.983(2) . ? Mn2 N42 1.985(2) . ? Mn2 N72B 2.311(10) . ? Mn2 O74 2.312(2) . ? Mn2 O71A 2.370(7) . ? Mn3 O51 1.8669(18) . ? Mn3 O70 1.8696(16) . ? Mn3 N62 1.971(2) . ? Mn3 N59 1.981(2) . ? Mn3 O79 2.271(2) . ? Mn3 O76 2.302(2) 1_666 ? O50 C49 1.318(3) . ? C49 C48 1.406(4) . ? C49 C44 1.414(4) . ? C48 C47 1.380(4) . ? C48 H48 0.9300 . ? C47 C46 1.386(5) . ? C47 H47 0.9300 . ? C12 O11 1.324(3) . ? C12 C13 1.400(4) . ? C12 C17 1.417(4) . ? C13 C14 1.373(4) . ? C13 H13 0.9300 . ? C14 C15 1.389(4) . ? C14 H14 0.9300 . ? C15 C16 1.371(4) . ? C15 H15 0.9300 . ? C16 C17 1.408(4) . ? C16 H16 0.9300 . ? C17 C18 1.443(4) . ? C18 N19 1.286(3) . ? C18 H18 0.9300 . ? C20 N19 1.471(3) . ? C20 C21 1.514(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N22 1.475(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C23 N22 1.280(3) . ? C23 C24 1.435(4) . ? C23 H23 0.9300 . ? C24 C25 1.382(4) . ? C24 C29 1.424(4) . ? C26 C25 1.356(5) . ? C26 C27 1.402(5) . ? C26 H26 0.9300 . ? C27 C28 1.358(4) . ? C27 H27 0.9300 . ? C28 C29 1.395(4) . ? C28 H28 0.9300 . ? C29 O30 1.313(3) . ? C32 O31 1.328(3) . ? C32 C33 1.392(4) . ? C32 C37 1.426(3) . ? C33 C34 1.379(3) . ? C33 H33 0.9300 . ? C34 C35 1.397(4) . ? C34 H34 0.9300 . ? C35 C36 1.349(4) . ? C35 H35 0.9300 . ? C36 C37 1.413(4) . ? C36 H36 0.9300 . ? C37 C38 1.431(4) . ? C38 N39 1.281(3) . ? C38 H38 0.9300 . ? C40 N39 1.468(3) . ? C40 C41 1.514(4) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N42 1.471(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? N42 C43 1.283(3) . ? N75 O74 1.242(2) . ? N75 O76 1.269(3) . ? N78 O79 1.246(3) . ? N78 O77 1.254(3) . ? C52 O51 1.319(3) . ? C52 C53 1.401(3) . ? C52 C57 1.419(3) . ? C53 C54 1.369(3) . ? C53 H53 0.9300 . ? C54 C55 1.390(4) . ? C54 H54 0.9300 . ? C55 C56 1.359(4) . ? C55 H55 0.9300 . ? C56 C57 1.415(3) . ? C56 H56 0.9300 . ? C57 C58 1.427(4) . ? C58 N59 1.281(3) . ? C58 H58 0.9300 . ? C60 N59 1.479(3) . ? C60 C61 1.509(3) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 N62 1.468(3) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? N62 C63 1.287(3) . ? C63 C64 1.438(3) . ? C63 H63 0.9300 . ? C64 C65 1.401(4) . ? C64 C69 1.418(4) . ? C65 C66 1.380(4) . ? C65 H66 0.9300 . ? C66 C67 1.386(5) . ? C66 H67 0.9300 . ? C67 C68 1.362(4) . ? C67 H68 0.9300 . ? C68 C69 1.404(3) . ? C68 H69 0.9300 . ? C69 O70 1.316(3) . ? N72A O73 1.192(7) . ? N72A O71A 1.254(11) . ? N72B O71B 1.217(16) . ? N72B O73 1.346(10) . ? O76 Mn3 2.302(2) 1_444 ? C25 H25 0.9300 . ? C44 C45 1.406(4) . ? C44 C43 1.440(4) . ? C45 C46 1.367(4) . ? C45 H45 0.9300 . ? C43 H43 0.9300 . ? C46 H46 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Mn1 O30 93.59(8) . . ? O11 Mn1 N22 174.38(9) . . ? O30 Mn1 N22 92.02(9) . . ? O11 Mn1 N19 92.17(9) . . ? O30 Mn1 N19 173.64(9) . . ? N22 Mn1 N19 82.22(10) . . ? O11 Mn1 O73 93.92(10) . . ? O30 Mn1 O73 87.94(10) . . ? N22 Mn1 O73 86.15(9) . . ? N19 Mn1 O73 88.99(9) . . ? O11 Mn1 O77 88.40(9) . . ? O30 Mn1 O77 80.90(9) . . ? N22 Mn1 O77 92.62(8) . . ? N19 Mn1 O77 101.96(8) . . ? O73 Mn1 O77 168.73(8) . . ? O50 Mn2 O31 94.90(8) . . ? O50 Mn2 N39 172.22(9) . . ? O31 Mn2 N39 92.23(9) . . ? O50 Mn2 N42 92.10(9) . . ? O31 Mn2 N42 170.96(9) . . ? N39 Mn2 N42 81.14(10) . . ? O50 Mn2 N72B 89.1(2) . . ? O31 Mn2 N72B 94.4(3) . . ? N39 Mn2 N72B 87.2(2) . . ? N42 Mn2 N72B 91.4(3) . . ? O50 Mn2 O74 94.56(7) . . ? O31 Mn2 O74 86.30(7) . . ? N39 Mn2 O74 89.01(8) . . ? N42 Mn2 O74 87.44(8) . . ? N72B Mn2 O74 176.2(2) . . ? O50 Mn2 O71A 86.54(16) . . ? O31 Mn2 O71A 77.18(17) . . ? N39 Mn2 O71A 92.01(16) . . ? N42 Mn2 O71A 109.02(18) . . ? N72B Mn2 O71A 17.71(17) . . ? O74 Mn2 O71A 163.47(17) . . ? O51 Mn3 O70 93.27(8) . . ? O51 Mn3 N62 175.49(8) . . ? O70 Mn3 N62 91.13(8) . . ? O51 Mn3 N59 92.68(8) . . ? O70 Mn3 N59 173.90(9) . . ? N62 Mn3 N59 82.90(9) . . ? O51 Mn3 O79 94.33(8) . . ? O70 Mn3 O79 89.22(8) . . ? N62 Mn3 O79 84.72(8) . . ? N59 Mn3 O79 88.99(8) . . ? O51 Mn3 O76 91.86(8) . 1_666 ? O70 Mn3 O76 85.84(7) . 1_666 ? N62 Mn3 O76 89.45(8) . 1_666 ? N59 Mn3 O76 95.31(8) . 1_666 ? O79 Mn3 O76 172.29(7) . 1_666 ? C49 O50 Mn2 128.99(17) . . ? O50 C49 C48 118.5(3) . . ? O50 C49 C44 124.2(3) . . ? C48 C49 C44 117.3(3) . . ? C47 C48 C49 121.3(3) . . ? C47 C48 H48 119.3 . . ? C49 C48 H48 119.3 . . ? C48 C47 C46 121.0(3) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? O11 C12 C13 118.1(3) . . ? O11 C12 C17 123.9(3) . . ? C13 C12 C17 118.1(3) . . ? C14 C13 C12 121.1(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 121.2(3) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 118.9(3) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 121.4(3) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 119.3(3) . . ? C16 C17 C18 118.1(3) . . ? C12 C17 C18 122.6(3) . . ? N19 C18 C17 125.1(3) . . ? N19 C18 H18 117.4 . . ? C17 C18 H18 117.4 . . ? N19 C20 C21 108.6(2) . . ? N19 C20 H20A 110.0 . . ? C21 C20 H20A 110.0 . . ? N19 C20 H20B 110.0 . . ? C21 C20 H20B 110.0 . . ? H20A C20 H20B 108.3 . . ? N22 C21 C20 106.9(2) . . ? N22 C21 H21A 110.3 . . ? C20 C21 H21A 110.3 . . ? N22 C21 H21B 110.3 . . ? C20 C21 H21B 110.3 . . ? H21A C21 H21B 108.6 . . ? N22 C23 C24 125.5(3) . . ? N22 C23 H23 117.2 . . ? C24 C23 H23 117.2 . . ? C25 C24 C29 119.0(3) . . ? C25 C24 C23 118.1(3) . . ? C29 C24 C23 122.9(3) . . ? C25 C26 C27 120.4(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 119.8(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 121.1(3) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? O30 C29 C28 118.4(2) . . ? O30 C29 C24 122.9(3) . . ? C28 C29 C24 118.7(3) . . ? O31 C32 C33 118.6(2) . . ? O31 C32 C37 123.2(2) . . ? C33 C32 C37 118.3(2) . . ? C34 C33 C32 121.1(3) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 120.9(3) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 119.1(3) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 122.1(3) . . ? C35 C36 H36 118.9 . . ? C37 C36 H36 118.9 . . ? C36 C37 C32 118.5(3) . . ? C36 C37 C38 118.4(3) . . ? C32 C37 C38 123.0(2) . . ? N39 C38 C37 125.7(2) . . ? N39 C38 H38 117.2 . . ? C37 C38 H38 117.2 . . ? N39 C40 C41 105.1(2) . . ? N39 C40 H40A 110.7 . . ? C41 C40 H40A 110.7 . . ? N39 C40 H40B 110.7 . . ? C41 C40 H40B 110.7 . . ? H40A C40 H40B 108.8 . . ? N42 C41 C40 107.0(2) . . ? N42 C41 H41A 110.3 . . ? C40 C41 H41A 110.3 . . ? N42 C41 H41B 110.3 . . ? C40 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C43 N42 C41 121.1(2) . . ? C43 N42 Mn2 125.6(2) . . ? C41 N42 Mn2 113.33(18) . . ? O74 N75 O76 115.4(2) . . ? O79 N78 O77 114.5(2) . . ? O51 C52 C53 117.8(2) . . ? O51 C52 C57 123.5(2) . . ? C53 C52 C57 118.7(2) . . ? C54 C53 C52 121.0(2) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 C55 120.6(3) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C56 C55 C54 119.8(3) . . ? C56 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? C55 C56 C57 121.6(3) . . ? C55 C56 H56 119.2 . . ? C57 C56 H56 119.2 . . ? C56 C57 C52 118.2(2) . . ? C56 C57 C58 118.6(2) . . ? C52 C57 C58 123.1(2) . . ? N59 C58 C57 125.8(2) . . ? N59 C58 H58 117.1 . . ? C57 C58 H58 117.1 . . ? N59 C60 C61 108.9(2) . . ? N59 C60 H60A 109.9 . . ? C61 C60 H60A 109.9 . . ? N59 C60 H60B 109.9 . . ? C61 C60 H60B 109.9 . . ? H60A C60 H60B 108.3 . . ? N62 C61 C60 107.3(2) . . ? N62 C61 H61A 110.3 . . ? C60 C61 H61A 110.3 . . ? N62 C61 H61B 110.3 . . ? C60 C61 H61B 110.3 . . ? H61A C61 H61B 108.5 . . ? C63 N62 C61 121.4(2) . . ? C63 N62 Mn3 125.59(18) . . ? C61 N62 Mn3 112.98(16) . . ? N62 C63 C64 124.1(2) . . ? N62 C63 H63 117.9 . . ? C64 C63 H63 117.9 . . ? C65 C64 C69 118.8(2) . . ? C65 C64 C63 118.4(3) . . ? C69 C64 C63 122.4(2) . . ? C66 C65 C64 121.0(3) . . ? C66 C65 H66 119.5 . . ? C64 C65 H66 119.5 . . ? C65 C66 C67 119.3(3) . . ? C65 C66 H67 120.4 . . ? C67 C66 H67 120.4 . . ? C68 C67 C66 121.3(3) . . ? C68 C67 H68 119.3 . . ? C66 C67 H68 119.3 . . ? C67 C68 C69 120.5(3) . . ? C67 C68 H69 119.7 . . ? C69 C68 H69 119.7 . . ? O70 C69 C68 117.7(2) . . ? O70 C69 C64 123.4(2) . . ? C68 C69 C64 118.9(2) . . ? C12 O11 Mn1 128.36(18) . . ? C29 O30 Mn1 127.97(17) . . ? C32 O31 Mn2 127.08(16) . . ? O73 N72A O71A 111.5(7) . . ? N72A O71A Mn2 123.3(6) . . ? O71B N72B O73 116.2(10) . . ? O71B N72B Mn2 128.9(9) . . ? O73 N72B Mn2 114.5(6) . . ? N72A O73 N72B 42.4(4) . . ? N72A O73 Mn1 112.7(3) . . ? N72B O73 Mn1 148.0(4) . . ? N75 O74 Mn2 114.85(16) . . ? N75 O76 Mn3 138.25(15) . 1_444 ? N78 O77 Mn1 129.53(17) . . ? N78 O79 Mn3 122.95(18) . . ? C52 O51 Mn3 129.37(16) . . ? C69 O70 Mn3 128.12(16) . . ? C18 N19 C20 120.7(2) . . ? C18 N19 Mn1 125.62(18) . . ? C20 N19 Mn1 113.62(18) . . ? C23 N22 C21 121.0(2) . . ? C23 N22 Mn1 124.9(2) . . ? C21 N22 Mn1 114.03(18) . . ? C38 N39 C40 120.9(2) . . ? C38 N39 Mn2 125.1(2) . . ? C40 N39 Mn2 113.94(18) . . ? C58 N59 C60 121.3(2) . . ? C58 N59 Mn3 125.42(18) . . ? C60 N59 Mn3 113.03(15) . . ? C26 C25 C24 121.1(3) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C45 C44 C49 120.0(3) . . ? C45 C44 C43 117.6(3) . . ? C49 C44 C43 122.4(3) . . ? C46 C45 C44 121.3(3) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? N42 C43 C44 125.7(3) . . ? N42 C43 H43 117.2 . . ? C44 C43 H43 117.2 . . ? C45 C46 C47 119.1(3) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.403 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.073 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END