# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Jie Zhang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; _publ_contact_author_email Zhangjie@fjirsm.ac.cn loop_ _publ_author_name _publ_author_address 'Jian-Ke Sun' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; 'Wei Li' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; 'Li-Xuan Cai' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; 'Jie Zhang' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; _publ_section_title ; Structural Diversity of the Mixed-Ligand System Mn-cpdba-2,2'-bpy Controlled by Temperature ; data_1 _database_code_depnum_ccdc_archive 'CCDC 780232' #TrackingRef '- compound 1-sjk.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H15 Mn N5 O8' _chemical_formula_sum 'C24 H15 Mn N5 O8' _chemical_formula_weight 556.35 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' Mn Mn 0.3368 0.7283 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5909(8) _cell_length_b 27.272(2) _cell_length_c 10.5706(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.897(5) _cell_angle_gamma 90.00 _cell_volume 2381.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5815 _cell_measurement_theta_min 3.0058 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6883 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 18278 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5428 _reflns_number_gt 4653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.9944P] 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 5428 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.80905(4) 0.037293(11) 0.32663(3) 0.03388(11) Uani 1 1 d . . . O1 O 0.7338(2) 0.11380(5) 0.32384(16) 0.0439(4) Uani 1 1 d . . . O2 O 0.8326(2) 0.09336(5) 0.15895(16) 0.0474(4) Uani 1 1 d . . . O3 O 0.21467(18) 0.50090(5) 0.00315(15) 0.0397(4) Uani 1 1 d . . . O4 O 0.0497(2) 0.44234(7) -0.0983(2) 0.0642(6) Uani 1 1 d . . . O5 O 0.6310(3) 0.32767(8) 0.2995(2) 0.0817(7) Uani 1 1 d . . . O6 O 0.4431(4) 0.27313(10) 0.2786(4) 0.1255(13) Uani 1 1 d . . . O7 O 1.0062(3) 0.22863(8) -0.0705(3) 0.0997(9) Uani 1 1 d . . . O8 O 0.9730(2) 0.30314(7) -0.0234(2) 0.0716(6) Uani 1 1 d . . . N1 N 0.5497(2) 0.01927(7) 0.21339(18) 0.0392(4) Uani 1 1 d . . . N2 N 0.8120(2) -0.03509(6) 0.22656(19) 0.0399(4) Uani 1 1 d . . . N3 N 0.9462(3) 0.25947(8) -0.0153(2) 0.0557(6) Uani 1 1 d . . . N4 N 0.5652(4) 0.28885(10) 0.2573(3) 0.0702(8) Uani 1 1 d . . . N5 N 0.7118(2) 0.32395(6) 0.0527(2) 0.0430(5) Uani 1 1 d . . . H5 H 0.7931 0.3367 0.0283 0.063(9) Uiso 1 1 calc R . . C1 C 0.7757(3) 0.12399(7) 0.2211(2) 0.0390(5) Uani 1 1 d . . . C2 C 0.7561(3) 0.17596(8) 0.1741(2) 0.0401(5) Uani 1 1 d . . . C3 C 0.6564(3) 0.20811(9) 0.2179(3) 0.0477(6) Uani 1 1 d . . . H3 H 0.5937 0.1963 0.2729 0.057 Uiso 1 1 calc R . . C4 C 0.6474(3) 0.25672(9) 0.1827(3) 0.0480(6) Uani 1 1 d . . . C5 C 0.7317(3) 0.27728(8) 0.0979(2) 0.0400(5) Uani 1 1 d . . . C6 C 0.8383(3) 0.24355(8) 0.0614(2) 0.0413(5) Uani 1 1 d . . . C7 C 0.8473(3) 0.19466(8) 0.0971(2) 0.0412(5) Uani 1 1 d . . . H7 H 0.9181 0.1735 0.0677 0.049 Uiso 1 1 calc R . . C8 C 0.5747(3) 0.35475(7) 0.0401(2) 0.0373(5) Uani 1 1 d . . . C9 C 0.4184(3) 0.33822(8) -0.0100(3) 0.0458(6) Uani 1 1 d . . . H9 H 0.3978 0.3044 -0.0291 0.055 Uiso 1 1 calc R . . C10 C 0.2907(3) 0.37145(8) -0.0326(3) 0.0438(5) Uani 1 1 d . . . H10 H 0.1828 0.3602 -0.0683 0.053 Uiso 1 1 calc R . . C11 C 0.3195(2) 0.42087(7) -0.0035(2) 0.0330(4) Uani 1 1 d . . . C12 C 0.4769(2) 0.43630(7) 0.0488(2) 0.0337(4) Uani 1 1 d . . . H12 H 0.4979 0.4699 0.0708 0.040 Uiso 1 1 calc R . . C13 C 0.6044(3) 0.40372(7) 0.0697(2) 0.0363(5) Uani 1 1 d . . . H13 H 0.7123 0.4150 0.1045 0.044 Uiso 1 1 calc R . . C14 C 0.1837(3) 0.45737(7) -0.0342(2) 0.0341(4) Uani 1 1 d . . . C15 C 0.4223(3) 0.04803(10) 0.2089(3) 0.0490(6) Uani 1 1 d . . . H15 H 0.4408 0.0795 0.2485 0.059 Uiso 1 1 calc R . . C16 C 0.2643(3) 0.03386(12) 0.1490(3) 0.0626(8) Uani 1 1 d . . . H16 H 0.1756 0.0548 0.1483 0.075 Uiso 1 1 calc R . . C17 C 0.2408(3) -0.01155(13) 0.0905(3) 0.0658(8) Uani 1 1 d . . . H17 H 0.1343 -0.0221 0.0467 0.079 Uiso 1 1 calc R . . C18 C 0.3694(3) -0.04170(11) 0.0950(3) 0.0559(7) Uani 1 1 d . . . H18 H 0.3529 -0.0732 0.0553 0.067 Uiso 1 1 calc R . . C19 C 0.5237(3) -0.02561(9) 0.1579(2) 0.0403(5) Uani 1 1 d . . . C20 C 0.6692(3) -0.05632(8) 0.1696(2) 0.0417(5) Uani 1 1 d . . . C21 C 0.6607(4) -0.10465(10) 0.1267(3) 0.0626(8) Uani 1 1 d . . . H21 H 0.5589 -0.1195 0.0875 0.075 Uiso 1 1 calc R . . C22 C 0.8015(4) -0.13063(11) 0.1417(4) 0.0776(10) Uani 1 1 d . . . H22 H 0.7973 -0.1637 0.1129 0.093 Uiso 1 1 calc R . . C23 C 0.9469(4) -0.10912(11) 0.1976(4) 0.0718(9) Uani 1 1 d . . . H23 H 1.0451 -0.1266 0.2073 0.086 Uiso 1 1 calc R . . C24 C 0.9476(3) -0.06139(10) 0.2397(3) 0.0537(6) Uani 1 1 d . . . H24 H 1.0488 -0.0463 0.2800 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 0.03195(19) 0.02329(17) 0.0430(2) 0.00301(13) 0.00447(15) -0.00212(11) O1 0.0565(10) 0.0266(7) 0.0519(10) 0.0065(7) 0.0202(8) 0.0036(7) O2 0.0695(11) 0.0265(8) 0.0458(9) 0.0000(7) 0.0150(8) 0.0053(7) O3 0.0435(9) 0.0288(8) 0.0460(9) -0.0011(7) 0.0111(7) 0.0071(6) O4 0.0322(9) 0.0558(11) 0.0920(15) -0.0272(11) -0.0040(9) 0.0095(8) O5 0.129(2) 0.0549(13) 0.0664(14) 0.0039(11) 0.0349(14) 0.0373(13) O6 0.139(2) 0.0799(18) 0.211(3) 0.038(2) 0.137(3) 0.0402(17) O7 0.127(2) 0.0598(13) 0.153(2) 0.0178(15) 0.107(2) 0.0271(13) O8 0.0611(12) 0.0403(10) 0.1274(19) 0.0256(11) 0.0495(13) 0.0070(8) N1 0.0359(10) 0.0420(10) 0.0376(10) 0.0033(8) 0.0064(8) -0.0031(8) N2 0.0415(10) 0.0342(10) 0.0428(11) -0.0013(8) 0.0097(9) -0.0018(7) N3 0.0531(13) 0.0411(12) 0.0822(16) 0.0177(11) 0.0345(12) 0.0137(9) N4 0.095(2) 0.0531(15) 0.0803(18) 0.0275(14) 0.0538(16) 0.0333(14) N5 0.0408(10) 0.0266(9) 0.0648(13) 0.0112(9) 0.0196(10) 0.0085(7) C1 0.0402(12) 0.0264(10) 0.0460(13) 0.0023(9) 0.0043(10) 0.0005(8) C2 0.0458(12) 0.0261(10) 0.0479(13) 0.0073(9) 0.0121(10) 0.0080(9) C3 0.0512(14) 0.0386(12) 0.0585(15) 0.0163(11) 0.0239(12) 0.0100(10) C4 0.0568(15) 0.0358(12) 0.0579(15) 0.0124(11) 0.0268(13) 0.0181(10) C5 0.0421(12) 0.0273(10) 0.0510(13) 0.0063(9) 0.0136(10) 0.0069(8) C6 0.0427(12) 0.0306(11) 0.0538(14) 0.0095(10) 0.0184(11) 0.0075(9) C7 0.0453(12) 0.0280(10) 0.0519(13) 0.0047(10) 0.0161(11) 0.0101(9) C8 0.0379(11) 0.0278(10) 0.0481(13) 0.0080(9) 0.0149(10) 0.0070(8) C9 0.0470(13) 0.0235(10) 0.0681(16) -0.0002(10) 0.0175(12) -0.0002(9) C10 0.0350(11) 0.0331(11) 0.0629(15) -0.0042(11) 0.0128(11) -0.0038(9) C11 0.0347(10) 0.0279(10) 0.0369(11) -0.0010(8) 0.0105(9) 0.0040(8) C12 0.0361(11) 0.0257(9) 0.0370(11) -0.0001(8) 0.0060(9) 0.0022(8) C13 0.0326(10) 0.0301(10) 0.0439(12) 0.0030(9) 0.0066(9) 0.0025(8) C14 0.0325(10) 0.0326(10) 0.0365(11) -0.0041(9) 0.0081(9) 0.0049(8) C15 0.0395(13) 0.0597(15) 0.0459(14) 0.0075(12) 0.0087(11) 0.0048(11) C16 0.0378(14) 0.094(2) 0.0544(17) 0.0185(16) 0.0091(12) 0.0086(13) C17 0.0394(14) 0.100(3) 0.0509(16) 0.0066(17) -0.0003(12) -0.0150(15) C18 0.0489(15) 0.0708(18) 0.0432(14) -0.0038(13) 0.0041(12) -0.0221(13) C19 0.0427(12) 0.0466(13) 0.0305(11) 0.0010(10) 0.0080(9) -0.0130(10) C20 0.0522(13) 0.0366(12) 0.0385(12) -0.0020(9) 0.0165(11) -0.0100(10) C21 0.0709(19) 0.0462(15) 0.0735(19) -0.0170(14) 0.0244(16) -0.0206(13) C22 0.098(3) 0.0406(15) 0.099(3) -0.0224(16) 0.035(2) -0.0018(16) C23 0.076(2) 0.0492(16) 0.092(2) -0.0123(16) 0.0268(18) 0.0119(15) C24 0.0544(15) 0.0436(13) 0.0627(17) -0.0046(12) 0.0153(13) 0.0060(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 2.0772(16) 4_666 ? Mn1 O3 2.1131(15) 2_645 ? Mn1 O1 2.1822(15) . ? Mn1 N2 2.2429(18) . ? Mn1 N1 2.2755(18) . ? Mn1 O2 2.3910(16) . ? Mn1 C1 2.596(2) . ? O1 C1 1.265(3) . ? O2 C1 1.243(3) . ? O3 C14 1.256(2) . ? O3 Mn1 2.1131(15) 2_655 ? O4 C14 1.235(3) . ? O4 Mn1 2.0772(16) 4_465 ? O5 N4 1.225(4) . ? O6 N4 1.211(4) . ? O7 N3 1.216(3) . ? O8 N3 1.220(3) . ? N1 C15 1.337(3) . ? N1 C19 1.349(3) . ? N2 C20 1.341(3) . ? N2 C24 1.343(3) . ? N3 C6 1.455(3) . ? N4 C4 1.481(3) . ? N5 C5 1.354(3) . ? N5 C8 1.423(3) . ? N5 H5 0.8800 . ? C1 C2 1.496(3) . ? C2 C7 1.373(3) . ? C2 C3 1.391(3) . ? C3 C4 1.373(3) . ? C3 H3 0.9500 . ? C4 C5 1.413(3) . ? C5 C6 1.424(3) . ? C6 C7 1.382(3) . ? C7 H7 0.9500 . ? C8 C9 1.378(3) . ? C8 C13 1.380(3) . ? C9 C10 1.392(3) . ? C9 H9 0.9500 . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 C12 1.379(3) . ? C11 C14 1.500(3) . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 C17 1.374(4) . ? C16 H16 0.9500 . ? C17 C18 1.368(4) . ? C17 H17 0.9500 . ? C18 C19 1.382(3) . ? C18 H18 0.9500 . ? C19 C20 1.482(3) . ? C20 C21 1.389(3) . ? C21 C22 1.373(4) . ? C21 H21 0.9500 . ? C22 C23 1.360(5) . ? C22 H22 0.9500 . ? C23 C24 1.375(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O3 96.79(7) 4_666 2_645 ? O4 Mn1 O1 90.56(7) 4_666 . ? O3 Mn1 O1 111.30(6) 2_645 . ? O4 Mn1 N2 106.08(8) 4_666 . ? O3 Mn1 N2 90.25(6) 2_645 . ? O1 Mn1 N2 151.24(7) . . ? O4 Mn1 N1 170.95(8) 4_666 . ? O3 Mn1 N1 92.15(6) 2_645 . ? O1 Mn1 N1 87.46(7) . . ? N2 Mn1 N1 72.40(7) . . ? O4 Mn1 O2 80.49(7) 4_666 . ? O3 Mn1 O2 168.26(6) 2_645 . ? O1 Mn1 O2 57.55(6) . . ? N2 Mn1 O2 101.48(6) . . ? N1 Mn1 O2 91.01(6) . . ? O4 Mn1 C1 84.37(7) 4_666 . ? O3 Mn1 C1 140.21(7) 2_645 . ? O1 Mn1 C1 29.08(6) . . ? N2 Mn1 C1 127.81(7) . . ? N1 Mn1 C1 89.64(7) . . ? O2 Mn1 C1 28.48(6) . . ? C1 O1 Mn1 93.94(13) . . ? C1 O2 Mn1 84.97(13) . . ? C14 O3 Mn1 130.54(14) . 2_655 ? C14 O4 Mn1 143.29(16) . 4_465 ? C15 N1 C19 118.7(2) . . ? C15 N1 Mn1 124.47(17) . . ? C19 N1 Mn1 116.51(15) . . ? C20 N2 C24 118.5(2) . . ? C20 N2 Mn1 117.71(15) . . ? C24 N2 Mn1 122.88(17) . . ? O7 N3 O8 121.9(2) . . ? O7 N3 C6 118.7(2) . . ? O8 N3 C6 119.5(2) . . ? O6 N4 O5 125.1(3) . . ? O6 N4 C4 117.0(3) . . ? O5 N4 C4 117.8(3) . . ? C5 N5 C8 127.52(19) . . ? C5 N5 H5 116.2 . . ? C8 N5 H5 116.2 . . ? O2 C1 O1 123.50(19) . . ? O2 C1 C2 119.0(2) . . ? O1 C1 C2 117.45(19) . . ? O2 C1 Mn1 66.54(11) . . ? O1 C1 Mn1 56.98(10) . . ? C2 C1 Mn1 174.01(17) . . ? C7 C2 C3 117.82(19) . . ? C7 C2 C1 121.24(19) . . ? C3 C2 C1 120.7(2) . . ? C4 C3 C2 120.8(2) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 123.7(2) . . ? C3 C4 N4 115.2(2) . . ? C5 C4 N4 120.3(2) . . ? N5 C5 C4 124.1(2) . . ? N5 C5 C6 122.7(2) . . ? C4 C5 C6 113.27(19) . . ? C7 C6 C5 122.8(2) . . ? C7 C6 N3 116.32(19) . . ? C5 C6 N3 120.92(19) . . ? C2 C7 C6 121.4(2) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C9 C8 C13 120.26(19) . . ? C9 C8 N5 122.5(2) . . ? C13 C8 N5 116.98(19) . . ? C8 C9 C10 119.5(2) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 120.6(2) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 118.70(19) . . ? C12 C11 C14 120.22(18) . . ? C10 C11 C14 121.01(19) . . ? C11 C12 C13 121.04(19) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 119.9(2) . . ? C8 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? O4 C14 O3 124.9(2) . . ? O4 C14 C11 116.82(19) . . ? O3 C14 C11 118.29(19) . . ? N1 C15 C16 122.8(3) . . ? N1 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C17 C16 C15 117.5(3) . . ? C17 C16 H16 121.3 . . ? C15 C16 H16 121.3 . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.0(3) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? N1 C19 C18 121.4(2) . . ? N1 C19 C20 116.19(19) . . ? C18 C19 C20 122.5(2) . . ? N2 C20 C21 121.1(2) . . ? N2 C20 C19 116.1(2) . . ? C21 C20 C19 122.8(2) . . ? C22 C21 C20 119.1(3) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 118.1(3) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? N2 C24 C23 123.0(3) . . ? N2 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.290 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.052 data_2 _database_code_depnum_ccdc_archive 'CCDC 780233' #TrackingRef '- compound 2-sjk.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 Mn2 N8 O21' _chemical_formula_sum 'C38 H32 Mn2 N8 O21' _chemical_formula_weight 1046.60 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.913(8) _cell_length_b 9.364(4) _cell_length_c 28.085(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.681(9) _cell_angle_gamma 90.00 _cell_volume 4356(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3609 _cell_measurement_theta_min 2.2968 _cell_measurement_theta_max 27.4758 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.3500 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7499 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 33250 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9915 _reflns_number_gt 7793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1136P)^2^+8.9719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9915 _refine_ls_number_parameters 617 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0876 _refine_ls_wR_factor_ref 0.2446 _refine_ls_wR_factor_gt 0.2292 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.5000 0.5000 0.0000 0.0272(2) Uani 1 2 d S . . Mn2 Mn 0.66287(4) 0.36961(7) -0.04567(2) 0.03279(19) Uani 1 1 d . . . Mn3 Mn 0.50278(9) -0.11098(16) 0.50303(6) 0.0445(4) Uiso 0.50 1 d P . . O1 O 0.62236(18) 0.4041(3) 0.02471(11) 0.0370(7) Uani 1 1 d . . . O2 O 0.7533(2) 0.4136(5) 0.03154(13) 0.0563(10) Uani 1 1 d . . . O3 O 1.0717(2) 0.1476(4) 0.38822(13) 0.0493(9) Uani 1 1 d . . . O4 O 0.9913(2) 0.1522(4) 0.44183(12) 0.0513(9) Uani 1 1 d . . . O5 O 0.6494(2) 0.1919(5) 0.31828(14) 0.0620(11) Uani 1 1 d . . . O6 O 0.7154(3) 0.2349(9) 0.38890(17) 0.123(3) Uani 1 1 d . . . O7 O 0.8223(3) 0.0086(4) 0.20250(14) 0.0619(11) Uani 1 1 d . . . O8 O 0.9431(3) 0.0949(6) 0.21389(15) 0.0796(14) Uani 1 1 d . . . O9 O 0.4513(2) 0.3523(4) 0.04528(12) 0.0464(8) Uani 1 1 d . . . O10 O 0.3338(2) 0.4155(3) 0.06407(13) 0.0460(8) Uani 1 1 d . . . O11 O 0.3794(4) -0.1987(7) 0.41798(19) 0.107(2) Uani 1 1 d . . . O12 O 0.4754(4) -0.0252(7) 0.4259(3) 0.107(2) Uiso 1 1 d . . . O13 O 0.2887(4) -0.4245(7) 0.2615(2) 0.112(2) Uani 1 1 d . . . O14 O 0.3599(3) -0.4042(5) 0.20713(17) 0.0703(12) Uani 1 1 d . . . O15 O 0.5602(3) 0.0299(6) 0.23593(16) 0.0735(13) Uani 1 1 d . . . O16 O 0.4912(3) 0.2013(5) 0.2613(2) 0.0907(17) Uani 1 1 d . . . N4 N 0.6745(3) 0.1383(4) -0.02377(15) 0.0419(9) Uani 1 1 d . . . N10 N 0.4142(3) -0.1397(4) 0.19602(14) 0.0394(9) Uani 1 1 d . . . H10 H 0.396(4) -0.212(6) 0.180(2) 0.053(17) Uiso 1 1 d . . . N15 N 0.7274(3) 0.2043(5) 0.24550(15) 0.0472(10) Uani 1 1 d . . . H15 H 0.691(4) 0.213(7) 0.253(2) 0.06(2) Uiso 1 1 d . . . N21 N 0.7544(2) 0.2748(4) -0.08289(14) 0.0425(9) Uani 1 1 d . . . N26 N 0.8790(3) 0.0739(5) 0.22655(15) 0.0510(10) Uani 1 1 d . . . N32 N 0.3401(3) -0.3645(5) 0.2445(2) 0.0629(13) Uani 1 1 d . . . N35 N 0.5064(3) 0.0758(6) 0.25565(17) 0.0607(13) Uani 1 1 d . . . N41 N 0.7130(3) 0.2088(6) 0.34654(15) 0.0572(12) Uani 1 1 d . . . C1 C 0.6935(3) 0.3993(5) 0.05089(15) 0.0334(8) Uani 1 1 d . . . C2 C 0.7039(3) 0.3584(4) 0.10304(15) 0.0342(9) Uani 1 1 d . . . C3 C 0.6389(3) 0.3030(5) 0.11994(15) 0.0390(10) Uani 1 1 d . . . H3 H 0.5870 0.3015 0.0991 0.047 Uiso 1 1 calc R . . C4 C 0.6483(3) 0.2501(6) 0.16651(16) 0.0446(11) Uani 1 1 d . . . H4 H 0.6036 0.2086 0.1771 0.053 Uiso 1 1 calc R . . C5 C 0.7227(3) 0.2572(5) 0.19806(15) 0.0396(10) Uani 1 1 d . . . C6 C 0.7873(3) 0.3217(5) 0.18241(17) 0.0442(11) Uani 1 1 d . . . H6 H 0.8376 0.3334 0.2044 0.053 Uiso 1 1 calc R . . C7 C 0.7782(3) 0.3689(5) 0.13475(16) 0.0413(10) Uani 1 1 d . . . H7 H 0.8230 0.4085 0.1238 0.050 Uiso 1 1 calc R . . C8 C 0.7930(3) 0.1758(5) 0.28087(16) 0.0403(10) Uani 1 1 d . . . C9 C 0.7889(3) 0.1893(5) 0.33078(16) 0.0414(10) Uani 1 1 d . . . C10 C 0.9319(3) 0.1505(5) 0.35803(16) 0.0388(10) Uani 1 1 d . . . C11 C 0.8562(3) 0.1779(5) 0.36783(16) 0.0421(10) Uani 1 1 d . . . H11 H 0.8505 0.1891 0.4006 0.051 Uiso 1 1 calc R . . C12 C 0.9368(3) 0.1237(5) 0.31040(16) 0.0408(10) Uani 1 1 d . . . H12 H 0.9874 0.0995 0.3029 0.049 Uiso 1 1 calc R . . C13 C 0.8694(3) 0.1314(5) 0.27372(16) 0.0403(10) Uani 1 1 d . . . C14 C 1.0031(3) 0.1483(5) 0.39877(17) 0.0418(11) Uani 1 1 d . . . C15 C 0.3950(3) 0.3361(5) 0.06791(16) 0.0379(10) Uani 1 1 d . . . C16 C 0.4012(3) 0.2135(5) 0.10274(15) 0.0349(9) Uani 1 1 d . . . C17 C 0.3525(3) 0.2078(5) 0.13719(17) 0.0415(10) Uani 1 1 d . . . H17 H 0.3152 0.2826 0.1388 0.050 Uiso 1 1 calc R . . C18 C 0.3583(3) 0.0938(5) 0.16907(17) 0.0418(10) Uani 1 1 d . . . H18 H 0.3257 0.0913 0.1929 0.050 Uiso 1 1 calc R . . C19 C 0.4115(3) -0.0166(4) 0.16617(15) 0.0345(9) Uani 1 1 d . . . C20 C 0.4601(3) -0.0110(4) 0.13198(16) 0.0369(9) Uani 1 1 d . . . H20 H 0.4974 -0.0857 0.1303 0.044 Uiso 1 1 calc R . . C21 C 0.4541(3) 0.1029(5) 0.10045(15) 0.0352(9) Uani 1 1 d . . . H21 H 0.4870 0.1054 0.0768 0.042 Uiso 1 1 calc R . . C22 C 0.4182(3) -0.1380(5) 0.24495(16) 0.0376(10) Uani 1 1 d . . . C23 C 0.3818(3) -0.2418(6) 0.27048(19) 0.0472(11) Uani 1 1 d . . . C24 C 0.3830(4) -0.2343(7) 0.3197(2) 0.0602(16) Uani 1 1 d . . . H24 H 0.3552 -0.3047 0.3343 0.072 Uiso 1 1 calc R . . C25 C 0.4232(4) -0.1278(7) 0.3476(2) 0.0605(16) Uani 1 1 d . . . C26 C 0.4622(4) -0.0251(7) 0.32509(18) 0.0550(14) Uani 1 1 d . . . H26 H 0.4915 0.0494 0.3438 0.066 Uiso 1 1 calc R . . C27 C 0.4584(3) -0.0309(5) 0.27554(17) 0.0451(11) Uani 1 1 d . . . C28 C 0.4306(6) -0.1148(10) 0.4049(3) 0.100(4) Uani 1 1 d . . . C29 C 0.7831(4) 0.3434(7) -0.1177(2) 0.0586(14) Uani 1 1 d . . . H29 H 0.7700 0.4412 -0.1238 0.070 Uiso 1 1 calc R . . C30 C 0.8317(4) 0.2749(8) -0.1452(3) 0.076(2) Uani 1 1 d . . . H30 H 0.8507 0.3249 -0.1701 0.091 Uiso 1 1 calc R . . C31 C 0.8517(4) 0.1337(8) -0.1358(3) 0.082(2) Uani 1 1 d . . . H31 H 0.8854 0.0856 -0.1539 0.098 Uiso 1 1 calc R . . C32 C 0.8230(4) 0.0635(7) -0.1005(2) 0.0642(16) Uani 1 1 d . . . H32 H 0.8370 -0.0335 -0.0935 0.077 Uiso 1 1 calc R . . C33 C 0.7725(3) 0.1356(5) -0.07463(19) 0.0465(11) Uani 1 1 d . . . C34 C 0.7337(3) 0.0637(5) -0.03820(17) 0.0445(11) Uani 1 1 d . . . C35 C 0.7540(4) -0.0742(6) -0.0213(2) 0.0662(17) Uani 1 1 d . . . H35 H 0.7963 -0.1249 -0.0314 0.079 Uiso 1 1 calc R . . C36 C 0.7116(5) -0.1354(6) 0.0102(2) 0.076(2) Uani 1 1 d . . . H36 H 0.7250 -0.2287 0.0224 0.091 Uiso 1 1 calc R . . C37 C 0.6502(5) -0.0615(7) 0.0238(2) 0.0730(19) Uani 1 1 d . . . H37 H 0.6195 -0.1036 0.0449 0.088 Uiso 1 1 calc R . . C38 C 0.6335(4) 0.0754(6) 0.0063(2) 0.0571(14) Uani 1 1 d . . . H38 H 0.5911 0.1268 0.0161 0.069 Uiso 1 1 calc R . . O1W O 0.3820(4) -0.0385(6) 0.5003(2) 0.0973(17) Uiso 1 1 d . . . O2W O 0.4747(6) -0.3148(10) 0.5419(3) 0.070(2) Uiso 0.50 1 d P . . O3W O 0.4369(8) -0.3111(15) 0.5815(5) 0.110(4) Uiso 0.50 1 d P . . O4W O 0.9052(9) 0.0692(18) 0.0893(6) 0.127(5) Uiso 0.50 1 d P . . O5W O 0.9206(7) -0.0542(13) 0.0936(4) 0.093(3) Uiso 0.50 1 d P . . O6W O 0.9779(8) -0.0614(15) 0.0337(5) 0.103(4) Uiso 0.50 1 d P . . O8W O 0.9402(6) 0.1859(10) 0.0266(4) 0.073(2) Uiso 0.50 1 d P . . O7W O 0.9679(7) 0.0653(13) 0.0272(4) 0.094(3) Uiso 0.50 1 d P . . O9W O 0.9002(8) 0.1968(15) 0.0651(5) 0.114(4) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0297(4) 0.0340(4) 0.0180(4) 0.0016(3) 0.0050(3) -0.0007(3) Mn2 0.0374(4) 0.0359(4) 0.0241(3) 0.0028(2) 0.0041(3) 0.0030(3) O1 0.0346(16) 0.0482(17) 0.0262(15) 0.0064(12) 0.0016(12) 0.0052(13) O2 0.0398(19) 0.092(3) 0.037(2) 0.0186(18) 0.0076(15) -0.0070(18) O3 0.0420(19) 0.055(2) 0.043(2) 0.0100(15) -0.0083(15) -0.0069(15) O4 0.077(3) 0.0470(19) 0.0230(16) 0.0075(13) -0.0063(16) -0.0036(17) O5 0.042(2) 0.102(3) 0.039(2) 0.0040(19) 0.0012(16) -0.008(2) O6 0.063(3) 0.263(8) 0.042(3) -0.045(4) 0.010(2) 0.017(4) O7 0.071(3) 0.070(3) 0.039(2) -0.0133(17) -0.0009(19) -0.006(2) O8 0.066(3) 0.139(4) 0.039(2) -0.008(2) 0.022(2) -0.006(3) O9 0.0461(19) 0.0504(19) 0.043(2) 0.0197(15) 0.0107(15) -0.0065(14) O10 0.0473(19) 0.0389(17) 0.051(2) 0.0157(14) 0.0077(15) -0.0022(14) O11 0.134(5) 0.145(5) 0.059(3) 0.037(3) 0.058(3) 0.055(4) O13 0.121(5) 0.101(4) 0.137(5) 0.004(4) 0.084(4) -0.046(4) O14 0.093(3) 0.057(2) 0.066(3) 0.001(2) 0.027(3) -0.020(2) O15 0.062(3) 0.110(4) 0.048(2) 0.004(2) 0.012(2) -0.032(2) O16 0.105(4) 0.059(3) 0.089(4) 0.013(2) -0.023(3) -0.015(3) N4 0.051(2) 0.036(2) 0.037(2) -0.0025(15) 0.0055(17) -0.0007(16) N10 0.053(2) 0.038(2) 0.0271(19) 0.0056(15) 0.0081(17) -0.0062(17) N15 0.040(2) 0.075(3) 0.024(2) 0.0106(18) 0.0001(17) -0.008(2) N21 0.035(2) 0.053(2) 0.039(2) -0.0041(17) 0.0067(16) 0.0004(16) N26 0.059(3) 0.065(3) 0.028(2) -0.0008(18) 0.0047(19) 0.000(2) N32 0.068(3) 0.056(3) 0.070(3) 0.018(2) 0.026(3) -0.011(2) N35 0.066(3) 0.067(3) 0.041(3) 0.007(2) -0.009(2) -0.019(2) N41 0.047(2) 0.094(4) 0.029(2) -0.003(2) 0.0051(18) -0.002(2) C1 0.036(2) 0.038(2) 0.025(2) 0.0032(15) 0.0052(16) -0.0003(17) C2 0.039(2) 0.040(2) 0.023(2) 0.0031(15) 0.0031(16) -0.0024(17) C3 0.032(2) 0.058(3) 0.024(2) 0.0060(18) 0.0001(16) -0.0028(19) C4 0.036(2) 0.067(3) 0.029(2) 0.009(2) 0.0042(18) -0.005(2) C5 0.047(3) 0.048(3) 0.022(2) 0.0049(17) 0.0029(18) -0.007(2) C6 0.038(2) 0.058(3) 0.031(2) 0.0061(19) -0.0055(18) -0.013(2) C7 0.040(2) 0.052(3) 0.029(2) 0.0089(18) -0.0004(18) -0.0110(19) C8 0.042(2) 0.052(3) 0.023(2) 0.0052(17) -0.0017(17) -0.010(2) C9 0.040(2) 0.055(3) 0.028(2) 0.0010(18) 0.0047(18) -0.008(2) C10 0.042(2) 0.046(2) 0.024(2) 0.0079(17) -0.0013(17) -0.0111(19) C11 0.053(3) 0.050(3) 0.020(2) 0.0011(17) 0.0010(18) -0.011(2) C12 0.041(2) 0.049(3) 0.030(2) 0.0062(18) 0.0022(18) -0.0070(19) C13 0.047(3) 0.049(3) 0.022(2) 0.0015(17) 0.0024(18) -0.007(2) C14 0.054(3) 0.035(2) 0.031(2) 0.0087(17) -0.006(2) -0.0069(19) C15 0.038(2) 0.040(2) 0.032(2) 0.0084(17) -0.0009(18) -0.0055(18) C16 0.041(2) 0.038(2) 0.025(2) 0.0057(16) 0.0062(17) -0.0068(17) C17 0.042(2) 0.047(3) 0.039(2) 0.0091(19) 0.016(2) 0.0084(19) C18 0.042(2) 0.052(3) 0.036(2) 0.0103(19) 0.018(2) 0.001(2) C19 0.044(2) 0.036(2) 0.024(2) 0.0061(15) 0.0091(17) -0.0048(17) C20 0.049(3) 0.033(2) 0.030(2) 0.0030(16) 0.0103(19) -0.0004(18) C21 0.040(2) 0.040(2) 0.027(2) 0.0027(16) 0.0120(17) -0.0048(17) C22 0.039(2) 0.046(2) 0.030(2) 0.0118(17) 0.0125(18) 0.0048(18) C23 0.051(3) 0.050(3) 0.044(3) 0.016(2) 0.019(2) 0.003(2) C24 0.071(4) 0.072(4) 0.047(3) 0.028(3) 0.033(3) 0.021(3) C25 0.065(4) 0.084(4) 0.037(3) 0.023(3) 0.021(3) 0.031(3) C26 0.060(3) 0.076(4) 0.028(2) -0.001(2) 0.006(2) 0.017(3) C27 0.051(3) 0.052(3) 0.032(2) 0.0063(19) 0.009(2) 0.001(2) C28 0.130(7) 0.113(6) 0.086(5) 0.062(5) 0.088(6) 0.076(6) C29 0.057(3) 0.070(4) 0.052(3) -0.005(3) 0.018(3) -0.013(3) C30 0.076(4) 0.093(5) 0.070(4) -0.025(4) 0.042(4) -0.030(4) C31 0.062(4) 0.094(5) 0.100(6) -0.044(4) 0.040(4) -0.015(4) C32 0.052(3) 0.068(4) 0.075(4) -0.025(3) 0.019(3) 0.001(3) C33 0.041(2) 0.047(3) 0.047(3) -0.014(2) -0.003(2) 0.004(2) C34 0.052(3) 0.044(3) 0.031(2) -0.0052(18) -0.007(2) 0.003(2) C35 0.089(4) 0.051(3) 0.049(3) -0.003(3) -0.010(3) 0.019(3) C36 0.137(7) 0.045(3) 0.036(3) 0.007(2) -0.007(4) 0.012(4) C37 0.129(6) 0.052(3) 0.037(3) 0.010(2) 0.015(3) -0.011(4) C38 0.086(4) 0.046(3) 0.041(3) 0.005(2) 0.016(3) -0.005(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 O4 2.150(3) 4_565 ? Mn1 O4 2.150(3) 2_655 ? Mn1 O9 2.152(3) 3_665 ? Mn1 O9 2.152(3) . ? Mn1 O1 2.234(3) 3_665 ? Mn1 O1 2.234(3) . ? Mn2 O10 2.081(3) 3_665 ? Mn2 O3 2.166(3) 4_565 ? Mn2 N21 2.221(4) . ? Mn2 O1 2.242(3) . ? Mn2 N4 2.249(4) . ? Mn2 O2 2.423(4) . ? Mn3 Mn3 2.086(3) 3_656 ? Mn3 O1W 2.139(6) . ? Mn3 O12 2.268(7) . ? Mn3 O2W 2.295(10) . ? Mn3 O12 2.333(7) 3_656 ? Mn3 O8W 2.359(10) 2_645 ? Mn3 O1W 2.416(6) 3_656 ? O1 C1 1.277(5) . ? O2 C1 1.249(5) . ? O3 C14 1.254(6) . ? O3 Mn2 2.166(3) 4_666 ? O4 C14 1.266(6) . ? O4 Mn1 2.150(3) 2_645 ? O5 N41 1.210(6) . ? O6 N41 1.207(6) . ? O7 N26 1.219(6) . ? O8 N26 1.223(6) . ? O9 C15 1.256(6) . ? O10 C15 1.262(6) . ? O10 Mn2 2.081(3) 3_665 ? O11 C28 1.278(11) . ? O12 C28 1.202(12) . ? O12 Mn3 2.333(7) 3_656 ? O13 N32 1.213(6) . ? O14 N32 1.221(7) . ? O15 N35 1.234(7) . ? O16 N35 1.221(7) . ? N4 C38 1.333(7) . ? N4 C34 1.349(6) . ? N10 C22 1.362(6) . ? N10 C19 1.421(5) . ? N10 H10 0.84(6) . ? N15 C8 1.357(6) . ? N15 C5 1.408(6) . ? N15 H15 0.70(6) . ? N21 C29 1.341(7) . ? N21 C33 1.348(6) . ? N26 C13 1.469(6) . ? N32 C23 1.464(8) . ? N35 C27 1.467(7) . ? N41 C9 1.452(6) . ? C1 C2 1.489(6) . ? C2 C3 1.385(6) . ? C2 C7 1.388(6) . ? C3 C4 1.377(6) . ? C3 H3 0.9500 . ? C4 C5 1.387(6) . ? C4 H4 0.9500 . ? C5 C6 1.395(6) . ? C6 C7 1.388(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.411(7) . ? C8 C9 1.423(6) . ? C9 C11 1.382(6) . ? C10 C12 1.380(6) . ? C10 C11 1.387(7) . ? C10 C14 1.483(6) . ? C11 H11 0.9500 . ? C12 C13 1.375(6) . ? C12 H12 0.9500 . ? C15 C16 1.498(6) . ? C16 C21 1.380(6) . ? C16 C17 1.392(6) . ? C17 C18 1.384(6) . ? C17 H17 0.9500 . ? C18 C19 1.384(7) . ? C18 H18 0.9500 . ? C19 C20 1.385(6) . ? C20 C21 1.377(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.403(7) . ? C22 C23 1.420(6) . ? C23 C24 1.380(7) . ? C24 C25 1.363(10) . ? C24 H24 0.9500 . ? C25 C26 1.390(9) . ? C25 C28 1.591(10) . ? C26 C27 1.381(7) . ? C26 H26 0.9500 . ? C29 C30 1.393(8) . ? C29 H29 0.9500 . ? C30 C31 1.378(11) . ? C30 H30 0.9500 . ? C31 C32 1.357(10) . ? C31 H31 0.9500 . ? C32 C33 1.403(7) . ? C32 H32 0.9500 . ? C33 C34 1.483(8) . ? C34 C35 1.394(8) . ? C35 C36 1.370(10) . ? C35 H35 0.9500 . ? C36 C37 1.365(11) . ? C36 H36 0.9500 . ? C37 C38 1.382(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? O1W Mn3 2.416(6) 3_656 ? O2W O6W 1.185(14) 4_556 ? O2W O3W 1.391(15) . ? O3W O5W 1.350(17) 4_556 ? O4W O5W 1.185(18) . ? O4W O9W 1.367(19) . ? O5W O3W 1.350(17) 4_655 ? O6W O2W 1.185(14) 4_655 ? O6W O7W 1.207(16) . ? O8W O7W 1.221(14) . ? O8W O9W 1.391(15) . ? O8W Mn3 2.359(10) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O4 180.0(2) 4_565 2_655 ? O4 Mn1 O9 87.29(15) 4_565 3_665 ? O4 Mn1 O9 92.71(15) 2_655 3_665 ? O4 Mn1 O9 92.71(15) 4_565 . ? O4 Mn1 O9 87.29(15) 2_655 . ? O9 Mn1 O9 180.00(18) 3_665 . ? O4 Mn1 O1 96.52(13) 4_565 3_665 ? O4 Mn1 O1 83.48(13) 2_655 3_665 ? O9 Mn1 O1 89.95(12) 3_665 3_665 ? O9 Mn1 O1 90.05(12) . 3_665 ? O4 Mn1 O1 83.48(13) 4_565 . ? O4 Mn1 O1 96.52(13) 2_655 . ? O9 Mn1 O1 90.05(12) 3_665 . ? O9 Mn1 O1 89.95(12) . . ? O1 Mn1 O1 180.00(15) 3_665 . ? O10 Mn2 O3 84.82(14) 3_665 4_565 ? O10 Mn2 N21 102.29(15) 3_665 . ? O3 Mn2 N21 90.57(15) 4_565 . ? O10 Mn2 O1 96.21(13) 3_665 . ? O3 Mn2 O1 118.33(13) 4_565 . ? N21 Mn2 O1 147.02(13) . . ? O10 Mn2 N4 173.56(15) 3_665 . ? O3 Mn2 N4 99.80(14) 4_565 . ? N21 Mn2 N4 73.33(15) . . ? O1 Mn2 N4 85.59(13) . . ? O10 Mn2 O2 90.79(14) 3_665 . ? O3 Mn2 O2 172.24(14) 4_565 . ? N21 Mn2 O2 96.62(14) . . ? O1 Mn2 O2 55.73(12) . . ? N4 Mn2 O2 85.11(15) . . ? Mn3 Mn3 O1W 69.76(18) 3_656 . ? Mn3 Mn3 O12 64.7(2) 3_656 . ? O1W Mn3 O12 81.0(2) . . ? Mn3 Mn3 O2W 149.0(3) 3_656 . ? O1W Mn3 O2W 89.6(3) . . ? O12 Mn3 O2W 136.6(3) . . ? Mn3 Mn3 O12 61.46(19) 3_656 3_656 ? O1W Mn3 O12 80.9(2) . 3_656 ? O12 Mn3 O12 126.11(18) . 3_656 ? O2W Mn3 O12 93.4(3) . 3_656 ? Mn3 Mn3 O8W 142.1(3) 3_656 2_645 ? O1W Mn3 O8W 134.3(3) . 2_645 ? O12 Mn3 O8W 88.1(3) . 2_645 ? O2W Mn3 O8W 68.6(3) . 2_645 ? O12 Mn3 O8W 137.5(3) 3_656 2_645 ? Mn3 Mn3 O1W 56.16(16) 3_656 3_656 ? O1W Mn3 O1W 125.92(16) . 3_656 ? O12 Mn3 O1W 76.6(2) . 3_656 ? O2W Mn3 O1W 138.2(3) . 3_656 ? O12 Mn3 O1W 74.2(2) 3_656 3_656 ? O8W Mn3 O1W 93.6(3) 2_645 3_656 ? C1 O1 Mn1 153.9(3) . . ? C1 O1 Mn2 94.7(2) . . ? Mn1 O1 Mn2 102.32(12) . . ? C1 O2 Mn2 87.2(3) . . ? C14 O3 Mn2 109.3(3) . 4_666 ? C14 O4 Mn1 135.0(3) . 2_645 ? C15 O9 Mn1 142.7(3) . . ? C15 O10 Mn2 121.8(3) . 3_665 ? C28 O12 Mn3 102.1(5) . . ? C28 O12 Mn3 141.0(6) . 3_656 ? Mn3 O12 Mn3 53.89(18) . 3_656 ? C38 N4 C34 118.3(5) . . ? C38 N4 Mn2 124.8(4) . . ? C34 N4 Mn2 116.4(3) . . ? C22 N10 C19 125.1(4) . . ? C22 N10 H10 119(4) . . ? C19 N10 H10 112(4) . . ? C8 N15 C5 130.0(4) . . ? C8 N15 H15 116(5) . . ? C5 N15 H15 111(5) . . ? C29 N21 C33 119.1(5) . . ? C29 N21 Mn2 122.8(4) . . ? C33 N21 Mn2 117.4(3) . . ? O7 N26 O8 124.3(5) . . ? O7 N26 C13 117.8(4) . . ? O8 N26 C13 117.9(4) . . ? O13 N32 O14 122.8(6) . . ? O13 N32 C23 118.6(6) . . ? O14 N32 C23 118.6(4) . . ? O16 N35 O15 126.0(6) . . ? O16 N35 C27 117.3(6) . . ? O15 N35 C27 116.7(5) . . ? O6 N41 O5 121.4(5) . . ? O6 N41 C9 118.0(5) . . ? O5 N41 C9 120.4(4) . . ? O2 C1 O1 119.8(4) . . ? O2 C1 C2 120.7(4) . . ? O1 C1 C2 119.1(4) . . ? C3 C2 C7 119.0(4) . . ? C3 C2 C1 119.3(4) . . ? C7 C2 C1 121.6(4) . . ? C4 C3 C2 120.9(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 119.1(4) . . ? C4 C5 N15 117.2(4) . . ? C6 C5 N15 123.6(4) . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 120.4(4) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? N15 C8 C13 126.2(4) . . ? N15 C8 C9 120.6(5) . . ? C13 C8 C9 113.2(4) . . ? C11 C9 C8 122.6(4) . . ? C11 C9 N41 115.1(4) . . ? C8 C9 N41 122.2(4) . . ? C12 C10 C11 117.7(4) . . ? C12 C10 C14 123.2(5) . . ? C11 C10 C14 119.1(4) . . ? C9 C11 C10 121.2(4) . . ? C9 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C10 120.9(5) . . ? C13 C12 H12 119.5 . . ? C10 C12 H12 119.5 . . ? C12 C13 C8 123.6(4) . . ? C12 C13 N26 115.5(4) . . ? C8 C13 N26 120.5(4) . . ? O3 C14 O4 124.0(4) . . ? O3 C14 C10 117.5(4) . . ? O4 C14 C10 118.5(5) . . ? O9 C15 O10 125.4(4) . . ? O9 C15 C16 117.6(4) . . ? O10 C15 C16 117.0(4) . . ? C21 C16 C17 119.0(4) . . ? C21 C16 C15 120.3(4) . . ? C17 C16 C15 120.7(4) . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 119.8(4) . . ? C18 C19 N10 121.0(4) . . ? C20 C19 N10 119.1(4) . . ? C21 C20 C19 119.9(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C16 121.0(4) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? N10 C22 C27 123.0(4) . . ? N10 C22 C23 124.3(5) . . ? C27 C22 C23 112.7(4) . . ? C24 C23 C22 123.4(5) . . ? C24 C23 N32 116.6(5) . . ? C22 C23 N32 120.0(5) . . ? C25 C24 C23 121.3(5) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 118.1(5) . . ? C24 C25 C28 124.5(6) . . ? C26 C25 C28 117.4(7) . . ? C27 C26 C25 120.2(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C22 124.3(5) . . ? C26 C27 N35 116.1(5) . . ? C22 C27 N35 119.3(4) . . ? O12 C28 O11 133.1(8) . . ? O12 C28 C25 117.6(7) . . ? O11 C28 C25 108.9(9) . . ? N21 C29 C30 121.7(6) . . ? N21 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C31 C30 C29 119.0(6) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C32 C31 C30 119.7(6) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.4(6) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? N21 C33 C32 121.1(5) . . ? N21 C33 C34 116.2(4) . . ? C32 C33 C34 122.7(5) . . ? N4 C34 C35 121.5(5) . . ? N4 C34 C33 115.5(4) . . ? C35 C34 C33 122.9(5) . . ? C36 C35 C34 118.9(6) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C37 C36 C35 119.7(5) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 118.9(6) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? N4 C38 C37 122.6(6) . . ? N4 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? Mn3 O1W Mn3 54.08(16) . 3_656 ? O6W O2W O3W 103.1(11) 4_556 . ? O6W O2W Mn3 134.3(9) 4_556 . ? O3W O2W Mn3 122.1(8) . . ? O5W O3W O2W 109.2(11) 4_556 . ? O5W O4W O9W 153.3(16) . . ? O4W O5W O3W 159.5(14) . 4_655 ? O2W O6W O7W 168.6(14) 4_655 . ? O7W O8W O9W 107.6(11) . . ? O7W O8W Mn3 124.6(8) . 2_655 ? O9W O8W Mn3 120.9(8) . 2_655 ? O6W O7W O8W 162.3(13) . . ? O4W O9W O8W 109.3(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.633 _refine_diff_density_min -1.500 _refine_diff_density_rms 0.104 data_4 _database_code_depnum_ccdc_archive 'CCDC 780234' #TrackingRef '- compound 4-sjk.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Mn N5 O9.50' _chemical_formula_sum 'C24 H18 Mn N5 O9.50' _chemical_formula_weight 583.37 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 24.820(2) _cell_length_b 13.4888(9) _cell_length_c 7.3141(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2448.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5680 _cell_measurement_theta_min 3.0202 _cell_measurement_theta_max 27.4835 _exptl_crystal_description needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.6000 _exptl_crystal_size_mid 0.0600 _exptl_crystal_size_min 0.0600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7982 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 18635 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5554 _reflns_number_gt 4633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.4134P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 5554 _refine_ls_number_parameters 365 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.695457(16) 0.91871(3) 0.73789(9) 0.02916(12) Uani 1 1 d . . . O1 O 0.81539(9) 0.84981(17) 0.5128(4) 0.0377(6) Uani 1 1 d . . . O2 O 0.74221(10) 0.79481(16) 0.6614(4) 0.0429(6) Uani 1 1 d . . . O3 O 0.74049(13) 0.4779(2) 0.9537(5) 0.0654(9) Uani 1 1 d . . . O4 O 0.81575(15) 0.4406(3) 1.0837(5) 0.0727(10) Uani 1 1 d . . . O5 O 0.97665(11) 0.6481(2) 0.5448(6) 0.0767(11) Uani 1 1 d . . . O6 O 0.98124(11) 0.5139(2) 0.6956(7) 0.0921(15) Uani 1 1 d . . . O7 O 0.81558(9) -0.01897(16) 0.9613(4) 0.0356(6) Uani 1 1 d . . . O8 O 0.74631(10) 0.03711(16) 0.7981(4) 0.0451(7) Uani 1 1 d . . . N1 N 0.89378(13) 0.4242(2) 0.8038(5) 0.0411(8) Uani 1 1 d . . . N2 N 0.78942(15) 0.4811(2) 0.9645(5) 0.0460(8) Uani 1 1 d . . . N3 N 0.95518(12) 0.5833(2) 0.6331(5) 0.0467(9) Uani 1 1 d . . . N4 N 0.62280(11) 1.0131(2) 0.8179(4) 0.0364(7) Uani 1 1 d . . . N5 N 0.61922(11) 0.8290(2) 0.6789(4) 0.0359(7) Uani 1 1 d . . . C1 C 0.81947(13) 0.6954(2) 0.6678(5) 0.0292(7) Uani 1 1 d . . . C2 C 0.79322(13) 0.6263(2) 0.7737(5) 0.0336(8) Uani 1 1 d . . . H2 H 0.7570 0.6379 0.8096 0.040 Uiso 1 1 calc R . . C3 C 0.81863(14) 0.5403(2) 0.8286(5) 0.0330(7) Uani 1 1 d . . . C4 C 0.87114(12) 0.5146(2) 0.7717(5) 0.0326(8) Uani 1 1 d . . . C5 C 0.89818(12) 0.5913(2) 0.6780(5) 0.0316(7) Uani 1 1 d . . . C6 C 0.87309(12) 0.6790(2) 0.6245(5) 0.0307(7) Uani 1 1 d . . . H6 H 0.8928 0.7276 0.5583 0.037 Uiso 1 1 calc R . . C7 C 0.79040(13) 0.7885(2) 0.6081(5) 0.0325(7) Uani 1 1 d . . . C8 C 0.86722(13) 0.3311(2) 0.8162(5) 0.0338(7) Uani 1 1 d . . . C9 C 0.81806(13) 0.3128(2) 0.7300(6) 0.0393(8) Uani 1 1 d . . . H9 H 0.8014 0.3631 0.6589 0.047 Uiso 1 1 calc R . . C10 C 0.79382(13) 0.2213(2) 0.7486(6) 0.0363(7) Uani 1 1 d . . . H10 H 0.7596 0.2097 0.6944 0.044 Uiso 1 1 calc R . . C11 C 0.81906(13) 0.1455(2) 0.8463(5) 0.0287(7) Uani 1 1 d . . . C12 C 0.86943(13) 0.1637(2) 0.9212(5) 0.0347(8) Uani 1 1 d . . . H12 H 0.8879 0.1117 0.9825 0.042 Uiso 1 1 calc R . . C13 C 0.89317(13) 0.2557(2) 0.9082(6) 0.0372(8) Uani 1 1 d . . . H13 H 0.9274 0.2672 0.9627 0.045 Uiso 1 1 calc R . . C14 C 0.79204(13) 0.0467(2) 0.8719(5) 0.0314(8) Uani 1 1 d . . . C15 C 0.62704(16) 1.1075(3) 0.8694(6) 0.0475(10) Uani 1 1 d . . . H15 H 0.6611 1.1311 0.9095 0.057 Uiso 1 1 calc R . . C16 C 0.5838(2) 1.1727(3) 0.8670(7) 0.0603(12) Uani 1 1 d . . . H16 H 0.5879 1.2393 0.9070 0.072 Uiso 1 1 calc R . . C17 C 0.53504(18) 1.1384(3) 0.8050(7) 0.0630(13) Uani 1 1 d . . . H17 H 0.5050 1.1818 0.7984 0.076 Uiso 1 1 calc R . . C18 C 0.52984(14) 1.0412(3) 0.7528(7) 0.0524(10) Uani 1 1 d . . . H18 H 0.4962 1.0167 0.7107 0.063 Uiso 1 1 calc R . . C19 C 0.57435(13) 0.9791(3) 0.7621(5) 0.0384(8) Uani 1 1 d . . . C20 C 0.57179(13) 0.8732(2) 0.7116(5) 0.0363(8) Uani 1 1 d . . . C21 C 0.52333(15) 0.8215(3) 0.6987(6) 0.0523(11) Uani 1 1 d . . . H21 H 0.4900 0.8538 0.7215 0.063 Uiso 1 1 calc R . . C22 C 0.52474(18) 0.7231(4) 0.6524(7) 0.0648(13) Uani 1 1 d . . . H22 H 0.4922 0.6865 0.6422 0.078 Uiso 1 1 calc R . . C23 C 0.57308(19) 0.6774(3) 0.6209(6) 0.0575(12) Uani 1 1 d . . . H23 H 0.5747 0.6091 0.5903 0.069 Uiso 1 1 calc R . . C24 C 0.61887(17) 0.7330(3) 0.6348(6) 0.0482(10) Uani 1 1 d . . . H24 H 0.6524 0.7015 0.6117 0.058 Uiso 1 1 calc R . . H1 H 0.9282(15) 0.426(2) 0.805(5) 0.032(10) Uiso 1 1 d . . . O1W O 0.9080(5) 0.4315(8) 1.3586(19) 0.150(5) Uani 0.50 1 d P . . O2W O 0.59468(10) 0.9189(2) 0.2362(6) 0.0639(7) 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 Mn1 0.0234(2) 0.0239(2) 0.0401(3) 0.0052(2) -0.0003(3) -0.00010(17) O1 0.0377(13) 0.0310(13) 0.0443(16) 0.0139(11) 0.0002(11) 0.0005(10) O2 0.0324(13) 0.0329(12) 0.0634(17) 0.0060(13) 0.0101(12) 0.0071(10) O3 0.055(2) 0.0562(17) 0.085(2) 0.0135(18) 0.0335(18) -0.0124(14) O4 0.099(3) 0.064(2) 0.055(2) 0.0320(17) 0.015(2) 0.0110(18) O5 0.0410(16) 0.068(2) 0.121(3) 0.049(2) 0.0249(18) 0.0060(14) O6 0.0328(14) 0.0525(16) 0.191(5) 0.053(3) 0.013(2) 0.0119(12) O7 0.0388(13) 0.0249(12) 0.0432(15) 0.0093(11) 0.0020(11) -0.0008(9) O8 0.0352(12) 0.0320(12) 0.0682(19) 0.0095(12) -0.0143(13) -0.0081(10) N1 0.0310(14) 0.0228(13) 0.069(2) 0.0084(14) -0.0008(15) -0.0017(11) N2 0.058(2) 0.0337(17) 0.046(2) 0.0078(15) 0.0176(17) -0.0044(14) N3 0.0315(15) 0.0295(15) 0.079(2) 0.0125(16) 0.0063(16) 0.0011(12) N4 0.0331(15) 0.0372(16) 0.0388(17) 0.0031(14) -0.0030(13) 0.0063(12) N5 0.0314(14) 0.0359(15) 0.0403(17) -0.0001(14) 0.0020(13) -0.0055(11) C1 0.0325(16) 0.0213(15) 0.0339(17) -0.0006(13) 0.0025(14) 0.0025(12) C2 0.0297(15) 0.0279(15) 0.043(2) 0.0021(15) 0.0042(15) -0.0024(12) C3 0.0357(17) 0.0232(16) 0.040(2) 0.0076(15) 0.0056(15) -0.0046(13) C4 0.0310(15) 0.0214(14) 0.045(2) 0.0055(14) 0.0009(15) -0.0012(11) C5 0.0261(14) 0.0266(15) 0.0422(19) 0.0038(15) 0.0036(13) -0.0003(12) C6 0.0300(16) 0.0242(15) 0.038(2) 0.0054(14) 0.0031(14) -0.0036(12) C7 0.0353(17) 0.0264(16) 0.0358(19) 0.0047(15) -0.0009(15) 0.0013(13) C8 0.0359(17) 0.0209(15) 0.045(2) 0.0066(15) -0.0003(15) -0.0030(12) C9 0.0419(17) 0.0271(15) 0.049(2) 0.0122(19) -0.008(2) 0.0021(12) C10 0.0363(16) 0.0287(15) 0.044(2) 0.0085(19) -0.0104(19) -0.0004(12) C11 0.0298(15) 0.0202(15) 0.0362(19) 0.0016(14) -0.0027(14) -0.0012(11) C12 0.0350(18) 0.0214(15) 0.048(2) 0.0104(15) -0.0062(16) -0.0013(12) C13 0.0313(16) 0.0251(16) 0.055(2) 0.0081(16) -0.0059(17) -0.0013(13) C14 0.0292(16) 0.0236(16) 0.041(2) 0.0020(15) 0.0027(14) -0.0031(12) C15 0.047(2) 0.042(2) 0.053(3) -0.0040(18) -0.0029(19) 0.0093(17) C16 0.072(3) 0.050(3) 0.059(3) -0.008(2) 0.011(2) 0.020(2) C17 0.057(3) 0.064(3) 0.068(3) 0.006(2) 0.008(2) 0.032(2) C18 0.0309(17) 0.069(2) 0.057(3) 0.007(3) -0.001(2) 0.0134(16) C19 0.0278(15) 0.051(2) 0.036(2) 0.0040(18) 0.0036(16) 0.0051(13) C20 0.0284(15) 0.0450(17) 0.035(2) 0.0070(17) -0.0015(15) -0.0086(13) C21 0.0313(18) 0.064(2) 0.061(3) 0.011(2) -0.0043(18) -0.0099(16) C22 0.050(3) 0.071(3) 0.073(3) 0.008(3) -0.002(2) -0.031(2) C23 0.066(3) 0.050(2) 0.056(3) -0.007(2) 0.006(2) -0.028(2) C24 0.051(2) 0.042(2) 0.051(3) -0.0057(19) 0.0057(19) -0.0077(17) O1W 0.181(12) 0.127(8) 0.142(10) -0.008(7) -0.020(9) -0.009(7) O2W 0.0384(13) 0.0788(18) 0.074(2) -0.0057(18) 0.000(2) 0.0005(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 Mn1 O8 2.083(2) 1_565 ? Mn1 O2 2.110(2) . ? Mn1 O7 2.208(3) 3_664 ? Mn1 O1 2.232(3) 3_655 ? Mn1 N4 2.284(3) . ? Mn1 N5 2.287(3) . ? O1 C7 1.247(4) . ? O1 Mn1 2.232(2) 3_654 ? O2 C7 1.261(4) . ? O3 N2 1.218(4) . ? O4 N2 1.219(5) . ? O5 N3 1.210(4) . ? O6 N3 1.226(4) . ? O7 C14 1.246(4) . ? O7 Mn1 2.208(3) 3_645 ? O8 C14 1.263(4) . ? O8 Mn1 2.083(2) 1_545 ? N1 C4 1.363(4) . ? N1 C8 1.422(4) . ? N2 C3 1.467(4) . ? N3 C5 1.456(4) . ? N4 C15 1.331(5) . ? N4 C19 1.350(4) . ? N5 C24 1.334(4) . ? N5 C20 1.341(4) . ? C1 C2 1.377(4) . ? C1 C6 1.386(4) . ? C1 C7 1.512(4) . ? C2 C3 1.379(5) . ? C3 C4 1.411(5) . ? C4 C5 1.411(4) . ? C5 C6 1.393(4) . ? C8 C13 1.379(4) . ? C8 C9 1.395(5) . ? C9 C10 1.380(4) . ? C10 C11 1.396(5) . ? C11 C12 1.386(4) . ? C11 C14 1.504(4) . ? C12 C13 1.377(4) . ? C15 C16 1.388(5) . ? C16 C17 1.373(7) . ? C17 C18 1.371(6) . ? C18 C19 1.388(5) . ? C19 C20 1.477(5) . ? C20 C21 1.393(5) . ? C21 C22 1.371(6) . ? C22 C23 1.368(6) . ? C23 C24 1.365(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Mn1 O2 109.28(9) 1_565 . ? O8 Mn1 O7 88.68(10) 1_565 3_664 ? O2 Mn1 O7 97.29(10) . 3_664 ? O8 Mn1 O1 101.65(11) 1_565 3_655 ? O2 Mn1 O1 88.59(10) . 3_655 ? O7 Mn1 O1 165.77(8) 3_664 3_655 ? O8 Mn1 N4 89.81(11) 1_565 . ? O2 Mn1 N4 160.70(10) . . ? O7 Mn1 N4 85.66(10) 3_664 . ? O1 Mn1 N4 84.62(10) 3_655 . ? O8 Mn1 N5 161.27(10) 1_565 . ? O2 Mn1 N5 89.18(10) . . ? O7 Mn1 N5 85.75(10) 3_664 . ? O1 Mn1 N5 81.37(10) 3_655 . ? N4 Mn1 N5 71.96(10) . . ? C7 O1 Mn1 136.0(2) . 3_654 ? C7 O2 Mn1 131.1(2) . . ? C14 O7 Mn1 133.9(2) . 3_645 ? C14 O8 Mn1 135.5(2) . 1_545 ? C4 N1 C8 127.6(3) . . ? O3 N2 O4 124.4(4) . . ? O3 N2 C3 117.9(3) . . ? O4 N2 C3 117.7(3) . . ? O5 N3 O6 121.2(3) . . ? O5 N3 C5 119.6(3) . . ? O6 N3 C5 119.0(3) . . ? C15 N4 C19 118.7(3) . . ? C15 N4 Mn1 122.9(2) . . ? C19 N4 Mn1 115.9(2) . . ? C24 N5 C20 118.0(3) . . ? C24 N5 Mn1 124.4(3) . . ? C20 N5 Mn1 117.2(2) . . ? C2 C1 C6 118.3(3) . . ? C2 C1 C7 119.9(3) . . ? C6 C1 C7 121.7(3) . . ? C1 C2 C3 121.1(3) . . ? C2 C3 C4 122.9(3) . . ? C2 C3 N2 115.4(3) . . ? C4 C3 N2 121.5(3) . . ? N1 C4 C5 122.9(3) . . ? N1 C4 C3 123.4(3) . . ? C5 C4 C3 113.7(3) . . ? C6 C5 C4 123.1(3) . . ? C6 C5 N3 115.7(3) . . ? C4 C5 N3 121.1(3) . . ? C1 C6 C5 120.1(3) . . ? O1 C7 O2 126.8(3) . . ? O1 C7 C1 118.3(3) . . ? O2 C7 C1 114.8(3) . . ? C13 C8 C9 119.9(3) . . ? C13 C8 N1 117.8(3) . . ? C9 C8 N1 122.2(3) . . ? C10 C9 C8 119.7(3) . . ? C9 C10 C11 120.6(3) . . ? C12 C11 C10 118.5(3) . . ? C12 C11 C14 120.6(3) . . ? C10 C11 C14 120.8(3) . . ? C13 C12 C11 121.2(3) . . ? C12 C13 C8 119.9(3) . . ? O7 C14 O8 124.9(3) . . ? O7 C14 C11 119.1(3) . . ? O8 C14 C11 116.0(3) . . ? N4 C15 C16 122.8(4) . . ? C17 C16 C15 118.1(4) . . ? C18 C17 C16 119.9(4) . . ? C17 C18 C19 119.2(4) . . ? N4 C19 C18 121.2(3) . . ? N4 C19 C20 116.3(3) . . ? C18 C19 C20 122.5(3) . . ? N5 C20 C21 121.5(3) . . ? N5 C20 C19 115.9(3) . . ? C21 C20 C19 122.5(3) . . ? C22 C21 C20 118.6(4) . . ? C23 C22 C21 120.0(4) . . ? C24 C23 C22 118.1(4) . . ? N5 C24 C23 123.8(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.373 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.053 data_5 _database_code_depnum_ccdc_archive 'CCDC 780235' #TrackingRef '- compound 5-sjk.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H56 Mn4 N18 O34' _chemical_formula_sum 'C86 H56 Mn4 N18 O34' _chemical_formula_weight 2105.25 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' Mn Mn 0.3368 0.7283 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 33.857(13) _cell_length_b 9.373(3) _cell_length_c 29.727(11) _cell_angle_alpha 90.00 _cell_angle_beta 112.200(7) _cell_angle_gamma 90.00 _cell_volume 8734(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6466 _cell_measurement_theta_min 2.2680 _cell_measurement_theta_max 27.4758 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4280 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7513 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 62325 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.45 _reflns_number_total 19811 _reflns_number_gt 12792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+2.7806P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19811 _refine_ls_number_parameters 1295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1959 _refine_ls_wR_factor_gt 0.1696 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.395539(16) 0.37296(5) 0.454527(16) 0.03087(13) Uani 1 1 d . . . Mn2 Mn 0.5000 0.5000 0.5000 0.02585(16) Uani 1 2 d S . . Mn3 Mn 0.250239(19) 0.88868(7) 0.003152(19) 0.04889(18) Uani 1 1 d . . . Mn4 Mn 0.0000 1.5000 -0.5000 0.02617(16) Uani 1 2 d S . . Mn5 Mn 0.104070(16) 1.63335(5) -0.454224(16) 0.03183(13) Uani 1 1 d . . . O1 O 0.38794(8) 0.4052(3) 0.53093(8) 0.0447(6) Uani 1 1 d . . . O2 O 0.45106(7) 0.4074(3) 0.52587(7) 0.0352(5) Uani 1 1 d . . . O3 O 0.40489(8) 0.1412(3) 0.88587(9) 0.0442(6) Uani 1 1 d . . . O4 O 0.47126(9) 0.1473(3) 0.94055(8) 0.0445(6) Uani 1 1 d . . . O5 O 0.19461(10) 1.0172(4) -0.00065(11) 0.0784(11) Uani 1 1 d . . . O6 O 0.43847(10) 0.0008(3) 0.70198(9) 0.0589(8) Uani 1 1 d . . . O7 O 0.58499(10) 0.2169(5) 0.88984(10) 0.0930(14) Uani 1 1 d . . . O8 O 0.58256(8) 0.1842(3) 0.81802(9) 0.0532(7) Uani 1 1 d . . . O9 O 0.31393(11) 0.9332(4) -0.00044(11) 0.0830(12) Uani 1 1 d . . . O10 O 0.45436(8) 0.6544(3) 0.45678(9) 0.0438(6) Uani 1 1 d . . . O11 O 0.27699(10) 0.9958(4) 0.07436(9) 0.0654(9) Uani 1 1 d . . . O12 O 0.23394(10) 1.1744(3) 0.07780(10) 0.0677(9) Uani 1 1 d . . . O13 O 0.36966(13) 0.7928(4) 0.24192(13) 0.0851(12) Uani 1 1 d . . . O14 O 0.41447(10) 0.9697(4) 0.26574(10) 0.0730(10) Uani 1 1 d . . . O15 O 0.32386(10) 1.3982(3) 0.28805(10) 0.0625(8) Uani 1 1 d . . . O16 O 0.26239(11) 1.4138(4) 0.23084(13) 0.0893(12) Uani 1 1 d . . . O17 O 0.22863(9) 0.9337(3) -0.07421(9) 0.0565(8) Uani 1 1 d . . . O18 O 0.27311(10) 0.7755(4) -0.08558(10) 0.0702(9) Uani 1 1 d . . . O19 O 0.04830(7) 1.3594(3) -0.45276(8) 0.0398(6) Uani 1 1 d . . . O20 O 0.11674(8) 1.4211(3) -0.43337(9) 0.0423(6) Uani 1 1 d . . . O21 O 0.17118(10) 0.5898(3) -0.29768(10) 0.0618(8) Uani 1 1 d . . . O22 O 0.23538(11) 0.5677(4) -0.24591(13) 0.0918(13) Uani 1 1 d . . . O23 O 0.09051(10) 1.0313(4) -0.26208(10) 0.0692(10) Uani 1 1 d . . . O24 O 0.13928(13) 1.1946(4) -0.23555(13) 0.0765(10) Uani 1 1 d . . . O25 O -0.04868(7) 1.4017(3) -0.47586(7) 0.0354(5) Uani 1 1 d . . . O26 O -0.10949(8) 1.4247(4) -0.46721(9) 0.0599(8) Uani 1 1 d . . . O27 O -0.02108(9) 1.1563(3) -0.05721(8) 0.0429(6) Uani 1 1 d . . . O28 O -0.08863(8) 1.1531(3) -0.10972(8) 0.0424(6) Uani 1 1 d . . . O29 O 0.08805(12) 1.2600(6) -0.11198(11) 0.126(2) Uani 1 1 d . . . O30 O 0.08662(9) 1.2031(4) -0.18090(9) 0.0629(8) Uani 1 1 d . . . O31 O -0.05865(11) 1.0167(3) -0.29715(9) 0.0624(8) Uani 1 1 d . . . O32 O -0.11278(10) 1.1022(5) -0.28460(11) 0.0817(11) Uani 1 1 d . . . O33 O 0.38619(8) 0.5903(3) 0.43862(9) 0.0417(6) Uani 1 1 d . . . O34 O 0.38376(10) 0.0892(4) 0.71236(10) 0.0736(10) Uani 1 1 d . . . N1 N 0.50721(10) 0.1993(4) 0.74515(9) 0.0405(7) Uani 1 1 d . . . H1 H 0.5347(14) 0.196(5) 0.7553(15) 0.061(13) Uiso 1 1 d . . . N2 N 0.56503(10) 0.1967(4) 0.84687(10) 0.0452(8) Uani 1 1 d . . . N3 N 0.42226(10) 0.0681(4) 0.72544(10) 0.0458(8) Uani 1 1 d . . . N4 N 0.40003(10) 0.1407(3) 0.47534(10) 0.0389(7) Uani 1 1 d . . . N5 N 0.33087(9) 0.2815(3) 0.41689(10) 0.0411(7) Uani 1 1 d . . . N6 N 0.35891(10) 1.1381(3) 0.30271(10) 0.0367(7) Uani 1 1 d . . . H6 H 0.3582(11) 1.217(4) 0.3136(13) 0.036(11) Uiso 1 1 d . . . N7 N 0.29687(11) 1.3556(3) 0.24990(12) 0.0496(8) Uani 1 1 d . . . N8 N 0.37828(13) 0.9193(4) 0.24622(12) 0.0562(10) Uani 1 1 d . . . N9 N 0.28389(10) 0.6855(4) 0.04126(11) 0.0554(9) Uani 1 1 d . . . N10 N 0.20656(11) 0.6882(4) -0.02705(12) 0.0599(10) Uani 1 1 d . . . N11 N 0.12783(12) 1.0707(4) -0.24219(11) 0.0522(9) Uani 1 1 d . . . N12 N 0.20086(11) 0.6275(4) -0.26070(11) 0.0518(9) Uani 1 1 d . . . N13 N 0.14066(9) 0.8580(3) -0.30568(10) 0.0373(7) Uani 1 1 d . . . H13 H 0.1330 0.7756 -0.3206 0.049(12) Uiso 1 1 calc R . . N14 N 0.09839(11) 1.8641(3) -0.47680(10) 0.0424(7) Uani 1 1 d . . . N15 N 0.16818(9) 1.7308(3) -0.41773(10) 0.0408(7) Uani 1 1 d . . . N16 N 0.01110(10) 1.2110(4) -0.25448(10) 0.0436(8) Uani 1 1 d . . . H16 H 0.0402(12) 1.209(4) -0.2429(12) 0.037(10) Uiso 1 1 d . . . N17 N -0.07419(11) 1.0826(4) -0.27277(10) 0.0504(8) Uani 1 1 d . . . N18 N 0.06876(11) 1.2239(4) -0.15328(10) 0.0518(9) Uani 1 1 d . . . C1 C 0.42742(10) 0.3950(3) 0.55045(11) 0.0308(7) Uani 1 1 d . . . C2 C 0.44805(11) 0.3531(3) 0.60244(10) 0.0311(7) Uani 1 1 d . . . C3 C 0.42626(11) 0.3595(4) 0.63390(12) 0.0370(8) Uani 1 1 d . . . H3 H 0.3980 0.3958 0.6224 0.044 Uiso 1 1 calc R . . C4 C 0.44523(12) 0.3137(4) 0.68181(12) 0.0409(8) Uani 1 1 d . . . H4 H 0.4308 0.3245 0.7035 0.049 Uiso 1 1 calc R . . C5 C 0.50777(11) 0.2488(4) 0.66686(12) 0.0439(9) Uani 1 1 d . . . H5 H 0.5358 0.2105 0.6780 0.053 Uiso 1 1 calc R . . C6 C 0.48557(11) 0.2517(4) 0.69771(10) 0.0354(8) Uani 1 1 d . . . C7 C 0.48954(11) 0.3010(4) 0.62020(11) 0.0367(8) Uani 1 1 d . . . H7 H 0.5055 0.3014 0.5999 0.044 Uiso 1 1 calc R . . C8 C 0.49246(11) 0.1675(4) 0.78064(11) 0.0323(7) Uani 1 1 d . . . C9 C 0.45041(11) 0.1243(4) 0.77288(10) 0.0347(8) Uani 1 1 d . . . C10 C 0.43448(11) 0.1167(4) 0.80910(11) 0.0365(8) Uani 1 1 d . . . H10 H 0.4053 0.0938 0.8012 0.044 Uiso 1 1 calc R . . C11 C 0.46086(11) 0.1423(4) 0.85713(11) 0.0330(7) Uani 1 1 d . . . C12 C 0.50354(11) 0.1676(4) 0.86735(11) 0.0353(7) Uani 1 1 d . . . H12 H 0.5226 0.1773 0.9002 0.042 Uiso 1 1 calc R . . C13 C 0.51886(11) 0.1790(4) 0.83064(11) 0.0350(7) Uani 1 1 d . . . C14 C 0.43487(18) -0.0569(5) 0.52448(15) 0.0675(14) Uani 1 1 d . . . H14 H 0.4605 -0.0994 0.5460 0.081 Uiso 1 1 calc R . . C15 C 0.43513(14) 0.0771(4) 0.50603(14) 0.0525(10) Uani 1 1 d . . . H15 H 0.4615 0.1268 0.5155 0.063 Uiso 1 1 calc R . . C16 C 0.44462(12) 0.1420(3) 0.89718(11) 0.0350(8) Uani 1 1 d . . . C17 C 0.3968(2) -0.1282(5) 0.51124(15) 0.0683(15) Uani 1 1 d . . . H17 H 0.3958 -0.2200 0.5243 0.082 Uiso 1 1 calc R . . C18 C 0.35975(17) -0.0663(4) 0.47878(15) 0.0576(11) Uani 1 1 d . . . H18 H 0.3332 -0.1151 0.4688 0.069 Uiso 1 1 calc R . . C19 C 0.36265(13) 0.0695(4) 0.46132(12) 0.0409(8) Uani 1 1 d . . . C20 C 0.32541(12) 0.1425(4) 0.42469(13) 0.0415(8) Uani 1 1 d . . . C21 C 0.28724(14) 0.0713(5) 0.39839(17) 0.0610(12) Uani 1 1 d . . . H21 H 0.2833 -0.0255 0.4051 0.073 Uiso 1 1 calc R . . C22 C 0.25599(15) 0.1437(6) 0.3631(2) 0.0769(16) Uani 1 1 d . . . H22 H 0.2299 0.0970 0.3449 0.092 Uiso 1 1 calc R . . C23 C 0.26166(14) 0.2842(6) 0.35324(18) 0.0715(14) Uani 1 1 d . . . H23 H 0.2403 0.3344 0.3278 0.086 Uiso 1 1 calc R . . C24 C 0.29949(13) 0.3497(5) 0.38157(15) 0.0541(10) Uani 1 1 d . . . H24 H 0.3034 0.4473 0.3757 0.065 Uiso 1 1 calc R . . C25 C 0.41456(11) 0.6694(4) 0.43415(11) 0.0338(7) Uani 1 1 d . . . C26 C 0.40013(11) 0.7914(4) 0.39877(11) 0.0327(7) Uani 1 1 d . . . C27 C 0.42771(11) 0.9013(4) 0.40018(11) 0.0346(7) Uani 1 1 d . . . H27 H 0.4561 0.8995 0.4235 0.041 Uiso 1 1 calc R . . C28 C 0.41436(11) 1.0138(4) 0.36796(11) 0.0360(8) Uani 1 1 d . . . H28 H 0.4336 1.0889 0.3691 0.043 Uiso 1 1 calc R . . C29 C 0.37294(11) 1.0171(4) 0.33397(11) 0.0328(7) Uani 1 1 d . . . C30 C 0.34516(11) 0.9077(4) 0.33206(12) 0.0417(8) Uani 1 1 d . . . H30 H 0.3169 0.9097 0.3085 0.050 Uiso 1 1 calc R . . C31 C 0.35827(11) 0.7951(4) 0.36431(12) 0.0405(8) Uani 1 1 d . . . H31 H 0.3389 0.7204 0.3631 0.049 Uiso 1 1 calc R . . C32 C 0.33721(11) 1.1312(4) 0.25337(11) 0.0337(7) Uani 1 1 d . . . C33 C 0.30637(11) 1.2323(4) 0.22620(12) 0.0392(8) Uani 1 1 d . . . C34 C 0.28327(12) 1.2192(4) 0.17668(13) 0.0456(9) Uani 1 1 d . . . H34 H 0.2619 1.2878 0.1606 0.055 Uiso 1 1 calc R . . C35 C 0.29062(12) 1.1094(4) 0.15044(12) 0.0444(9) Uani 1 1 d . . . C36 C 0.32151(13) 1.0092(4) 0.17510(12) 0.0453(9) Uani 1 1 d . . . H36 H 0.3274 0.9321 0.1578 0.054 Uiso 1 1 calc R . . C37 C 0.34370(12) 1.0215(4) 0.22465(12) 0.0403(8) Uani 1 1 d . . . C38 C 0.26508(14) 1.0937(5) 0.09628(13) 0.0516(11) Uani 1 1 d . . . C39 C 0.32092(14) 0.6885(6) 0.07975(15) 0.0682(14) Uani 1 1 d . . . H39 H 0.3329 0.7789 0.0919 0.082 Uiso 1 1 calc R . . C40 C 0.34252(17) 0.5686(7) 0.1026(2) 0.092(2) Uani 1 1 d . . . H40 H 0.3687 0.5758 0.1298 0.110 Uiso 1 1 calc R . . C41 C 0.3254(2) 0.4401(8) 0.0853(3) 0.111(2) Uani 1 1 d . . . H41 H 0.3393 0.3553 0.1009 0.133 Uiso 1 1 calc R . . C42 C 0.28795(19) 0.4317(6) 0.0453(2) 0.0931(19) Uani 1 1 d . . . H42 H 0.2763 0.3416 0.0323 0.112 Uiso 1 1 calc R . . C43 C 0.26743(14) 0.5572(5) 0.02417(16) 0.0581(11) Uani 1 1 d . . . C44 C 0.22567(14) 0.5596(5) -0.01799(16) 0.0578(11) Uani 1 1 d . . . C45 C 0.20823(18) 0.4391(6) -0.0454(2) 0.0800(15) Uani 1 1 d . . . H45 H 0.2225 0.3498 -0.0380 0.096 Uiso 1 1 calc R . . C46 C 0.1695(2) 0.4527(8) -0.0838(2) 0.094(2) Uani 1 1 d . . . H46 H 0.1574 0.3732 -0.1042 0.113 Uiso 1 1 calc R . . C47 C 0.14854(18) 0.5824(8) -0.09247(18) 0.0848(18) Uani 1 1 d . . . H47 H 0.1211 0.5926 -0.1175 0.102 Uiso 1 1 calc R . . C48 C 0.16873(15) 0.6965(6) -0.06364(15) 0.0734(14) Uani 1 1 d . . . H48 H 0.1548 0.7865 -0.0703 0.088 Uiso 1 1 calc R . . C49 C 0.24119(13) 0.8545(4) -0.10018(13) 0.0474(9) Uani 1 1 d . . . C50 C 0.21452(12) 0.8551(4) -0.15427(12) 0.0409(8) Uani 1 1 d . . . C51 C 0.21974(12) 0.7498(4) -0.18384(12) 0.0438(9) Uani 1 1 d . . . H51 H 0.2407 0.6779 -0.1704 0.053 Uiso 1 1 calc R . . C52 C 0.19468(11) 0.7478(4) -0.23311(12) 0.0387(8) Uani 1 1 d . . . C53 C 0.16417(10) 0.8551(4) -0.25668(11) 0.0336(7) Uani 1 1 d . . . C54 C 0.16065(11) 0.9586(4) -0.22417(12) 0.0379(8) Uani 1 1 d . . . C55 C 0.18396(12) 0.9590(4) -0.17514(12) 0.0414(8) Uani 1 1 d . . . H55 H 0.1791 1.0311 -0.1553 0.050 Uiso 1 1 calc R . . C56 C 0.12758(11) 0.9837(4) -0.33435(11) 0.0322(7) Uani 1 1 d . . . C57 C 0.08602(11) 0.9908(4) -0.36861(11) 0.0341(7) Uani 1 1 d . . . H57 H 0.0664 0.9160 -0.3711 0.041 Uiso 1 1 calc R . . C58 C 0.07372(11) 1.1070(4) -0.39883(11) 0.0334(7) Uani 1 1 d . . . H58 H 0.0455 1.1110 -0.4225 0.040 Uiso 1 1 calc R . . C59 C 0.10160(10) 1.2191(4) -0.39571(10) 0.0313(7) Uani 1 1 d . . . C60 C 0.14285(11) 1.2110(4) -0.36038(12) 0.0389(8) Uani 1 1 d . . . H60 H 0.1623 1.2869 -0.3573 0.047 Uiso 1 1 calc R . . C61 C 0.15578(11) 1.0944(4) -0.32987(12) 0.0403(8) Uani 1 1 d . . . H61 H 0.1839 1.0903 -0.3059 0.048 Uiso 1 1 calc R . . C62 C 0.08778(11) 1.3426(4) -0.42982(11) 0.0331(7) Uani 1 1 d . . . C63 C -0.07034(11) 1.4040(4) -0.44904(11) 0.0344(7) Uani 1 1 d . . . C64 C -0.04885(10) 1.3633(3) -0.39679(11) 0.0313(7) Uani 1 1 d . . . C65 C -0.00829(11) 1.3054(4) -0.38057(11) 0.0396(8) Uani 1 1 d . . . H65 H 0.0068 1.3015 -0.4018 0.047 Uiso 1 1 calc R . . C66 C 0.01052(11) 1.2529(4) -0.33359(11) 0.0418(9) Uani 1 1 d . . . H66 H 0.0379 1.2098 -0.3232 0.050 Uiso 1 1 calc R . . C67 C -0.01074(11) 1.2631(4) -0.30157(11) 0.0365(8) Uani 1 1 d . . . C68 C -0.05003(11) 1.3315(4) -0.31664(11) 0.0372(8) Uani 1 1 d . . . H68 H -0.0635 1.3468 -0.2943 0.045 Uiso 1 1 calc R . . C69 C -0.06958(11) 1.3773(4) -0.36435(12) 0.0366(8) Uani 1 1 d . . . H69 H -0.0973 1.4185 -0.3750 0.044 Uiso 1 1 calc R . . C70 C -0.00348(11) 1.1846(4) -0.21842(11) 0.0352(7) Uani 1 1 d . . . C71 C 0.02306(11) 1.1999(4) -0.16885(11) 0.0358(8) Uani 1 1 d . . . C72 C 0.00836(11) 1.1886(4) -0.13152(11) 0.0348(7) Uani 1 1 d . . . H72 H 0.0277 1.2013 -0.0989 0.042 Uiso 1 1 calc R . . C73 C -0.03384(11) 1.1592(4) -0.14091(11) 0.0333(7) Uani 1 1 d . . . C74 C -0.06066(12) 1.1310(4) -0.18848(11) 0.0375(8) Uani 1 1 d . . . H74 H -0.0896 1.1056 -0.1956 0.045 Uiso 1 1 calc R . . C75 C -0.04548(12) 1.1396(4) -0.22549(11) 0.0379(8) Uani 1 1 d . . . C76 C -0.04925(12) 1.1540(4) -0.09980(11) 0.0345(8) Uani 1 1 d . . . C77 C 0.06231(15) 1.9259(5) -0.50664(14) 0.0583(11) Uani 1 1 d . . . H77 H 0.0366 1.8720 -0.5168 0.070 Uiso 1 1 calc R . . C78 C 0.0607(2) 2.0640(5) -0.52327(15) 0.0731(15) Uani 1 1 d . . . H78 H 0.0343 2.1046 -0.5439 0.088 Uiso 1 1 calc R . . C79 C 0.0972(2) 2.1410(5) -0.50983(16) 0.0694(15) Uani 1 1 d . . . H79 H 0.0968 2.2351 -0.5218 0.083 Uiso 1 1 calc R . . C80 C 0.13514(17) 2.0819(4) -0.47850(16) 0.0602(12) Uani 1 1 d . . . H80 H 0.1609 2.1349 -0.4685 0.072 Uiso 1 1 calc R . . C81 C 0.13460(13) 1.9420(4) -0.46192(13) 0.0443(9) Uani 1 1 d . . . C82 C 0.17257(12) 1.8702(4) -0.42625(13) 0.0427(9) Uani 1 1 d . . . C83 C 0.21026(15) 1.9434(5) -0.40056(17) 0.0625(12) Uani 1 1 d . . . H83 H 0.2131 2.0411 -0.4072 0.075 Uiso 1 1 calc R . . C84 C 0.24299(15) 1.8730(6) -0.3658(2) 0.0748(16) Uani 1 1 d . . . H84 H 0.2690 1.9211 -0.3484 0.090 Uiso 1 1 calc R . . C85 C 0.23804(14) 1.7332(6) -0.35618(19) 0.0726(14) Uani 1 1 d . . . H85 H 0.2600 1.6839 -0.3312 0.087 Uiso 1 1 calc R . . C86 C 0.20019(13) 1.6640(5) -0.38370(15) 0.0537(10) Uani 1 1 d . . . H86 H 0.1972 1.5657 -0.3779 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 0.0357(3) 0.0317(3) 0.0240(2) 0.0025(2) 0.0098(2) -0.0012(2) Mn2 0.0262(3) 0.0293(4) 0.0191(3) 0.0018(3) 0.0053(3) 0.0019(3) Mn3 0.0434(3) 0.0656(4) 0.0303(3) 0.0030(3) 0.0055(2) -0.0106(3) Mn4 0.0254(3) 0.0324(4) 0.0182(3) 0.0018(3) 0.0055(3) 0.0014(3) Mn5 0.0352(3) 0.0337(3) 0.0249(2) 0.0036(2) 0.0094(2) -0.0008(2) O1 0.0347(13) 0.0669(18) 0.0303(12) 0.0106(12) 0.0098(10) 0.0114(12) O2 0.0386(13) 0.0423(14) 0.0261(10) 0.0057(10) 0.0137(10) -0.0018(10) O3 0.0496(16) 0.0505(16) 0.0420(13) 0.0051(12) 0.0283(12) 0.0054(12) O4 0.0675(18) 0.0425(15) 0.0229(11) 0.0042(11) 0.0163(12) 0.0078(13) O5 0.0437(18) 0.124(3) 0.0558(18) -0.028(2) 0.0057(14) -0.0067(18) O6 0.069(2) 0.068(2) 0.0407(14) -0.0171(14) 0.0219(14) -0.0063(15) O7 0.0528(19) 0.189(4) 0.0310(14) -0.027(2) 0.0083(14) -0.034(2) O8 0.0390(15) 0.088(2) 0.0374(13) 0.0004(14) 0.0194(12) 0.0025(14) O9 0.066(2) 0.132(3) 0.0509(17) -0.011(2) 0.0214(16) -0.052(2) O10 0.0453(15) 0.0409(15) 0.0419(13) 0.0144(12) 0.0126(12) 0.0129(11) O11 0.0545(19) 0.095(3) 0.0350(14) -0.0088(16) 0.0038(13) -0.0083(17) O12 0.064(2) 0.068(2) 0.0431(15) 0.0073(15) -0.0127(14) -0.0016(16) O13 0.132(3) 0.058(2) 0.088(2) 0.021(2) 0.067(2) 0.038(2) O14 0.054(2) 0.118(3) 0.0400(15) -0.0003(18) 0.0101(15) 0.035(2) O15 0.067(2) 0.0551(19) 0.0471(16) -0.0048(15) 0.0008(15) 0.0153(15) O16 0.061(2) 0.093(3) 0.084(2) -0.004(2) -0.0069(18) 0.0426(19) O17 0.0569(18) 0.075(2) 0.0326(13) 0.0028(14) 0.0110(13) 0.0043(15) O18 0.064(2) 0.081(2) 0.0409(15) 0.0014(16) -0.0078(14) 0.0224(17) O19 0.0368(13) 0.0447(15) 0.0338(12) 0.0150(11) 0.0087(10) 0.0133(11) O20 0.0431(14) 0.0390(14) 0.0456(14) 0.0115(12) 0.0178(12) 0.0071(11) O21 0.0645(19) 0.0546(19) 0.0482(16) -0.0107(15) 0.0007(14) 0.0138(15) O22 0.074(2) 0.094(3) 0.079(2) -0.022(2) -0.0038(19) 0.050(2) O23 0.054(2) 0.109(3) 0.0391(15) 0.0074(17) 0.0112(14) 0.0386(18) O24 0.116(3) 0.050(2) 0.081(2) 0.0133(18) 0.057(2) 0.026(2) O25 0.0367(13) 0.0455(14) 0.0251(10) 0.0053(10) 0.0130(10) -0.0015(10) O26 0.0365(15) 0.103(3) 0.0389(14) 0.0221(16) 0.0128(12) 0.0148(15) O27 0.0600(16) 0.0445(15) 0.0234(11) 0.0042(11) 0.0148(11) -0.0017(12) O28 0.0473(16) 0.0490(16) 0.0368(13) 0.0033(12) 0.0226(12) 0.0038(12) O29 0.069(2) 0.267(6) 0.0438(17) -0.055(3) 0.0252(17) -0.075(3) O30 0.0466(17) 0.104(3) 0.0410(14) 0.0023(16) 0.0201(13) 0.0067(16) O31 0.086(2) 0.065(2) 0.0371(14) -0.0155(14) 0.0236(15) -0.0035(17) O32 0.0465(19) 0.140(4) 0.0451(16) -0.015(2) 0.0022(14) -0.006(2) O33 0.0489(15) 0.0333(13) 0.0436(13) 0.0114(12) 0.0183(12) 0.0060(11) O34 0.0433(18) 0.119(3) 0.0446(16) -0.0168(18) 0.0008(13) -0.0024(18) N1 0.0381(17) 0.062(2) 0.0208(13) 0.0092(14) 0.0104(12) 0.0059(15) N2 0.0421(18) 0.062(2) 0.0289(14) -0.0014(15) 0.0111(13) -0.0038(15) N3 0.0476(19) 0.060(2) 0.0260(14) -0.0015(15) 0.0099(14) -0.0014(16) N4 0.0492(18) 0.0328(16) 0.0321(14) 0.0012(13) 0.0126(13) -0.0002(13) N5 0.0379(16) 0.0462(19) 0.0413(16) -0.0025(15) 0.0174(13) -0.0020(14) N6 0.0454(18) 0.0317(17) 0.0268(14) 0.0066(13) 0.0065(13) 0.0085(13) N7 0.0462(19) 0.0426(19) 0.0515(19) 0.0102(16) 0.0088(16) 0.0139(15) N8 0.073(3) 0.066(3) 0.0349(17) 0.0078(18) 0.0265(18) 0.029(2) N9 0.0414(18) 0.076(3) 0.0413(17) 0.0133(18) 0.0072(14) -0.0076(17) N10 0.046(2) 0.074(3) 0.0449(18) 0.0026(19) 0.0002(15) -0.0107(18) N11 0.062(2) 0.060(2) 0.0367(17) 0.0115(17) 0.0214(17) 0.0282(19) N12 0.057(2) 0.046(2) 0.0414(17) 0.0064(16) 0.0055(16) 0.0198(16) N13 0.0435(17) 0.0330(17) 0.0275(13) 0.0040(13) 0.0046(12) 0.0068(13) N14 0.058(2) 0.0355(17) 0.0342(15) 0.0013(13) 0.0179(15) 0.0013(14) N15 0.0374(16) 0.0440(18) 0.0427(16) -0.0045(15) 0.0173(13) 0.0000(13) N16 0.0399(18) 0.069(2) 0.0228(13) 0.0072(14) 0.0131(13) 0.0112(16) N17 0.059(2) 0.060(2) 0.0271(15) 0.0025(15) 0.0105(15) -0.0025(17) N18 0.0472(19) 0.081(3) 0.0274(14) -0.0021(16) 0.0138(14) -0.0094(17) C1 0.0337(17) 0.0318(18) 0.0272(15) 0.0033(14) 0.0118(13) 0.0031(14) C2 0.0372(18) 0.0344(18) 0.0215(14) 0.0005(13) 0.0108(13) 0.0024(14) C3 0.0379(19) 0.043(2) 0.0308(16) 0.0065(15) 0.0135(14) 0.0116(15) C4 0.046(2) 0.053(2) 0.0276(16) 0.0072(16) 0.0191(15) 0.0098(17) C5 0.0358(19) 0.068(3) 0.0299(16) 0.0083(18) 0.0150(15) 0.0126(18) C6 0.0421(19) 0.044(2) 0.0190(14) 0.0021(14) 0.0105(13) 0.0050(15) C7 0.0365(18) 0.049(2) 0.0280(15) 0.0050(16) 0.0162(14) 0.0079(16) C8 0.0369(18) 0.0361(18) 0.0240(14) 0.0023(14) 0.0117(13) 0.0041(14) C9 0.0418(19) 0.041(2) 0.0183(13) 0.0008(14) 0.0076(13) 0.0032(15) C10 0.0351(18) 0.042(2) 0.0313(16) 0.0038(15) 0.0106(14) 0.0050(15) C11 0.0400(19) 0.0364(19) 0.0242(14) 0.0066(14) 0.0138(14) 0.0082(14) C12 0.0420(19) 0.0387(19) 0.0236(15) 0.0000(14) 0.0106(14) 0.0038(15) C13 0.0342(18) 0.044(2) 0.0246(15) -0.0002(15) 0.0089(13) 0.0015(15) C14 0.100(4) 0.042(3) 0.039(2) 0.008(2) 0.002(2) 0.017(3) C15 0.063(3) 0.041(2) 0.040(2) 0.0008(18) 0.0048(19) 0.0096(19) C16 0.052(2) 0.0275(18) 0.0288(16) 0.0048(14) 0.0192(16) 0.0063(15) C17 0.127(5) 0.037(2) 0.040(2) 0.007(2) 0.030(3) 0.002(3) C18 0.089(3) 0.042(2) 0.051(2) -0.002(2) 0.037(2) -0.008(2) C19 0.062(2) 0.0320(19) 0.0352(17) -0.0020(16) 0.0260(17) -0.0061(17) C20 0.047(2) 0.039(2) 0.0439(19) -0.0058(17) 0.0242(17) -0.0053(16) C21 0.052(3) 0.055(3) 0.073(3) -0.020(2) 0.020(2) -0.013(2) C22 0.043(3) 0.072(4) 0.100(4) -0.030(3) 0.009(3) -0.007(2) C23 0.045(3) 0.079(4) 0.070(3) -0.018(3) -0.001(2) 0.014(2) C24 0.046(2) 0.056(3) 0.054(2) 0.000(2) 0.0111(19) 0.0086(19) C25 0.0397(19) 0.0328(18) 0.0290(15) 0.0039(14) 0.0130(14) 0.0095(15) C26 0.0374(18) 0.0330(18) 0.0261(15) 0.0036(14) 0.0103(13) 0.0081(14) C27 0.0350(18) 0.0360(19) 0.0258(15) 0.0043(14) 0.0037(13) 0.0047(14) C28 0.0357(19) 0.0355(19) 0.0297(16) -0.0001(15) 0.0042(14) -0.0019(14) C29 0.0376(19) 0.0359(19) 0.0228(14) 0.0074(14) 0.0091(14) 0.0099(14) C30 0.0304(18) 0.051(2) 0.0362(18) 0.0114(17) 0.0041(14) 0.0040(16) C31 0.0347(19) 0.043(2) 0.0408(18) 0.0145(17) 0.0105(15) 0.0011(15) C32 0.0330(17) 0.0350(19) 0.0289(15) 0.0065(14) 0.0068(13) 0.0012(14) C33 0.0338(18) 0.041(2) 0.0362(17) 0.0088(16) 0.0063(15) 0.0024(15) C34 0.039(2) 0.043(2) 0.0407(19) 0.0114(18) -0.0001(16) 0.0001(17) C35 0.040(2) 0.053(2) 0.0311(17) 0.0124(18) 0.0034(15) -0.0055(17) C36 0.049(2) 0.053(2) 0.0314(17) -0.0020(17) 0.0121(17) -0.0017(18) C37 0.042(2) 0.045(2) 0.0300(16) 0.0077(16) 0.0092(15) 0.0097(16) C38 0.055(3) 0.056(3) 0.0310(18) 0.0053(19) 0.0019(18) -0.018(2) C39 0.048(3) 0.092(4) 0.050(2) 0.021(3) 0.003(2) -0.009(2) C40 0.055(3) 0.112(5) 0.082(4) 0.056(4) -0.003(3) -0.008(3) C41 0.077(4) 0.097(5) 0.131(6) 0.070(5) 0.009(4) 0.005(4) C42 0.083(4) 0.068(4) 0.113(5) 0.030(4) 0.021(4) -0.015(3) C43 0.055(3) 0.061(3) 0.059(2) 0.016(2) 0.021(2) -0.008(2) C44 0.049(2) 0.069(3) 0.056(2) 0.001(2) 0.022(2) -0.016(2) C45 0.075(4) 0.076(4) 0.092(4) -0.010(3) 0.034(3) -0.025(3) C46 0.074(4) 0.116(6) 0.090(4) -0.040(4) 0.027(3) -0.046(4) C47 0.060(3) 0.130(6) 0.052(3) -0.016(3) 0.008(2) -0.029(3) C48 0.051(3) 0.095(4) 0.052(2) 0.003(3) -0.005(2) -0.013(3) C49 0.049(2) 0.052(2) 0.0328(18) 0.0100(18) 0.0066(17) 0.0011(19) C50 0.040(2) 0.045(2) 0.0312(17) 0.0116(16) 0.0057(15) 0.0018(16) C51 0.041(2) 0.045(2) 0.0346(17) 0.0142(17) 0.0018(15) 0.0069(16) C52 0.041(2) 0.035(2) 0.0348(17) 0.0067(16) 0.0085(15) 0.0073(15) C53 0.0296(17) 0.040(2) 0.0267(15) 0.0082(14) 0.0060(13) 0.0020(14) C54 0.0360(19) 0.042(2) 0.0329(17) 0.0141(16) 0.0095(15) 0.0098(15) C55 0.047(2) 0.047(2) 0.0305(16) 0.0033(17) 0.0149(16) 0.0008(17) C56 0.0378(19) 0.0326(18) 0.0224(14) 0.0058(13) 0.0072(14) 0.0096(14) C57 0.0371(19) 0.0320(19) 0.0289(16) 0.0013(14) 0.0074(14) 0.0016(14) C58 0.0311(17) 0.0378(19) 0.0256(14) 0.0010(14) 0.0043(13) 0.0058(14) C59 0.0331(17) 0.0364(18) 0.0221(14) 0.0025(14) 0.0078(13) 0.0053(14) C60 0.0359(18) 0.041(2) 0.0328(16) 0.0098(16) 0.0051(14) 0.0006(15) C61 0.0320(18) 0.047(2) 0.0343(17) 0.0098(17) 0.0042(14) 0.0028(16) C62 0.0401(19) 0.0346(18) 0.0259(15) 0.0044(14) 0.0140(14) 0.0073(15) C63 0.0330(18) 0.043(2) 0.0275(15) 0.0065(15) 0.0115(14) 0.0021(15) C64 0.0340(17) 0.0354(19) 0.0250(15) 0.0040(14) 0.0117(13) 0.0005(14) C65 0.0381(19) 0.055(2) 0.0287(15) 0.0098(16) 0.0166(14) 0.0109(17) C66 0.0359(19) 0.061(3) 0.0294(16) 0.0078(17) 0.0138(14) 0.0126(17) C67 0.0410(19) 0.047(2) 0.0224(14) 0.0034(15) 0.0126(14) 0.0063(16) C68 0.043(2) 0.047(2) 0.0277(15) 0.0001(15) 0.0200(15) 0.0096(16) C69 0.0388(19) 0.040(2) 0.0330(16) 0.0057(15) 0.0163(15) 0.0085(15) C70 0.045(2) 0.0367(19) 0.0245(15) 0.0044(15) 0.0132(14) 0.0089(15) C71 0.0362(18) 0.046(2) 0.0249(15) 0.0002(15) 0.0110(14) 0.0029(15) C72 0.0419(19) 0.0375(19) 0.0222(14) -0.0020(14) 0.0090(14) 0.0037(15) C73 0.0429(19) 0.0348(18) 0.0227(14) 0.0058(14) 0.0131(14) 0.0073(15) C74 0.0392(19) 0.043(2) 0.0284(16) 0.0036(15) 0.0106(14) 0.0046(15) C75 0.045(2) 0.044(2) 0.0210(14) 0.0000(15) 0.0088(14) 0.0035(16) C76 0.049(2) 0.0317(18) 0.0253(15) 0.0018(14) 0.0165(15) 0.0045(15) C77 0.074(3) 0.047(3) 0.039(2) 0.0048(19) 0.003(2) 0.009(2) C78 0.113(4) 0.051(3) 0.041(2) 0.011(2) 0.013(3) 0.019(3) C79 0.131(5) 0.039(3) 0.044(2) 0.009(2) 0.041(3) 0.007(3) C80 0.101(4) 0.039(2) 0.055(2) -0.002(2) 0.045(3) -0.012(2) C81 0.067(3) 0.037(2) 0.0390(18) -0.0061(17) 0.0309(19) -0.0094(18) C82 0.047(2) 0.043(2) 0.046(2) -0.0146(18) 0.0264(18) -0.0102(17) C83 0.058(3) 0.059(3) 0.077(3) -0.027(3) 0.033(2) -0.017(2) C84 0.044(3) 0.084(4) 0.091(4) -0.047(3) 0.019(3) -0.011(2) C85 0.044(3) 0.083(4) 0.081(3) -0.025(3) 0.013(2) 0.011(2) C86 0.041(2) 0.060(3) 0.056(2) -0.002(2) 0.0133(19) 0.0081(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O33 2.088(2) . ? Mn1 O3 2.185(2) 4_565 ? Mn1 N5 2.220(3) . ? Mn1 N4 2.253(3) . ? Mn1 O2 2.263(2) . ? Mn1 O1 2.399(2) . ? Mn2 O10 2.152(2) . ? Mn2 O10 2.152(2) 3_666 ? Mn2 O4 2.163(2) 2_656 ? Mn2 O4 2.163(2) 4_565 ? Mn2 O2 2.248(2) . ? Mn2 O2 2.248(2) 3_666 ? Mn3 O17 2.175(3) . ? Mn3 O5 2.202(4) . ? Mn3 O11 2.205(3) . ? Mn3 O9 2.238(3) . ? Mn3 N9 2.288(4) . ? Mn3 N10 2.350(4) . ? Mn4 O27 2.152(2) 2_554 ? Mn4 O27 2.152(2) 4_585 ? Mn4 O19 2.156(2) . ? Mn4 O19 2.156(2) 3_584 ? Mn4 O25 2.230(2) . ? Mn4 O25 2.230(2) 3_584 ? Mn5 O20 2.080(3) . ? Mn5 O28 2.161(2) 2_554 ? Mn5 N15 2.223(3) . ? Mn5 O25 2.236(2) 3_584 ? Mn5 N14 2.251(3) . ? Mn5 O26 2.471(3) 3_584 ? O1 C1 1.244(4) . ? O2 C1 1.277(4) . ? O3 C16 1.257(4) . ? O3 Mn1 2.184(2) 4_566 ? O4 C16 1.265(4) . ? O4 Mn2 2.163(2) 2_646 ? O6 N3 1.214(4) . ? O7 N2 1.213(4) . ? O8 N2 1.219(4) . ? O10 C25 1.266(4) . ? O11 C38 1.276(5) . ? O12 C38 1.244(5) . ? O13 N8 1.217(5) . ? O14 N8 1.234(5) . ? O15 N7 1.224(4) . ? O16 N7 1.217(4) . ? O17 C49 1.255(5) . ? O18 C49 1.246(5) . ? O19 C62 1.260(4) . ? O20 C62 1.262(4) . ? O21 N12 1.228(4) . ? O22 N12 1.219(4) . ? O23 N11 1.232(5) . ? O24 N11 1.217(5) . ? O25 C63 1.271(4) . ? O25 Mn5 2.236(2) 3_584 ? O26 C63 1.243(4) . ? O26 Mn5 2.471(3) 3_584 ? O27 C76 1.265(4) . ? O27 Mn4 2.152(2) 2_544 ? O28 C76 1.252(4) . ? O28 Mn5 2.161(2) 2_544 ? O29 N18 1.201(4) . ? O30 N18 1.206(4) . ? O31 N17 1.213(4) . ? O32 N17 1.232(5) . ? O33 C25 1.260(4) . ? O34 N3 1.227(4) . ? N1 C8 1.360(4) . ? N1 C6 1.410(4) . ? N1 H1 0.86(4) . ? N2 C13 1.461(4) . ? N3 C9 1.469(4) . ? N4 C15 1.334(5) . ? N4 C19 1.350(5) . ? N5 C24 1.340(5) . ? N5 C20 1.349(5) . ? N6 C32 1.372(4) . ? N6 C29 1.429(4) . ? N6 H6 0.81(4) . ? N7 C33 1.451(5) . ? N8 C37 1.460(5) . ? N9 C39 1.341(5) . ? N9 C43 1.342(6) . ? N10 C48 1.333(5) . ? N10 C44 1.346(6) . ? N11 C54 1.475(5) . ? N12 C52 1.456(5) . ? N13 C53 1.371(4) . ? N13 C56 1.423(4) . ? N13 H13 0.8800 . ? N14 C77 1.340(5) . ? N14 C81 1.350(5) . ? N15 C86 1.327(5) . ? N15 C82 1.350(5) . ? N16 C70 1.362(4) . ? N16 C67 1.401(4) . ? N16 H16 0.91(4) . ? N17 C75 1.474(4) . ? N18 C71 1.455(5) . ? C1 C2 1.489(4) . ? C2 C7 1.389(5) . ? C2 C3 1.394(4) . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 C6 1.392(5) . ? C4 H4 0.9500 . ? C5 C7 1.377(4) . ? C5 C6 1.389(4) . ? C5 H5 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.413(5) . ? C8 C13 1.420(4) . ? C9 C10 1.376(5) . ? C10 C11 1.389(4) . ? C10 H10 0.9500 . ? C11 C12 1.380(5) . ? C11 C16 1.488(4) . ? C12 C13 1.378(4) . ? C12 H12 0.9500 . ? C14 C17 1.370(7) . ? C14 C15 1.372(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C17 C18 1.389(7) . ? C17 H17 0.9500 . ? C18 C19 1.392(5) . ? C18 H18 0.9500 . ? C19 C20 1.485(5) . ? C20 C21 1.401(5) . ? C21 C22 1.358(7) . ? C21 H21 0.9500 . ? C22 C23 1.378(7) . ? C22 H22 0.9500 . ? C23 C24 1.383(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.505(4) . ? C26 C27 1.381(5) . ? C26 C31 1.401(5) . ? C27 C28 1.381(5) . ? C27 H27 0.9500 . ? C28 C29 1.385(4) . ? C28 H28 0.9500 . ? C29 C30 1.378(5) . ? C30 C31 1.381(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.406(5) . ? C32 C33 1.416(5) . ? C33 C34 1.387(5) . ? C34 C35 1.370(6) . ? C34 H34 0.9500 . ? C35 C36 1.390(5) . ? C35 C38 1.520(5) . ? C36 C37 1.383(5) . ? C36 H36 0.9500 . ? C39 C40 1.373(7) . ? C39 H39 0.9500 . ? C40 C41 1.350(9) . ? C40 H40 0.9500 . ? C41 C42 1.375(8) . ? C41 H41 0.9500 . ? C42 C43 1.389(7) . ? C42 H42 0.9500 . ? C43 C44 1.494(6) . ? C44 C45 1.388(7) . ? C45 C46 1.380(8) . ? C45 H45 0.9500 . ? C46 C47 1.383(9) . ? C46 H46 0.9500 . ? C47 C48 1.379(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.518(5) . ? C50 C51 1.377(5) . ? C50 C55 1.386(5) . ? C51 C52 1.388(5) . ? C51 H51 0.9500 . ? C52 C53 1.422(5) . ? C53 C54 1.406(5) . ? C54 C55 1.370(5) . ? C55 H55 0.9500 . ? C56 C61 1.382(5) . ? C56 C57 1.392(4) . ? C57 C58 1.372(4) . ? C57 H57 0.9500 . ? C58 C59 1.392(5) . ? C58 H58 0.9500 . ? C59 C60 1.397(4) . ? C59 C62 1.493(4) . ? C60 C61 1.382(5) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C63 C64 1.494(4) . ? C64 C65 1.383(5) . ? C64 C69 1.397(4) . ? C65 C66 1.388(4) . ? C65 H65 0.9500 . ? C66 C67 1.397(4) . ? C66 H66 0.9500 . ? C67 C68 1.389(5) . ? C68 C69 1.387(4) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C71 1.414(4) . ? C70 C75 1.420(5) . ? C71 C72 1.381(4) . ? C72 C73 1.376(5) . ? C72 H72 0.9500 . ? C73 C74 1.387(4) . ? C73 C76 1.500(4) . ? C74 C75 1.381(5) . ? C74 H74 0.9500 . ? C77 C78 1.380(6) . ? C77 H77 0.9500 . ? C78 C79 1.355(8) . ? C78 H78 0.9500 . ? C79 C80 1.386(7) . ? C79 H79 0.9500 . ? C80 C81 1.403(5) . ? C80 H80 0.9500 . ? C81 C82 1.483(6) . ? C82 C83 1.395(5) . ? C83 C84 1.366(7) . ? C83 H83 0.9500 . ? C84 C85 1.365(8) . ? C84 H84 0.9500 . ? C85 C86 1.393(6) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? 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 O33 Mn1 O3 84.88(10) . 4_565 ? O33 Mn1 N5 103.07(11) . . ? O3 Mn1 N5 88.23(10) 4_565 . ? O33 Mn1 N4 173.58(11) . . ? O3 Mn1 N4 100.33(10) 4_565 . ? N5 Mn1 N4 73.55(12) . . ? O33 Mn1 O2 94.25(10) . . ? O3 Mn1 O2 121.46(9) 4_565 . ? N5 Mn1 O2 147.04(10) . . ? N4 Mn1 O2 86.25(10) . . ? O33 Mn1 O1 91.74(10) . . ? O3 Mn1 O1 175.76(10) 4_565 . ? N5 Mn1 O1 95.03(10) . . ? N4 Mn1 O1 83.22(10) . . ? O2 Mn1 O1 56.17(8) . . ? O10 Mn2 O10 180.00(13) . 3_666 ? O10 Mn2 O4 93.36(10) . 2_656 ? O10 Mn2 O4 86.64(10) 3_666 2_656 ? O10 Mn2 O4 86.64(10) . 4_565 ? O10 Mn2 O4 93.36(10) 3_666 4_565 ? O4 Mn2 O4 180.000(1) 2_656 4_565 ? O10 Mn2 O2 90.45(9) . . ? O10 Mn2 O2 89.55(9) 3_666 . ? O4 Mn2 O2 97.41(9) 2_656 . ? O4 Mn2 O2 82.59(9) 4_565 . ? O10 Mn2 O2 89.55(9) . 3_666 ? O10 Mn2 O2 90.45(9) 3_666 3_666 ? O4 Mn2 O2 82.59(9) 2_656 3_666 ? O4 Mn2 O2 97.41(9) 4_565 3_666 ? O2 Mn2 O2 180.00(9) . 3_666 ? O17 Mn3 O5 84.26(12) . . ? O17 Mn3 O11 141.14(13) . . ? O5 Mn3 O11 80.40(12) . . ? O17 Mn3 O9 81.87(11) . . ? O5 Mn3 O9 135.75(15) . . ? O11 Mn3 O9 84.68(12) . . ? O17 Mn3 N9 126.21(12) . . ? O5 Mn3 N9 137.48(13) . . ? O11 Mn3 N9 87.52(13) . . ? O9 Mn3 N9 82.55(14) . . ? O17 Mn3 N10 80.76(12) . . ? O5 Mn3 N10 90.87(14) . . ? O11 Mn3 N10 134.60(12) . . ? O9 Mn3 N10 127.55(14) . . ? N9 Mn3 N10 69.34(13) . . ? O27 Mn4 O27 180.00(15) 2_554 4_585 ? O27 Mn4 O19 87.59(10) 2_554 . ? O27 Mn4 O19 92.41(10) 4_585 . ? O27 Mn4 O19 92.41(10) 2_554 3_584 ? O27 Mn4 O19 87.59(10) 4_585 3_584 ? O19 Mn4 O19 180.00(12) . 3_584 ? O27 Mn4 O25 95.25(9) 2_554 . ? O27 Mn4 O25 84.75(9) 4_585 . ? O19 Mn4 O25 90.52(9) . . ? O19 Mn4 O25 89.49(9) 3_584 . ? O27 Mn4 O25 84.75(9) 2_554 3_584 ? O27 Mn4 O25 95.25(9) 4_585 3_584 ? O19 Mn4 O25 89.48(9) . 3_584 ? O19 Mn4 O25 90.51(9) 3_584 3_584 ? O25 Mn4 O25 180.00(6) . 3_584 ? O20 Mn5 O28 84.90(10) . 2_554 ? O20 Mn5 N15 101.19(11) . . ? O28 Mn5 N15 92.96(10) 2_554 . ? O20 Mn5 O25 98.19(10) . 3_584 ? O28 Mn5 O25 115.68(9) 2_554 3_584 ? N15 Mn5 O25 146.65(10) . 3_584 ? O20 Mn5 N14 173.06(11) . . ? O28 Mn5 N14 99.10(10) 2_554 . ? N15 Mn5 N14 73.06(12) . . ? O25 Mn5 N14 85.24(10) 3_584 . ? O20 Mn5 O26 89.46(10) . 3_584 ? O28 Mn5 O26 168.21(10) 2_554 3_584 ? N15 Mn5 O26 98.29(10) . 3_584 ? O25 Mn5 O26 54.89(9) 3_584 3_584 ? N14 Mn5 O26 87.60(11) . 3_584 ? C1 O1 Mn1 87.20(19) . . ? C1 O2 Mn2 159.0(2) . . ? C1 O2 Mn1 92.58(19) . . ? Mn2 O2 Mn1 101.13(8) . . ? C16 O3 Mn1 105.6(2) . 4_566 ? C16 O4 Mn2 137.3(2) . 2_646 ? C25 O10 Mn2 140.5(2) . . ? C38 O11 Mn3 136.3(3) . . ? C49 O17 Mn3 118.6(2) . . ? C62 O19 Mn4 144.8(2) . . ? C62 O20 Mn5 120.2(2) . . ? C63 O25 Mn4 150.1(2) . . ? C63 O25 Mn5 96.05(19) . 3_584 ? Mn4 O25 Mn5 102.94(9) . 3_584 ? C63 O26 Mn5 85.9(2) . 3_584 ? C76 O27 Mn4 132.7(2) . 2_544 ? C76 O28 Mn5 112.5(2) . 2_544 ? C25 O33 Mn1 122.8(2) . . ? C8 N1 C6 130.4(3) . . ? C8 N1 H1 113(3) . . ? C6 N1 H1 116(3) . . ? O7 N2 O8 122.0(3) . . ? O7 N2 C13 117.8(3) . . ? O8 N2 C13 120.1(3) . . ? O6 N3 O34 123.9(3) . . ? O6 N3 C9 117.9(3) . . ? O34 N3 C9 118.2(3) . . ? C15 N4 C19 118.6(3) . . ? C15 N4 Mn1 124.7(3) . . ? C19 N4 Mn1 115.8(2) . . ? C24 N5 C20 118.4(3) . . ? C24 N5 Mn1 123.4(3) . . ? C20 N5 Mn1 117.4(2) . . ? C32 N6 C29 124.8(3) . . ? C32 N6 H6 113(3) . . ? C29 N6 H6 121(3) . . ? O16 N7 O15 122.3(4) . . ? O16 N7 C33 118.7(3) . . ? O15 N7 C33 119.0(3) . . ? O13 N8 O14 125.4(4) . . ? O13 N8 C37 118.2(4) . . ? O14 N8 C37 116.4(4) . . ? C39 N9 C43 117.5(4) . . ? C39 N9 Mn3 122.4(3) . . ? C43 N9 Mn3 120.1(3) . . ? C48 N10 C44 117.2(4) . . ? C48 N10 Mn3 122.5(4) . . ? C44 N10 Mn3 117.0(3) . . ? O24 N11 O23 124.7(4) . . ? O24 N11 C54 118.1(4) . . ? O23 N11 C54 117.1(4) . . ? O22 N12 O21 122.7(3) . . ? O22 N12 C52 118.4(3) . . ? O21 N12 C52 118.9(3) . . ? C53 N13 C56 125.3(3) . . ? C53 N13 H13 117.4 . . ? C56 N13 H13 117.4 . . ? C77 N14 C81 118.1(4) . . ? C77 N14 Mn5 124.5(3) . . ? C81 N14 Mn5 117.2(3) . . ? C86 N15 C82 118.9(3) . . ? C86 N15 Mn5 122.9(3) . . ? C82 N15 Mn5 117.5(2) . . ? C70 N16 C67 129.7(3) . . ? C70 N16 H16 111(2) . . ? C67 N16 H16 118(2) . . ? O31 N17 O32 123.9(3) . . ? O31 N17 C75 118.4(3) . . ? O32 N17 C75 117.6(3) . . ? O29 N18 O30 121.5(4) . . ? O29 N18 C71 118.1(3) . . ? O30 N18 C71 120.3(3) . . ? O1 C1 O2 121.5(3) . . ? O1 C1 C2 120.3(3) . . ? O2 C1 C2 117.9(3) . . ? C7 C2 C3 118.4(3) . . ? C7 C2 C1 119.8(3) . . ? C3 C2 C1 121.7(3) . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C6 119.4(3) . . ? C3 C4 H4 120.3 . . ? C6 C4 H4 120.3 . . ? C7 C5 C6 120.6(3) . . ? C7 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C4 119.4(3) . . ? C5 C6 N1 116.6(3) . . ? C4 C6 N1 123.9(3) . . ? C5 C7 C2 120.8(3) . . ? C5 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? N1 C8 C9 125.4(3) . . ? N1 C8 C13 121.7(3) . . ? C9 C8 C13 112.9(3) . . ? C10 C9 C8 123.8(3) . . ? C10 C9 N3 115.4(3) . . ? C8 C9 N3 120.5(3) . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 118.0(3) . . ? C12 C11 C16 119.8(3) . . ? C10 C11 C16 122.2(3) . . ? C13 C12 C11 121.0(3) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C8 123.1(3) . . ? C12 C13 N2 115.0(3) . . ? C8 C13 N2 121.8(3) . . ? C17 C14 C15 118.6(4) . . ? C17 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? N4 C15 C14 122.9(4) . . ? N4 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? O3 C16 O4 123.5(3) . . ? O3 C16 C11 117.9(3) . . ? O4 C16 C11 118.6(3) . . ? C14 C17 C18 120.0(4) . . ? C14 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 118.0(4) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? N4 C19 C18 121.8(4) . . ? N4 C19 C20 115.8(3) . . ? C18 C19 C20 122.3(4) . . ? N5 C20 C21 121.4(4) . . ? N5 C20 C19 115.9(3) . . ? C21 C20 C19 122.6(4) . . ? C22 C21 C20 118.6(4) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C21 C22 C23 120.7(4) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C24 117.8(4) . . ? C22 C23 H23 121.1 . . ? C24 C23 H23 121.1 . . ? N5 C24 C23 122.9(4) . . ? N5 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? O33 C25 O10 125.4(3) . . ? O33 C25 C26 117.5(3) . . ? O10 C25 C26 117.1(3) . . ? C27 C26 C31 119.3(3) . . ? C27 C26 C25 120.6(3) . . ? C31 C26 C25 120.1(3) . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.9(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.1(3) . . ? C30 C29 N6 120.6(3) . . ? C28 C29 N6 119.2(3) . . ? C29 C30 C31 120.3(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C26 119.9(3) . . ? C30 C31 H31 120.1 . . ? C26 C31 H31 120.1 . . ? N6 C32 C37 122.7(3) . . ? N6 C32 C33 124.1(3) . . ? C37 C32 C33 113.2(3) . . ? C34 C33 C32 123.0(4) . . ? C34 C33 N7 116.5(3) . . ? C32 C33 N7 120.5(3) . . ? C35 C34 C33 121.3(3) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C34 C35 C36 118.0(3) . . ? C34 C35 C38 121.5(4) . . ? C36 C35 C38 120.5(4) . . ? C37 C36 C35 120.2(4) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C32 124.1(3) . . ? C36 C37 N8 115.9(3) . . ? C32 C37 N8 119.8(3) . . ? O12 C38 O11 126.2(4) . . ? O12 C38 C35 117.2(4) . . ? O11 C38 C35 116.6(4) . . ? N9 C39 C40 123.9(5) . . ? N9 C39 H39 118.1 . . ? C40 C39 H39 118.1 . . ? C41 C40 C39 118.0(5) . . ? C41 C40 H40 121.0 . . ? C39 C40 H40 121.0 . . ? C40 C41 C42 120.2(6) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C43 118.9(6) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? N9 C43 C42 121.5(4) . . ? N9 C43 C44 115.4(4) . . ? C42 C43 C44 123.1(5) . . ? N10 C44 C45 123.1(5) . . ? N10 C44 C43 114.4(4) . . ? C45 C44 C43 122.6(5) . . ? C46 C45 C44 118.1(6) . . ? C46 C45 H45 120.9 . . ? C44 C45 H45 120.9 . . ? C45 C46 C47 119.7(6) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C48 C47 C46 117.8(5) . . ? C48 C47 H47 121.1 . . ? C46 C47 H47 121.1 . . ? N10 C48 C47 124.0(6) . . ? N10 C48 H48 118.0 . . ? C47 C48 H48 118.0 . . ? O18 C49 O17 126.1(3) . . ? O18 C49 C50 117.5(4) . . ? O17 C49 C50 116.4(3) . . ? C51 C50 C55 118.2(3) . . ? C51 C50 C49 120.4(3) . . ? C55 C50 C49 121.4(4) . . ? C50 C51 C52 120.6(3) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C51 C52 C53 123.4(3) . . ? C51 C52 N12 116.4(3) . . ? C53 C52 N12 120.2(3) . . ? N13 C53 C54 123.4(3) . . ? N13 C53 C52 124.0(3) . . ? C54 C53 C52 112.6(3) . . ? C55 C54 C53 124.7(3) . . ? C55 C54 N11 115.9(3) . . ? C53 C54 N11 119.3(3) . . ? C54 C55 C50 120.5(4) . . ? C54 C55 H55 119.8 . . ? C50 C55 H55 119.8 . . ? C61 C56 C57 120.3(3) . . ? C61 C56 N13 121.1(3) . . ? C57 C56 N13 118.5(3) . . ? C58 C57 C56 119.3(3) . . ? C58 C57 H57 120.3 . . ? C56 C57 H57 120.3 . . ? C57 C58 C59 121.7(3) . . ? C57 C58 H58 119.2 . . ? C59 C58 H58 119.2 . . ? C58 C59 C60 118.0(3) . . ? C58 C59 C62 120.6(3) . . ? C60 C59 C62 121.4(3) . . ? C61 C60 C59 121.0(3) . . ? C61 C60 H60 119.5 . . ? C59 C60 H60 119.5 . . ? C60 C61 C56 119.6(3) . . ? C60 C61 H61 120.2 . . ? C56 C61 H61 120.2 . . ? O19 C62 O20 125.5(3) . . ? O19 C62 C59 117.4(3) . . ? O20 C62 C59 117.0(3) . . ? O26 C63 O25 120.2(3) . . ? O26 C63 C64 120.8(3) . . ? O25 C63 C64 118.5(3) . . ? C65 C64 C69 119.2(3) . . ? C65 C64 C63 119.5(3) . . ? C69 C64 C63 121.3(3) . . ? C64 C65 C66 120.5(3) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C65 C66 C67 120.2(3) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C68 C67 C66 119.3(3) . . ? C68 C67 N16 124.2(3) . . ? C66 C67 N16 116.3(3) . . ? C69 C68 C67 120.1(3) . . ? C69 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C68 C69 C64 120.4(3) . . ? C68 C69 H69 119.8 . . ? C64 C69 H69 119.8 . . ? N16 C70 C71 121.7(3) . . ? N16 C70 C75 125.3(3) . . ? C71 C70 C75 113.0(3) . . ? C72 C71 C70 123.3(3) . . ? C72 C71 N18 114.8(3) . . ? C70 C71 N18 121.8(3) . . ? C73 C72 C71 120.9(3) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C72 C73 C74 118.3(3) . . ? C72 C73 C76 119.7(3) . . ? C74 C73 C76 122.0(3) . . ? C75 C74 C73 120.2(3) . . ? C75 C74 H74 119.9 . . ? C73 C74 H74 119.9 . . ? C74 C75 C70 123.5(3) . . ? C74 C75 N17 115.4(3) . . ? C70 C75 N17 120.7(3) . . ? O28 C76 O27 124.7(3) . . ? O28 C76 C73 118.4(3) . . ? O27 C76 C73 116.9(3) . . ? N14 C77 C78 123.1(5) . . ? N14 C77 H77 118.5 . . ? C78 C77 H77 118.5 . . ? C79 C78 C77 119.0(5) . . ? C79 C78 H78 120.5 . . ? C77 C78 H78 120.5 . . ? C78 C79 C80 119.8(4) . . ? C78 C79 H79 120.1 . . ? C80 C79 H79 120.1 . . ? C79 C80 C81 118.5(5) . . ? C79 C80 H80 120.7 . . ? C81 C80 H80 120.7 . . ? N14 C81 C80 121.4(4) . . ? N14 C81 C82 115.0(3) . . ? C80 C81 C82 123.5(4) . . ? N15 C82 C83 121.1(4) . . ? N15 C82 C81 116.5(3) . . ? C83 C82 C81 122.3(4) . . ? C84 C83 C82 119.3(5) . . ? C84 C83 H83 120.3 . . ? C82 C83 H83 120.3 . . ? C85 C84 C83 119.5(4) . . ? C85 C84 H84 120.2 . . ? C83 C84 H84 120.2 . . ? C84 C85 C86 118.8(5) . . ? C84 C85 H85 120.6 . . ? C86 C85 H85 120.6 . . ? N15 C86 C85 122.3(4) . . ? N15 C86 H86 118.9 . . ? C85 C86 H86 118.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O33 Mn1 O1 C1 -103.1(2) . . . . ? O3 Mn1 O1 C1 -66.2(13) 4_565 . . . ? N5 Mn1 O1 C1 153.6(2) . . . . ? N4 Mn1 O1 C1 80.9(2) . . . . ? O2 Mn1 O1 C1 -9.14(19) . . . . ? O10 Mn2 O2 C1 -79.0(6) . . . . ? O10 Mn2 O2 C1 101.0(6) 3_666 . . . ? O4 Mn2 O2 C1 14.4(6) 2_656 . . . ? O4 Mn2 O2 C1 -165.6(6) 4_565 . . . ? O2 Mn2 O2 C1 -171(89) 3_666 . . . ? O10 Mn2 O2 Mn1 50.83(10) . . . . ? O10 Mn2 O2 Mn1 -129.17(10) 3_666 . . . ? O4 Mn2 O2 Mn1 144.27(10) 2_656 . . . ? O4 Mn2 O2 Mn1 -35.73(10) 4_565 . . . ? O2 Mn2 O2 Mn1 -41(89) 3_666 . . . ? O33 Mn1 O2 C1 98.14(19) . . . . ? O3 Mn1 O2 C1 -175.27(18) 4_565 . . . ? N5 Mn1 O2 C1 -24.0(3) . . . . ? N4 Mn1 O2 C1 -75.4(2) . . . . ? O1 Mn1 O2 C1 8.90(18) . . . . ? O33 Mn1 O2 Mn2 -65.87(10) . . . . ? O3 Mn1 O2 Mn2 20.72(14) 4_565 . . . ? N5 Mn1 O2 Mn2 172.03(16) . . . . ? N4 Mn1 O2 Mn2 120.55(11) . . . . ? O1 Mn1 O2 Mn2 -155.11(14) . . . . ? O10 Mn2 O10 C25 160(100) 3_666 . . . ? O4 Mn2 O10 C25 -126.6(4) 2_656 . . . ? O4 Mn2 O10 C25 53.4(4) 4_565 . . . ? O2 Mn2 O10 C25 -29.1(4) . . . . ? O2 Mn2 O10 C25 150.9(4) 3_666 . . . ? O17 Mn3 O11 C38 61.3(5) . . . . ? O5 Mn3 O11 C38 -6.9(4) . . . . ? O9 Mn3 O11 C38 131.3(4) . . . . ? N9 Mn3 O11 C38 -146.0(4) . . . . ? N10 Mn3 O11 C38 -88.5(4) . . . . ? O5 Mn3 O17 C49 -160.1(3) . . . . ? O11 Mn3 O17 C49 133.0(3) . . . . ? O9 Mn3 O17 C49 62.0(3) . . . . ? N9 Mn3 O17 C49 -12.5(4) . . . . ? N10 Mn3 O17 C49 -68.3(3) . . . . ? O27 Mn4 O19 C62 -61.4(4) 2_554 . . . ? O27 Mn4 O19 C62 118.6(4) 4_585 . . . ? O19 Mn4 O19 C62 55(91) 3_584 . . . ? O25 Mn4 O19 C62 -156.6(4) . . . . ? O25 Mn4 O19 C62 23.4(4) 3_584 . . . ? O28 Mn5 O20 C62 59.8(2) 2_554 . . . ? N15 Mn5 O20 C62 151.8(2) . . . . ? O25 Mn5 O20 C62 -55.5(3) 3_584 . . . ? N14 Mn5 O20 C62 -174.7(8) . . . . ? O26 Mn5 O20 C62 -109.8(2) 3_584 . . . ? O27 Mn4 O25 C63 10.4(4) 2_554 . . . ? O27 Mn4 O25 C63 -169.6(4) 4_585 . . . ? O19 Mn4 O25 C63 98.0(4) . . . . ? O19 Mn4 O25 C63 -82.0(4) 3_584 . . . ? O25 Mn4 O25 C63 -128(100) 3_584 . . . ? O27 Mn4 O25 Mn5 138.38(10) 2_554 . . 3_584 ? O27 Mn4 O25 Mn5 -41.62(10) 4_585 . . 3_584 ? O19 Mn4 O25 Mn5 -134.00(10) . . . 3_584 ? O19 Mn4 O25 Mn5 46.00(10) 3_584 . . 3_584 ? O25 Mn4 O25 Mn5 0(100) 3_584 . . 3_584 ? O3 Mn1 O33 C25 -61.5(3) 4_565 . . . ? N5 Mn1 O33 C25 -148.4(3) . . . . ? N4 Mn1 O33 C25 154.0(9) . . . . ? O2 Mn1 O33 C25 59.8(3) . . . . ? O1 Mn1 O33 C25 116.0(3) . . . . ? O33 Mn1 N4 C15 -118.6(9) . . . . ? O3 Mn1 N4 C15 97.4(3) 4_565 . . . ? N5 Mn1 N4 C15 -177.6(3) . . . . ? O2 Mn1 N4 C15 -24.0(3) . . . . ? O1 Mn1 N4 C15 -80.3(3) . . . . ? O33 Mn1 N4 C19 50.6(10) . . . . ? O3 Mn1 N4 C19 -93.5(2) 4_565 . . . ? N5 Mn1 N4 C19 -8.4(2) . . . . ? O2 Mn1 N4 C19 145.2(2) . . . . ? O1 Mn1 N4 C19 88.9(2) . . . . ? O33 Mn1 N5 C24 17.9(3) . . . . ? O3 Mn1 N5 C24 -66.4(3) 4_565 . . . ? N4 Mn1 N5 C24 -167.7(3) . . . . ? O2 Mn1 N5 C24 137.8(3) . . . . ? O1 Mn1 N5 C24 110.9(3) . . . . ? O33 Mn1 N5 C20 -173.0(2) . . . . ? O3 Mn1 N5 C20 102.6(3) 4_565 . . . ? N4 Mn1 N5 C20 1.3(2) . . . . ? O2 Mn1 N5 C20 -53.2(3) . . . . ? O1 Mn1 N5 C20 -80.1(3) . . . . ? O17 Mn3 N9 C39 127.5(3) . . . . ? O5 Mn3 N9 C39 -104.6(4) . . . . ? O11 Mn3 N9 C39 -31.7(3) . . . . ? O9 Mn3 N9 C39 53.3(3) . . . . ? N10 Mn3 N9 C39 -171.8(4) . . . . ? O17 Mn3 N9 C43 -50.1(4) . . . . ? O5 Mn3 N9 C43 77.8(4) . . . . ? O11 Mn3 N9 C43 150.7(3) . . . . ? O9 Mn3 N9 C43 -124.3(3) . . . . ? N10 Mn3 N9 C43 10.6(3) . . . . ? O17 Mn3 N10 C48 -41.5(4) . . . . ? O5 Mn3 N10 C48 42.5(4) . . . . ? O11 Mn3 N10 C48 119.9(4) . . . . ? O9 Mn3 N10 C48 -113.7(4) . . . . ? N9 Mn3 N10 C48 -176.0(4) . . . . ? O17 Mn3 N10 C44 117.2(3) . . . . ? O5 Mn3 N10 C44 -158.7(3) . . . . ? O11 Mn3 N10 C44 -81.4(4) . . . . ? O9 Mn3 N10 C44 45.0(4) . . . . ? N9 Mn3 N10 C44 -17.3(3) . . . . ? O20 Mn5 N14 C77 145.7(8) . . . . ? O28 Mn5 N14 C77 -89.5(3) 2_554 . . . ? N15 Mn5 N14 C77 -179.8(3) . . . . ? O25 Mn5 N14 C77 25.8(3) 3_584 . . . ? O26 Mn5 N14 C77 80.8(3) 3_584 . . . ? O20 Mn5 N14 C81 -29.3(10) . . . . ? O28 Mn5 N14 C81 95.5(3) 2_554 . . . ? N15 Mn5 N14 C81 5.2(2) . . . . ? O25 Mn5 N14 C81 -149.2(3) 3_584 . . . ? O26 Mn5 N14 C81 -94.2(2) 3_584 . . . ? O20 Mn5 N15 C86 -13.4(3) . . . . ? O28 Mn5 N15 C86 72.0(3) 2_554 . . . ? O25 Mn5 N15 C86 -137.8(3) 3_584 . . . ? N14 Mn5 N15 C86 170.6(3) . . . . ? O26 Mn5 N15 C86 -104.5(3) 3_584 . . . ? O20 Mn5 N15 C82 175.6(2) . . . . ? O28 Mn5 N15 C82 -99.0(3) 2_554 . . . ? O25 Mn5 N15 C82 51.2(3) 3_584 . . . ? N14 Mn5 N15 C82 -0.4(2) . . . . ? O26 Mn5 N15 C82 84.5(3) 3_584 . . . ? Mn1 O1 C1 O2 15.9(3) . . . . ? Mn1 O1 C1 C2 -157.8(3) . . . . ? Mn2 O2 C1 O1 114.1(6) . . . . ? Mn1 O2 C1 O1 -16.9(3) . . . . ? Mn2 O2 C1 C2 -72.0(7) . . . . ? Mn1 O2 C1 C2 156.9(3) . . . . ? O1 C1 C2 C7 160.9(3) . . . . ? O2 C1 C2 C7 -13.1(5) . . . . ? O1 C1 C2 C3 -16.7(5) . . . . ? O2 C1 C2 C3 169.4(3) . . . . ? C7 C2 C3 C4 -0.7(5) . . . . ? C1 C2 C3 C4 176.9(3) . . . . ? C2 C3 C4 C6 -4.2(6) . . . . ? C7 C5 C6 C4 -2.8(6) . . . . ? C7 C5 C6 N1 -178.5(4) . . . . ? C3 C4 C6 C5 5.9(6) . . . . ? C3 C4 C6 N1 -178.7(4) . . . . ? C8 N1 C6 C5 -168.5(4) . . . . ? C8 N1 C6 C4 16.0(6) . . . . ? C6 C5 C7 C2 -2.2(6) . . . . ? C3 C2 C7 C5 3.9(5) . . . . ? C1 C2 C7 C5 -173.7(3) . . . . ? C6 N1 C8 C9 27.8(6) . . . . ? C6 N1 C8 C13 -150.6(4) . . . . ? N1 C8 C9 C10 -168.4(3) . . . . ? C13 C8 C9 C10 10.1(5) . . . . ? N1 C8 C9 N3 18.8(5) . . . . ? C13 C8 C9 N3 -162.7(3) . . . . ? O6 N3 C9 C10 -140.7(4) . . . . ? O34 N3 C9 C10 37.8(5) . . . . ? O6 N3 C9 C8 32.7(5) . . . . ? O34 N3 C9 C8 -148.8(4) . . . . ? C8 C9 C10 C11 -4.7(5) . . . . ? N3 C9 C10 C11 168.4(3) . . . . ? C9 C10 C11 C12 -3.5(5) . . . . ? C9 C10 C11 C16 177.1(3) . . . . ? C10 C11 C12 C13 5.3(5) . . . . ? C16 C11 C12 C13 -175.2(3) . . . . ? C11 C12 C13 C8 0.8(6) . . . . ? C11 C12 C13 N2 -176.3(3) . . . . ? N1 C8 C13 C12 170.4(3) . . . . ? C9 C8 C13 C12 -8.1(5) . . . . ? N1 C8 C13 N2 -12.7(5) . . . . ? C9 C8 C13 N2 168.8(3) . . . . ? O7 N2 C13 C12 -8.6(6) . . . . ? O8 N2 C13 C12 167.9(3) . . . . ? O7 N2 C13 C8 174.3(4) . . . . ? O8 N2 C13 C8 -9.2(6) . . . . ? C19 N4 C15 C14 -0.8(6) . . . . ? Mn1 N4 C15 C14 168.1(3) . . . . ? C17 C14 C15 N4 -0.7(7) . . . . ? Mn1 O3 C16 O4 -6.0(4) 4_566 . . . ? Mn1 O3 C16 C11 176.5(2) 4_566 . . . ? Mn2 O4 C16 O3 81.3(5) 2_646 . . . ? Mn2 O4 C16 C11 -101.2(4) 2_646 . . . ? C12 C11 C16 O3 169.0(3) . . . . ? C10 C11 C16 O3 -11.6(5) . . . . ? C12 C11 C16 O4 -8.7(5) . . . . ? C10 C11 C16 O4 170.8(3) . . . . ? C15 C14 C17 C18 1.7(7) . . . . ? C14 C17 C18 C19 -1.2(6) . . . . ? C15 N4 C19 C18 1.4(5) . . . . ? Mn1 N4 C19 C18 -168.5(3) . . . . ? C15 N4 C19 C20 -176.2(3) . . . . ? Mn1 N4 C19 C20 13.9(4) . . . . ? C17 C18 C19 N4 -0.4(6) . . . . ? C17 C18 C19 C20 177.0(3) . . . . ? C24 N5 C20 C21 -3.0(5) . . . . ? Mn1 N5 C20 C21 -172.6(3) . . . . ? C24 N5 C20 C19 174.9(3) . . . . ? Mn1 N5 C20 C19 5.3(4) . . . . ? N4 C19 C20 N5 -12.9(5) . . . . ? C18 C19 C20 N5 169.6(3) . . . . ? N4 C19 C20 C21 165.0(4) . . . . ? C18 C19 C20 C21 -12.5(6) . . . . ? N5 C20 C21 C22 2.6(6) . . . . ? C19 C20 C21 C22 -175.1(4) . . . . ? C20 C21 C22 C23 0.0(8) . . . . ? C21 C22 C23 C24 -2.1(8) . . . . ? C20 N5 C24 C23 0.8(6) . . . . ? Mn1 N5 C24 C23 169.7(3) . . . . ? C22 C23 C24 N5 1.8(7) . . . . ? Mn1 O33 C25 O10 -31.8(5) . . . . ? Mn1 O33 C25 C26 147.8(2) . . . . ? Mn2 O10 C25 O33 14.4(6) . . . . ? Mn2 O10 C25 C26 -165.1(2) . . . . ? O33 C25 C26 C27 164.3(3) . . . . ? O10 C25 C26 C27 -16.1(5) . . . . ? O33 C25 C26 C31 -15.0(5) . . . . ? O10 C25 C26 C31 164.6(3) . . . . ? C31 C26 C27 C28 -0.2(5) . . . . ? C25 C26 C27 C28 -179.5(3) . . . . ? C26 C27 C28 C29 0.2(5) . . . . ? C27 C28 C29 C30 -0.5(5) . . . . ? C27 C28 C29 N6 176.5(3) . . . . ? C32 N6 C29 C30 -50.3(5) . . . . ? C32 N6 C29 C28 132.7(4) . . . . ? C28 C29 C30 C31 0.7(5) . . . . ? N6 C29 C30 C31 -176.2(3) . . . . ? C29 C30 C31 C26 -0.7(6) . . . . ? C27 C26 C31 C30 0.4(5) . . . . ? C25 C26 C31 C30 179.7(3) . . . . ? C29 N6 C32 C37 -32.4(5) . . . . ? C29 N6 C32 C33 147.7(3) . . . . ? N6 C32 C33 C34 -176.6(3) . . . . ? C37 C32 C33 C34 3.5(5) . . . . ? N6 C32 C33 N7 2.2(5) . . . . ? C37 C32 C33 N7 -177.7(3) . . . . ? O16 N7 C33 C34 22.4(6) . . . . ? O15 N7 C33 C34 -157.0(4) . . . . ? O16 N7 C33 C32 -156.5(4) . . . . ? O15 N7 C33 C32 24.2(5) . . . . ? C32 C33 C34 C35 -3.3(6) . . . . ? N7 C33 C34 C35 177.9(4) . . . . ? C33 C34 C35 C36 1.2(6) . . . . ? C33 C34 C35 C38 179.4(4) . . . . ? C34 C35 C36 C37 0.3(6) . . . . ? C38 C35 C36 C37 -177.9(4) . . . . ? C35 C36 C37 C32 0.3(6) . . . . ? C35 C36 C37 N8 -174.1(4) . . . . ? N6 C32 C37 C36 178.1(4) . . . . ? C33 C32 C37 C36 -2.0(5) . . . . ? N6 C32 C37 N8 -7.7(6) . . . . ? C33 C32 C37 N8 172.2(3) . . . . ? O13 N8 C37 C36 -58.8(5) . . . . ? O14 N8 C37 C36 118.3(4) . . . . ? O13 N8 C37 C32 126.6(4) . . . . ? O14 N8 C37 C32 -56.4(5) . . . . ? Mn3 O11 C38 O12 -11.3(7) . . . . ? Mn3 O11 C38 C35 166.5(3) . . . . ? C34 C35 C38 O12 -8.2(6) . . . . ? C36 C35 C38 O12 169.9(4) . . . . ? C34 C35 C38 O11 173.7(4) . . . . ? C36 C35 C38 O11 -8.2(6) . . . . ? C43 N9 C39 C40 -0.5(7) . . . . ? Mn3 N9 C39 C40 -178.1(4) . . . . ? N9 C39 C40 C41 -0.1(9) . . . . ? C39 C40 C41 C42 1.4(10) . . . . ? C40 C41 C42 C43 -2.2(11) . . . . ? C39 N9 C43 C42 -0.3(7) . . . . ? Mn3 N9 C43 C42 177.4(4) . . . . ? C39 N9 C43 C44 178.6(4) . . . . ? Mn3 N9 C43 C44 -3.7(5) . . . . ? C41 C42 C43 N9 1.6(9) . . . . ? C41 C42 C43 C44 -177.2(6) . . . . ? C48 N10 C44 C45 1.4(7) . . . . ? Mn3 N10 C44 C45 -158.5(4) . . . . ? C48 N10 C44 C43 -178.6(4) . . . . ? Mn3 N10 C44 C43 21.5(5) . . . . ? N9 C43 C44 N10 -12.0(6) . . . . ? C42 C43 C44 N10 166.9(5) . . . . ? N9 C43 C44 C45 167.9(4) . . . . ? C42 C43 C44 C45 -13.2(7) . . . . ? N10 C44 C45 C46 0.2(8) . . . . ? C43 C44 C45 C46 -179.7(5) . . . . ? C44 C45 C46 C47 -2.9(9) . . . . ? C45 C46 C47 C48 3.8(9) . . . . ? C44 N10 C48 C47 -0.4(7) . . . . ? Mn3 N10 C48 C47 158.3(4) . . . . ? C46 C47 C48 N10 -2.2(8) . . . . ? Mn3 O17 C49 O18 -20.1(6) . . . . ? Mn3 O17 C49 C50 159.3(3) . . . . ? O18 C49 C50 C51 14.4(6) . . . . ? O17 C49 C50 C51 -165.1(4) . . . . ? O18 C49 C50 C55 -166.7(4) . . . . ? O17 C49 C50 C55 13.8(6) . . . . ? C55 C50 C51 C52 -0.6(6) . . . . ? C49 C50 C51 C52 178.3(4) . . . . ? C50 C51 C52 C53 3.4(6) . . . . ? C50 C51 C52 N12 -176.4(4) . . . . ? O22 N12 C52 C51 -26.3(6) . . . . ? O21 N12 C52 C51 153.4(4) . . . . ? O22 N12 C52 C53 153.9(4) . . . . ? O21 N12 C52 C53 -26.4(5) . . . . ? C56 N13 C53 C54 34.0(5) . . . . ? C56 N13 C53 C52 -146.0(4) . . . . ? C51 C52 C53 N13 176.8(3) . . . . ? N12 C52 C53 N13 -3.4(6) . . . . ? C51 C52 C53 C54 -3.2(5) . . . . ? N12 C52 C53 C54 176.6(3) . . . . ? N13 C53 C54 C55 -179.4(4) . . . . ? C52 C53 C54 C55 0.6(5) . . . . ? N13 C53 C54 N11 5.1(5) . . . . ? C52 C53 C54 N11 -174.9(3) . . . . ? O24 N11 C54 C55 59.6(5) . . . . ? O23 N11 C54 C55 -118.9(4) . . . . ? O24 N11 C54 C53 -124.5(4) . . . . ? O23 N11 C54 C53 57.0(5) . . . . ? C53 C54 C55 C50 2.0(6) . . . . ? N11 C54 C55 C50 177.6(3) . . . . ? C51 C50 C55 C54 -1.9(6) . . . . ? C49 C50 C55 C54 179.1(3) . . . . ? C53 N13 C56 C61 45.7(5) . . . . ? C53 N13 C56 C57 -136.8(3) . . . . ? C61 C56 C57 C58 1.8(5) . . . . ? N13 C56 C57 C58 -175.7(3) . . . . ? C56 C57 C58 C59 -0.8(5) . . . . ? C57 C58 C59 C60 -0.5(5) . . . . ? C57 C58 C59 C62 178.5(3) . . . . ? C58 C59 C60 C61 0.9(5) . . . . ? C62 C59 C60 C61 -178.1(3) . . . . ? C59 C60 C61 C56 0.1(5) . . . . ? C57 C56 C61 C60 -1.5(5) . . . . ? N13 C56 C61 C60 175.9(3) . . . . ? Mn4 O19 C62 O20 -8.7(6) . . . . ? Mn4 O19 C62 C59 171.6(2) . . . . ? Mn5 O20 C62 O19 26.3(5) . . . . ? Mn5 O20 C62 C59 -154.0(2) . . . . ? C58 C59 C62 O19 17.0(5) . . . . ? C60 C59 C62 O19 -164.1(3) . . . . ? C58 C59 C62 O20 -162.7(3) . . . . ? C60 C59 C62 O20 16.2(5) . . . . ? Mn5 O26 C63 O25 16.4(3) 3_584 . . . ? Mn5 O26 C63 C64 -155.8(3) 3_584 . . . ? Mn4 O25 C63 O26 111.2(4) . . . . ? Mn5 O25 C63 O26 -18.2(4) 3_584 . . . ? Mn4 O25 C63 C64 -76.4(5) . . . . ? Mn5 O25 C63 C64 154.2(3) 3_584 . . . ? O26 C63 C64 C65 163.2(4) . . . . ? O25 C63 C64 C65 -9.1(5) . . . . ? O26 C63 C64 C69 -14.1(5) . . . . ? O25 C63 C64 C69 173.5(3) . . . . ? C69 C64 C65 C66 4.3(6) . . . . ? C63 C64 C65 C66 -173.1(3) . . . . ? C64 C65 C66 C67 -2.5(6) . . . . ? C65 C66 C67 C68 -2.6(6) . . . . ? C65 C66 C67 N16 -178.2(4) . . . . ? C70 N16 C67 C68 16.8(6) . . . . ? C70 N16 C67 C66 -167.8(4) . . . . ? C66 C67 C68 C69 5.8(6) . . . . ? N16 C67 C68 C69 -178.9(4) . . . . ? C67 C68 C69 C64 -4.0(6) . . . . ? C65 C64 C69 C68 -1.1(5) . . . . ? C63 C64 C69 C68 176.3(3) . . . . ? C67 N16 C70 C71 -148.5(4) . . . . ? C67 N16 C70 C75 31.7(6) . . . . ? N16 C70 C71 C72 173.0(3) . . . . ? C75 C70 C71 C72 -7.1(5) . . . . ? N16 C70 C71 N18 -9.3(6) . . . . ? C75 C70 C71 N18 170.6(3) . . . . ? O29 N18 C71 C72 -14.6(6) . . . . ? O30 N18 C71 C72 162.9(4) . . . . ? O29 N18 C71 C70 167.5(5) . . . . ? O30 N18 C71 C70 -15.0(6) . . . . ? C70 C71 C72 C73 0.9(6) . . . . ? N18 C71 C72 C73 -177.0(3) . . . . ? C71 C72 C73 C74 4.6(5) . . . . ? C71 C72 C73 C76 -177.3(3) . . . . ? C72 C73 C74 C75 -3.2(5) . . . . ? C76 C73 C74 C75 178.7(3) . . . . ? C73 C74 C75 C70 -3.7(5) . . . . ? C73 C74 C75 N17 169.3(3) . . . . ? N16 C70 C75 C74 -171.6(3) . . . . ? C71 C70 C75 C74 8.5(5) . . . . ? N16 C70 C75 N17 15.7(6) . . . . ? C71 C70 C75 N17 -164.2(3) . . . . ? O31 N17 C75 C74 -141.0(4) . . . . ? O32 N17 C75 C74 37.4(5) . . . . ? O31 N17 C75 C70 32.2(5) . . . . ? O32 N17 C75 C70 -149.4(4) . . . . ? Mn5 O28 C76 O27 -6.1(4) 2_544 . . . ? Mn5 O28 C76 C73 176.8(2) 2_544 . . . ? Mn4 O27 C76 O28 70.8(5) 2_544 . . . ? Mn4 O27 C76 C73 -112.0(3) 2_544 . . . ? C72 C73 C76 O28 167.2(3) . . . . ? C74 C73 C76 O28 -14.8(5) . . . . ? C72 C73 C76 O27 -10.2(5) . . . . ? C74 C73 C76 O27 167.9(3) . . . . ? C81 N14 C77 C78 1.0(6) . . . . ? Mn5 N14 C77 C78 -174.0(3) . . . . ? N14 C77 C78 C79 1.4(7) . . . . ? C77 C78 C79 C80 -2.1(7) . . . . ? C78 C79 C80 C81 0.7(6) . . . . ? C77 N14 C81 C80 -2.5(5) . . . . ? Mn5 N14 C81 C80 172.9(3) . . . . ? C77 N14 C81 C82 175.8(3) . . . . ? Mn5 N14 C81 C82 -8.9(4) . . . . ? C79 C80 C81 N14 1.7(6) . . . . ? C79 C80 C81 C82 -176.5(4) . . . . ? C86 N15 C82 C83 1.2(5) . . . . ? Mn5 N15 C82 C83 172.5(3) . . . . ? C86 N15 C82 C81 -175.4(3) . . . . ? Mn5 N15 C82 C81 -4.0(4) . . . . ? N14 C81 C82 N15 8.5(5) . . . . ? C80 C81 C82 N15 -173.3(3) . . . . ? N14 C81 C82 C83 -168.0(3) . . . . ? C80 C81 C82 C83 10.3(6) . . . . ? N15 C82 C83 C84 -0.9(6) . . . . ? C81 C82 C83 C84 175.4(4) . . . . ? C82 C83 C84 C85 -1.0(7) . . . . ? C83 C84 C85 C86 2.6(7) . . . . ? C82 N15 C86 C85 0.5(6) . . . . ? Mn5 N15 C86 C85 -170.4(3) . . . . ? C84 C85 C86 N15 -2.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.378 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.078