# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global # Name of the journal to which the paper has been or will be submitted _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_address ; Division of Structural Chemistry Stockholm University SE-106 91 Stockholm Sweden ; # E-mail address of contact person _publ_contact_author_email lerik@struc.su.se # Name of contact person _publ_contact_author_name 'Lars Eriksson' _publ_section_title ; Synthesis, structure and reactivity of two tetranuclear carboxylate bridged Mn-complexes. ; loop_ _publ_author_name 'Gustav Berggren' 'Anders Thapper' 'Ping Huang' 'Philip Kurz' 'Lars Eriksson' 'Stenbj\"on Styring' ; M.Anderlund ; data_gb294 _database_code_depnum_ccdc_archive 'CCDC 712176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H100 Mn4 N16 O8, 2(C2 H3 N), 4(Cl O4)' _chemical_formula_sum 'C96 H106 Cl4 Mn4 N18 O24' _chemical_formula_weight 2257.55 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' Cl Cl 0.1484 0.1585 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.6096(7) _cell_length_b 24.6816(15) _cell_length_c 28.0200(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.043(5) _cell_angle_gamma 90.00 _cell_volume 10595.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2573 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 24.95 _exptl_crystal_description needle _exptl_crystal_colour colour_less _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4672 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? # Crystallization solvent _exptl_crystal_preparation 'acetonitrile : diethylether' _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 'STOE IPDS' _diffrn_measurement_method '\f scan' _diffrn_detector_area_resol_mean 6.8 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 31743 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.3094 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.37 _reflns_number_total 19069 _reflns_number_gt 6931 _reflns_threshold_expression I>2\s1(I) _computing_data_collection 'Expose (Stoe, 1997)' _computing_cell_refinement 'Cell (Stoe, 1997)' _computing_data_reduction 'Integrate (Stoe, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Bergerhoff, 1996)' _computing_publication_material 'PLATON (Spek,2003)' _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^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.29(3) _refine_ls_number_reflns 19069 _refine_ls_number_parameters 1170 _refine_ls_number_restraints 500 _refine_ls_R_factor_all 0.2124 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 0.806 _refine_ls_restrained_S_all 0.804 _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 Cl1 Cl -0.0340(2) 0.92078(15) -0.18866(14) 0.0914(12) Uani 1 1 d DU . . O11 O -0.0343(8) 0.9642(4) -0.2202(4) 0.151(4) Uani 1 1 d DU . . O12 O -0.0603(9) 0.8768(4) -0.2140(5) 0.189(5) Uani 1 1 d DU . . O13 O 0.0445(7) 0.9131(6) -0.1637(5) 0.212(6) Uani 1 1 d DU . . O14 O -0.0905(10) 0.9319(8) -0.1595(5) 0.269(8) Uani 1 1 d DU . . Cl2 Cl 0.0242(3) 0.81292(15) 0.18393(15) 0.0938(12) Uani 1 1 d DU . . O21 O 0.0300(12) 0.8554(6) 0.2130(6) 0.268(8) Uani 1 1 d DU . . O22 O -0.0196(11) 0.7755(5) 0.2017(7) 0.294(10) Uani 1 1 d DU . . O23 O -0.0226(13) 0.8268(9) 0.1394(5) 0.317(11) Uani 1 1 d DU . . O24 O 0.0997(8) 0.7966(6) 0.1788(7) 0.265(9) Uani 1 1 d DU . . Cl3 Cl 0.0263(2) 0.55327(15) 0.33594(12) 0.0908(11) Uani 1 1 d DU . . O31 O 0.0317(9) 0.5990(4) 0.3158(7) 0.238(8) Uani 1 1 d DU . . O32 O 0.0967(9) 0.5340(9) 0.3629(5) 0.316(10) Uani 1 1 d DU . . O33 O -0.0431(10) 0.5492(9) 0.3569(7) 0.347(12) Uani 1 1 d DU . . O34 O 0.0039(16) 0.5179(6) 0.2974(6) 0.347(12) Uani 1 1 d DU . . Cl4 Cl 0.0330(3) 0.32269(14) 0.16430(18) 0.1151(16) Uani 1 1 d DU . . O41 O 0.0056(13) 0.3629(5) 0.1915(4) 0.251(8) Uani 1 1 d DU . . O42 O 0.1095(8) 0.3383(9) 0.1574(6) 0.322(10) Uani 1 1 d DU . . O43 O -0.0177(6) 0.3199(3) 0.1197(3) 0.119(3) Uani 1 1 d DU . . O44 O 0.0323(10) 0.2795(4) 0.1908(5) 0.250(8) Uani 1 1 d DU . . Mn1 Mn 0.00058(9) 0.58883(5) 0.09979(5) 0.0384(4) Uani 1 1 d U . . N101 N 0.0016(5) 0.5092(3) 0.1436(3) 0.0465(11) Uani 1 1 d U . . C102 C 0.0922(7) 0.5075(4) 0.1730(4) 0.050(2) Uani 1 1 d U . . H10A H 0.0951 0.4790 0.1972 0.061 Uiso 1 1 calc R . . H10B H 0.1322 0.4980 0.1518 0.061 Uiso 1 1 calc R . . C103 C 0.1204(4) 0.5564(2) 0.1970(2) 0.046(2) Uani 1 1 d GU . . C104 C 0.1806(5) 0.5598(3) 0.2404(2) 0.076(3) Uani 1 1 d GU . . H104 H 0.2032 0.5284 0.2563 0.091 Uiso 1 1 calc R . . C105 C 0.2071(5) 0.6102(3) 0.2600(2) 0.081(4) Uani 1 1 d GU . . H105 H 0.2474 0.6125 0.2890 0.097 Uiso 1 1 calc R . . C106 C 0.1733(5) 0.6572(3) 0.2362(3) 0.068(3) Uani 1 1 d GU . . H106 H 0.1910 0.6909 0.2493 0.081 Uiso 1 1 calc R . . C107 C 0.1131(4) 0.6537(2) 0.1928(2) 0.051(2) Uani 1 1 d GU . . H107 H 0.0905 0.6852 0.1769 0.061 Uiso 1 1 calc R . . N108 N 0.0866(4) 0.6034(2) 0.17320(18) 0.0447(16) Uani 1 1 d GU . . C109 C -0.0118(8) 0.4648(4) 0.1084(4) 0.061(2) Uani 1 1 d U . . H10C H -0.0735 0.4621 0.0946 0.074 Uiso 1 1 calc R . . H10D H 0.0060 0.4311 0.1253 0.074 Uiso 1 1 calc R . . C110 C 0.0368(4) 0.4713(2) 0.0687(2) 0.055(3) Uani 1 1 d GU . . C111 C 0.0584(5) 0.42846(18) 0.0411(3) 0.072(3) Uani 1 1 d GU . . H111 H 0.0516 0.3930 0.0508 0.087 Uiso 1 1 calc R . . C112 C 0.0900(5) 0.4387(2) -0.0012(2) 0.067(3) Uani 1 1 d GU . . H112 H 0.1044 0.4100 -0.0197 0.080 Uiso 1 1 calc R . . C113 C 0.1001(5) 0.4917(3) -0.0158(2) 0.061(3) Uani 1 1 d GU . . H113 H 0.1212 0.4986 -0.0440 0.073 Uiso 1 1 calc R . . C114 C 0.0785(5) 0.5346(2) 0.0119(2) 0.054(2) Uani 1 1 d GU . . H114 H 0.0853 0.5701 0.0021 0.065 Uiso 1 1 calc R . . N115 N 0.0469(4) 0.5244(2) 0.0541(2) 0.0435(15) Uani 1 1 d GU . . C116 C -0.0628(6) 0.5121(4) 0.1728(4) 0.052(2) Uani 1 1 d U . . H11A H -0.0381 0.5298 0.2033 0.062 Uiso 1 1 calc R . . H11B H -0.0792 0.4756 0.1803 0.062 Uiso 1 1 calc R . . C117 C -0.1467(6) 0.5437(4) 0.1479(3) 0.0418(18) Uani 1 1 d U . . H11C H -0.1725 0.5262 0.1175 0.050 Uiso 1 1 calc R . . H11D H -0.1894 0.5437 0.1689 0.050 Uiso 1 1 calc R . . N118 N -0.1216(5) 0.6007(3) 0.1384(3) 0.0406(12) Uani 1 1 d U . . C119 C -0.1086(7) 0.6334(4) 0.1851(3) 0.048(2) Uani 1 1 d U . . H11E H -0.0609 0.6172 0.2080 0.058 Uiso 1 1 calc R . . H11F H -0.0901 0.6696 0.1780 0.058 Uiso 1 1 calc R . . C120 C -0.1827(4) 0.6388(3) 0.2094(2) 0.049(2) Uani 1 1 d GU . . C121 C -0.2434(5) 0.6802(3) 0.1977(2) 0.073(3) Uani 1 1 d GU . . H121 H -0.2359 0.7062 0.1748 0.088 Uiso 1 1 calc R . . C122 C -0.3153(5) 0.6829(3) 0.2202(3) 0.090(4) Uani 1 1 d GU . . H122 H -0.3559 0.7106 0.2123 0.107 Uiso 1 1 calc R . . C123 C -0.3265(4) 0.6441(4) 0.2544(3) 0.106(5) Uani 1 1 d GU . . H123 H -0.3746 0.6459 0.2695 0.128 Uiso 1 1 calc R . . C124 C -0.2658(6) 0.6026(3) 0.2662(3) 0.088(4) Uani 1 1 d GU . . H124 H -0.2734 0.5767 0.2891 0.105 Uiso 1 1 calc R . . C125 C -0.1940(5) 0.6000(3) 0.2436(3) 0.078(3) Uani 1 1 d GU . . H125 H -0.1534 0.5723 0.2515 0.093 Uiso 1 1 calc R . . C126 C -0.1906(7) 0.6250(4) 0.1018(3) 0.046(2) Uani 1 1 d U . . H12A H -0.1872 0.6642 0.1039 0.055 Uiso 1 1 calc R . . H12B H -0.2474 0.6139 0.1075 0.055 Uiso 1 1 calc R . . C127 C -0.1789(6) 0.6060(4) 0.0496(3) 0.036(2) Uiso 1 1 d U . . O128 O -0.1166(4) 0.5846(3) 0.0440(2) 0.0424(13) Uani 1 1 d U . . O129 O -0.2459(4) 0.6223(3) 0.0196(2) 0.0501(14) Uani 1 1 d U . . Mn2 Mn 0.27925(9) 0.64604(6) 0.05570(5) 0.0392(4) Uani 1 1 d U . . N201 N 0.3646(5) 0.6597(3) 0.1317(3) 0.0482(12) Uani 1 1 d U . . C202 C 0.4571(7) 0.6510(4) 0.1292(4) 0.056(2) Uani 1 1 d U . . H20A H 0.4939 0.6677 0.1572 0.067 Uiso 1 1 calc R . . H20B H 0.4696 0.6125 0.1302 0.067 Uiso 1 1 calc R . . C203 C 0.4770(4) 0.6744(3) 0.08440(19) 0.055(2) Uani 1 1 d GU . . C204 C 0.5599(4) 0.6927(4) 0.0812(2) 0.079(4) Uani 1 1 d GU . . H204 H 0.6036 0.6941 0.1089 0.095 Uiso 1 1 calc R . . C205 C 0.5777(4) 0.7089(4) 0.0366(3) 0.108(5) Uani 1 1 d GU . . H205 H 0.6332 0.7211 0.0344 0.129 Uiso 1 1 calc R . . C206 C 0.5125(5) 0.7068(3) -0.0048(2) 0.072(3) Uani 1 1 d GU . . H206 H 0.5244 0.7176 -0.0347 0.086 Uiso 1 1 calc R . . C207 C 0.4296(4) 0.6885(3) -0.00163(19) 0.059(3) Uani 1 1 d GU . . H207 H 0.3860 0.6871 -0.0293 0.070 Uiso 1 1 calc R . . N208 N 0.4118(3) 0.6723(3) 0.0430(2) 0.0499(16) Uani 1 1 d GU . . C209 C 0.3325(8) 0.6174(4) 0.1628(4) 0.059(2) Uani 1 1 d U . . H20C H 0.3717 0.6158 0.1942 0.070 Uiso 1 1 calc R . . H20D H 0.2751 0.6275 0.1683 0.070 Uiso 1 1 calc R . . C210 C 0.3278(5) 0.5650(2) 0.1403(2) 0.057(3) Uani 1 1 d GU . . C211 C 0.3395(6) 0.5166(3) 0.16612(19) 0.074(3) Uani 1 1 d GU . . H211 H 0.3532 0.5171 0.1999 0.089 Uiso 1 1 calc R . . C212 C 0.3308(6) 0.4674(2) 0.1414(3) 0.099(4) Uani 1 1 d GU . . H212 H 0.3386 0.4351 0.1587 0.119 Uiso 1 1 calc R . . C213 C 0.3103(6) 0.4667(2) 0.0909(3) 0.086(4) Uani 1 1 d GU . . H213 H 0.3044 0.4338 0.0744 0.103 Uiso 1 1 calc R . . C214 C 0.2986(5) 0.5151(3) 0.06511(19) 0.062(3) Uani 1 1 d GU . . H214 H 0.2849 0.5146 0.0313 0.074 Uiso 1 1 calc R . . N215 N 0.3074(4) 0.5642(2) 0.0898(2) 0.0525(16) Uani 1 1 d GU . . C216 C 0.3490(6) 0.7147(4) 0.1463(4) 0.050(2) Uani 1 1 d U . . H21A H 0.3880 0.7390 0.1335 0.061 Uiso 1 1 calc R . . H21B H 0.3635 0.7170 0.1815 0.061 Uiso 1 1 calc R . . C217 C 0.2571(6) 0.7339(4) 0.1297(3) 0.0420(18) Uani 1 1 d U . . H21C H 0.2181 0.7117 0.1445 0.050 Uiso 1 1 calc R . . H21D H 0.2521 0.7710 0.1404 0.050 Uiso 1 1 calc R . . N218 N 0.2300(5) 0.7312(3) 0.0756(3) 0.0392(12) Uani 1 1 d U . . C219 C 0.2657(6) 0.7758(3) 0.0502(4) 0.0466(19) Uani 1 1 d U . . H21E H 0.2547 0.7678 0.0157 0.056 Uiso 1 1 calc R . . H21F H 0.3285 0.7769 0.0614 0.056 Uiso 1 1 calc R . . C220 C 0.2287(4) 0.8312(2) 0.0576(2) 0.045(2) Uani 1 1 d GU . . C221 C 0.1561(4) 0.8506(3) 0.0255(2) 0.058(3) Uani 1 1 d GU . . H221 H 0.1295 0.8293 -0.0006 0.070 Uiso 1 1 calc R . . C222 C 0.1232(4) 0.9017(3) 0.0323(3) 0.079(3) Uani 1 1 d GU . . H222 H 0.0746 0.9147 0.0108 0.095 Uiso 1 1 calc R . . C223 C 0.1629(5) 0.9335(2) 0.0712(3) 0.092(4) Uani 1 1 d GU . . H223 H 0.1409 0.9677 0.0758 0.110 Uiso 1 1 calc R . . C224 C 0.2355(5) 0.9141(3) 0.1034(2) 0.075(3) Uani 1 1 d GU . . H224 H 0.2621 0.9354 0.1294 0.090 Uiso 1 1 calc R . . C225 C 0.2684(4) 0.8630(3) 0.0965(2) 0.067(3) Uani 1 1 d GU . . H225 H 0.3170 0.8500 0.1180 0.081 Uiso 1 1 calc R . . C226 C 0.1350(6) 0.7284(3) 0.0625(3) 0.0374(17) Uani 1 1 d U . . H22A H 0.1166 0.7368 0.0282 0.045 Uiso 1 1 calc R . . H22B H 0.1096 0.7552 0.0810 0.045 Uiso 1 1 calc R . . C227 C 0.1026(7) 0.6731(4) 0.0726(3) 0.0335(18) Uani 1 1 d U . . O228 O 0.1535(4) 0.6342(2) 0.0771(2) 0.0457(14) Uani 1 1 d U . . O229 O 0.0253(4) 0.6686(3) 0.0782(2) 0.0456(13) Uani 1 1 d U . . Mn3 Mn -0.27986(9) 0.60673(6) -0.05522(5) 0.0379(4) Uani 1 1 d U . . N301 N -0.3657(5) 0.5906(3) -0.1303(3) 0.0442(11) Uani 1 1 d U . . C302 C -0.4587(7) 0.5972(5) -0.1260(4) 0.061(2) Uani 1 1 d U . . H30A H -0.4732 0.6354 -0.1283 0.073 Uiso 1 1 calc R . . H30B H -0.4951 0.5790 -0.1533 0.073 Uiso 1 1 calc R . . C303 C -0.4789(4) 0.5764(3) -0.08222(17) 0.045(2) Uani 1 1 d GU . . C304 C -0.5602(4) 0.5564(3) -0.0777(2) 0.072(4) Uani 1 1 d GU . . H304 H -0.6049 0.5541 -0.1048 0.086 Uiso 1 1 calc R . . C305 C -0.5748(4) 0.5397(3) -0.0325(3) 0.091(4) Uani 1 1 d GU . . H305 H -0.6292 0.5264 -0.0295 0.109 Uiso 1 1 calc R . . C306 C -0.5081(5) 0.5431(3) 0.0081(2) 0.070(3) Uani 1 1 d GU . . H306 H -0.5179 0.5320 0.0383 0.084 Uiso 1 1 calc R . . C307 C -0.4268(4) 0.5631(3) 0.00355(18) 0.056(3) Uani 1 1 d GU . . H307 H -0.3822 0.5653 0.0307 0.067 Uiso 1 1 calc R . . N308 N -0.4122(3) 0.5797(2) -0.0416(2) 0.0401(14) Uani 1 1 d GU . . C309 C -0.3431(8) 0.6306(4) -0.1635(4) 0.056(2) Uani 1 1 d U . . H30C H -0.3865 0.6304 -0.1934 0.068 Uiso 1 1 calc R . . H30D H -0.2870 0.6216 -0.1715 0.068 Uiso 1 1 calc R . . C310 C -0.3389(5) 0.6854(2) -0.1411(2) 0.047(2) Uani 1 1 d GU . . C311 C -0.3585(5) 0.7327(3) -0.16786(18) 0.084(4) Uani 1 1 d GU . . H311 H -0.3758 0.7309 -0.2015 0.100 Uiso 1 1 calc R . . C312 C -0.3522(6) 0.7826(2) -0.1444(3) 0.100(4) Uani 1 1 d GU . . H312 H -0.3654 0.8142 -0.1624 0.120 Uiso 1 1 calc R . . C313 C -0.3263(6) 0.7852(2) -0.0942(3) 0.078(3) Uani 1 1 d GU . . H313 H -0.3221 0.8185 -0.0785 0.094 Uiso 1 1 calc R . . C314 C -0.3067(4) 0.7379(3) -0.06736(18) 0.061(3) Uani 1 1 d GU . . H314 H -0.2893 0.7396 -0.0337 0.073 Uiso 1 1 calc R . . N315 N -0.3130(4) 0.6880(2) -0.0908(2) 0.0450(14) Uani 1 1 d GU . . C316 C -0.3483(7) 0.5325(4) -0.1443(3) 0.051(2) Uani 1 1 d U . . H31A H -0.3853 0.5081 -0.1302 0.062 Uiso 1 1 calc R . . H31B H -0.3633 0.5288 -0.1794 0.062 Uiso 1 1 calc R . . C317 C -0.2551(7) 0.5170(4) -0.1273(3) 0.052(2) Uani 1 1 d U . . H31C H -0.2183 0.5401 -0.1429 0.062 Uiso 1 1 calc R . . H31D H -0.2466 0.4799 -0.1368 0.062 Uiso 1 1 calc R . . N318 N -0.2283(5) 0.5222(3) -0.0731(3) 0.0392(11) Uani 1 1 d U . . C319 C -0.2609(6) 0.4751(3) -0.0467(4) 0.0451(19) Uani 1 1 d U . . H31E H -0.2469 0.4828 -0.0121 0.054 Uiso 1 1 calc R . . H31F H -0.3240 0.4742 -0.0559 0.054 Uiso 1 1 calc R . . C320 C -0.2288(4) 0.42144(19) -0.0540(2) 0.0354(18) Uani 1 1 d GU . . C321 C -0.1568(4) 0.4024(2) -0.0212(2) 0.050(2) Uani 1 1 d GU . . H321 H -0.1306 0.4241 0.0046 0.060 Uiso 1 1 calc R . . C322 C -0.1241(4) 0.3509(3) -0.0270(3) 0.076(3) Uani 1 1 d GU . . H322 H -0.0760 0.3382 -0.0051 0.092 Uiso 1 1 calc R . . C323 C -0.1633(5) 0.3185(2) -0.0657(3) 0.076(3) Uani 1 1 d GU . . H323 H -0.1414 0.2841 -0.0696 0.091 Uiso 1 1 calc R . . C324 C -0.2352(5) 0.3376(2) -0.0985(2) 0.084(4) Uani 1 1 d GU . . H324 H -0.2615 0.3159 -0.1243 0.101 Uiso 1 1 calc R . . C325 C -0.2680(4) 0.3890(3) -0.0927(2) 0.058(3) Uani 1 1 d GU . . H325 H -0.3161 0.4018 -0.1146 0.069 Uiso 1 1 calc R . . C326 C -0.1311(6) 0.5244(4) -0.0603(4) 0.047(2) Uani 1 1 d U . . H32A H -0.1064 0.4959 -0.0774 0.057 Uiso 1 1 calc R . . H32B H -0.1121 0.5185 -0.0256 0.057 Uiso 1 1 calc R . . C327 C -0.0997(7) 0.5785(4) -0.0740(4) 0.038(2) Uani 1 1 d U . . O328 O -0.1565(4) 0.6199(2) -0.0776(2) 0.0431(13) Uani 1 1 d U . . O329 O -0.0241(4) 0.5843(3) -0.0800(2) 0.0470(13) Uani 1 1 d U . . Mn4 Mn 0.00023(9) 0.66416(6) -0.10082(5) 0.0399(4) Uani 1 1 d U . . N401 N -0.0082(6) 0.7433(3) -0.1442(3) 0.0522(13) Uani 1 1 d U . . C402 C -0.0883(9) 0.7482(5) -0.1749(5) 0.072(3) Uani 1 1 d U . . H40A H -0.0837 0.7750 -0.1997 0.087 Uiso 1 1 calc R . . H40B H -0.1306 0.7614 -0.1564 0.087 Uiso 1 1 calc R . . C403 C -0.1214(4) 0.6952(2) -0.1997(2) 0.062(3) Uani 1 1 d GU . . C404 C -0.1808(4) 0.6893(3) -0.2432(2) 0.068(3) Uani 1 1 d GU . . H404 H -0.2059 0.7198 -0.2598 0.081 Uiso 1 1 calc R . . C405 C -0.2028(4) 0.6379(3) -0.26189(19) 0.070(3) Uani 1 1 d GU . . H405 H -0.2425 0.6340 -0.2910 0.084 Uiso 1 1 calc R . . C406 C -0.1653(5) 0.5924(2) -0.2371(2) 0.058(3) Uani 1 1 d GU . . H406 H -0.1800 0.5580 -0.2495 0.070 Uiso 1 1 calc R . . C407 C -0.1059(4) 0.5983(2) -0.1936(2) 0.052(2) Uani 1 1 d GU . . H407 H -0.0809 0.5678 -0.1770 0.063 Uiso 1 1 calc R . . N408 N -0.0840(3) 0.6497(2) -0.17491(18) 0.0415(15) Uani 1 1 d GU . . C409 C 0.0070(8) 0.7893(4) -0.1102(4) 0.065(2) Uani 1 1 d U . . H40C H 0.0692 0.7931 -0.0981 0.078 Uiso 1 1 calc R . . H40D H -0.0136 0.8223 -0.1275 0.078 Uiso 1 1 calc R . . C410 C -0.0373(4) 0.7824(2) -0.0690(2) 0.053(2) Uani 1 1 d GU . . C411 C -0.0620(5) 0.8249(2) -0.0421(3) 0.079(3) Uani 1 1 d GU . . H411 H -0.0551 0.8606 -0.0515 0.094 Uiso 1 1 calc R . . C412 C -0.0970(5) 0.8142(3) -0.0011(3) 0.100(4) Uani 1 1 d GU . . H412 H -0.1135 0.8427 0.0170 0.120 Uiso 1 1 calc R . . C413 C -0.1073(5) 0.7610(3) 0.0131(2) 0.081(3) Uani 1 1 d GU . . H413 H -0.1307 0.7539 0.0405 0.097 Uiso 1 1 calc R . . C414 C -0.0826(4) 0.7185(2) -0.0139(2) 0.049(2) Uani 1 1 d GU . . H414 H -0.0894 0.6829 -0.0044 0.058 Uiso 1 1 calc R . . N415 N -0.0476(4) 0.7292(2) -0.0549(2) 0.0508(16) Uani 1 1 d GU . . C416 C 0.0648(7) 0.7398(4) -0.1741(4) 0.061(2) Uani 1 1 d U . . H41A H 0.0431 0.7207 -0.2043 0.073 Uiso 1 1 calc R . . H41B H 0.0812 0.7761 -0.1821 0.073 Uiso 1 1 calc R . . C417 C 0.1451(7) 0.7104(4) -0.1463(4) 0.054(2) Uani 1 1 d U . . H41C H 0.1921 0.7123 -0.1644 0.065 Uiso 1 1 calc R . . H41D H 0.1645 0.7275 -0.1149 0.065 Uiso 1 1 calc R . . N418 N 0.1223(5) 0.6538(3) -0.1396(3) 0.0434(12) Uani 1 1 d U . . C419 C 0.1127(7) 0.6219(4) -0.1846(3) 0.0438(19) Uani 1 1 d U . . H41E H 0.0681 0.6387 -0.2089 0.053 Uiso 1 1 calc R . . H41F H 0.0919 0.5861 -0.1782 0.053 Uiso 1 1 calc R . . C420 C 0.1963(4) 0.6152(3) -0.2063(2) 0.052(2) Uani 1 1 d GU . . C421 C 0.2481(5) 0.5697(3) -0.1939(3) 0.061(3) Uani 1 1 d GU . . H421 H 0.2311 0.5431 -0.1741 0.074 Uiso 1 1 calc R . . C422 C 0.3254(5) 0.5638(3) -0.2112(3) 0.106(4) Uani 1 1 d GU . . H422 H 0.3601 0.5333 -0.2029 0.127 Uiso 1 1 calc R . . C423 C 0.3508(4) 0.6035(4) -0.2408(3) 0.092(4) Uani 1 1 d GU . . H423 H 0.4026 0.5996 -0.2523 0.111 Uiso 1 1 calc R . . C424 C 0.2990(5) 0.6491(4) -0.2532(3) 0.106(5) Uani 1 1 d GU . . H424 H 0.3160 0.6756 -0.2730 0.127 Uiso 1 1 calc R . . C425 C 0.2217(5) 0.6549(3) -0.2359(3) 0.072(3) Uani 1 1 d GU . . H425 H 0.1871 0.6854 -0.2442 0.086 Uiso 1 1 calc R . . C426 C 0.1907(7) 0.6294(5) -0.1028(4) 0.056(2) Uani 1 1 d U . . H42A H 0.1889 0.5906 -0.1084 0.067 Uiso 1 1 calc R . . H42B H 0.2464 0.6422 -0.1089 0.067 Uiso 1 1 calc R . . C427 C 0.1903(6) 0.6380(4) -0.0517(4) 0.0411(14) Uani 1 1 d U . . O428 O 0.1185(4) 0.6681(3) -0.0440(2) 0.0469(12) Uani 1 1 d U . . O429 O 0.2491(5) 0.6323(3) -0.0180(2) 0.0598(15) Uani 1 1 d U . . N601 N -0.0864(11) 0.2090(6) -0.1265(5) 0.132(6) Uani 1 1 d U . . C601 C -0.0837(15) 0.2381(8) -0.1554(6) 0.128(8) Uani 1 1 d U . . C603 C -0.0853(10) 0.2773(7) -0.1907(6) 0.126(6) Uani 1 1 d U . . H60A H -0.0533 0.3085 -0.1767 0.190 Uiso 1 1 calc R . . H60B H -0.1446 0.2874 -0.2036 0.190 Uiso 1 1 calc R . . H60C H -0.0590 0.2633 -0.2165 0.190 Uiso 1 1 calc R . . N604 N -0.3916(10) 0.4504(6) -0.3673(5) 0.128(5) Uani 1 1 d U . . C605 C -0.4020(10) 0.4828(7) -0.3331(7) 0.096(5) Uani 1 1 d U . . C606 C -0.4007(13) 0.5189(9) -0.2969(7) 0.168(9) Uani 1 1 d U . . H60D H -0.3585 0.5079 -0.2690 0.253 Uiso 1 1 calc R . . H60E H -0.4574 0.5206 -0.2884 0.253 Uiso 1 1 calc R . . H60F H -0.3854 0.5540 -0.3075 0.253 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 Cl1 0.091(3) 0.077(2) 0.095(3) 0.0198(19) -0.011(2) -0.013(2) O11 0.186(11) 0.115(6) 0.142(10) 0.068(6) 0.004(7) 0.008(7) O12 0.245(13) 0.128(7) 0.169(11) -0.019(5) -0.025(8) -0.089(10) O13 0.143(6) 0.231(14) 0.207(13) 0.110(10) -0.108(7) -0.063(8) O14 0.279(13) 0.42(2) 0.135(12) -0.012(12) 0.112(10) -0.016(17) Cl2 0.106(3) 0.084(3) 0.097(3) -0.009(2) 0.034(2) 0.015(2) O21 0.35(2) 0.225(13) 0.234(14) -0.146(12) 0.074(14) 0.049(13) O22 0.36(2) 0.155(10) 0.46(2) 0.121(12) 0.31(2) 0.058(11) O23 0.327(18) 0.41(3) 0.160(11) 0.068(10) -0.101(13) -0.116(18) O24 0.133(8) 0.265(19) 0.43(2) -0.147(17) 0.124(11) 0.005(9) Cl3 0.104(3) 0.107(3) 0.066(2) 0.014(2) 0.027(2) -0.010(2) O31 0.223(13) 0.082(6) 0.45(3) 0.067(8) 0.180(14) -0.011(8) O32 0.188(10) 0.57(3) 0.172(13) 0.124(15) -0.015(8) 0.111(15) O33 0.245(14) 0.51(3) 0.35(2) 0.31(2) 0.225(16) 0.137(18) O34 0.55(3) 0.188(12) 0.250(19) -0.116(13) -0.060(14) -0.03(2) Cl4 0.090(3) 0.055(2) 0.167(4) 0.019(2) -0.061(3) -0.013(2) O41 0.47(2) 0.145(10) 0.132(9) 0.018(7) 0.029(12) 0.076(14) O42 0.118(8) 0.61(3) 0.204(17) 0.042(16) -0.050(6) -0.131(14) O43 0.112(7) 0.090(6) 0.133(6) 0.029(5) -0.032(5) -0.051(6) O44 0.297(14) 0.083(6) 0.264(13) 0.088(7) -0.211(12) -0.061(8) Mn1 0.0480(10) 0.0336(8) 0.0324(9) 0.0024(7) 0.0049(7) -0.0025(7) N101 0.053(3) 0.036(2) 0.051(3) 0.0085(18) 0.013(2) -0.006(2) C102 0.054(4) 0.052(3) 0.047(6) 0.017(3) 0.012(3) 0.008(5) C103 0.036(5) 0.065(3) 0.038(4) 0.015(3) 0.011(3) -0.003(4) C104 0.109(9) 0.094(5) 0.021(6) 0.023(4) -0.001(4) -0.007(6) C105 0.076(10) 0.117(7) 0.045(7) -0.016(5) 0.000(5) 0.000(7) C106 0.057(8) 0.088(5) 0.057(7) -0.029(5) 0.008(4) -0.017(6) C107 0.049(7) 0.063(3) 0.044(5) -0.018(4) 0.017(4) -0.013(5) N108 0.047(3) 0.051(3) 0.035(3) 0.002(2) 0.004(2) -0.008(3) C109 0.086(8) 0.036(2) 0.064(6) 0.002(3) 0.018(4) -0.010(5) C110 0.062(7) 0.037(2) 0.068(6) -0.017(4) 0.013(5) -0.018(5) C111 0.097(9) 0.043(3) 0.077(8) -0.015(4) 0.020(6) -0.003(6) C112 0.059(8) 0.072(4) 0.067(7) -0.019(5) 0.005(6) 0.009(7) C113 0.063(8) 0.079(5) 0.038(6) -0.020(4) 0.004(5) -0.006(6) C114 0.040(6) 0.068(4) 0.060(6) -0.005(4) 0.021(5) 0.005(6) N115 0.045(4) 0.042(2) 0.043(3) -0.001(2) 0.006(3) 0.004(3) C116 0.054(4) 0.052(5) 0.051(6) 0.014(3) 0.013(4) -0.007(4) C117 0.048(4) 0.047(3) 0.029(6) -0.008(3) 0.003(4) -0.012(3) N118 0.047(3) 0.044(3) 0.030(3) -0.007(2) 0.005(2) -0.006(2) C119 0.070(6) 0.043(5) 0.031(3) -0.008(3) 0.010(3) -0.008(4) C120 0.066(6) 0.058(6) 0.020(5) -0.009(3) 0.002(4) 0.005(4) C121 0.074(7) 0.091(8) 0.042(7) -0.017(5) -0.019(5) 0.025(6) C122 0.076(7) 0.112(9) 0.071(9) -0.058(6) -0.010(6) 0.026(7) C123 0.081(9) 0.146(13) 0.095(12) -0.057(7) 0.024(9) -0.015(7) C124 0.113(10) 0.084(8) 0.079(9) -0.031(6) 0.053(7) -0.036(6) C125 0.107(9) 0.082(8) 0.053(8) 0.008(5) 0.039(6) 0.003(6) C126 0.058(3) 0.049(5) 0.031(3) -0.010(4) 0.008(3) 0.009(4) O128 0.039(3) 0.055(4) 0.034(2) -0.007(3) 0.0081(18) 0.002(2) O129 0.042(3) 0.073(4) 0.0333(16) -0.002(2) 0.000(2) 0.005(3) Mn2 0.0478(9) 0.0384(9) 0.0300(8) -0.0006(7) 0.0038(7) 0.0052(8) N201 0.058(3) 0.048(3) 0.034(2) 0.002(2) -0.0039(19) 0.005(2) C202 0.057(3) 0.073(7) 0.033(4) -0.022(5) -0.003(2) 0.000(4) C203 0.047(3) 0.051(7) 0.061(4) 0.011(5) -0.003(2) 0.007(5) C204 0.045(4) 0.117(11) 0.072(6) 0.000(8) 0.002(4) 0.000(7) C205 0.081(7) 0.151(13) 0.089(7) 0.011(10) 0.011(5) -0.051(10) C206 0.057(6) 0.089(9) 0.075(6) 0.021(7) 0.026(4) 0.015(6) C207 0.051(5) 0.083(9) 0.048(4) -0.009(6) 0.024(3) 0.015(6) N208 0.042(2) 0.060(5) 0.047(3) 0.008(4) 0.0057(19) 0.012(3) C209 0.080(7) 0.059(3) 0.035(2) 0.012(3) 0.009(5) 0.012(6) C210 0.068(8) 0.053(3) 0.049(3) 0.015(2) 0.010(6) 0.001(5) C211 0.093(9) 0.060(4) 0.066(4) 0.023(3) 0.009(7) 0.006(7) C212 0.163(13) 0.054(3) 0.089(6) 0.023(4) 0.041(10) -0.005(8) C213 0.121(10) 0.042(2) 0.092(6) 0.008(4) 0.010(9) -0.009(7) C214 0.078(8) 0.041(2) 0.071(5) 0.000(3) 0.023(7) 0.009(6) N215 0.057(4) 0.0420(17) 0.053(3) 0.0037(19) -0.004(4) 0.008(2) C216 0.050(4) 0.053(3) 0.044(5) -0.013(3) -0.002(4) -0.008(4) C217 0.052(4) 0.037(5) 0.036(3) -0.006(3) 0.006(4) -0.007(4) N218 0.044(3) 0.0373(18) 0.038(3) 0.008(2) 0.011(3) 0.0004(19) C219 0.053(4) 0.0367(19) 0.053(5) 0.009(3) 0.016(5) -0.004(3) C220 0.027(5) 0.032(2) 0.077(7) -0.005(3) 0.014(4) -0.017(3) C221 0.056(7) 0.037(5) 0.077(7) 0.001(5) 0.004(4) -0.004(4) C222 0.105(9) 0.048(6) 0.087(8) 0.018(5) 0.026(6) 0.023(6) C223 0.150(12) 0.035(6) 0.099(10) 0.001(5) 0.046(7) 0.022(6) C224 0.120(10) 0.038(5) 0.077(8) -0.008(5) 0.040(5) -0.023(5) C225 0.078(8) 0.037(5) 0.079(7) -0.002(4) -0.003(5) -0.019(5) C226 0.045(3) 0.031(3) 0.036(5) -0.005(4) 0.008(3) -0.002(2) C227 0.049(3) 0.032(3) 0.018(5) -0.004(4) 0.005(4) -0.004(2) O228 0.052(2) 0.035(2) 0.051(4) 0.003(4) 0.010(3) -0.0005(19) O229 0.049(2) 0.0373(18) 0.050(4) 0.011(2) 0.006(3) -0.001(2) Mn3 0.0446(9) 0.0397(8) 0.0272(8) 0.0009(7) 0.0014(7) -0.0056(8) N301 0.044(3) 0.059(3) 0.028(2) 0.004(2) 0.0033(18) 0.002(2) C302 0.036(2) 0.085(7) 0.056(4) 0.032(6) -0.008(2) 0.012(4) C303 0.046(3) 0.050(6) 0.040(3) -0.020(5) 0.011(2) -0.003(5) C304 0.054(5) 0.121(11) 0.043(5) -0.028(7) 0.014(4) -0.023(7) C305 0.066(6) 0.156(13) 0.060(6) -0.015(8) 0.034(4) -0.020(8) C306 0.087(7) 0.084(9) 0.047(5) 0.001(6) 0.032(4) -0.023(7) C307 0.068(5) 0.058(7) 0.045(4) 0.011(6) 0.020(3) -0.001(6) N308 0.051(2) 0.034(4) 0.037(3) -0.004(3) 0.012(2) -0.009(3) C309 0.067(7) 0.067(3) 0.032(2) 0.013(3) 0.001(5) -0.004(6) C310 0.045(6) 0.062(3) 0.041(3) 0.018(2) 0.021(5) 0.010(5) C311 0.127(11) 0.072(4) 0.056(4) 0.029(3) 0.028(7) 0.027(8) C312 0.153(13) 0.063(3) 0.081(6) 0.031(5) 0.015(9) 0.009(8) C313 0.109(10) 0.050(3) 0.081(6) 0.018(4) 0.030(8) 0.019(7) C314 0.078(8) 0.041(2) 0.063(4) 0.010(3) 0.013(6) -0.010(6) N315 0.054(4) 0.0466(17) 0.042(3) 0.0109(19) 0.029(4) 0.002(2) C316 0.066(5) 0.059(3) 0.024(5) -0.005(3) -0.004(3) -0.005(4) C317 0.071(5) 0.052(6) 0.031(3) -0.003(3) 0.006(4) 0.010(4) N318 0.043(2) 0.0408(18) 0.033(3) 0.005(2) 0.005(3) -0.0058(19) C319 0.054(4) 0.0385(19) 0.045(5) 0.000(3) 0.016(5) -0.013(3) C320 0.029(5) 0.036(2) 0.045(5) -0.005(3) 0.018(3) -0.020(3) C321 0.070(7) 0.041(5) 0.038(6) 0.010(4) 0.004(4) -0.013(4) C322 0.061(7) 0.047(6) 0.117(10) 0.015(5) 0.009(6) -0.005(5) C323 0.122(10) 0.029(6) 0.089(9) 0.009(4) 0.050(6) 0.005(5) C324 0.157(12) 0.037(5) 0.056(7) -0.010(5) 0.016(6) -0.015(6) C325 0.066(7) 0.065(6) 0.042(6) -0.018(4) 0.007(4) -0.004(5) C326 0.042(3) 0.045(3) 0.054(6) 0.021(5) 0.009(3) -0.001(2) C327 0.045(3) 0.039(3) 0.029(6) 0.003(4) 0.002(4) -0.008(2) O328 0.047(2) 0.040(2) 0.043(4) 0.004(3) 0.009(2) -0.0062(18) O329 0.045(3) 0.0419(19) 0.052(4) 0.020(2) 0.005(3) -0.002(2) Mn4 0.0478(9) 0.0354(9) 0.0355(9) 0.0062(7) 0.0051(7) -0.0052(7) N401 0.077(4) 0.040(2) 0.037(3) 0.0119(18) 0.004(2) -0.003(2) C402 0.091(5) 0.057(3) 0.059(7) 0.003(4) -0.010(4) 0.033(6) C403 0.059(7) 0.072(4) 0.048(5) 0.012(4) -0.006(4) 0.003(5) C404 0.060(8) 0.103(6) 0.037(6) 0.003(4) 0.002(4) 0.020(6) C405 0.067(8) 0.119(7) 0.026(6) 0.000(4) 0.016(4) -0.020(6) C406 0.045(7) 0.096(5) 0.039(6) -0.029(4) 0.021(4) -0.007(5) C407 0.052(7) 0.067(3) 0.041(5) -0.005(4) 0.016(4) -0.025(5) N408 0.043(3) 0.055(3) 0.028(3) 0.007(2) 0.011(2) -0.010(3) C409 0.089(8) 0.036(2) 0.072(6) 0.000(3) 0.021(4) -0.014(5) C410 0.059(7) 0.044(2) 0.053(5) -0.010(4) 0.000(5) -0.006(5) C411 0.074(9) 0.056(3) 0.108(9) -0.030(5) 0.024(7) -0.008(7) C412 0.090(10) 0.085(5) 0.141(12) -0.052(7) 0.063(9) -0.012(8) C413 0.067(8) 0.100(6) 0.083(8) -0.027(6) 0.034(7) -0.001(8) C414 0.036(6) 0.073(5) 0.032(5) -0.009(4) -0.006(4) -0.006(5) N415 0.065(4) 0.050(2) 0.035(3) 0.002(3) 0.004(3) 0.005(3) C416 0.093(6) 0.041(5) 0.052(6) 0.010(3) 0.021(4) -0.021(4) C417 0.070(5) 0.055(4) 0.041(6) -0.010(4) 0.021(5) -0.026(4) N418 0.047(3) 0.052(3) 0.0301(19) 0.002(2) 0.0038(19) -0.012(2) C419 0.056(5) 0.041(5) 0.032(3) 0.004(3) 0.003(3) 0.002(4) C420 0.048(5) 0.073(6) 0.030(6) -0.008(4) -0.003(4) 0.000(4) C421 0.058(6) 0.082(7) 0.036(6) -0.022(5) -0.011(5) 0.013(5) C422 0.079(9) 0.152(11) 0.087(11) -0.031(8) 0.013(7) 0.042(8) C423 0.030(6) 0.195(13) 0.048(8) -0.051(7) -0.004(5) -0.001(6) C424 0.064(8) 0.230(14) 0.026(6) 0.031(9) 0.015(6) 0.018(7) C425 0.071(7) 0.091(7) 0.061(8) 0.000(5) 0.030(6) 0.000(6) C426 0.046(3) 0.091(7) 0.029(2) 0.006(5) 0.005(3) -0.003(4) C427 0.0421(18) 0.049(2) 0.0317(15) 0.0056(18) 0.0056(14) -0.0155(17) O428 0.056(3) 0.053(4) 0.029(2) 0.004(3) 0.0013(18) -0.005(2) O429 0.059(3) 0.083(4) 0.0324(16) -0.006(2) -0.0024(19) 0.008(3) N601 0.180(13) 0.138(13) 0.090(11) 0.020(7) 0.053(10) 0.071(11) C601 0.23(2) 0.117(14) 0.039(10) -0.017(6) 0.046(12) 0.058(15) C603 0.110(13) 0.132(15) 0.134(15) 0.032(9) 0.016(11) -0.010(11) N604 0.143(12) 0.114(12) 0.115(12) 0.000(7) 0.000(9) -0.045(9) C605 0.063(8) 0.091(13) 0.126(15) 0.013(7) 0.000(10) -0.030(9) C606 0.130(15) 0.22(2) 0.142(18) -0.052(13) -0.007(13) -0.006(15) _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 Cl1 O13 1.304(9) . ? Cl1 O12 1.319(9) . ? Cl1 O14 1.341(11) . ? Cl1 O11 1.390(8) . ? Cl2 O24 1.279(10) . ? Cl2 O22 1.302(10) . ? Cl2 O21 1.320(10) . ? Cl2 O23 1.363(11) . ? Cl3 O31 1.271(9) . ? Cl3 O32 1.299(11) . ? Cl3 O33 1.331(10) . ? Cl3 O34 1.380(11) . ? Cl4 O44 1.299(9) . ? Cl4 O42 1.304(11) . ? Cl4 O43 1.347(8) . ? Cl4 O41 1.369(11) . ? Mn1 O229 2.116(6) . ? Mn1 O128 2.170(6) . ? Mn1 N115 2.246(4) . ? Mn1 N108 2.259(5) . ? Mn1 N101 2.314(7) . ? Mn1 N118 2.384(8) . ? N101 C116 1.416(12) . ? N101 C109 1.463(12) . ? N101 C102 1.495(13) . ? C102 C103 1.410(12) . ? C102 H10A 0.9700 . ? C102 H10B 0.9700 . ? C103 C104 1.3900 . ? C103 N108 1.3900 . ? C104 C105 1.3900 . ? C104 H104 0.9300 . ? C105 C106 1.3900 . ? C105 H105 0.9300 . ? C106 C107 1.3900 . ? C106 H106 0.9300 . ? C107 N108 1.3900 . ? C107 H107 0.9300 . ? C109 C110 1.470(11) . ? C109 H10C 0.9700 . ? C109 H10D 0.9700 . ? C110 C111 1.3900 . ? C110 N115 1.3900 . ? C111 C112 1.3900 . ? C111 H111 0.9300 . ? C112 C113 1.3900 . ? C112 H112 0.9300 . ? C113 C114 1.3900 . ? C113 H113 0.9300 . ? C114 N115 1.3900 . ? C114 H114 0.9300 . ? C116 C117 1.568(13) . ? C116 H11A 0.9700 . ? C116 H11B 0.9700 . ? C117 N118 1.499(12) . ? C117 H11C 0.9700 . ? C117 H11D 0.9700 . ? N118 C126 1.467(12) . ? N118 C119 1.518(12) . ? C119 C120 1.457(11) . ? C119 H11E 0.9700 . ? C119 H11F 0.9700 . ? C120 C121 1.3900 . ? C120 C125 1.3900 . ? C121 C122 1.3900 . ? C121 H121 0.9300 . ? C122 C123 1.3900 . ? C122 H122 0.9300 . ? C123 C124 1.3900 . ? C123 H123 0.9300 . ? C124 C125 1.3900 . ? C124 H124 0.9300 . ? C125 H125 0.9300 . ? C126 C127 1.579(13) . ? C126 H12A 0.9700 . ? C126 H12B 0.9700 . ? C127 O128 1.143(10) . ? C127 O129 1.275(10) . ? O129 Mn3 2.097(6) . ? Mn2 O429 2.056(7) . ? Mn2 O228 2.180(6) . ? Mn2 N215 2.241(5) . ? Mn2 N208 2.261(5) . ? Mn2 N201 2.309(8) . ? Mn2 N218 2.343(7) . ? N201 C216 1.454(12) . ? N201 C202 1.475(13) . ? N201 C209 1.506(13) . ? C202 C203 1.469(11) . ? C202 H20A 0.9700 . ? C202 H20B 0.9700 . ? C203 C204 1.3900 . ? C203 N208 1.3900 . ? C204 C205 1.3900 . ? C204 H204 0.9300 . ? C205 C206 1.3900 . ? C205 H205 0.9300 . ? C206 C207 1.3900 . ? C206 H206 0.9300 . ? C207 N208 1.3900 . ? C207 H207 0.9300 . ? C209 C210 1.435(11) . ? C209 H20C 0.9700 . ? C209 H20D 0.9700 . ? C210 C211 1.3900 . ? C210 N215 1.3900 . ? C211 C212 1.3900 . ? C211 H211 0.9300 . ? C212 C213 1.3900 . ? C212 H212 0.9300 . ? C213 C214 1.3900 . ? C213 H213 0.9300 . ? C214 N215 1.3900 . ? C214 H214 0.9300 . ? C216 C217 1.499(13) . ? C216 H21A 0.9700 . ? C216 H21B 0.9700 . ? C217 N218 1.495(11) . ? C217 H21C 0.9700 . ? C217 H21D 0.9700 . ? N218 C226 1.460(11) . ? N218 C219 1.475(11) . ? C219 C220 1.514(10) . ? C219 H21E 0.9700 . ? C219 H21F 0.9700 . ? C220 C221 1.3900 . ? C220 C225 1.3900 . ? C221 C222 1.3900 . ? C221 H221 0.9300 . ? C222 C223 1.3900 . ? C222 H222 0.9300 . ? C223 C224 1.3900 . ? C223 H223 0.9300 . ? C224 C225 1.3900 . ? C224 H224 0.9300 . ? C225 H225 0.9300 . ? C226 C227 1.501(12) . ? C226 H22A 0.9700 . ? C226 H22B 0.9700 . ? C227 O228 1.238(10) . ? C227 O229 1.251(11) . ? Mn3 O328 2.161(6) . ? Mn3 N315 2.255(5) . ? Mn3 N308 2.272(5) . ? Mn3 N301 2.301(8) . ? Mn3 N318 2.326(7) . ? N301 C309 1.446(12) . ? N301 C302 1.488(12) . ? N301 C316 1.525(12) . ? C302 C303 1.422(11) . ? C302 H30A 0.9700 . ? C302 H30B 0.9700 . ? C303 C304 1.3900 . ? C303 N308 1.3900 . ? C304 C305 1.3900 . ? C304 H304 0.9300 . ? C305 C306 1.3900 . ? C305 H305 0.9300 . ? C306 C307 1.3900 . ? C306 H306 0.9300 . ? C307 N308 1.3900 . ? C307 H307 0.9300 . ? C309 C310 1.489(12) . ? C309 H30C 0.9700 . ? C309 H30D 0.9700 . ? C310 C311 1.3900 . ? C310 N315 1.3900 . ? C311 C312 1.3900 . ? C311 H311 0.9300 . ? C312 C313 1.3900 . ? C312 H312 0.9300 . ? C313 C314 1.3900 . ? C313 H313 0.9300 . ? C314 N315 1.3900 . ? C314 H314 0.9300 . ? C316 C317 1.491(13) . ? C316 H31A 0.9700 . ? C316 H31B 0.9700 . ? C317 N318 1.501(11) . ? C317 H31C 0.9700 . ? C317 H31D 0.9700 . ? N318 C326 1.491(12) . ? N318 C319 1.518(11) . ? C319 C320 1.444(10) . ? C319 H31E 0.9700 . ? C319 H31F 0.9700 . ? C320 C321 1.3900 . ? C320 C325 1.3900 . ? C321 C322 1.3900 . ? C321 H321 0.9300 . ? C322 C323 1.3900 . ? C322 H322 0.9300 . ? C323 C324 1.3900 . ? C323 H323 0.9300 . ? C324 C325 1.3900 . ? C324 H324 0.9300 . ? C325 H325 0.9300 . ? C326 C327 1.499(13) . ? C326 H32A 0.9700 . ? C326 H32B 0.9700 . ? C327 O329 1.231(11) . ? C327 O328 1.343(11) . ? O329 Mn4 2.111(6) . ? Mn4 O428 2.197(6) . ? Mn4 N408 2.263(5) . ? Mn4 N415 2.270(5) . ? Mn4 N401 2.290(8) . ? Mn4 N418 2.382(9) . ? N401 C402 1.381(13) . ? N401 C409 1.472(12) . ? N401 C416 1.540(12) . ? C402 C403 1.525(13) . ? C402 H40A 0.9700 . ? C402 H40B 0.9700 . ? C403 C404 1.3900 . ? C403 N408 1.3900 . ? C404 C405 1.3900 . ? C404 H404 0.9300 . ? C405 C406 1.3900 . ? C405 H405 0.9300 . ? C406 C407 1.3900 . ? C406 H406 0.9300 . ? C407 N408 1.3900 . ? C407 H407 0.9300 . ? C409 C410 1.464(11) . ? C409 H40C 0.9700 . ? C409 H40D 0.9700 . ? C410 C411 1.3900 . ? C410 N415 1.3900 . ? C411 C412 1.3900 . ? C411 H411 0.9300 . ? C412 C413 1.3900 . ? C412 H412 0.9300 . ? C413 C414 1.3900 . ? C413 H413 0.9300 . ? C414 N415 1.3900 . ? C414 H414 0.9300 . ? C416 C417 1.526(15) . ? C416 H41A 0.9700 . ? C416 H41B 0.9700 . ? C417 N418 1.462(12) . ? C417 H41C 0.9700 . ? C417 H41D 0.9700 . ? N418 C426 1.465(12) . ? N418 C419 1.469(12) . ? C419 C420 1.550(11) . ? C419 H41E 0.9700 . ? C419 H41F 0.9700 . ? C420 C421 1.3900 . ? C420 C425 1.3900 . ? C421 C422 1.3900 . ? C421 H421 0.9300 . ? C422 C423 1.3900 . ? C422 H422 0.9300 . ? C423 C424 1.3900 . ? C423 H423 0.9300 . ? C424 C425 1.3900 . ? C424 H424 0.9300 . ? C425 H425 0.9300 . ? C426 C427 1.450(13) . ? C426 H42A 0.9700 . ? C426 H42B 0.9700 . ? C427 O429 1.192(10) . ? C427 O428 1.395(11) . ? N601 C601 1.089(19) . ? C601 C603 1.38(2) . ? C603 H60A 0.9600 . ? C603 H60B 0.9600 . ? C603 H60C 0.9600 . ? N604 C605 1.28(2) . ? C605 C606 1.35(2) . ? C606 H60D 0.9600 . ? C606 H60E 0.9600 . ? C606 H60F 0.9600 . ? 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 O13 Cl1 O12 109.5(9) . . ? O13 Cl1 O14 111.2(9) . . ? O12 Cl1 O14 108.8(9) . . ? O13 Cl1 O11 110.0(7) . . ? O12 Cl1 O11 109.3(7) . . ? O14 Cl1 O11 107.9(9) . . ? O24 Cl2 O22 112.4(10) . . ? O24 Cl2 O21 111.4(10) . . ? O22 Cl2 O21 107.8(10) . . ? O24 Cl2 O23 108.7(11) . . ? O22 Cl2 O23 107.4(11) . . ? O21 Cl2 O23 109.0(11) . . ? O31 Cl3 O32 117.5(11) . . ? O31 Cl3 O33 113.0(9) . . ? O32 Cl3 O33 112.7(9) . . ? O31 Cl3 O34 104.1(11) . . ? O32 Cl3 O34 106.4(11) . . ? O33 Cl3 O34 101.1(11) . . ? O44 Cl4 O42 115.8(10) . . ? O44 Cl4 O43 114.8(6) . . ? O42 Cl4 O43 105.6(8) . . ? O44 Cl4 O41 103.9(10) . . ? O42 Cl4 O41 105.1(10) . . ? O43 Cl4 O41 111.3(8) . . ? O229 Mn1 O128 90.8(3) . . ? O229 Mn1 N115 113.5(3) . . ? O128 Mn1 N115 82.8(2) . . ? O229 Mn1 N108 90.2(2) . . ? O128 Mn1 N108 159.4(2) . . ? N115 Mn1 N108 115.5(2) . . ? O229 Mn1 N101 163.3(3) . . ? O128 Mn1 N101 105.1(3) . . ? N115 Mn1 N101 74.4(3) . . ? N108 Mn1 N101 73.1(3) . . ? O229 Mn1 N118 102.8(3) . . ? O128 Mn1 N118 72.3(2) . . ? N115 Mn1 N118 135.9(2) . . ? N108 Mn1 N118 87.4(2) . . ? N101 Mn1 N118 77.8(3) . . ? C116 N101 C109 113.7(8) . . ? C116 N101 C102 112.5(8) . . ? C109 N101 C102 110.3(8) . . ? C116 N101 Mn1 109.3(6) . . ? C109 N101 Mn1 107.1(6) . . ? C102 N101 Mn1 103.2(6) . . ? C103 C102 N101 114.4(8) . . ? C103 C102 H10A 108.7 . . ? N101 C102 H10A 108.7 . . ? C103 C102 H10B 108.7 . . ? N101 C102 H10B 108.7 . . ? H10A C102 H10B 107.6 . . ? C104 C103 N108 120.0 . . ? C104 C103 C102 124.4(6) . . ? N108 C103 C102 115.5(6) . . ? C103 C104 C105 120.0 . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C106 C105 C104 120.0 . . ? C106 C105 H105 120.0 . . ? C104 C105 H105 120.0 . . ? C107 C106 C105 120.0 . . ? C107 C106 H106 120.0 . . ? C105 C106 H106 120.0 . . ? C106 C107 N108 120.0 . . ? C106 C107 H107 120.0 . . ? N108 C107 H107 120.0 . . ? C107 N108 C103 120.0 . . ? C107 N108 Mn1 125.6(3) . . ? C103 N108 Mn1 114.1(3) . . ? N101 C109 C110 113.5(8) . . ? N101 C109 H10C 108.9 . . ? C110 C109 H10C 108.9 . . ? N101 C109 H10D 108.9 . . ? C110 C109 H10D 108.9 . . ? H10C C109 H10D 107.7 . . ? C111 C110 N115 120.0 . . ? C111 C110 C109 123.6(6) . . ? N115 C110 C109 115.5(6) . . ? C112 C111 C110 120.0 . . ? C112 C111 H111 120.0 . . ? C110 C111 H111 120.0 . . ? C111 C112 C113 120.0 . . ? C111 C112 H112 120.0 . . ? C113 C112 H112 120.0 . . ? C114 C113 C112 120.0 . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? N115 C114 C113 120.0 . . ? N115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C114 N115 C110 120.0 . . ? C114 N115 Mn1 124.2(3) . . ? C110 N115 Mn1 115.7(3) . . ? N101 C116 C117 113.1(8) . . ? N101 C116 H11A 109.0 . . ? C117 C116 H11A 109.0 . . ? N101 C116 H11B 109.0 . . ? C117 C116 H11B 109.0 . . ? H11A C116 H11B 107.8 . . ? N118 C117 C116 108.7(7) . . ? N118 C117 H11C 109.9 . . ? C116 C117 H11C 109.9 . . ? N118 C117 H11D 109.9 . . ? C116 C117 H11D 109.9 . . ? H11C C117 H11D 108.3 . . ? C126 N118 C117 109.1(7) . . ? C126 N118 C119 110.2(8) . . ? C117 N118 C119 110.1(7) . . ? C126 N118 Mn1 106.0(6) . . ? C117 N118 Mn1 102.9(6) . . ? C119 N118 Mn1 118.0(6) . . ? C120 C119 N118 117.6(8) . . ? C120 C119 H11E 107.9 . . ? N118 C119 H11E 107.9 . . ? C120 C119 H11F 107.9 . . ? N118 C119 H11F 107.9 . . ? H11E C119 H11F 107.2 . . ? C121 C120 C125 120.0 . . ? C121 C120 C119 121.5(6) . . ? C125 C120 C119 118.4(6) . . ? C120 C121 C122 120.0 . . ? C120 C121 H121 120.0 . . ? C122 C121 H121 120.0 . . ? C123 C122 C121 120.0 . . ? C123 C122 H122 120.0 . . ? C121 C122 H122 120.0 . . ? C122 C123 C124 120.0 . . ? C122 C123 H123 120.0 . . ? C124 C123 H123 120.0 . . ? C125 C124 C123 120.0 . . ? C125 C124 H124 120.0 . . ? C123 C124 H124 120.0 . . ? C124 C125 C120 120.0 . . ? C124 C125 H125 120.0 . . ? C120 C125 H125 120.0 . . ? N118 C126 C127 109.0(8) . . ? N118 C126 H12A 109.9 . . ? C127 C126 H12A 109.9 . . ? N118 C126 H12B 109.9 . . ? C127 C126 H12B 109.9 . . ? H12A C126 H12B 108.3 . . ? O128 C127 O129 131.7(10) . . ? O128 C127 C126 121.3(9) . . ? O129 C127 C126 106.9(8) . . ? C127 O128 Mn1 119.9(6) . . ? C127 O129 Mn3 128.4(6) . . ? O429 Mn2 O228 102.1(3) . . ? O429 Mn2 N215 105.6(3) . . ? O228 Mn2 N215 82.8(2) . . ? O429 Mn2 N208 86.0(3) . . ? O228 Mn2 N208 169.0(2) . . ? N215 Mn2 N208 102.4(2) . . ? O429 Mn2 N201 158.5(3) . . ? O228 Mn2 N201 99.0(3) . . ? N215 Mn2 N201 73.0(3) . . ? N208 Mn2 N201 73.7(3) . . ? O429 Mn2 N218 111.4(3) . . ? O228 Mn2 N218 72.6(2) . . ? N215 Mn2 N218 138.9(3) . . ? N208 Mn2 N218 97.6(2) . . ? N201 Mn2 N218 78.9(3) . . ? C216 N201 C202 111.5(8) . . ? C216 N201 C209 113.1(8) . . ? C202 N201 C209 111.3(8) . . ? C216 N201 Mn2 107.4(6) . . ? C202 N201 Mn2 109.5(6) . . ? C209 N201 Mn2 103.7(6) . . ? C203 C202 N201 110.6(8) . . ? C203 C202 H20A 109.5 . . ? N201 C202 H20A 109.5 . . ? C203 C202 H20B 109.5 . . ? N201 C202 H20B 109.5 . . ? H20A C202 H20B 108.1 . . ? C204 C203 N208 120.0 . . ? C204 C203 C202 122.3(6) . . ? N208 C203 C202 117.3(6) . . ? C205 C204 C203 120.0 . . ? C205 C204 H204 120.0 . . ? C203 C204 H204 120.0 . . ? C204 C205 C206 120.0 . . ? C204 C205 H205 120.0 . . ? C206 C205 H205 120.0 . . ? C205 C206 C207 120.0 . . ? C205 C206 H206 120.0 . . ? C207 C206 H206 120.0 . . ? C206 C207 N208 120.0 . . ? C206 C207 H207 120.0 . . ? N208 C207 H207 120.0 . . ? C207 N208 C203 120.0 . . ? C207 N208 Mn2 124.8(3) . . ? C203 N208 Mn2 115.1(3) . . ? C210 C209 N201 111.4(8) . . ? C210 C209 H20C 109.3 . . ? N201 C209 H20C 109.3 . . ? C210 C209 H20D 109.3 . . ? N201 C209 H20D 109.3 . . ? H20C C209 H20D 108.0 . . ? C211 C210 N215 120.0 . . ? C211 C210 C209 123.7(6) . . ? N215 C210 C209 116.2(6) . . ? C210 C211 C212 120.0 . . ? C210 C211 H211 120.0 . . ? C212 C211 H211 120.0 . . ? C213 C212 C211 120.0 . . ? C213 C212 H212 120.0 . . ? C211 C212 H212 120.0 . . ? C212 C213 C214 120.0 . . ? C212 C213 H213 120.0 . . ? C214 C213 H213 120.0 . . ? N215 C214 C213 120.0 . . ? N215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C214 N215 C210 120.0 . . ? C214 N215 Mn2 125.5(3) . . ? C210 N215 Mn2 114.2(3) . . ? N201 C216 C217 114.2(8) . . ? N201 C216 H21A 108.7 . . ? C217 C216 H21A 108.7 . . ? N201 C216 H21B 108.7 . . ? C217 C216 H21B 108.7 . . ? H21A C216 H21B 107.6 . . ? N218 C217 C216 111.7(8) . . ? N218 C217 H21C 109.3 . . ? C216 C217 H21C 109.3 . . ? N218 C217 H21D 109.3 . . ? C216 C217 H21D 109.3 . . ? H21C C217 H21D 108.0 . . ? C226 N218 C219 111.9(7) . . ? C226 N218 C217 109.5(7) . . ? C219 N218 C217 113.3(7) . . ? C226 N218 Mn2 105.2(5) . . ? C219 N218 Mn2 112.5(5) . . ? C217 N218 Mn2 103.9(5) . . ? N218 C219 C220 114.7(7) . . ? N218 C219 H21E 108.6 . . ? C220 C219 H21E 108.6 . . ? N218 C219 H21F 108.6 . . ? C220 C219 H21F 108.6 . . ? H21E C219 H21F 107.6 . . ? C221 C220 C225 120.0 . . ? C221 C220 C219 120.5(6) . . ? C225 C220 C219 119.5(6) . . ? C220 C221 C222 120.0 . . ? C220 C221 H221 120.0 . . ? C222 C221 H221 120.0 . . ? C223 C222 C221 120.0 . . ? C223 C222 H222 120.0 . . ? C221 C222 H222 120.0 . . ? C222 C223 C224 120.0 . . ? C222 C223 H223 120.0 . . ? C224 C223 H223 120.0 . . ? C223 C224 C225 120.0 . . ? C223 C224 H224 120.0 . . ? C225 C224 H224 120.0 . . ? C224 C225 C220 120.0 . . ? C224 C225 H225 120.0 . . ? C220 C225 H225 120.0 . . ? N218 C226 C227 111.0(8) . . ? N218 C226 H22A 109.4 . . ? C227 C226 H22A 109.4 . . ? N218 C226 H22B 109.4 . . ? C227 C226 H22B 109.4 . . ? H22A C226 H22B 108.0 . . ? O228 C227 O229 122.1(9) . . ? O228 C227 C226 119.6(9) . . ? O229 C227 C226 118.2(9) . . ? C227 O228 Mn2 117.4(6) . . ? C227 O229 Mn1 110.7(6) . . ? O129 Mn3 O328 101.2(3) . . ? O129 Mn3 N315 105.8(3) . . ? O328 Mn3 N315 83.1(2) . . ? O129 Mn3 N308 87.1(2) . . ? O328 Mn3 N308 169.2(2) . . ? N315 Mn3 N308 101.3(2) . . ? O129 Mn3 N301 159.5(3) . . ? O328 Mn3 N301 98.9(3) . . ? N315 Mn3 N301 72.9(3) . . ? N308 Mn3 N301 73.4(3) . . ? O129 Mn3 N318 110.3(3) . . ? O328 Mn3 N318 73.0(2) . . ? N315 Mn3 N318 139.7(2) . . ? N308 Mn3 N318 97.8(2) . . ? N301 Mn3 N318 79.2(3) . . ? C309 N301 C302 109.8(8) . . ? C309 N301 C316 113.4(8) . . ? C302 N301 C316 110.3(8) . . ? C309 N301 Mn3 107.5(6) . . ? C302 N301 Mn3 108.3(6) . . ? C316 N301 Mn3 107.3(5) . . ? C303 C302 N301 114.3(8) . . ? C303 C302 H30A 108.7 . . ? N301 C302 H30A 108.7 . . ? C303 C302 H30B 108.7 . . ? N301 C302 H30B 108.7 . . ? H30A C302 H30B 107.6 . . ? C304 C303 N308 120.0 . . ? C304 C303 C302 124.4(6) . . ? N308 C303 C302 115.5(6) . . ? C305 C304 C303 120.0 . . ? C305 C304 H304 120.0 . . ? C303 C304 H304 120.0 . . ? C304 C305 C306 120.0 . . ? C304 C305 H305 120.0 . . ? C306 C305 H305 120.0 . . ? C307 C306 C305 120.0 . . ? C307 C306 H306 120.0 . . ? C305 C306 H306 120.0 . . ? N308 C307 C306 120.0 . . ? N308 C307 H307 120.0 . . ? C306 C307 H307 120.0 . . ? C307 N308 C303 120.0 . . ? C307 N308 Mn3 123.5(3) . . ? C303 N308 Mn3 116.3(3) . . ? N301 C309 C310 110.1(8) . . ? N301 C309 H30C 109.6 . . ? C310 C309 H30C 109.6 . . ? N301 C309 H30D 109.6 . . ? C310 C309 H30D 109.6 . . ? H30C C309 H30D 108.2 . . ? C311 C310 N315 120.0 . . ? C311 C310 C309 123.2(6) . . ? N315 C310 C309 116.8(6) . . ? C312 C311 C310 120.0 . . ? C312 C311 H311 120.0 . . ? C310 C311 H311 120.0 . . ? C311 C312 C313 120.0 . . ? C311 C312 H312 120.0 . . ? C313 C312 H312 120.0 . . ? C312 C313 C314 120.0 . . ? C312 C313 H313 120.0 . . ? C314 C313 H313 120.0 . . ? N315 C314 C313 120.0 . . ? N315 C314 H314 120.0 . . ? C313 C314 H314 120.0 . . ? C314 N315 C310 120.0 . . ? C314 N315 Mn3 126.1(3) . . ? C310 N315 Mn3 113.8(3) . . ? C317 C316 N301 111.7(8) . . ? C317 C316 H31A 109.3 . . ? N301 C316 H31A 109.3 . . ? C317 C316 H31B 109.3 . . ? N301 C316 H31B 109.3 . . ? H31A C316 H31B 107.9 . . ? C316 C317 N318 111.6(8) . . ? C316 C317 H31C 109.3 . . ? N318 C317 H31C 109.3 . . ? C316 C317 H31D 109.3 . . ? N318 C317 H31D 109.3 . . ? H31C C317 H31D 108.0 . . ? C326 N318 C317 108.7(7) . . ? C326 N318 C319 109.4(7) . . ? C317 N318 C319 112.0(7) . . ? C326 N318 Mn3 107.1(5) . . ? C317 N318 Mn3 104.6(5) . . ? C319 N318 Mn3 114.8(5) . . ? C320 C319 N318 118.3(7) . . ? C320 C319 H31E 107.7 . . ? N318 C319 H31E 107.7 . . ? C320 C319 H31F 107.7 . . ? N318 C319 H31F 107.7 . . ? H31E C319 H31F 107.1 . . ? C321 C320 C325 120.0 . . ? C321 C320 C319 118.3(6) . . ? C325 C320 C319 121.7(6) . . ? C322 C321 C320 120.0 . . ? C322 C321 H321 120.0 . . ? C320 C321 H321 120.0 . . ? C321 C322 C323 120.0 . . ? C321 C322 H322 120.0 . . ? C323 C322 H322 120.0 . . ? C324 C323 C322 120.0 . . ? C324 C323 H323 120.0 . . ? C322 C323 H323 120.0 . . ? C323 C324 C325 120.0 . . ? C323 C324 H324 120.0 . . ? C325 C324 H324 120.0 . . ? C324 C325 C320 120.0 . . ? C324 C325 H325 120.0 . . ? C320 C325 H325 120.0 . . ? N318 C326 C327 109.8(8) . . ? N318 C326 H32A 109.7 . . ? C327 C326 H32A 109.7 . . ? N318 C326 H32B 109.7 . . ? C327 C326 H32B 109.7 . . ? H32A C326 H32B 108.2 . . ? O329 C327 O328 122.6(8) . . ? O329 C327 C326 120.5(9) . . ? O328 C327 C326 116.9(9) . . ? C327 O328 Mn3 118.5(6) . . ? C327 O329 Mn4 111.9(6) . . ? O329 Mn4 O428 90.7(2) . . ? O329 Mn4 N408 90.1(2) . . ? O428 Mn4 N408 158.7(2) . . ? O329 Mn4 N415 114.1(3) . . ? O428 Mn4 N415 83.1(2) . . ? N408 Mn4 N415 115.8(2) . . ? O329 Mn4 N401 161.4(3) . . ? O428 Mn4 N401 107.6(3) . . ? N408 Mn4 N401 71.5(3) . . ? N415 Mn4 N401 72.9(3) . . ? O329 Mn4 N418 103.2(3) . . ? O428 Mn4 N418 72.6(3) . . ? N408 Mn4 N418 86.5(2) . . ? N415 Mn4 N418 135.5(3) . . ? N401 Mn4 N418 79.5(3) . . ? C402 N401 C409 110.4(9) . . ? C402 N401 C416 110.0(9) . . ? C409 N401 C416 110.5(8) . . ? C402 N401 Mn4 111.1(7) . . ? C409 N401 Mn4 109.2(6) . . ? C416 N401 Mn4 105.5(6) . . ? N401 C402 C403 113.3(9) . . ? N401 C402 H40A 108.9 . . ? C403 C402 H40A 108.9 . . ? N401 C402 H40B 108.9 . . ? C403 C402 H40B 108.9 . . ? H40A C402 H40B 107.7 . . ? C404 C403 N408 120.0 . . ? C404 C403 C402 126.9(6) . . ? N408 C403 C402 113.1(6) . . ? C403 C404 C405 120.0 . . ? C403 C404 H404 120.0 . . ? C405 C404 H404 120.0 . . ? C406 C405 C404 120.0 . . ? C406 C405 H405 120.0 . . ? C404 C405 H405 120.0 . . ? C405 C406 C407 120.0 . . ? C405 C406 H406 120.0 . . ? C407 C406 H406 120.0 . . ? N408 C407 C406 120.0 . . ? N408 C407 H407 120.0 . . ? C406 C407 H407 120.0 . . ? C407 N408 C403 120.0 . . ? C407 N408 Mn4 123.2(3) . . ? C403 N408 Mn4 116.5(3) . . ? C410 C409 N401 112.3(8) . . ? C410 C409 H40C 109.2 . . ? N401 C409 H40C 109.2 . . ? C410 C409 H40D 109.2 . . ? N401 C409 H40D 109.2 . . ? H40C C409 H40D 107.9 . . ? C411 C410 N415 120.0 . . ? C411 C410 C409 124.3(6) . . ? N415 C410 C409 115.5(6) . . ? C410 C411 C412 120.0 . . ? C410 C411 H411 120.0 . . ? C412 C411 H411 120.0 . . ? C411 C412 C413 120.0 . . ? C411 C412 H412 120.0 . . ? C413 C412 H412 120.0 . . ? C412 C413 C414 120.0 . . ? C412 C413 H413 120.0 . . ? C414 C413 H413 120.0 . . ? N415 C414 C413 120.0 . . ? N415 C414 H414 120.0 . . ? C413 C414 H414 120.0 . . ? C414 N415 C410 120.0 . . ? C414 N415 Mn4 123.9(3) . . ? C410 N415 Mn4 116.0(3) . . ? C417 C416 N401 111.7(8) . . ? C417 C416 H41A 109.3 . . ? N401 C416 H41A 109.3 . . ? C417 C416 H41B 109.3 . . ? N401 C416 H41B 109.3 . . ? H41A C416 H41B 107.9 . . ? N418 C417 C416 108.8(8) . . ? N418 C417 H41C 109.9 . . ? C416 C417 H41C 109.9 . . ? N418 C417 H41D 109.9 . . ? C416 C417 H41D 109.9 . . ? H41C C417 H41D 108.3 . . ? C417 N418 C426 108.7(8) . . ? C417 N418 C419 113.0(7) . . ? C426 N418 C419 108.8(8) . . ? C417 N418 Mn4 101.0(6) . . ? C426 N418 Mn4 105.1(6) . . ? C419 N418 Mn4 119.3(6) . . ? N418 C419 C420 116.0(8) . . ? N418 C419 H41E 108.3 . . ? C420 C419 H41E 108.3 . . ? N418 C419 H41F 108.3 . . ? C420 C419 H41F 108.3 . . ? H41E C419 H41F 107.4 . . ? C421 C420 C425 120.0 . . ? C421 C420 C419 118.7(6) . . ? C425 C420 C419 121.2(6) . . ? C422 C421 C420 120.0 . . ? C422 C421 H421 120.0 . . ? C420 C421 H421 120.0 . . ? C421 C422 C423 120.0 . . ? C421 C422 H422 120.0 . . ? C423 C422 H422 120.0 . . ? C424 C423 C422 120.0 . . ? C424 C423 H423 120.0 . . ? C422 C423 H423 120.0 . . ? C423 C424 C425 120.0 . . ? C423 C424 H424 120.0 . . ? C425 C424 H424 120.0 . . ? C424 C425 C420 120.0 . . ? C424 C425 H425 120.0 . . ? C420 C425 H425 120.0 . . ? C427 C426 N418 119.7(9) . . ? C427 C426 H42A 107.4 . . ? N418 C426 H42A 107.4 . . ? C427 C426 H42B 107.4 . . ? N418 C426 H42B 107.4 . . ? H42A C426 H42B 106.9 . . ? O429 C427 O428 117.4(9) . . ? O429 C427 C426 128.1(10) . . ? O428 C427 C426 112.7(9) . . ? C427 O428 Mn4 117.0(5) . . ? C427 O429 Mn2 140.3(7) . . ? N601 C601 C603 175(2) . . ? C601 C603 H60A 109.5 . . ? C601 C603 H60B 109.5 . . ? H60A C603 H60B 109.5 . . ? C601 C603 H60C 109.5 . . ? H60A C603 H60C 109.5 . . ? H60B C603 H60C 109.5 . . ? N604 C605 C606 171.6(18) . . ? C605 C606 H60D 109.5 . . ? C605 C606 H60E 109.5 . . ? H60D C606 H60E 109.5 . . ? C605 C606 H60F 109.5 . . ? H60D C606 H60F 109.5 . . ? H60E C606 H60F 109.5 . . ? 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 O229 Mn1 N101 C116 88.1(12) . . . . ? O128 Mn1 N101 C116 -73.4(7) . . . . ? N115 Mn1 N101 C116 -151.2(7) . . . . ? N108 Mn1 N101 C116 85.2(7) . . . . ? N118 Mn1 N101 C116 -5.7(6) . . . . ? O229 Mn1 N101 C109 -148.3(10) . . . . ? O128 Mn1 N101 C109 50.2(7) . . . . ? N115 Mn1 N101 C109 -27.6(6) . . . . ? N108 Mn1 N101 C109 -151.2(7) . . . . ? N118 Mn1 N101 C109 117.9(7) . . . . ? O229 Mn1 N101 C102 -31.8(13) . . . . ? O128 Mn1 N101 C102 166.7(6) . . . . ? N115 Mn1 N101 C102 88.9(6) . . . . ? N108 Mn1 N101 C102 -34.7(6) . . . . ? N118 Mn1 N101 C102 -125.7(6) . . . . ? C116 N101 C102 C103 -70.2(11) . . . . ? C109 N101 C102 C103 161.7(8) . . . . ? Mn1 N101 C102 C103 47.5(9) . . . . ? N101 C102 C103 C104 151.1(6) . . . . ? N101 C102 C103 N108 -31.7(10) . . . . ? N108 C103 C104 C105 0.0 . . . . ? C102 C103 C104 C105 177.1(8) . . . . ? C103 C104 C105 C106 0.0 . . . . ? C104 C105 C106 C107 0.0 . . . . ? C105 C106 C107 N108 0.0 . . . . ? C106 C107 N108 C103 0.0 . . . . ? C106 C107 N108 Mn1 -173.4(5) . . . . ? C104 C103 N108 C107 0.0 . . . . ? C102 C103 N108 C107 -177.3(7) . . . . ? C104 C103 N108 Mn1 174.1(4) . . . . ? C102 C103 N108 Mn1 -3.3(7) . . . . ? O229 Mn1 N108 C107 17.0(4) . . . . ? O128 Mn1 N108 C107 -75.8(8) . . . . ? N115 Mn1 N108 C107 133.4(4) . . . . ? N101 Mn1 N108 C107 -163.8(4) . . . . ? N118 Mn1 N108 C107 -85.8(4) . . . . ? O229 Mn1 N108 C103 -156.7(4) . . . . ? O128 Mn1 N108 C103 110.5(7) . . . . ? N115 Mn1 N108 C103 -40.3(4) . . . . ? N101 Mn1 N108 C103 22.5(3) . . . . ? N118 Mn1 N108 C103 100.5(4) . . . . ? C116 N101 C109 C110 162.1(8) . . . . ? C102 N101 C109 C110 -70.4(11) . . . . ? Mn1 N101 C109 C110 41.2(10) . . . . ? N101 C109 C110 C111 157.8(6) . . . . ? N101 C109 C110 N115 -33.5(11) . . . . ? N115 C110 C111 C112 0.0 . . . . ? C109 C110 C111 C112 168.3(8) . . . . ? C110 C111 C112 C113 0.0 . . . . ? C111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 N115 0.0 . . . . ? C113 C114 N115 C110 0.0 . . . . ? C113 C114 N115 Mn1 -175.5(4) . . . . ? C111 C110 N115 C114 0.0 . . . . ? C109 C110 N115 C114 -169.2(7) . . . . ? C111 C110 N115 Mn1 175.9(4) . . . . ? C109 C110 N115 Mn1 6.7(7) . . . . ? O229 Mn1 N115 C114 -8.0(4) . . . . ? O128 Mn1 N115 C114 79.7(4) . . . . ? N108 Mn1 N115 C114 -110.2(4) . . . . ? N101 Mn1 N115 C114 -172.3(4) . . . . ? N118 Mn1 N115 C114 134.9(4) . . . . ? O229 Mn1 N115 C110 176.3(3) . . . . ? O128 Mn1 N115 C110 -96.0(4) . . . . ? N108 Mn1 N115 C110 74.0(4) . . . . ? N101 Mn1 N115 C110 12.0(4) . . . . ? N118 Mn1 N115 C110 -40.8(5) . . . . ? C109 N101 C116 C117 -84.3(10) . . . . ? C102 N101 C116 C117 149.3(8) . . . . ? Mn1 N101 C116 C117 35.3(10) . . . . ? N101 C116 C117 N118 -61.1(10) . . . . ? C116 C117 N118 C126 161.5(8) . . . . ? C116 C117 N118 C119 -77.5(10) . . . . ? C116 C117 N118 Mn1 49.2(7) . . . . ? O229 Mn1 N118 C126 58.3(6) . . . . ? O128 Mn1 N118 C126 -28.4(5) . . . . ? N115 Mn1 N118 C126 -87.1(6) . . . . ? N108 Mn1 N118 C126 147.9(6) . . . . ? N101 Mn1 N118 C126 -138.8(6) . . . . ? O229 Mn1 N118 C117 172.8(5) . . . . ? O128 Mn1 N118 C117 86.1(5) . . . . ? N115 Mn1 N118 C117 27.4(7) . . . . ? N108 Mn1 N118 C117 -97.6(5) . . . . ? N101 Mn1 N118 C117 -24.3(5) . . . . ? O229 Mn1 N118 C119 -65.7(7) . . . . ? O128 Mn1 N118 C119 -152.4(7) . . . . ? N115 Mn1 N118 C119 148.9(6) . . . . ? N108 Mn1 N118 C119 23.9(7) . . . . ? N101 Mn1 N118 C119 97.2(7) . . . . ? C126 N118 C119 C120 60.2(11) . . . . ? C117 N118 C119 C120 -60.1(11) . . . . ? Mn1 N118 C119 C120 -177.8(6) . . . . ? N118 C119 C120 C121 -87.9(9) . . . . ? N118 C119 C120 C125 89.5(9) . . . . ? C125 C120 C121 C122 0.0 . . . . ? C119 C120 C121 C122 177.4(8) . . . . ? C120 C121 C122 C123 0.0 . . . . ? C121 C122 C123 C124 0.0 . . . . ? C122 C123 C124 C125 0.0 . . . . ? C123 C124 C125 C120 0.0 . . . . ? C121 C120 C125 C124 0.0 . . . . ? C119 C120 C125 C124 -177.5(7) . . . . ? C117 N118 C126 C127 -80.9(9) . . . . ? C119 N118 C126 C127 158.2(8) . . . . ? Mn1 N118 C126 C127 29.4(8) . . . . ? N118 C126 C127 O128 -12.0(13) . . . . ? N118 C126 C127 O129 172.0(8) . . . . ? O129 C127 O128 Mn1 158.0(8) . . . . ? C126 C127 O128 Mn1 -16.9(12) . . . . ? O229 Mn1 O128 C127 -77.3(8) . . . . ? N115 Mn1 O128 C127 169.0(8) . . . . ? N108 Mn1 O128 C127 15.4(12) . . . . ? N101 Mn1 O128 C127 97.5(8) . . . . ? N118 Mn1 O128 C127 25.9(7) . . . . ? O128 C127 O129 Mn3 9.7(16) . . . . ? C126 C127 O129 Mn3 -174.9(6) . . . . ? O429 Mn2 N201 C216 113.9(9) . . . . ? O228 Mn2 N201 C216 -77.3(6) . . . . ? N215 Mn2 N201 C216 -156.9(7) . . . . ? N208 Mn2 N201 C216 94.2(6) . . . . ? N218 Mn2 N201 C216 -7.2(6) . . . . ? O429 Mn2 N201 C202 -7.4(12) . . . . ? O228 Mn2 N201 C202 161.4(6) . . . . ? N215 Mn2 N201 C202 81.9(6) . . . . ? N208 Mn2 N201 C202 -27.0(6) . . . . ? N218 Mn2 N201 C202 -128.4(7) . . . . ? O429 Mn2 N201 C209 -126.2(9) . . . . ? O228 Mn2 N201 C209 42.6(6) . . . . ? N215 Mn2 N201 C209 -36.9(6) . . . . ? N208 Mn2 N201 C209 -145.9(6) . . . . ? N218 Mn2 N201 C209 112.8(6) . . . . ? C216 N201 C202 C203 -78.0(9) . . . . ? C209 N201 C202 C203 154.7(8) . . . . ? Mn2 N201 C202 C203 40.7(9) . . . . ? N201 C202 C203 C204 152.3(6) . . . . ? N201 C202 C203 N208 -34.7(10) . . . . ? N208 C203 C204 C205 0.0 . . . . ? C202 C203 C204 C205 172.8(8) . . . . ? C203 C204 C205 C206 0.0 . . . . ? C204 C205 C206 C207 0.0 . . . . ? C205 C206 C207 N208 0.0 . . . . ? C206 C207 N208 C203 0.0 . . . . ? C206 C207 N208 Mn2 176.4(5) . . . . ? C204 C203 N208 C207 0.0 . . . . ? C202 C203 N208 C207 -173.2(8) . . . . ? C204 C203 N208 Mn2 -176.8(4) . . . . ? C202 C203 N208 Mn2 10.1(7) . . . . ? O429 Mn2 N208 C207 20.2(4) . . . . ? O228 Mn2 N208 C207 -117.2(13) . . . . ? N215 Mn2 N208 C207 125.3(4) . . . . ? N201 Mn2 N208 C207 -166.9(5) . . . . ? N218 Mn2 N208 C207 -90.8(4) . . . . ? O429 Mn2 N208 C203 -163.2(4) . . . . ? O228 Mn2 N208 C203 59.4(14) . . . . ? N215 Mn2 N208 C203 -58.1(4) . . . . ? N201 Mn2 N208 C203 9.7(4) . . . . ? N218 Mn2 N208 C203 85.7(4) . . . . ? C216 N201 C209 C210 164.9(8) . . . . ? C202 N201 C209 C210 -68.6(11) . . . . ? Mn2 N201 C209 C210 48.9(9) . . . . ? N201 C209 C210 C211 149.8(6) . . . . ? N201 C209 C210 N215 -32.5(11) . . . . ? N215 C210 C211 C212 0.0 . . . . ? C209 C210 C211 C212 177.7(9) . . . . ? C210 C211 C212 C213 0.0 . . . . ? C211 C212 C213 C214 0.0 . . . . ? C212 C213 C214 N215 0.0 . . . . ? C213 C214 N215 C210 0.0 . . . . ? C213 C214 N215 Mn2 -174.0(5) . . . . ? C211 C210 N215 C214 0.0 . . . . ? C209 C210 N215 C214 -177.8(8) . . . . ? C211 C210 N215 Mn2 174.7(4) . . . . ? C209 C210 N215 Mn2 -3.2(7) . . . . ? O429 Mn2 N215 C214 -4.6(5) . . . . ? O228 Mn2 N215 C214 96.0(4) . . . . ? N208 Mn2 N215 C214 -93.8(4) . . . . ? N201 Mn2 N215 C214 -162.2(5) . . . . ? N218 Mn2 N215 C214 148.9(4) . . . . ? O429 Mn2 N215 C210 -178.9(4) . . . . ? O228 Mn2 N215 C210 -78.3(4) . . . . ? N208 Mn2 N215 C210 91.9(4) . . . . ? N201 Mn2 N215 C210 23.5(4) . . . . ? N218 Mn2 N215 C210 -25.4(5) . . . . ? C202 N201 C216 C217 155.1(8) . . . . ? C209 N201 C216 C217 -78.6(11) . . . . ? Mn2 N201 C216 C217 35.2(10) . . . . ? N201 C216 C217 N218 -58.0(11) . . . . ? C216 C217 N218 C226 157.0(7) . . . . ? C216 C217 N218 C219 -77.2(9) . . . . ? C216 C217 N218 Mn2 45.2(8) . . . . ? O429 Mn2 N218 C226 64.8(6) . . . . ? O228 Mn2 N218 C226 -31.6(5) . . . . ? N215 Mn2 N218 C226 -87.7(6) . . . . ? N208 Mn2 N218 C226 153.5(5) . . . . ? N201 Mn2 N218 C226 -134.9(6) . . . . ? O429 Mn2 N218 C219 -57.3(7) . . . . ? O228 Mn2 N218 C219 -153.7(6) . . . . ? N215 Mn2 N218 C219 150.3(6) . . . . ? N208 Mn2 N218 C219 31.4(6) . . . . ? N201 Mn2 N218 C219 103.1(6) . . . . ? O429 Mn2 N218 C217 179.8(5) . . . . ? O228 Mn2 N218 C217 83.4(5) . . . . ? N215 Mn2 N218 C217 27.3(7) . . . . ? N208 Mn2 N218 C217 -91.6(5) . . . . ? N201 Mn2 N218 C217 -19.9(5) . . . . ? C226 N218 C219 C220 55.7(10) . . . . ? C217 N218 C219 C220 -68.7(10) . . . . ? Mn2 N218 C219 C220 173.8(6) . . . . ? N218 C219 C220 C221 -91.4(8) . . . . ? N218 C219 C220 C225 89.2(8) . . . . ? C225 C220 C221 C222 0.0 . . . . ? C219 C220 C221 C222 -179.3(7) . . . . ? C220 C221 C222 C223 0.0 . . . . ? C221 C222 C223 C224 0.0 . . . . ? C222 C223 C224 C225 0.0 . . . . ? C223 C224 C225 C220 0.0 . . . . ? C221 C220 C225 C224 0.0 . . . . ? C219 C220 C225 C224 179.3(7) . . . . ? C219 N218 C226 C227 158.6(7) . . . . ? C217 N218 C226 C227 -74.9(9) . . . . ? Mn2 N218 C226 C227 36.2(8) . . . . ? N218 C226 C227 O228 -19.3(12) . . . . ? N218 C226 C227 O229 157.6(8) . . . . ? O229 C227 O228 Mn2 171.1(7) . . . . ? C226 C227 O228 Mn2 -12.0(11) . . . . ? O429 Mn2 O228 C227 -84.0(7) . . . . ? N215 Mn2 O228 C227 171.6(7) . . . . ? N208 Mn2 O228 C227 52.4(16) . . . . ? N201 Mn2 O228 C227 100.2(7) . . . . ? N218 Mn2 O228 C227 24.9(6) . . . . ? O228 C227 O229 Mn1 3.3(11) . . . . ? C226 C227 O229 Mn1 -173.5(6) . . . . ? O128 Mn1 O229 C227 -130.6(6) . . . . ? N115 Mn1 O229 C227 -48.1(7) . . . . ? N108 Mn1 O229 C227 70.0(6) . . . . ? N101 Mn1 O229 C227 67.2(12) . . . . ? N118 Mn1 O229 C227 157.4(6) . . . . ? C127 O129 Mn3 O328 -44.9(8) . . . . ? C127 O129 Mn3 N315 -130.8(7) . . . . ? C127 O129 Mn3 N308 128.3(8) . . . . ? C127 O129 Mn3 N301 145.9(9) . . . . ? C127 O129 Mn3 N318 31.0(8) . . . . ? O129 Mn3 N301 C309 125.2(9) . . . . ? O328 Mn3 N301 C309 -44.1(7) . . . . ? N315 Mn3 N301 C309 35.8(6) . . . . ? N308 Mn3 N301 C309 143.6(7) . . . . ? N318 Mn3 N301 C309 -114.7(7) . . . . ? O129 Mn3 N301 C302 6.6(12) . . . . ? O328 Mn3 N301 C302 -162.7(6) . . . . ? N315 Mn3 N301 C302 -82.8(6) . . . . ? N308 Mn3 N301 C302 25.0(6) . . . . ? N318 Mn3 N301 C302 126.7(6) . . . . ? O129 Mn3 N301 C316 -112.5(9) . . . . ? O328 Mn3 N301 C316 78.2(6) . . . . ? N315 Mn3 N301 C316 158.1(6) . . . . ? N308 Mn3 N301 C316 -94.0(6) . . . . ? N318 Mn3 N301 C316 7.6(6) . . . . ? C309 N301 C302 C303 -156.4(9) . . . . ? C316 N301 C302 C303 77.8(10) . . . . ? Mn3 N301 C302 C303 -39.3(10) . . . . ? N301 C302 C303 C304 -151.1(7) . . . . ? N301 C302 C303 N308 32.4(11) . . . . ? N308 C303 C304 C305 0.0 . . . . ? C302 C303 C304 C305 -176.3(8) . . . . ? C303 C304 C305 C306 0.0 . . . . ? C304 C305 C306 C307 0.0 . . . . ? C305 C306 C307 N308 0.0 . . . . ? C306 C307 N308 C303 0.0 . . . . ? C306 C307 N308 Mn3 -174.9(4) . . . . ? C304 C303 N308 C307 0.0 . . . . ? C302 C303 N308 C307 176.6(8) . . . . ? C304 C303 N308 Mn3 175.3(4) . . . . ? C302 C303 N308 Mn3 -8.1(7) . . . . ? O129 Mn3 N308 C307 -21.5(4) . . . . ? O328 Mn3 N308 C307 119.6(13) . . . . ? N315 Mn3 N308 C307 -127.1(4) . . . . ? N301 Mn3 N308 C307 164.8(4) . . . . ? N318 Mn3 N308 C307 88.6(4) . . . . ? O129 Mn3 N308 C303 163.4(4) . . . . ? O328 Mn3 N308 C303 -55.5(14) . . . . ? N315 Mn3 N308 C303 57.8(4) . . . . ? N301 Mn3 N308 C303 -10.3(4) . . . . ? N318 Mn3 N308 C303 -86.5(4) . . . . ? C302 N301 C309 C310 71.2(10) . . . . ? C316 N301 C309 C310 -164.8(8) . . . . ? Mn3 N301 C309 C310 -46.4(9) . . . . ? N301 C309 C310 C311 -149.5(6) . . . . ? N301 C309 C310 N315 31.2(10) . . . . ? N315 C310 C311 C312 0.0 . . . . ? C309 C310 C311 C312 -179.3(8) . . . . ? C310 C311 C312 C313 0.0 . . . . ? C311 C312 C313 C314 0.0 . . . . ? C312 C313 C314 N315 0.0 . . . . ? C313 C314 N315 C310 0.0 . . . . ? C313 C314 N315 Mn3 177.6(5) . . . . ? C311 C310 N315 C314 0.0 . . . . ? C309 C310 N315 C314 179.3(7) . . . . ? C311 C310 N315 Mn3 -177.9(4) . . . . ? C309 C310 N315 Mn3 1.4(7) . . . . ? O129 Mn3 N315 C314 3.3(4) . . . . ? O328 Mn3 N315 C314 -96.4(4) . . . . ? N308 Mn3 N315 C314 93.5(4) . . . . ? N301 Mn3 N315 C314 162.0(4) . . . . ? N318 Mn3 N315 C314 -149.7(4) . . . . ? O129 Mn3 N315 C310 -178.9(3) . . . . ? O328 Mn3 N315 C310 81.4(3) . . . . ? N308 Mn3 N315 C310 -88.7(3) . . . . ? N301 Mn3 N315 C310 -20.2(3) . . . . ? N318 Mn3 N315 C310 28.1(5) . . . . ? C309 N301 C316 C317 82.6(10) . . . . ? C302 N301 C316 C317 -153.7(8) . . . . ? Mn3 N301 C316 C317 -35.9(9) . . . . ? N301 C316 C317 N318 58.8(11) . . . . ? C316 C317 N318 C326 -161.4(8) . . . . ? C316 C317 N318 C319 77.7(10) . . . . ? C316 C317 N318 Mn3 -47.2(9) . . . . ? O129 Mn3 N318 C326 -63.5(6) . . . . ? O328 Mn3 N318 C326 32.5(5) . . . . ? N315 Mn3 N318 C326 88.8(6) . . . . ? N308 Mn3 N318 C326 -153.3(5) . . . . ? N301 Mn3 N318 C326 135.4(6) . . . . ? O129 Mn3 N318 C317 -178.7(5) . . . . ? O328 Mn3 N318 C317 -82.8(6) . . . . ? N315 Mn3 N318 C317 -26.5(7) . . . . ? N308 Mn3 N318 C317 91.4(6) . . . . ? N301 Mn3 N318 C317 20.1(6) . . . . ? O129 Mn3 N318 C319 58.1(6) . . . . ? O328 Mn3 N318 C319 154.1(6) . . . . ? N315 Mn3 N318 C319 -149.6(5) . . . . ? N308 Mn3 N318 C319 -31.7(6) . . . . ? N301 Mn3 N318 C319 -103.0(6) . . . . ? C326 N318 C319 C320 -56.9(10) . . . . ? C317 N318 C319 C320 63.7(10) . . . . ? Mn3 N318 C319 C320 -177.2(6) . . . . ? N318 C319 C320 C321 93.9(8) . . . . ? N318 C319 C320 C325 -86.2(8) . . . . ? C325 C320 C321 C322 0.0 . . . . ? C319 C320 C321 C322 179.8(6) . . . . ? C320 C321 C322 C323 0.0 . . . . ? C321 C322 C323 C324 0.0 . . . . ? C322 C323 C324 C325 0.0 . . . . ? C323 C324 C325 C320 0.0 . . . . ? C321 C320 C325 C324 0.0 . . . . ? C319 C320 C325 C324 -179.8(7) . . . . ? C317 N318 C326 C327 73.6(10) . . . . ? C319 N318 C326 C327 -163.9(8) . . . . ? Mn3 N318 C326 C327 -38.9(9) . . . . ? N318 C326 C327 O329 -158.9(9) . . . . ? N318 C326 C327 O328 23.4(12) . . . . ? O329 C327 O328 Mn3 -170.4(7) . . . . ? C326 C327 O328 Mn3 7.2(11) . . . . ? O129 Mn3 O328 C327 85.6(7) . . . . ? N315 Mn3 O328 C327 -169.6(6) . . . . ? N308 Mn3 O328 C327 -54.7(16) . . . . ? N301 Mn3 O328 C327 -98.2(6) . . . . ? N318 Mn3 O328 C327 -22.4(6) . . . . ? O328 C327 O329 Mn4 -3.9(12) . . . . ? C326 C327 O329 Mn4 178.6(7) . . . . ? C327 O329 Mn4 O428 130.0(7) . . . . ? C327 O329 Mn4 N408 -71.3(7) . . . . ? C327 O329 Mn4 N415 47.2(7) . . . . ? C327 O329 Mn4 N401 -61.3(12) . . . . ? C327 O329 Mn4 N418 -157.7(7) . . . . ? O329 Mn4 N401 C402 22.6(14) . . . . ? O428 Mn4 N401 C402 -169.3(7) . . . . ? N408 Mn4 N401 C402 33.1(7) . . . . ? N415 Mn4 N401 C402 -92.5(8) . . . . ? N418 Mn4 N401 C402 122.9(8) . . . . ? O329 Mn4 N401 C409 144.6(9) . . . . ? O428 Mn4 N401 C409 -47.3(7) . . . . ? N408 Mn4 N401 C409 155.1(7) . . . . ? N415 Mn4 N401 C409 29.5(6) . . . . ? N418 Mn4 N401 C409 -115.1(7) . . . . ? O329 Mn4 N401 C416 -96.6(11) . . . . ? O428 Mn4 N401 C416 71.5(6) . . . . ? N408 Mn4 N401 C416 -86.1(6) . . . . ? N415 Mn4 N401 C416 148.3(6) . . . . ? N418 Mn4 N401 C416 3.7(6) . . . . ? C409 N401 C402 C403 -161.8(9) . . . . ? C416 N401 C402 C403 76.0(11) . . . . ? Mn4 N401 C402 C403 -40.5(11) . . . . ? N401 C402 C403 C404 -156.1(7) . . . . ? N401 C402 C403 N408 22.2(12) . . . . ? N408 C403 C404 C405 0.0 . . . . ? C402 C403 C404 C405 178.2(9) . . . . ? C403 C404 C405 C406 0.0 . . . . ? C404 C405 C406 C407 0.0 . . . . ? C405 C406 C407 N408 0.0 . . . . ? C406 C407 N408 C403 0.0 . . . . ? C406 C407 N408 Mn4 173.2(4) . . . . ? C404 C403 N408 C407 0.0 . . . . ? C402 C403 N408 C407 -178.4(8) . . . . ? C404 C403 N408 Mn4 -173.7(4) . . . . ? C402 C403 N408 Mn4 7.9(7) . . . . ? O329 Mn4 N408 C407 -18.4(4) . . . . ? O428 Mn4 N408 C407 73.8(7) . . . . ? N415 Mn4 N408 C407 -135.4(3) . . . . ? N401 Mn4 N408 C407 165.0(4) . . . . ? N418 Mn4 N408 C407 84.8(4) . . . . ? O329 Mn4 N408 C403 155.1(3) . . . . ? O428 Mn4 N408 C403 -112.7(6) . . . . ? N415 Mn4 N408 C403 38.0(4) . . . . ? N401 Mn4 N408 C403 -21.6(4) . . . . ? N418 Mn4 N408 C403 -101.7(3) . . . . ? C402 N401 C409 C410 80.8(11) . . . . ? C416 N401 C409 C410 -157.3(8) . . . . ? Mn4 N401 C409 C410 -41.6(10) . . . . ? N401 C409 C410 C411 -155.1(6) . . . . ? N401 C409 C410 N415 30.2(11) . . . . ? N415 C410 C411 C412 0.0 . . . . ? C409 C410 C411 C412 -174.5(8) . . . . ? C410 C411 C412 C413 0.0 . . . . ? C411 C412 C413 C414 0.0 . . . . ? C412 C413 C414 N415 0.0 . . . . ? C413 C414 N415 C410 0.0 . . . . ? C413 C414 N415 Mn4 177.7(4) . . . . ? C411 C410 N415 C414 0.0 . . . . ? C409 C410 N415 C414 174.9(8) . . . . ? C411 C410 N415 Mn4 -177.8(4) . . . . ? C409 C410 N415 Mn4 -2.9(7) . . . . ? O329 Mn4 N415 C414 5.7(4) . . . . ? O428 Mn4 N415 C414 -81.9(4) . . . . ? N408 Mn4 N415 C414 108.4(4) . . . . ? N401 Mn4 N415 C414 167.2(5) . . . . ? N418 Mn4 N415 C414 -138.4(4) . . . . ? O329 Mn4 N415 C410 -176.5(3) . . . . ? O428 Mn4 N415 C410 95.8(4) . . . . ? N408 Mn4 N415 C410 -73.9(4) . . . . ? N401 Mn4 N415 C410 -15.0(4) . . . . ? N418 Mn4 N415 C410 39.3(5) . . . . ? C402 N401 C416 C417 -155.0(9) . . . . ? C409 N401 C416 C417 82.8(10) . . . . ? Mn4 N401 C416 C417 -35.0(9) . . . . ? N401 C416 C417 N418 65.9(10) . . . . ? C416 C417 N418 C426 -165.5(8) . . . . ? C416 C417 N418 C419 73.5(11) . . . . ? C416 C417 N418 Mn4 -55.2(8) . . . . ? O329 Mn4 N418 C417 -171.4(6) . . . . ? O428 Mn4 N418 C417 -84.9(6) . . . . ? N408 Mn4 N418 C417 99.3(6) . . . . ? N415 Mn4 N418 C417 -24.7(7) . . . . ? N401 Mn4 N418 C417 27.4(6) . . . . ? O329 Mn4 N418 C426 -58.3(7) . . . . ? O428 Mn4 N418 C426 28.2(6) . . . . ? N408 Mn4 N418 C426 -147.7(6) . . . . ? N415 Mn4 N418 C426 88.3(7) . . . . ? N401 Mn4 N418 C426 140.5(7) . . . . ? O329 Mn4 N418 C419 64.1(7) . . . . ? O428 Mn4 N418 C419 150.6(7) . . . . ? N408 Mn4 N418 C419 -25.3(7) . . . . ? N415 Mn4 N418 C419 -149.2(6) . . . . ? N401 Mn4 N418 C419 -97.1(7) . . . . ? C417 N418 C419 C420 63.9(11) . . . . ? C426 N418 C419 C420 -57.1(10) . . . . ? Mn4 N418 C419 C420 -177.6(5) . . . . ? N418 C419 C420 C421 93.7(8) . . . . ? N418 C419 C420 C425 -83.4(9) . . . . ? C425 C420 C421 C422 0.0 . . . . ? C419 C420 C421 C422 -177.2(7) . . . . ? C420 C421 C422 C423 0.0 . . . . ? C421 C422 C423 C424 0.0 . . . . ? C422 C423 C424 C425 0.0 . . . . ? C423 C424 C425 C420 0.0 . . . . ? C421 C420 C425 C424 0.0 . . . . ? C419 C420 C425 C424 177.1(7) . . . . ? C417 N418 C426 C427 81.2(11) . . . . ? C419 N418 C426 C427 -155.3(9) . . . . ? Mn4 N418 C426 C427 -26.4(11) . . . . ? N418 C426 C427 O429 -161.3(10) . . . . ? N418 C426 C427 O428 3.0(13) . . . . ? O429 C427 O428 Mn4 -167.5(7) . . . . ? C426 C427 O428 Mn4 26.4(10) . . . . ? O329 Mn4 O428 C427 72.6(6) . . . . ? N408 Mn4 O428 C427 -19.5(10) . . . . ? N415 Mn4 O428 C427 -173.2(6) . . . . ? N401 Mn4 O428 C427 -103.6(6) . . . . ? N418 Mn4 O428 C427 -31.0(6) . . . . ? O428 C427 O429 Mn2 8.9(16) . . . . ? C426 C427 O429 Mn2 172.6(8) . . . . ? O228 Mn2 O429 C427 33.0(12) . . . . ? N215 Mn2 O429 C427 118.8(11) . . . . ? N208 Mn2 O429 C427 -139.4(11) . . . . ? N201 Mn2 O429 C427 -158.3(10) . . . . ? N218 Mn2 O429 C427 -42.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.431 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.080 data_gb305 _database_code_depnum_ccdc_archive 'CCDC 712177' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H84 Mn4 N16 O8, 4(Cl O4), 2(O)' _chemical_formula_sum 'C68 H84 Cl4 Mn4 N16 O26' _chemical_formula_weight 1903.07 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7119(14) _cell_length_b 12.7287(14) _cell_length_c 16.245(2) _cell_angle_alpha 68.501(11) _cell_angle_beta 73.531(11) _cell_angle_gamma 69.659(11) _cell_volume 2078.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13970 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour colour_less _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Excalibur3 with Sapphire-3 CCD' _diffrn_measurement_method '\w scans at different \f' _diffrn_detector_area_resol_mean 12.0 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 13970 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8124 _reflns_number_gt 4472 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Bergerhoff, 1996)' _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^)+(0.1131P)^2^] 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 8124 _refine_ls_number_parameters 565 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1974 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.987 _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 Cl1 Cl 0.69415(15) 0.13965(13) 0.36783(15) 0.0825(5) Uani 1 1 d . . . O1 O 0.6627(7) 0.0338(5) 0.4021(5) 0.147(3) Uani 1 1 d . . . O2 O 0.7299(9) 0.1685(6) 0.2757(5) 0.178(3) Uani 1 1 d . . . O3 O 0.5927(4) 0.2319(4) 0.3885(4) 0.1205(19) Uani 1 1 d . . . O4 O 0.7906(5) 0.1338(5) 0.4031(5) 0.142(3) Uani 1 1 d . . . Cl2 Cl 0.33026(17) 0.23988(13) 0.02596(12) 0.0824(5) Uani 1 1 d . . . O5 O 0.3487(6) 0.1660(5) -0.0263(5) 0.141(2) Uani 1 1 d . . . O6 O 0.2635(7) 0.1995(5) 0.1101(4) 0.171(3) Uani 1 1 d . . . O7 O 0.2709(7) 0.3566(4) -0.0178(4) 0.153(3) Uani 1 1 d . . . O8 O 0.4499(7) 0.2299(7) 0.0355(6) 0.174(3) Uani 1 1 d . . . Mn1 Mn 0.93923(6) 0.52496(6) 0.32384(5) 0.0429(2) Uani 1 1 d . . . Mn2 Mn 1.24653(6) 0.70788(6) 0.33121(5) 0.0494(2) Uani 1 1 d . . . N115 N 1.1111(3) 0.3796(3) 0.3596(3) 0.0428(9) Uani 1 1 d . . . C12 C 1.1852(4) 0.3783(4) 0.4094(3) 0.0492(12) Uani 1 1 d . . . H12 H 1.1688 0.4435 0.4284 0.059 Uiso 1 1 calc R . . C13 C 1.2858(4) 0.2835(4) 0.4337(4) 0.0597(14) Uani 1 1 d . . . H13 H 1.3350 0.2841 0.4695 0.072 Uiso 1 1 calc R . . C14 C 1.3107(5) 0.1889(4) 0.4036(4) 0.0688(16) Uani 1 1 d . . . H14 H 1.3787 0.1249 0.4174 0.083 Uiso 1 1 calc R . . C15 C 1.2351(5) 0.1895(4) 0.3535(4) 0.0645(15) Uani 1 1 d . . . H15 H 1.2514 0.1259 0.3326 0.077 Uiso 1 1 calc R . . C16 C 1.1343(4) 0.2847(4) 0.3335(3) 0.0525(12) Uani 1 1 d . . . C17 C 1.0425(5) 0.2860(4) 0.2847(4) 0.0580(14) Uani 1 1 d . . . H17A H 1.0843 0.2393 0.2436 0.070 Uiso 1 1 calc R . . H17B H 0.9796 0.2507 0.3277 0.070 Uiso 1 1 calc R . . N101 N 0.9827(3) 0.4070(3) 0.2336(3) 0.0491(10) Uani 1 1 d . . . C19 C 1.0692(5) 0.4495(5) 0.1524(4) 0.0634(15) Uani 1 1 d . . . H19A H 1.0737 0.4144 0.1074 0.076 Uiso 1 1 calc R . . H19B H 1.1512 0.4252 0.1670 0.076 Uiso 1 1 calc R . . C20 C 1.0302(5) 0.5801(5) 0.1148(4) 0.0633(14) Uani 1 1 d . . . C21 C 1.0591(6) 0.6363(7) 0.0240(4) 0.086(2) Uani 1 1 d . . . H21 H 1.1037 0.5929 -0.0157 0.103 Uiso 1 1 calc R . . C22 C 1.0219(9) 0.7562(9) -0.0069(5) 0.114(3) Uani 1 1 d . . . H22 H 1.0414 0.7952 -0.0677 0.137 Uiso 1 1 calc R . . C23 C 0.9563(8) 0.8173(7) 0.0520(6) 0.102(3) Uani 1 1 d . . . H23 H 0.9292 0.8987 0.0317 0.122 Uiso 1 1 calc R . . C24 C 0.9291(6) 0.7583(5) 0.1430(4) 0.0725(17) Uani 1 1 d . . . H24 H 0.8833 0.8013 0.1829 0.087 Uiso 1 1 calc R . . N108 N 0.9680(4) 0.6398(4) 0.1748(3) 0.0596(11) Uani 1 1 d . . . C26 C 0.8637(4) 0.4158(5) 0.2118(4) 0.0548(13) Uani 1 1 d . . . H26A H 0.8715 0.3458 0.1973 0.066 Uiso 1 1 calc R . . H26B H 0.8456 0.4828 0.1595 0.066 Uiso 1 1 calc R . . C27 C 0.7586(4) 0.4289(4) 0.2898(4) 0.0529(12) Uani 1 1 d . . . H27A H 0.6830 0.4320 0.2743 0.064 Uiso 1 1 calc R . . H27B H 0.7759 0.3609 0.3416 0.064 Uiso 1 1 calc R . . N118 N 0.7398(3) 0.5369(3) 0.3135(3) 0.0463(9) Uani 1 1 d . . . C29 C 0.6752(4) 0.6416(5) 0.2486(3) 0.0606(14) Uani 1 1 d . . . H29A H 0.5931 0.6377 0.2535 0.091 Uiso 1 1 calc R . . H29B H 0.7199 0.6443 0.1887 0.091 Uiso 1 1 calc R . . H29C H 0.6707 0.7110 0.2613 0.091 Uiso 1 1 calc R . . C30 C 0.6671(4) 0.5282(4) 0.4041(3) 0.0544(13) Uani 1 1 d . . . H30A H 0.5975 0.4995 0.4104 0.065 Uiso 1 1 calc R . . H30B H 0.6343 0.6060 0.4117 0.065 Uiso 1 1 calc R . . C31 C 0.7411(5) 0.4476(4) 0.4778(4) 0.0498(12) Uani 1 1 d . . . O128 O 0.8573(3) 0.4210(3) 0.4569(2) 0.0563(9) Uani 1 1 d . . . O129 O 0.6814(3) 0.4148(3) 0.5555(2) 0.0594(9) Uani 1 1 d . . . O229 O 0.8882(3) 0.6755(3) 0.3680(3) 0.0645(10) Uani 1 1 d . . . C35 C 0.9827(5) 0.7064(4) 0.3598(4) 0.0525(12) Uani 1 1 d . . . O228 O 1.0894(3) 0.6537(3) 0.3297(2) 0.0526(8) Uani 1 1 d . . . C37 C 0.9664(5) 0.8099(5) 0.3905(5) 0.0685(16) Uani 1 1 d . . . H37A H 0.8922 0.8700 0.3729 0.082 Uiso 1 1 calc R . . H37B H 0.9550 0.7852 0.4556 0.082 Uiso 1 1 calc R . . N218 N 1.0699(4) 0.8592(3) 0.3538(3) 0.0528(10) Uani 1 1 d D . . C39 C 1.0740(6) 0.9174(7) 0.4144(7) 0.117(3) Uani 1 1 d . . . H39A H 0.9949 0.9719 0.4255 0.175 Uiso 1 1 calc R . . H39B H 1.1364 0.9589 0.3876 0.175 Uiso 1 1 calc R . . H39C H 1.0933 0.8600 0.4701 0.175 Uiso 1 1 calc R . . C40A C 1.0964(18) 0.9607(11) 0.2752(10) 0.057(6) Uani 0.312(18) 1 d PD . . H40A H 1.0254 1.0290 0.2733 0.068 Uiso 0.312(18) 1 calc PR . . H40B H 1.1668 0.9803 0.2801 0.068 Uiso 0.312(18) 1 calc PR . . C40B C 1.0463(9) 0.9329(8) 0.2593(6) 0.069(4) Uani 0.688(18) 1 d PD . . H40C H 1.0086 0.8932 0.2380 0.082 Uiso 0.688(18) 1 calc PR . . H40D H 0.9870 1.0074 0.2626 0.082 Uiso 0.688(18) 1 calc PR . . C41A C 1.1239(17) 0.925(2) 0.1922(18) 0.060(9) Uani 0.312(18) 1 d PD . . H41A H 1.1208 0.9938 0.1395 0.072 Uiso 0.312(18) 1 calc PR . . H41B H 1.0635 0.8876 0.1945 0.072 Uiso 0.312(18) 1 calc PR . . C41B C 1.1583(10) 0.9571(8) 0.1918(12) 0.079(5) Uani 0.688(18) 1 d PD . . H41C H 1.1933 1.0031 0.2089 0.095 Uiso 0.688(18) 1 calc PR . . H41D H 1.1357 1.0013 0.1331 0.095 Uiso 0.688(18) 1 calc PR . . N201 N 1.2527(4) 0.8408(4) 0.1878(3) 0.0631(12) Uani 1 1 d D . . C43 C 1.2440(6) 0.7806(6) 0.1295(4) 0.0756(17) Uani 1 1 d . . . H43A H 1.2733 0.8204 0.0675 0.091 Uiso 1 1 calc R . . H43B H 1.1578 0.7850 0.1351 0.091 Uiso 1 1 calc R . . C44 C 1.3186(5) 0.6526(5) 0.1522(4) 0.0660(15) Uani 1 1 d . . . C45 C 1.3501(7) 0.5913(8) 0.0915(5) 0.093(2) Uani 1 1 d . . . H45 H 1.3304 0.6276 0.0343 0.111 Uiso 1 1 calc R . . C46 C 1.4131(8) 0.4715(8) 0.1189(6) 0.105(3) Uani 1 1 d . . . H46 H 1.4319 0.4263 0.0805 0.126 Uiso 1 1 calc R . . C47 C 1.4464(7) 0.4219(6) 0.2002(6) 0.090(2) Uani 1 1 d . . . H47 H 1.4909 0.3434 0.2178 0.108 Uiso 1 1 calc R . . C48 C 1.4132(5) 0.4899(5) 0.2567(4) 0.0673(15) Uani 1 1 d . . . H48 H 1.4353 0.4557 0.3133 0.081 Uiso 1 1 calc R . . N215 N 1.3499(4) 0.6039(4) 0.2334(3) 0.0565(11) Uani 1 1 d . . . C50 C 1.3712(6) 0.8706(5) 0.1596(4) 0.0744(17) Uani 1 1 d . . . H50A H 1.3636 0.9444 0.1116 0.089 Uiso 1 1 calc R . . H50B H 1.4345 0.8104 0.1362 0.089 Uiso 1 1 calc R . . C51 C 1.4099(5) 0.8812(5) 0.2365(5) 0.0686(16) Uani 1 1 d . . . C52 C 1.4836(7) 0.9534(6) 0.2209(6) 0.090(2) Uani 1 1 d . . . H52 H 1.5067 0.9996 0.1630 0.108 Uiso 1 1 calc R . . C53 C 1.5215(7) 0.9555(6) 0.2915(7) 0.097(2) Uani 1 1 d . . . H53 H 1.5707 1.0041 0.2819 0.117 Uiso 1 1 calc R . . C54 C 1.4891(6) 0.8883(6) 0.3754(6) 0.082(2) Uani 1 1 d . . . H54 H 1.5159 0.8887 0.4240 0.098 Uiso 1 1 calc R . . C55 C 1.4137(5) 0.8179(5) 0.3870(4) 0.0658(15) Uani 1 1 d . . . H55 H 1.3893 0.7723 0.4448 0.079 Uiso 1 1 calc R . . N208 N 1.3750(4) 0.8130(4) 0.3190(3) 0.0634(12) Uani 1 1 d . . . O1AQ O 0.702(3) 0.138(3) 0.1118(10) 0.278(19) Uani 0.58(2) 1 d P . . O2AQ O 0.8149(17) 1.0345(17) 0.1599(18) 0.162(11) Uani 0.42(2) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0681(9) 0.0625(9) 0.1283(16) -0.0328(9) -0.0337(10) -0.0137(7) O1 0.178(6) 0.082(3) 0.209(7) -0.016(4) -0.067(5) -0.069(4) O2 0.249(9) 0.132(5) 0.123(6) -0.050(5) -0.003(6) -0.027(5) O3 0.072(3) 0.090(3) 0.173(6) -0.031(3) -0.023(3) 0.001(3) O4 0.084(4) 0.124(4) 0.261(8) -0.093(5) -0.081(5) 0.000(3) Cl2 0.0889(11) 0.0700(9) 0.0734(11) -0.0248(8) -0.0015(9) -0.0107(8) O5 0.149(5) 0.135(5) 0.151(6) -0.086(4) -0.002(4) -0.028(4) O6 0.187(6) 0.102(4) 0.097(4) -0.002(3) 0.046(4) 0.025(4) O7 0.206(7) 0.082(3) 0.083(4) 0.002(3) 0.000(4) 0.017(4) O8 0.143(6) 0.163(6) 0.233(9) -0.051(6) -0.061(6) -0.049(5) Mn1 0.0385(4) 0.0445(4) 0.0502(5) -0.0217(3) -0.0121(3) -0.0052(3) Mn2 0.0430(4) 0.0523(4) 0.0540(5) -0.0216(4) -0.0128(3) -0.0049(3) N115 0.0358(19) 0.047(2) 0.048(2) -0.0204(18) -0.0054(17) -0.0080(15) C12 0.041(2) 0.048(3) 0.064(3) -0.022(2) -0.013(2) -0.009(2) C13 0.044(3) 0.063(3) 0.073(4) -0.016(3) -0.021(3) -0.012(2) C14 0.055(3) 0.050(3) 0.096(5) -0.023(3) -0.025(3) 0.004(2) C15 0.056(3) 0.046(3) 0.098(5) -0.035(3) -0.024(3) 0.001(2) C16 0.049(3) 0.049(3) 0.059(3) -0.026(2) -0.013(2) -0.001(2) C17 0.059(3) 0.047(3) 0.073(4) -0.032(3) -0.013(3) -0.003(2) N101 0.039(2) 0.058(2) 0.053(3) -0.026(2) -0.0079(18) -0.0077(17) C19 0.056(3) 0.083(4) 0.056(3) -0.034(3) -0.013(3) -0.009(3) C20 0.059(3) 0.080(4) 0.059(4) -0.020(3) -0.023(3) -0.020(3) C21 0.092(5) 0.107(5) 0.051(4) -0.017(4) -0.015(3) -0.023(4) C22 0.153(8) 0.139(8) 0.058(5) -0.003(5) -0.038(5) -0.062(6) C23 0.127(7) 0.081(5) 0.101(6) 0.017(5) -0.066(6) -0.042(5) C24 0.081(4) 0.065(4) 0.083(5) -0.013(3) -0.042(4) -0.022(3) N108 0.063(3) 0.062(3) 0.061(3) -0.014(2) -0.020(2) -0.023(2) C26 0.054(3) 0.062(3) 0.062(3) -0.034(3) -0.015(3) -0.012(2) C27 0.047(3) 0.058(3) 0.063(3) -0.022(3) -0.020(2) -0.013(2) N118 0.041(2) 0.053(2) 0.044(2) -0.0196(18) -0.0106(17) -0.0044(17) C29 0.043(3) 0.071(3) 0.054(3) -0.014(3) -0.015(2) 0.001(2) C30 0.044(3) 0.062(3) 0.052(3) -0.017(2) -0.013(2) -0.006(2) C31 0.050(3) 0.050(3) 0.052(3) -0.021(2) -0.012(2) -0.007(2) O128 0.0407(19) 0.067(2) 0.053(2) -0.0180(16) -0.0123(16) -0.0015(15) O129 0.0467(19) 0.075(2) 0.049(2) -0.0175(18) -0.0066(17) -0.0103(17) O229 0.050(2) 0.071(2) 0.095(3) -0.050(2) -0.0048(19) -0.0242(17) C35 0.055(3) 0.047(3) 0.066(4) -0.024(2) -0.017(3) -0.013(2) O228 0.053(2) 0.0412(16) 0.067(2) -0.0289(16) -0.0142(17) -0.0017(14) C37 0.043(3) 0.071(3) 0.108(5) -0.058(3) -0.002(3) -0.011(2) N218 0.049(2) 0.045(2) 0.071(3) -0.030(2) -0.008(2) -0.0095(17) C39 0.065(4) 0.135(6) 0.206(9) -0.134(7) -0.025(5) -0.004(4) C40A 0.028(9) 0.045(9) 0.105(17) -0.032(10) -0.004(10) -0.015(7) C40B 0.052(6) 0.056(5) 0.080(8) -0.013(5) -0.006(5) -0.006(4) C41A 0.076(18) 0.049(13) 0.038(13) 0.004(10) -0.024(13) -0.003(12) C41B 0.065(6) 0.061(8) 0.095(10) -0.015(7) -0.030(7) 0.004(6) N201 0.055(3) 0.064(3) 0.057(3) -0.014(2) -0.016(2) -0.001(2) C43 0.065(4) 0.112(5) 0.055(4) -0.024(3) -0.016(3) -0.027(3) C44 0.057(3) 0.089(4) 0.055(4) -0.029(3) -0.003(3) -0.022(3) C45 0.098(5) 0.151(7) 0.065(4) -0.055(5) 0.006(4) -0.069(5) C46 0.106(6) 0.125(7) 0.112(7) -0.081(6) 0.039(5) -0.060(5) C47 0.093(5) 0.088(5) 0.089(5) -0.050(4) 0.016(4) -0.026(4) C48 0.055(3) 0.069(3) 0.084(4) -0.037(3) 0.005(3) -0.024(3) N215 0.044(2) 0.068(3) 0.061(3) -0.030(2) -0.004(2) -0.012(2) C50 0.073(4) 0.058(3) 0.078(4) -0.011(3) -0.006(3) -0.017(3) C51 0.055(3) 0.047(3) 0.098(5) -0.022(3) -0.014(3) -0.007(2) C52 0.088(5) 0.068(4) 0.109(6) -0.008(4) -0.026(4) -0.027(4) C53 0.095(5) 0.076(5) 0.138(8) -0.033(5) -0.037(5) -0.029(4) C54 0.071(4) 0.065(4) 0.122(6) -0.045(4) -0.038(4) 0.001(3) C55 0.053(3) 0.068(3) 0.087(4) -0.034(3) -0.023(3) -0.008(3) N208 0.049(2) 0.059(3) 0.080(4) -0.027(3) -0.019(2) 0.000(2) O1AQ 0.37(4) 0.43(4) 0.089(10) -0.037(15) 0.018(14) -0.26(4) O2AQ 0.126(14) 0.157(16) 0.20(2) -0.083(15) -0.015(13) -0.010(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 Cl1 O4 1.373(5) . ? Cl1 O2 1.378(7) . ? Cl1 O1 1.393(5) . ? Cl1 O3 1.413(5) . ? Cl2 O6 1.379(6) . ? Cl2 O7 1.408(5) . ? Cl2 O8 1.410(7) . ? Cl2 O5 1.412(6) . ? Mn1 O229 2.124(3) . ? Mn1 O128 2.226(4) . ? Mn1 N115 2.258(3) . ? Mn1 N101 2.306(4) . ? Mn1 N108 2.323(5) . ? Mn1 N118 2.337(4) . ? Mn2 O129 2.097(3) 2_766 ? Mn2 O228 2.186(3) . ? Mn2 N215 2.254(4) . ? Mn2 N208 2.265(5) . ? Mn2 N201 2.324(4) . ? Mn2 N218 2.332(4) . ? N115 C12 1.336(6) . ? N115 C16 1.340(6) . ? C12 C13 1.388(6) . ? C12 H12 0.9300 . ? C13 C14 1.372(7) . ? C13 H13 0.9300 . ? C14 C15 1.359(7) . ? C14 H14 0.9300 . ? C15 C16 1.379(6) . ? C15 H15 0.9300 . ? C16 C17 1.499(7) . ? C17 N101 1.482(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? N101 C19 1.470(7) . ? N101 C26 1.491(6) . ? C19 C20 1.493(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N108 1.347(7) . ? C20 C21 1.383(9) . ? C21 C22 1.369(11) . ? C21 H21 0.9300 . ? C22 C23 1.350(11) . ? C22 H22 0.9300 . ? C23 C24 1.392(10) . ? C23 H23 0.9300 . ? C24 N108 1.355(7) . ? C24 H24 0.9300 . ? C26 C27 1.508(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N118 1.489(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? N118 C30 1.463(6) . ? N118 C29 1.477(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.519(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 O129 1.254(6) . ? C31 O128 1.259(6) . ? O129 Mn2 2.097(3) 2_766 ? O229 C35 1.256(6) . ? C35 O228 1.250(6) . ? C35 C37 1.508(7) . ? C37 N218 1.436(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? N218 C39 1.452(7) . ? N218 C40A 1.498(11) . ? N218 C40B 1.522(8) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40A C41A 1.490(15) . ? C40A H40A 0.9700 . ? C40A H40B 0.9700 . ? C40B C41B 1.495(12) . ? C40B H40C 0.9700 . ? C40B H40D 0.9700 . ? C41A N201 1.519(11) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C41B N201 1.519(8) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? N201 C43 1.462(7) . ? N201 C50 1.468(8) . ? C43 C44 1.519(8) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N215 1.332(7) . ? C44 C45 1.368(8) . ? C45 C46 1.405(11) . ? C45 H45 0.9300 . ? C46 C47 1.344(11) . ? C46 H46 0.9300 . ? C47 C48 1.375(9) . ? C47 H47 0.9300 . ? C48 N215 1.344(7) . ? C48 H48 0.9300 . ? C50 C51 1.507(9) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 N208 1.342(8) . ? C51 C52 1.381(9) . ? C52 C53 1.354(10) . ? C52 H52 0.9300 . ? C53 C54 1.346(10) . ? C53 H53 0.9300 . ? C54 C55 1.395(8) . ? C54 H54 0.9300 . ? C55 N208 1.337(7) . ? C55 H55 0.9300 . ? O1AQ O2AQ 1.65(3) 1_545 ? O2AQ O1AQ 1.65(3) 1_565 ? 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 Cl1 O2 107.6(5) . . ? O4 Cl1 O1 111.3(4) . . ? O2 Cl1 O1 111.0(5) . . ? O4 Cl1 O3 107.8(4) . . ? O2 Cl1 O3 108.1(4) . . ? O1 Cl1 O3 110.8(4) . . ? O6 Cl2 O7 111.3(3) . . ? O6 Cl2 O8 108.5(5) . . ? O7 Cl2 O8 111.1(5) . . ? O6 Cl2 O5 110.1(5) . . ? O7 Cl2 O5 110.6(4) . . ? O8 Cl2 O5 105.1(5) . . ? O229 Mn1 O128 92.03(14) . . ? O229 Mn1 N115 119.66(14) . . ? O128 Mn1 N115 80.94(12) . . ? O229 Mn1 N101 161.77(15) . . ? O128 Mn1 N101 103.19(14) . . ? N115 Mn1 N101 73.33(13) . . ? O229 Mn1 N108 90.62(16) . . ? O128 Mn1 N108 162.66(14) . . ? N115 Mn1 N108 112.40(15) . . ? N101 Mn1 N108 71.88(15) . . ? O229 Mn1 N118 96.30(13) . . ? O128 Mn1 N118 73.06(13) . . ? N115 Mn1 N118 136.16(13) . . ? N101 Mn1 N118 78.96(13) . . ? N108 Mn1 N118 89.62(14) . . ? O129 Mn2 O228 104.44(14) 2_766 . ? O129 Mn2 N215 97.48(15) 2_766 . ? O228 Mn2 N215 84.01(13) . . ? O129 Mn2 N208 88.24(16) 2_766 . ? O228 Mn2 N208 164.46(13) . . ? N215 Mn2 N208 103.51(16) . . ? O129 Mn2 N201 156.20(15) 2_766 . ? O228 Mn2 N201 96.28(15) . . ? N215 Mn2 N201 72.87(16) . . ? N208 Mn2 N201 73.52(18) . . ? O129 Mn2 N218 117.95(15) 2_766 . ? O228 Mn2 N218 73.53(12) . . ? N215 Mn2 N218 141.52(16) . . ? N208 Mn2 N218 92.71(14) . . ? N201 Mn2 N218 78.90(15) . . ? C12 N115 C16 118.4(4) . . ? C12 N115 Mn1 125.0(3) . . ? C16 N115 Mn1 116.4(3) . . ? N115 C12 C13 122.6(4) . . ? N115 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C14 C13 C12 118.1(5) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C15 C14 C13 119.5(4) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? N115 C16 C15 121.4(5) . . ? N115 C16 C17 116.5(4) . . ? C15 C16 C17 122.0(4) . . ? N101 C17 C16 111.5(4) . . ? N101 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? N101 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C19 N101 C17 109.9(4) . . ? C19 N101 C26 111.8(4) . . ? C17 N101 C26 112.1(4) . . ? C19 N101 Mn1 107.6(3) . . ? C17 N101 Mn1 107.3(3) . . ? C26 N101 Mn1 107.8(3) . . ? N101 C19 C20 111.7(4) . . ? N101 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? N101 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? N108 C20 C21 122.1(6) . . ? N108 C20 C19 116.0(5) . . ? C21 C20 C19 121.9(6) . . ? C22 C21 C20 119.6(7) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 C21 119.1(7) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 120.1(7) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? N108 C24 C23 121.4(6) . . ? N108 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C20 N108 C24 117.7(5) . . ? C20 N108 Mn1 115.3(3) . . ? C24 N108 Mn1 127.0(4) . . ? N101 C26 C27 111.1(4) . . ? N101 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? N101 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? N118 C27 C26 111.8(4) . . ? N118 C27 H27A 109.2 . . ? C26 C27 H27A 109.2 . . ? N118 C27 H27B 109.2 . . ? C26 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C30 N118 C29 109.5(3) . . ? C30 N118 C27 110.0(4) . . ? C29 N118 C27 110.4(4) . . ? C30 N118 Mn1 105.7(3) . . ? C29 N118 Mn1 118.0(3) . . ? C27 N118 Mn1 102.9(2) . . ? N118 C29 H29A 109.5 . . ? N118 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N118 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N118 C30 C31 113.3(4) . . ? N118 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? N118 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? O129 C31 O128 124.9(4) . . ? O129 C31 C30 117.2(4) . . ? O128 C31 C30 117.8(5) . . ? C31 O128 Mn1 117.2(3) . . ? C31 O129 Mn2 126.8(3) . 2_766 ? C35 O229 Mn1 109.9(3) . . ? O228 C35 O229 123.2(4) . . ? O228 C35 C37 118.6(4) . . ? O229 C35 C37 118.1(4) . . ? C35 O228 Mn2 118.9(3) . . ? N218 C37 C35 112.9(4) . . ? N218 C37 H37A 109.0 . . ? C35 C37 H37A 109.0 . . ? N218 C37 H37B 109.0 . . ? C35 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 N218 C39 108.2(5) . . ? C37 N218 C40A 134.0(9) . . ? C39 N218 C40A 89.9(9) . . ? C37 N218 C40B 102.3(6) . . ? C39 N218 C40B 118.7(7) . . ? C40A N218 C40B 35.2(7) . . ? C37 N218 Mn2 107.7(3) . . ? C39 N218 Mn2 114.6(3) . . ? C40A N218 Mn2 101.8(7) . . ? C40B N218 Mn2 104.2(4) . . ? N218 C39 H39A 109.5 . . ? N218 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N218 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41A C40A N218 107.5(18) . . ? C41A C40A H40A 110.2 . . ? N218 C40A H40A 110.2 . . ? C41A C40A H40B 110.2 . . ? N218 C40A H40B 110.2 . . ? H40A C40A H40B 108.5 . . ? C41B C40B N218 115.3(12) . . ? C41B C40B H40C 108.4 . . ? N218 C40B H40C 108.4 . . ? C41B C40B H40D 108.4 . . ? N218 C40B H40D 108.4 . . ? H40C C40B H40D 107.5 . . ? C40A C41A N201 107.2(12) . . ? C40A C41A H41A 110.3 . . ? N201 C41A H41A 110.3 . . ? C40A C41A H41B 110.3 . . ? N201 C41A H41B 110.3 . . ? H41A C41A H41B 108.5 . . ? C40B C41B N201 108.8(8) . . ? C40B C41B H41C 109.9 . . ? N201 C41B H41C 109.9 . . ? C40B C41B H41D 109.9 . . ? N201 C41B H41D 109.9 . . ? H41C C41B H41D 108.3 . . ? C43 N201 C50 110.3(5) . . ? C43 N201 C41A 99.5(9) . . ? C50 N201 C41A 127.1(14) . . ? C43 N201 C41B 119.0(8) . . ? C50 N201 C41B 103.1(6) . . ? C41A N201 C41B 25.1(12) . . ? C43 N201 Mn2 106.0(4) . . ? C50 N201 Mn2 108.8(3) . . ? C41A N201 Mn2 103.2(12) . . ? C41B N201 Mn2 109.3(7) . . ? N201 C43 C44 112.6(4) . . ? N201 C43 H43A 109.1 . . ? C44 C43 H43A 109.1 . . ? N201 C43 H43B 109.1 . . ? C44 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? N215 C44 C45 122.4(6) . . ? N215 C44 C43 116.9(5) . . ? C45 C44 C43 120.7(6) . . ? C44 C45 C46 117.6(7) . . ? C44 C45 H45 121.2 . . ? C46 C45 H45 121.2 . . ? C47 C46 C45 120.4(7) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 118.4(7) . . ? C46 C47 H47 120.8 . . ? C48 C47 H47 120.8 . . ? N215 C48 C47 122.5(6) . . ? N215 C48 H48 118.7 . . ? C47 C48 H48 118.7 . . ? C44 N215 C48 118.5(5) . . ? C44 N215 Mn2 114.7(3) . . ? C48 N215 Mn2 124.6(4) . . ? N201 C50 C51 111.7(5) . . ? N201 C50 H50A 109.3 . . ? C51 C50 H50A 109.3 . . ? N201 C50 H50B 109.3 . . ? C51 C50 H50B 109.3 . . ? H50A C50 H50B 108.0 . . ? N208 C51 C52 122.3(7) . . ? N208 C51 C50 116.8(5) . . ? C52 C51 C50 120.8(7) . . ? C53 C52 C51 118.7(8) . . ? C53 C52 H52 120.6 . . ? C51 C52 H52 120.6 . . ? C54 C53 C52 121.0(7) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 C55 117.6(7) . . ? C53 C54 H54 121.2 . . ? C55 C54 H54 121.2 . . ? N208 C55 C54 123.1(7) . . ? N208 C55 H55 118.4 . . ? C54 C55 H55 118.4 . . ? C55 N208 C51 117.2(5) . . ? C55 N208 Mn2 125.9(4) . . ? C51 N208 Mn2 116.9(4) . . ? 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 O229 Mn1 N115 C12 1.5(4) . . . . ? O128 Mn1 N115 C12 -85.7(4) . . . . ? N101 Mn1 N115 C12 167.5(4) . . . . ? N108 Mn1 N115 C12 105.9(4) . . . . ? N118 Mn1 N115 C12 -139.4(4) . . . . ? O229 Mn1 N115 C16 176.7(3) . . . . ? O128 Mn1 N115 C16 89.5(4) . . . . ? N101 Mn1 N115 C16 -17.2(3) . . . . ? N108 Mn1 N115 C16 -78.9(4) . . . . ? N118 Mn1 N115 C16 35.9(4) . . . . ? C16 N115 C12 C13 1.0(7) . . . . ? Mn1 N115 C12 C13 176.1(4) . . . . ? N115 C12 C13 C14 1.4(8) . . . . ? C12 C13 C14 C15 -1.7(9) . . . . ? C13 C14 C15 C16 -0.2(9) . . . . ? C12 N115 C16 C15 -3.0(8) . . . . ? Mn1 N115 C16 C15 -178.5(4) . . . . ? C12 N115 C16 C17 174.9(5) . . . . ? Mn1 N115 C16 C17 -0.7(6) . . . . ? C14 C15 C16 N115 2.6(9) . . . . ? C14 C15 C16 C17 -175.1(6) . . . . ? N115 C16 C17 N101 29.7(7) . . . . ? C15 C16 C17 N101 -152.5(5) . . . . ? C16 C17 N101 C19 75.0(5) . . . . ? C16 C17 N101 C26 -160.0(4) . . . . ? C16 C17 N101 Mn1 -41.7(5) . . . . ? O229 Mn1 N101 C19 50.5(6) . . . . ? O128 Mn1 N101 C19 -163.6(3) . . . . ? N115 Mn1 N101 C19 -87.4(3) . . . . ? N108 Mn1 N101 C19 33.7(3) . . . . ? N118 Mn1 N101 C19 126.9(3) . . . . ? O229 Mn1 N101 C17 168.8(4) . . . . ? O128 Mn1 N101 C17 -45.3(3) . . . . ? N115 Mn1 N101 C17 30.8(3) . . . . ? N108 Mn1 N101 C17 151.9(3) . . . . ? N118 Mn1 N101 C17 -114.8(3) . . . . ? O229 Mn1 N101 C26 -70.2(6) . . . . ? O128 Mn1 N101 C26 75.7(3) . . . . ? N115 Mn1 N101 C26 151.8(3) . . . . ? N108 Mn1 N101 C26 -87.1(3) . . . . ? N118 Mn1 N101 C26 6.2(3) . . . . ? C17 N101 C19 C20 -162.0(4) . . . . ? C26 N101 C19 C20 72.8(5) . . . . ? Mn1 N101 C19 C20 -45.4(5) . . . . ? N101 C19 C20 N108 30.4(6) . . . . ? N101 C19 C20 C21 -151.2(5) . . . . ? N108 C20 C21 C22 -1.3(10) . . . . ? C19 C20 C21 C22 -179.6(6) . . . . ? C20 C21 C22 C23 -0.6(12) . . . . ? C21 C22 C23 C24 1.0(12) . . . . ? C22 C23 C24 N108 0.5(11) . . . . ? C21 C20 N108 C24 2.8(8) . . . . ? C19 C20 N108 C24 -178.9(5) . . . . ? C21 C20 N108 Mn1 -177.2(5) . . . . ? C19 C20 N108 Mn1 1.1(6) . . . . ? C23 C24 N108 C20 -2.4(8) . . . . ? C23 C24 N108 Mn1 177.6(4) . . . . ? O229 Mn1 N108 C20 165.6(4) . . . . ? O128 Mn1 N108 C20 -95.6(6) . . . . ? N115 Mn1 N108 C20 42.9(4) . . . . ? N101 Mn1 N108 C20 -19.6(3) . . . . ? N118 Mn1 N108 C20 -98.1(4) . . . . ? O229 Mn1 N108 C24 -14.5(4) . . . . ? O128 Mn1 N108 C24 84.4(6) . . . . ? N115 Mn1 N108 C24 -137.1(4) . . . . ? N101 Mn1 N108 C24 160.3(5) . . . . ? N118 Mn1 N108 C24 81.8(4) . . . . ? C19 N101 C26 C27 -152.9(4) . . . . ? C17 N101 C26 C27 83.1(5) . . . . ? Mn1 N101 C26 C27 -34.8(5) . . . . ? N101 C26 C27 N118 60.6(5) . . . . ? C26 C27 N118 C30 -162.0(4) . . . . ? C26 C27 N118 C29 77.0(5) . . . . ? C26 C27 N118 Mn1 -49.7(4) . . . . ? O229 Mn1 N118 C30 -60.1(3) . . . . ? O128 Mn1 N118 C30 30.1(3) . . . . ? N115 Mn1 N118 C30 86.4(3) . . . . ? N101 Mn1 N118 C30 137.7(3) . . . . ? N108 Mn1 N118 C30 -150.7(3) . . . . ? O229 Mn1 N118 C29 62.7(3) . . . . ? O128 Mn1 N118 C29 152.9(3) . . . . ? N115 Mn1 N118 C29 -150.8(3) . . . . ? N101 Mn1 N118 C29 -99.5(3) . . . . ? N108 Mn1 N118 C29 -27.9(3) . . . . ? O229 Mn1 N118 C27 -175.5(3) . . . . ? O128 Mn1 N118 C27 -85.3(3) . . . . ? N115 Mn1 N118 C27 -29.0(4) . . . . ? N101 Mn1 N118 C27 22.3(3) . . . . ? N108 Mn1 N118 C27 93.9(3) . . . . ? C29 N118 C30 C31 -162.6(4) . . . . ? C27 N118 C30 C31 75.9(5) . . . . ? Mn1 N118 C30 C31 -34.5(5) . . . . ? N118 C30 C31 O129 -164.7(4) . . . . ? N118 C30 C31 O128 16.9(7) . . . . ? O129 C31 O128 Mn1 -165.2(4) . . . . ? C30 C31 O128 Mn1 13.0(6) . . . . ? O229 Mn1 O128 C31 71.3(3) . . . . ? N115 Mn1 O128 C31 -169.0(4) . . . . ? N101 Mn1 O128 C31 -98.6(3) . . . . ? N108 Mn1 O128 C31 -27.4(7) . . . . ? N118 Mn1 O128 C31 -24.7(3) . . . . ? O128 C31 O129 Mn2 -7.9(7) . . . 2_766 ? C30 C31 O129 Mn2 173.9(3) . . . 2_766 ? O128 Mn1 O229 C35 121.8(4) . . . . ? N115 Mn1 O229 C35 41.1(4) . . . . ? N101 Mn1 O229 C35 -91.3(5) . . . . ? N108 Mn1 O229 C35 -75.3(4) . . . . ? N118 Mn1 O229 C35 -165.0(4) . . . . ? Mn1 O229 C35 O228 0.1(6) . . . . ? Mn1 O229 C35 C37 -178.1(4) . . . . ? O229 C35 O228 Mn2 -174.4(4) . . . . ? C37 C35 O228 Mn2 3.8(6) . . . . ? O129 Mn2 O228 C35 99.7(4) 2_766 . . . ? N215 Mn2 O228 C35 -164.1(4) . . . . ? N208 Mn2 O228 C35 -44.2(8) . . . . ? N201 Mn2 O228 C35 -92.1(4) . . . . ? N218 Mn2 O228 C35 -15.7(4) . . . . ? O228 C35 C37 N218 19.8(7) . . . . ? O229 C35 C37 N218 -162.0(5) . . . . ? C35 C37 N218 C39 -154.5(5) . . . . ? C35 C37 N218 C40A 97.2(10) . . . . ? C35 C37 N218 C40B 79.4(6) . . . . ? C35 C37 N218 Mn2 -30.1(6) . . . . ? O129 Mn2 N218 C37 -73.9(4) 2_766 . . . ? O228 Mn2 N218 C37 24.0(4) . . . . ? N215 Mn2 N218 C37 80.8(4) . . . . ? N208 Mn2 N218 C37 -163.3(4) . . . . ? N201 Mn2 N218 C37 124.0(4) . . . . ? O129 Mn2 N218 C39 46.6(5) 2_766 . . . ? O228 Mn2 N218 C39 144.5(5) . . . . ? N215 Mn2 N218 C39 -158.7(5) . . . . ? N208 Mn2 N218 C39 -42.9(5) . . . . ? N201 Mn2 N218 C39 -115.5(5) . . . . ? O129 Mn2 N218 C40A 141.9(9) 2_766 . . . ? O228 Mn2 N218 C40A -120.2(9) . . . . ? N215 Mn2 N218 C40A -63.4(9) . . . . ? N208 Mn2 N218 C40A 52.5(9) . . . . ? N201 Mn2 N218 C40A -20.2(9) . . . . ? O129 Mn2 N218 C40B 177.9(6) 2_766 . . . ? O228 Mn2 N218 C40B -84.2(6) . . . . ? N215 Mn2 N218 C40B -27.3(6) . . . . ? N208 Mn2 N218 C40B 88.5(6) . . . . ? N201 Mn2 N218 C40B 15.9(6) . . . . ? C37 N218 C40A C41A -74.8(16) . . . . ? C39 N218 C40A C41A 169.6(13) . . . . ? C40B N218 C40A C41A -43.7(11) . . . . ? Mn2 N218 C40A C41A 54.4(14) . . . . ? C37 N218 C40B C41B -156.4(10) . . . . ? C39 N218 C40B C41B 84.6(11) . . . . ? C40A N218 C40B C41B 46.0(13) . . . . ? Mn2 N218 C40B C41B -44.3(12) . . . . ? N218 C40A C41A N201 -74(3) . . . . ? N218 C40B C41B N201 57.0(18) . . . . ? C40A C41A N201 C43 157.8(19) . . . . ? C40A C41A N201 C50 -78(3) . . . . ? C40A C41A N201 C41B -59(2) . . . . ? C40A C41A N201 Mn2 49(2) . . . . ? C40B C41B N201 C43 85.2(15) . . . . ? C40B C41B N201 C50 -152.3(13) . . . . ? C40B C41B N201 C41A 43(3) . . . . ? C40B C41B N201 Mn2 -36.7(16) . . . . ? O129 Mn2 N201 C43 103.8(5) 2_766 . . . ? O228 Mn2 N201 C43 -46.8(3) . . . . ? N215 Mn2 N201 C43 35.0(3) . . . . ? N208 Mn2 N201 C43 145.2(4) . . . . ? N218 Mn2 N201 C43 -118.6(3) . . . . ? O129 Mn2 N201 C50 -14.8(6) 2_766 . . . ? O228 Mn2 N201 C50 -165.4(3) . . . . ? N215 Mn2 N201 C50 -83.7(4) . . . . ? N208 Mn2 N201 C50 26.6(3) . . . . ? N218 Mn2 N201 C50 122.8(4) . . . . ? O129 Mn2 N201 C41A -152.1(11) 2_766 . . . ? O228 Mn2 N201 C41A 57.3(11) . . . . ? N215 Mn2 N201 C41A 139.1(11) . . . . ? N208 Mn2 N201 C41A -110.7(11) . . . . ? N218 Mn2 N201 C41A -14.5(11) . . . . ? O129 Mn2 N201 C41B -126.8(7) 2_766 . . . ? O228 Mn2 N201 C41B 82.7(7) . . . . ? N215 Mn2 N201 C41B 164.4(7) . . . . ? N208 Mn2 N201 C41B -85.3(7) . . . . ? N218 Mn2 N201 C41B 10.9(7) . . . . ? C50 N201 C43 C44 77.8(6) . . . . ? C41A N201 C43 C44 -146.7(14) . . . . ? C41B N201 C43 C44 -163.4(7) . . . . ? Mn2 N201 C43 C44 -39.9(5) . . . . ? N201 C43 C44 N215 19.1(7) . . . . ? N201 C43 C44 C45 -161.7(6) . . . . ? N215 C44 C45 C46 2.7(9) . . . . ? C43 C44 C45 C46 -176.5(6) . . . . ? C44 C45 C46 C47 -3.5(11) . . . . ? C45 C46 C47 C48 2.5(11) . . . . ? C46 C47 C48 N215 -0.6(10) . . . . ? C45 C44 N215 C48 -0.9(8) . . . . ? C43 C44 N215 C48 178.3(5) . . . . ? C45 C44 N215 Mn2 -164.9(5) . . . . ? C43 C44 N215 Mn2 14.3(6) . . . . ? C47 C48 N215 C44 -0.2(8) . . . . ? C47 C48 N215 Mn2 162.1(5) . . . . ? O129 Mn2 N215 C44 174.7(4) 2_766 . . . ? O228 Mn2 N215 C44 70.9(4) . . . . ? N208 Mn2 N215 C44 -95.3(4) . . . . ? N201 Mn2 N215 C44 -27.6(4) . . . . ? N218 Mn2 N215 C44 17.1(5) . . . . ? O129 Mn2 N215 C48 11.9(4) 2_766 . . . ? O228 Mn2 N215 C48 -91.9(4) . . . . ? N208 Mn2 N215 C48 101.9(4) . . . . ? N201 Mn2 N215 C48 169.6(4) . . . . ? N218 Mn2 N215 C48 -145.8(4) . . . . ? C43 N201 C50 C51 -154.4(5) . . . . ? C41A N201 C50 C51 85.7(12) . . . . ? C41B N201 C50 C51 77.5(9) . . . . ? Mn2 N201 C50 C51 -38.5(5) . . . . ? N201 C50 C51 N208 31.1(6) . . . . ? N201 C50 C51 C52 -152.2(5) . . . . ? N208 C51 C52 C53 -0.2(9) . . . . ? C50 C51 C52 C53 -176.6(6) . . . . ? C51 C52 C53 C54 0.4(11) . . . . ? C52 C53 C54 C55 -0.9(10) . . . . ? C53 C54 C55 N208 1.3(8) . . . . ? C54 C55 N208 C51 -1.1(7) . . . . ? C54 C55 N208 Mn2 -177.3(4) . . . . ? C52 C51 N208 C55 0.5(7) . . . . ? C50 C51 N208 C55 177.1(5) . . . . ? C52 C51 N208 Mn2 177.1(5) . . . . ? C50 C51 N208 Mn2 -6.4(6) . . . . ? O129 Mn2 N208 C55 -30.6(4) 2_766 . . . ? O228 Mn2 N208 C55 114.5(6) . . . . ? N215 Mn2 N208 C55 -127.9(4) . . . . ? N201 Mn2 N208 C55 164.9(4) . . . . ? N218 Mn2 N208 C55 87.3(4) . . . . ? O129 Mn2 N208 C51 153.1(4) 2_766 . . . ? O228 Mn2 N208 C51 -61.8(7) . . . . ? N215 Mn2 N208 C51 55.8(4) . . . . ? N201 Mn2 N208 C51 -11.4(3) . . . . ? N218 Mn2 N208 C51 -89.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.770 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.086