# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email komil@chemistry.uoc.gr _publ_contact_author_name 'Constantinos J. Milios' _publ_author_name C.Milios data_af78a _database_code_depnum_ccdc_archive 'CCDC 837606' #TrackingRef 'complex_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H70 Mn6 N12 O22, 10(C H4 O)' _chemical_formula_sum 'C66 H110 Mn6 N12 O32' _chemical_formula_weight 1913.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.514(3) _cell_length_b 11.767(4) _cell_length_c 17.730(6) _cell_angle_alpha 95.80(5) _cell_angle_beta 105.73(5) _cell_angle_gamma 99.28(5) _cell_volume 2255.3(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11577 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 29.0 _exptl_crystal_description needle _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Xcalibur PX KM4CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25491 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.1266 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.96 _reflns_number_total 11459 _reflns_number_gt 5759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^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 11459 _refine_ls_number_parameters 537 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1390 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1942 _refine_ls_wR_factor_gt 0.1751 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.39093(6) 0.57200(6) 0.47263(4) 0.02235(18) Uani 1 1 d . . . Mn2 Mn 0.39274(6) 0.45224(7) 0.30187(4) 0.0269(2) Uani 1 1 d . A . Mn3 Mn 0.14852(6) 0.39153(7) 0.35537(4) 0.0295(2) Uani 1 1 d . A . O1 O 0.3197(2) 0.4530(3) 0.38478(17) 0.0224(7) Uani 1 1 d . . . O11 O 0.4413(2) 0.6797(3) 0.56752(18) 0.0236(7) Uani 1 1 d . . . O21 O 0.1224(3) 0.4847(3) 0.4442(2) 0.0362(9) Uani 1 1 d . . . N11 N 0.1294(3) 0.6058(4) 0.5847(3) 0.0388(12) Uani 1 1 d . . . H11A H 0.0578 0.5656 0.5543 0.047 Uiso 1 1 d R . . H11B H 0.1295 0.6463 0.6292 0.047 Uiso 1 1 d R . . N21 N 0.2305(3) 0.5593(3) 0.4917(2) 0.0255(9) Uani 1 1 d . . . C11 C 0.3325(4) 0.8178(4) 0.6186(3) 0.0300(11) Uani 1 1 d . . . C21 C 0.3240(5) 0.8838(5) 0.5584(4) 0.0471(15) Uani 1 1 d . . . H21 H 0.3332 0.8525 0.5093 0.057 Uiso 1 1 calc R . . C31 C 0.3022(7) 0.9960(6) 0.5691(5) 0.066(2) Uani 1 1 d . . . H31 H 0.2969 1.0418 0.5276 0.079 Uiso 1 1 calc R . . C41 C 0.2878(7) 1.0414(6) 0.6419(5) 0.066(2) Uani 1 1 d . . . H41 H 0.2714 1.1177 0.6492 0.080 Uiso 1 1 calc R . . C51 C 0.2972(6) 0.9778(6) 0.7005(4) 0.0564(18) Uani 1 1 d . . . H51 H 0.2883 1.0095 0.7496 0.068 Uiso 1 1 calc R . . C61 C 0.3202(5) 0.8648(5) 0.6905(3) 0.0409(13) Uani 1 1 d . . . H61 H 0.3273 0.8203 0.7328 0.049 Uiso 1 1 calc R . . C71 C 0.3498(4) 0.6931(4) 0.6068(3) 0.0239(10) Uani 1 1 d . . . H71 H 0.3756 0.6677 0.6600 0.029 Uiso 1 1 calc R . . C81 C 0.2278(4) 0.6149(4) 0.5584(3) 0.0236(10) Uani 1 1 d . . . O12 O 0.4987(3) 0.4562(3) 0.23723(18) 0.0299(8) Uani 1 1 d . . . O22 O 0.5544(2) 0.5834(3) 0.45752(17) 0.0211(7) Uani 1 1 d . . . N12 N 0.7438(3) 0.6452(3) 0.3977(2) 0.0291(9) Uani 1 1 d . . . H12A H 0.8122 0.6806 0.3901 0.035 Uiso 1 1 d R . . H12B H 0.7564 0.6815 0.4459 0.035 Uiso 1 1 d R . . N22 N 0.5394(3) 0.5533(3) 0.3765(2) 0.0233(8) Uani 1 1 d . . . C12 C 0.6273(5) 0.6303(5) 0.2164(3) 0.0367(13) Uani 1 1 d . . . C22 C 0.5277(7) 0.6819(5) 0.1875(3) 0.0527(17) Uani 1 1 d . . . H22 H 0.4531 0.6577 0.1998 0.063 Uiso 1 1 calc R . . C32 C 0.5363(8) 0.7701(6) 0.1400(4) 0.073(2) Uani 1 1 d . . . H32 H 0.4677 0.8050 0.1195 0.087 Uiso 1 1 calc R . . C42 C 0.6467(11) 0.8052(7) 0.1237(4) 0.088(3) Uani 1 1 d . . . H42 H 0.6532 0.8635 0.0909 0.106 Uiso 1 1 calc R . . C52 C 0.7452(9) 0.7575(7) 0.1539(4) 0.076(3) Uani 1 1 d . . . H52 H 0.8210 0.7840 0.1436 0.091 Uiso 1 1 calc R . . C62 C 0.7356(6) 0.6696(5) 0.2001(4) 0.0538(17) Uani 1 1 d . . . H62 H 0.8052 0.6362 0.2208 0.065 Uiso 1 1 calc R . . C72 C 0.6149(4) 0.5342(4) 0.2654(3) 0.0291(11) Uani 1 1 d . . . H72 H 0.6798 0.4880 0.2629 0.035 Uiso 1 1 calc R . . C82 C 0.6367(4) 0.5832(4) 0.3521(3) 0.0255(10) Uani 1 1 d . . . O13 O -0.0140(3) 0.3065(4) 0.3120(2) 0.0456(10) Uani 1 1 d . . . O23 O 0.2778(3) 0.3165(3) 0.2385(2) 0.0401(10) Uani 1 1 d . . . N13 N 0.0777(4) 0.1599(5) 0.1512(3) 0.0575(15) Uani 1 1 d . . . H13A H 0.0100 0.1124 0.1215 0.069 Uiso 1 1 d R . . H13B H 0.1529 0.1667 0.1471 0.069 Uiso 1 1 d R . . N23 N 0.1690(3) 0.3059(4) 0.2604(3) 0.0393(11) Uani 1 1 d . . . C13 C -0.1508(4) 0.2361(6) 0.1776(3) 0.0443(15) Uani 1 1 d . . . C23 C -0.1793(6) 0.3424(6) 0.1745(4) 0.0565(17) Uani 1 1 d . . . H23 H -0.1286 0.4089 0.2099 0.068 Uiso 1 1 calc R . . C33 C -0.2836(6) 0.3504(7) 0.1186(4) 0.070(2) Uani 1 1 d . . . H33 H -0.3035 0.4254 0.1153 0.084 Uiso 1 1 calc R . . C43 C -0.3619(6) 0.2585(8) 0.0669(4) 0.076(2) Uani 1 1 d . . . H43 H -0.4352 0.2695 0.0305 0.091 Uiso 1 1 calc R . . C53 C -0.3332(6) 0.1494(7) 0.0681(4) 0.069(2) Uani 1 1 d . . . H53 H -0.3852 0.0842 0.0320 0.083 Uiso 1 1 calc R . . C63 C -0.2237(5) 0.1367(6) 0.1247(4) 0.0537(17) Uani 1 1 d . . . H63 H -0.2002 0.0630 0.1268 0.064 Uiso 1 1 calc R . . C73 C -0.0397(5) 0.2180(5) 0.2446(3) 0.0393(13) Uani 1 1 d . . . H73 H -0.0592 0.1396 0.2605 0.047 Uiso 1 1 calc R . . C83 C 0.0754(5) 0.2265(5) 0.2168(3) 0.0376(13) Uani 1 1 d . . . O14 O 0.1048(4) 0.5370(4) 0.2837(3) 0.0650(13) Uani 1 1 d . . . O24 O 0.2841(4) 0.5738(4) 0.2475(3) 0.0616(13) Uani 1 1 d . . . C14 C 0.1651(7) 0.5664(7) 0.2353(4) 0.069(2) Uani 0.56(4) 1 d P A 1 C24 C 0.0832(16) 0.569(2) 0.1486(10) 0.084(7) Uiso 0.56(4) 1 d P A 1 H24D H 0.0638 0.4909 0.1176 0.127 Uiso 0.56(4) 1 calc PR A 1 H24E H 0.1283 0.6239 0.1234 0.127 Uiso 0.56(4) 1 calc PR A 1 H24F H 0.0067 0.5937 0.1508 0.127 Uiso 0.56(4) 1 calc PR A 1 C141 C 0.1651(7) 0.5664(7) 0.2353(4) 0.069(2) Uani 0.44(4) 1 d P A 2 C241 C 0.113(2) 0.648(4) 0.1691(16) 0.102(10) Uiso 0.44(4) 1 d P A 2 H24A H 0.0364 0.6680 0.1755 0.153 Uiso 0.44(4) 1 calc PR A 2 H24B H 0.0968 0.6050 0.1158 0.153 Uiso 0.44(4) 1 calc PR A 2 H24C H 0.1743 0.7194 0.1764 0.153 Uiso 0.44(4) 1 calc PR A 2 O1M O 0.3573(3) 0.7118(3) 0.3935(2) 0.0370(8) Uani 1 1 d . . . H1M H 0.3215 0.6762 0.3475 0.055 Uiso 1 1 calc R . . C1M C 0.4499(7) 0.8028(7) 0.3910(5) 0.077(2) Uani 1 1 d . . . H1M1 H 0.4636 0.8650 0.4355 0.115 Uiso 1 1 calc R . . H1M2 H 0.4249 0.8334 0.3410 0.115 Uiso 1 1 calc R . . H1M3 H 0.5262 0.7738 0.3950 0.115 Uiso 1 1 calc R . . O2M O 0.1820(3) 0.2460(3) 0.4332(2) 0.0417(10) Uani 1 1 d . . . H2M H 0.2384 0.2143 0.4245 0.050 Uiso 1 1 d R A . C2M C 0.0838(5) 0.1523(6) 0.4335(4) 0.0590(18) Uani 1 1 d . A . H2M1 H 0.0061 0.1803 0.4232 0.088 Uiso 1 1 calc R . . H2M2 H 0.1024 0.1259 0.4854 0.088 Uiso 1 1 calc R . . H2M3 H 0.0766 0.0874 0.3922 0.088 Uiso 1 1 calc R . . O3M O 0.6391(3) 0.8512(3) 0.5904(2) 0.0487(11) Uani 1 1 d . . . H3M H 0.5750 0.8005 0.5829 0.073 Uiso 1 1 calc R . . C3M C 0.6662(6) 0.9171(6) 0.6635(4) 0.0650(19) Uani 1 1 d . . . H3M1 H 0.6962 0.8706 0.7048 0.097 Uiso 1 1 calc R . . H3M2 H 0.5919 0.9421 0.6700 0.097 Uiso 1 1 calc R . . H3M3 H 0.7298 0.9857 0.6678 0.097 Uiso 1 1 calc R . . O4M O 0.3859(4) 0.3675(4) 0.0811(2) 0.0592(12) Uani 1 1 d . . . H4M H 0.4293 0.4001 0.1267 0.089 Uiso 1 1 d R B . C4M C 0.3011(12) 0.4265(11) 0.0533(7) 0.062(4) Uiso 0.559(15) 1 d P B 1 H4M1 H 0.3389 0.5091 0.0600 0.093 Uiso 0.559(15) 1 calc PR B 1 H4M2 H 0.2395 0.4174 0.0821 0.093 Uiso 0.559(15) 1 calc PR B 1 H4M3 H 0.2614 0.3974 -0.0032 0.093 Uiso 0.559(15) 1 calc PR B 1 C4MA C 0.3977(19) 0.4551(17) 0.0300(11) 0.087(7) Uiso 0.441(15) 1 d P B 2 H4M4 H 0.3454 0.4242 -0.0241 0.131 Uiso 0.441(15) 1 calc PR B 2 H4M5 H 0.4836 0.4753 0.0300 0.131 Uiso 0.441(15) 1 calc PR B 2 H4M6 H 0.3719 0.5249 0.0496 0.131 Uiso 0.441(15) 1 calc PR B 2 O5M O -0.0791(4) -0.0587(4) 0.0581(3) 0.0792(16) Uani 1 1 d . . . H5M H -0.1452 -0.0875 0.0225 0.119 Uiso 1 1 d R . . C5M C 0.0075(9) -0.1395(12) 0.0607(6) 0.151(5) Uani 1 1 d . . . H5M1 H 0.0601 -0.1179 0.0272 0.226 Uiso 1 1 calc R . . H5M2 H -0.0390 -0.2193 0.0411 0.226 Uiso 1 1 calc R . . H5M3 H 0.0587 -0.1347 0.1154 0.226 Uiso 1 1 calc R . . O6M O 0.9768(4) 0.6740(4) 0.3647(4) 0.0759(16) Uani 1 1 d . . . H6M H 1.0157 0.6227 0.3549 0.114 Uiso 1 1 calc R . . C6M C 1.0448(7) 0.7803(7) 0.3690(6) 0.105(3) Uani 1 1 d . . . H6M1 H 0.9934 0.8391 0.3690 0.157 Uiso 1 1 calc R . . H6M2 H 1.0770 0.7818 0.3232 0.157 Uiso 1 1 calc R . . H6M3 H 1.1136 0.7974 0.4180 0.157 Uiso 1 1 calc R . . O7M O 0.2815(4) 0.1453(4) 0.0717(3) 0.0706(14) Uani 1 1 d . . . H7M H 0.3156 0.2149 0.0743 0.106 Uiso 1 1 calc R . . C7M C 0.3619(7) 0.0893(8) 0.1265(5) 0.082(2) Uani 1 1 d . . . H7M1 H 0.4324 0.0788 0.1075 0.123 Uiso 1 1 calc R . . H7M2 H 0.3168 0.0132 0.1306 0.123 Uiso 1 1 calc R . . H7M3 H 0.3911 0.1379 0.1788 0.123 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0134(3) 0.0282(4) 0.0217(4) -0.0069(3) 0.0044(3) 0.0013(3) Mn2 0.0188(3) 0.0375(5) 0.0206(4) -0.0077(3) 0.0067(3) 0.0010(3) Mn3 0.0143(3) 0.0435(5) 0.0235(4) -0.0150(3) 0.0043(3) -0.0007(3) O1 0.0151(13) 0.0272(18) 0.0214(16) -0.0041(14) 0.0053(12) -0.0006(13) O11 0.0158(14) 0.0258(18) 0.0254(17) -0.0076(14) 0.0070(13) -0.0010(13) O21 0.0126(14) 0.049(2) 0.0355(19) -0.0226(17) 0.0036(14) -0.0039(14) N11 0.0168(18) 0.053(3) 0.036(2) -0.028(2) 0.0088(18) -0.0040(18) N21 0.0134(16) 0.033(2) 0.024(2) -0.0092(18) 0.0032(15) 0.0012(16) C11 0.020(2) 0.026(3) 0.038(3) -0.008(2) 0.004(2) 0.003(2) C21 0.056(4) 0.042(4) 0.044(3) 0.000(3) 0.010(3) 0.024(3) C31 0.088(5) 0.039(4) 0.076(5) 0.019(4) 0.023(4) 0.024(4) C41 0.075(5) 0.029(4) 0.095(6) -0.013(4) 0.032(5) 0.014(3) C51 0.062(4) 0.045(4) 0.060(4) -0.017(4) 0.028(4) 0.003(3) C61 0.046(3) 0.031(3) 0.041(3) -0.015(3) 0.017(3) 0.001(2) C71 0.017(2) 0.030(3) 0.022(2) -0.007(2) 0.0045(18) 0.0051(19) C81 0.0151(19) 0.024(3) 0.028(2) -0.005(2) 0.0047(18) 0.0010(18) O12 0.0282(17) 0.035(2) 0.0228(17) -0.0068(15) 0.0114(14) -0.0037(15) O22 0.0174(14) 0.0262(18) 0.0178(15) -0.0023(13) 0.0057(12) 0.0010(13) N12 0.0208(18) 0.033(2) 0.031(2) -0.0040(19) 0.0123(17) -0.0034(17) N22 0.0234(18) 0.028(2) 0.0178(19) -0.0007(17) 0.0086(16) 0.0022(16) C12 0.053(3) 0.030(3) 0.022(3) -0.004(2) 0.013(2) -0.005(3) C22 0.087(5) 0.034(3) 0.030(3) 0.000(3) 0.016(3) -0.002(3) C32 0.130(7) 0.039(4) 0.028(3) -0.006(3) 0.006(4) -0.010(4) C42 0.167(9) 0.042(5) 0.028(4) -0.006(3) 0.026(5) -0.045(5) C52 0.108(7) 0.062(5) 0.043(4) -0.004(4) 0.031(5) -0.033(5) C62 0.073(4) 0.043(4) 0.040(3) -0.006(3) 0.029(3) -0.017(3) C72 0.028(2) 0.033(3) 0.025(2) -0.006(2) 0.014(2) -0.005(2) C82 0.025(2) 0.029(3) 0.022(2) 0.000(2) 0.0091(19) 0.004(2) O13 0.0245(17) 0.067(3) 0.033(2) -0.0260(19) 0.0063(16) -0.0015(17) O23 0.0196(16) 0.057(3) 0.037(2) -0.0206(19) 0.0136(15) -0.0045(16) N13 0.036(3) 0.069(4) 0.056(3) -0.028(3) 0.018(2) -0.008(2) N23 0.0178(19) 0.056(3) 0.034(2) -0.018(2) 0.0057(18) -0.0019(19) C13 0.021(2) 0.063(4) 0.038(3) -0.010(3) 0.000(2) 0.004(3) C23 0.061(4) 0.064(5) 0.037(3) 0.014(3) -0.001(3) 0.014(4) C33 0.068(5) 0.099(6) 0.034(3) -0.012(4) 0.001(3) 0.030(4) C43 0.051(4) 0.113(7) 0.045(4) -0.031(4) -0.014(3) 0.041(4) C53 0.044(4) 0.100(6) 0.045(4) -0.025(4) -0.009(3) 0.018(4) C63 0.036(3) 0.069(5) 0.050(4) -0.005(3) 0.007(3) 0.012(3) C73 0.032(3) 0.048(4) 0.036(3) -0.005(3) 0.012(2) 0.005(2) C83 0.032(3) 0.043(3) 0.035(3) -0.004(3) 0.009(2) 0.006(2) O14 0.064(3) 0.080(4) 0.058(3) 0.015(3) 0.020(3) 0.028(3) O24 0.063(3) 0.090(4) 0.056(3) 0.037(3) 0.030(2) 0.045(3) C14 0.065(5) 0.087(6) 0.062(5) 0.026(4) 0.018(4) 0.023(4) C141 0.065(5) 0.087(6) 0.062(5) 0.026(4) 0.018(4) 0.023(4) O1M 0.041(2) 0.034(2) 0.034(2) 0.0023(18) 0.0089(17) 0.0079(17) C1M 0.093(6) 0.065(5) 0.092(6) 0.026(5) 0.051(5) 0.023(5) O2M 0.0284(18) 0.038(2) 0.053(2) -0.0161(19) 0.0204(18) -0.0105(16) C2M 0.039(3) 0.051(4) 0.083(5) -0.001(4) 0.027(3) -0.012(3) O3M 0.038(2) 0.037(2) 0.063(3) -0.014(2) 0.020(2) -0.0138(18) C3M 0.044(4) 0.067(5) 0.070(5) -0.013(4) 0.012(3) -0.003(3) O4M 0.064(3) 0.068(3) 0.033(2) -0.008(2) 0.003(2) 0.005(2) O5M 0.047(3) 0.068(3) 0.102(4) -0.027(3) 0.011(3) -0.003(2) C5M 0.090(8) 0.231(15) 0.098(8) 0.003(9) 0.020(7) -0.034(9) O6M 0.051(3) 0.056(3) 0.149(5) 0.030(3) 0.067(3) 0.018(2) C6M 0.045(4) 0.078(6) 0.175(10) -0.019(6) 0.027(6) -0.003(4) O7M 0.058(3) 0.070(4) 0.067(3) -0.008(3) 0.006(3) -0.005(3) C7M 0.062(5) 0.117(7) 0.070(5) 0.000(5) 0.021(4) 0.029(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.886(3) . ? Mn1 O11 1.891(3) . ? Mn1 N21 1.952(3) . ? Mn1 O22 1.958(3) . ? Mn1 O22 2.383(3) 2_666 ? Mn1 Mn2 3.2145(18) . ? Mn2 O1 1.881(3) . ? Mn2 O12 1.886(3) . ? Mn2 O23 1.927(4) . ? Mn2 N22 1.960(4) . ? Mn2 O24 2.177(4) . ? Mn2 Mn3 3.2019(15) . ? Mn3 O13 1.885(4) . ? Mn3 O1 1.894(3) . ? Mn3 O21 1.947(3) . ? Mn3 N23 1.963(4) . ? Mn3 O14 2.274(5) . ? Mn3 O2M 2.321(4) . ? O11 C71 1.433(5) . ? O21 N21 1.400(5) . ? N11 C81 1.330(5) . ? N11 H11A 0.8800 . ? N11 H11B 0.8800 . ? N21 C81 1.302(6) . ? C11 C21 1.374(8) . ? C11 C61 1.391(7) . ? C11 C71 1.513(7) . ? C21 C31 1.387(8) . ? C21 H21 0.9500 . ? C31 C41 1.409(10) . ? C31 H31 0.9500 . ? C41 C51 1.332(9) . ? C41 H41 0.9500 . ? C51 C61 1.401(8) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C71 C81 1.525(6) . ? C71 H71 1.0000 . ? O12 C72 1.425(5) . ? O22 N22 1.400(4) . ? O22 Mn1 2.383(3) 2_666 ? N12 C82 1.325(6) . ? N12 H12A 0.8800 . ? N12 H12B 0.8800 . ? N22 C82 1.316(5) . ? C12 C62 1.374(8) . ? C12 C22 1.383(8) . ? C12 C72 1.506(7) . ? C22 C32 1.410(9) . ? C22 H22 0.9500 . ? C32 C42 1.387(11) . ? C32 H32 0.9500 . ? C42 C52 1.350(12) . ? C42 H42 0.9500 . ? C52 C62 1.392(10) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C72 C82 1.525(6) . ? C72 H72 1.0000 . ? O13 C73 1.434(6) . ? O23 N23 1.399(5) . ? N13 C83 1.344(7) . ? N13 H13A 0.8800 . ? N13 H13B 0.8800 . ? N23 C83 1.307(6) . ? C13 C23 1.346(9) . ? C13 C63 1.409(8) . ? C13 C73 1.552(7) . ? C23 C33 1.358(8) . ? C23 H23 0.9500 . ? C33 C43 1.364(10) . ? C33 H33 0.9500 . ? C43 C53 1.377(10) . ? C43 H43 0.9500 . ? C53 C63 1.423(8) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? C73 C83 1.527(7) . ? C73 H73 1.0000 . ? O14 C14 1.283(8) . ? O24 C14 1.315(8) . ? C14 C24 1.578(17) . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? O1M C1M 1.397(8) . ? O1M H1M 0.8400 . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? O2M C2M 1.448(6) . ? O2M H2M 0.8400 . ? C2M H2M1 0.9800 . ? C2M H2M2 0.9800 . ? C2M H2M3 0.9800 . ? O3M C3M 1.370(7) . ? O3M H3M 0.8400 . ? C3M H3M1 0.9800 . ? C3M H3M2 0.9800 . ? C3M H3M3 0.9800 . ? O4M C4M 1.306(12) . ? O4M C4MA 1.454(19) . ? O4M H4M 0.8400 . ? C4M H4M1 0.9800 . ? C4M H4M2 0.9800 . ? C4M H4M3 0.9800 . ? C4MA H4M4 0.9800 . ? C4MA H4M5 0.9800 . ? C4MA H4M6 0.9800 . ? O5M C5M 1.479(13) . ? O5M H5M 0.8400 . ? C5M H5M1 0.9800 . ? C5M H5M2 0.9800 . ? C5M H5M3 0.9800 . ? O6M C6M 1.348(9) . ? O6M H6M 0.8400 . ? C6M H6M1 0.9800 . ? C6M H6M2 0.9800 . ? C6M H6M3 0.9800 . ? O7M C7M 1.440(8) . ? O7M H7M 0.8400 . ? C7M H7M1 0.9800 . ? C7M H7M2 0.9800 . ? C7M H7M3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O11 170.38(13) . . ? O1 Mn1 N21 88.75(15) . . ? O11 Mn1 N21 82.67(15) . . ? O1 Mn1 O22 92.39(13) . . ? O11 Mn1 O22 96.05(13) . . ? N21 Mn1 O22 177.83(15) . . ? O1 Mn1 O22 84.32(13) . 2_666 ? O11 Mn1 O22 91.98(13) . 2_666 ? N21 Mn1 O22 94.39(15) . 2_666 ? O22 Mn1 O22 83.89(13) . 2_666 ? O1 Mn1 Mn2 31.38(9) . . ? O11 Mn1 Mn2 158.24(9) . . ? N21 Mn1 Mn2 116.38(12) . . ? O22 Mn1 Mn2 65.22(10) . . ? O22 Mn1 Mn2 96.62(8) 2_666 . ? O1 Mn2 O12 167.26(14) . . ? O1 Mn2 O23 94.05(14) . . ? O12 Mn2 O23 94.71(14) . . ? O1 Mn2 N22 87.74(14) . . ? O12 Mn2 N22 81.11(14) . . ? O23 Mn2 N22 162.16(17) . . ? O1 Mn2 O24 91.24(14) . . ? O12 Mn2 O24 97.37(15) . . ? O23 Mn2 O24 93.87(19) . . ? N22 Mn2 O24 103.84(19) . . ? O1 Mn2 Mn3 32.09(9) . . ? O12 Mn2 Mn3 159.76(10) . . ? O23 Mn2 Mn3 66.32(10) . . ? N22 Mn2 Mn3 119.12(11) . . ? O24 Mn2 Mn3 77.86(12) . . ? O1 Mn2 Mn1 31.46(9) . . ? O12 Mn2 Mn1 138.87(11) . . ? O23 Mn2 Mn1 125.51(10) . . ? N22 Mn2 Mn1 58.01(11) . . ? O24 Mn2 Mn1 88.89(12) . . ? Mn3 Mn2 Mn1 61.21(5) . . ? O13 Mn3 O1 167.98(14) . . ? O13 Mn3 O21 97.55(14) . . ? O1 Mn3 O21 94.11(14) . . ? O13 Mn3 N23 81.57(16) . . ? O1 Mn3 N23 87.03(15) . . ? O21 Mn3 N23 175.53(19) . . ? O13 Mn3 O14 91.39(19) . . ? O1 Mn3 O14 92.00(16) . . ? O21 Mn3 O14 87.69(16) . . ? N23 Mn3 O14 87.96(19) . . ? O13 Mn3 O2M 86.53(17) . . ? O1 Mn3 O2M 90.81(14) . . ? O21 Mn3 O2M 88.77(15) . . ? N23 Mn3 O2M 95.54(17) . . ? O14 Mn3 O2M 175.62(14) . . ? O13 Mn3 Mn2 138.39(11) . . ? O1 Mn3 Mn2 31.86(9) . . ? O21 Mn3 Mn2 122.05(11) . . ? N23 Mn3 Mn2 57.93(13) . . ? O14 Mn3 Mn2 79.01(12) . . ? O2M Mn3 Mn2 105.07(9) . . ? Mn2 O1 Mn1 117.16(15) . . ? Mn2 O1 Mn3 116.04(16) . . ? Mn1 O1 Mn3 119.63(15) . . ? C71 O11 Mn1 116.7(2) . . ? N21 O21 Mn3 112.5(2) . . ? C81 N11 H11A 120.2 . . ? C81 N11 H11B 122.6 . . ? H11A N11 H11B 116.7 . . ? C81 N21 O21 117.9(3) . . ? C81 N21 Mn1 116.7(3) . . ? O21 N21 Mn1 124.9(3) . . ? C21 C11 C61 119.4(5) . . ? C21 C11 C71 121.1(4) . . ? C61 C11 C71 119.4(5) . . ? C11 C21 C31 120.3(6) . . ? C11 C21 H21 119.9 . . ? C31 C21 H21 119.9 . . ? C21 C31 C41 119.5(6) . . ? C21 C31 H31 120.3 . . ? C41 C31 H31 120.3 . . ? C51 C41 C31 120.2(6) . . ? C51 C41 H41 119.9 . . ? C31 C41 H41 119.9 . . ? C41 C51 C61 120.7(6) . . ? C41 C51 H51 119.7 . . ? C61 C51 H51 119.7 . . ? C11 C61 C51 119.9(6) . . ? C11 C61 H61 120.1 . . ? C51 C61 H61 120.1 . . ? O11 C71 C11 112.6(4) . . ? O11 C71 C81 109.1(3) . . ? C11 C71 C81 109.4(4) . . ? O11 C71 H71 108.6 . . ? C11 C71 H71 108.6 . . ? C81 C71 H71 108.6 . . ? N21 C81 N11 124.6(4) . . ? N21 C81 C71 114.4(4) . . ? N11 C81 C71 121.0(4) . . ? C72 O12 Mn2 118.1(3) . . ? N22 O22 Mn1 108.1(2) . . ? N22 O22 Mn1 110.6(2) . 2_666 ? Mn1 O22 Mn1 96.11(13) . 2_666 ? C82 N12 H12A 136.0 . . ? C82 N12 H12B 124.7 . . ? H12A N12 H12B 97.0 . . ? C82 N22 O22 116.7(4) . . ? C82 N22 Mn2 118.4(3) . . ? O22 N22 Mn2 124.3(2) . . ? C62 C12 C22 118.7(6) . . ? C62 C12 C72 121.8(5) . . ? C22 C12 C72 119.4(5) . . ? C12 C22 C32 120.4(7) . . ? C12 C22 H22 119.8 . . ? C32 C22 H22 119.8 . . ? C42 C32 C22 118.8(8) . . ? C42 C32 H32 120.6 . . ? C22 C32 H32 120.6 . . ? C52 C42 C32 120.8(7) . . ? C52 C42 H42 119.6 . . ? C32 C42 H42 119.6 . . ? C42 C52 C62 120.0(7) . . ? C42 C52 H52 120.0 . . ? C62 C52 H52 120.0 . . ? C12 C62 C52 121.2(7) . . ? C12 C62 H62 119.4 . . ? C52 C62 H62 119.4 . . ? O12 C72 C12 113.3(4) . . ? O12 C72 C82 109.0(3) . . ? C12 C72 C82 111.2(4) . . ? O12 C72 H72 107.7 . . ? C12 C72 H72 107.7 . . ? C82 C72 H72 107.7 . . ? N22 C82 N12 124.6(4) . . ? N22 C82 C72 112.4(4) . . ? N12 C82 C72 122.9(4) . . ? C73 O13 Mn3 118.3(3) . . ? N23 O23 Mn2 109.0(3) . . ? C83 N13 H13A 119.6 . . ? C83 N13 H13B 111.4 . . ? H13A N13 H13B 128.8 . . ? C83 N23 O23 117.1(4) . . ? C83 N23 Mn3 117.1(3) . . ? O23 N23 Mn3 125.6(3) . . ? C23 C13 C63 122.2(6) . . ? C23 C13 C73 120.1(5) . . ? C63 C13 C73 117.5(6) . . ? C13 C23 C33 117.2(7) . . ? C13 C23 H23 121.4 . . ? C33 C23 H23 121.4 . . ? C23 C33 C43 124.6(8) . . ? C23 C33 H33 117.7 . . ? C43 C33 H33 117.7 . . ? C33 C43 C53 119.1(6) . . ? C33 C43 H43 120.5 . . ? C53 C43 H43 120.5 . . ? C43 C53 C63 118.4(7) . . ? C43 C53 H53 120.8 . . ? C63 C53 H53 120.8 . . ? C13 C63 C53 118.4(6) . . ? C13 C63 H63 120.8 . . ? C53 C63 H63 120.8 . . ? O13 C73 C83 107.8(4) . . ? O13 C73 C13 110.0(4) . . ? C83 C73 C13 110.6(4) . . ? O13 C73 H73 109.4 . . ? C83 C73 H73 109.4 . . ? C13 C73 H73 109.4 . . ? N23 C83 N13 123.3(5) . . ? N23 C83 C73 114.5(4) . . ? N13 C83 C73 122.1(5) . . ? C14 O14 Mn3 120.6(4) . . ? C14 O24 Mn2 126.1(5) . . ? O14 C14 O24 125.9(6) . . ? O14 C14 C24 114.9(8) . . ? O24 C14 C24 118.1(8) . . ? H24A C241 H24B 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C1M O1M H1M 109.5 . . ? O1M C1M H1M1 109.5 . . ? O1M C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1M C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? C2M O2M Mn3 122.3(4) . . ? C2M O2M H2M 106.3 . . ? Mn3 O2M H2M 110.4 . . ? O2M C2M H2M1 109.5 . . ? O2M C2M H2M2 109.5 . . ? H2M1 C2M H2M2 109.5 . . ? O2M C2M H2M3 109.5 . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C3M O3M H3M 109.5 . . ? O3M C3M H3M1 109.5 . . ? O3M C3M H3M2 109.5 . . ? H3M1 C3M H3M2 109.5 . . ? O3M C3M H3M3 109.5 . . ? H3M1 C3M H3M3 109.5 . . ? H3M2 C3M H3M3 109.5 . . ? C4M O4M C4MA 55.6(9) . . ? C4M O4M H4M 109.8 . . ? C4MA O4M H4M 105.0 . . ? O4M C4M H4M1 109.5 . . ? O4M C4M H4M2 109.5 . . ? O4M C4M H4M3 109.5 . . ? O4M C4MA H4M4 109.5 . . ? O4M C4MA H4M5 109.5 . . ? H4M4 C4MA H4M5 109.5 . . ? O4M C4MA H4M6 109.5 . . ? H4M4 C4MA H4M6 109.5 . . ? H4M5 C4MA H4M6 109.5 . . ? C5M O5M H5M 109.1 . . ? O5M C5M H5M1 109.5 . . ? O5M C5M H5M2 109.5 . . ? H5M1 C5M H5M2 109.5 . . ? O5M C5M H5M3 109.5 . . ? H5M1 C5M H5M3 109.5 . . ? H5M2 C5M H5M3 109.5 . . ? C6M O6M H6M 109.5 . . ? O6M C6M H6M1 109.5 . . ? O6M C6M H6M2 109.5 . . ? H6M1 C6M H6M2 109.5 . . ? O6M C6M H6M3 109.5 . . ? H6M1 C6M H6M3 109.5 . . ? H6M2 C6M H6M3 109.5 . . ? C7M O7M H7M 109.5 . . ? O7M C7M H7M1 109.5 . . ? O7M C7M H7M2 109.5 . . ? H7M1 C7M H7M2 109.5 . . ? O7M C7M H7M3 109.5 . . ? H7M1 C7M H7M3 109.5 . . ? H7M2 C7M H7M3 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 O11 Mn1 Mn2 O1 -179.8(3) . . . . ? N21 Mn1 Mn2 O1 -30.7(2) . . . . ? O22 Mn1 Mn2 O1 147.7(2) . . . . ? O22 Mn1 Mn2 O1 67.57(19) 2_666 . . . ? O1 Mn1 Mn2 O12 -165.8(2) . . . . ? O11 Mn1 Mn2 O12 14.3(3) . . . . ? N21 Mn1 Mn2 O12 163.5(2) . . . . ? O22 Mn1 Mn2 O12 -18.2(2) . . . . ? O22 Mn1 Mn2 O12 -98.28(19) 2_666 . . . ? O1 Mn1 Mn2 O23 0.2(2) . . . . ? O11 Mn1 Mn2 O23 -179.6(3) . . . . ? N21 Mn1 Mn2 O23 -30.5(2) . . . . ? O22 Mn1 Mn2 O23 147.91(18) . . . . ? O22 Mn1 Mn2 O23 67.79(17) 2_666 . . . ? O1 Mn1 Mn2 N22 -158.7(2) . . . . ? O11 Mn1 Mn2 N22 21.5(3) . . . . ? N21 Mn1 Mn2 N22 170.61(19) . . . . ? O22 Mn1 Mn2 N22 -11.02(17) . . . . ? O22 Mn1 Mn2 N22 -91.14(15) 2_666 . . . ? O1 Mn1 Mn2 O24 94.2(2) . . . . ? O11 Mn1 Mn2 O24 -85.6(3) . . . . ? N21 Mn1 Mn2 O24 63.50(19) . . . . ? O22 Mn1 Mn2 O24 -118.12(17) . . . . ? O22 Mn1 Mn2 O24 161.76(15) 2_666 . . . ? O1 Mn1 Mn2 Mn3 17.45(18) . . . . ? O11 Mn1 Mn2 Mn3 -162.4(3) . . . . ? N21 Mn1 Mn2 Mn3 -13.24(14) . . . . ? O22 Mn1 Mn2 Mn3 165.13(11) . . . . ? O22 Mn1 Mn2 Mn3 85.01(8) 2_666 . . . ? O1 Mn2 Mn3 O13 -168.1(3) . . . . ? O12 Mn2 Mn3 O13 1.0(4) . . . . ? O23 Mn2 Mn3 O13 -20.5(2) . . . . ? N22 Mn2 Mn3 O13 178.5(2) . . . . ? O24 Mn2 Mn3 O13 79.3(2) . . . . ? Mn1 Mn2 Mn3 O13 174.7(2) . . . . ? O12 Mn2 Mn3 O1 169.1(4) . . . . ? O23 Mn2 Mn3 O1 147.6(2) . . . . ? N22 Mn2 Mn3 O1 -13.4(2) . . . . ? O24 Mn2 Mn3 O1 -112.6(2) . . . . ? Mn1 Mn2 Mn3 O1 -17.13(18) . . . . ? O1 Mn2 Mn3 O21 32.1(2) . . . . ? O12 Mn2 Mn3 O21 -158.8(3) . . . . ? O23 Mn2 Mn3 O21 179.71(19) . . . . ? N22 Mn2 Mn3 O21 18.70(19) . . . . ? O24 Mn2 Mn3 O21 -80.5(2) . . . . ? Mn1 Mn2 Mn3 O21 14.97(14) . . . . ? O1 Mn2 Mn3 N23 -153.2(3) . . . . ? O12 Mn2 Mn3 N23 16.0(4) . . . . ? O23 Mn2 Mn3 N23 -5.6(2) . . . . ? N22 Mn2 Mn3 N23 -166.6(2) . . . . ? O24 Mn2 Mn3 N23 94.2(2) . . . . ? Mn1 Mn2 Mn3 N23 -170.30(17) . . . . ? O1 Mn2 Mn3 O14 112.3(2) . . . . ? O12 Mn2 Mn3 O14 -78.6(4) . . . . ? O23 Mn2 Mn3 O14 -100.08(18) . . . . ? N22 Mn2 Mn3 O14 98.91(18) . . . . ? O24 Mn2 Mn3 O14 -0.31(18) . . . . ? Mn1 Mn2 Mn3 O14 95.18(13) . . . . ? O1 Mn2 Mn3 O2M -66.1(2) . . . . ? O12 Mn2 Mn3 O2M 103.1(3) . . . . ? O23 Mn2 Mn3 O2M 81.53(16) . . . . ? N22 Mn2 Mn3 O2M -79.47(17) . . . . ? O24 Mn2 Mn3 O2M -178.70(16) . . . . ? Mn1 Mn2 Mn3 O2M -83.21(10) . . . . ? O12 Mn2 O1 Mn1 46.8(7) . . . . ? O23 Mn2 O1 Mn1 -179.82(18) . . . . ? N22 Mn2 O1 Mn1 17.95(19) . . . . ? O24 Mn2 O1 Mn1 -85.8(2) . . . . ? Mn3 Mn2 O1 Mn1 -150.4(3) . . . . ? O12 Mn2 O1 Mn3 -162.8(6) . . . . ? O23 Mn2 O1 Mn3 -29.5(2) . . . . ? N22 Mn2 O1 Mn3 168.32(19) . . . . ? O24 Mn2 O1 Mn3 64.5(2) . . . . ? Mn1 Mn2 O1 Mn3 150.4(3) . . . . ? N21 Mn1 O1 Mn2 152.8(2) . . . . ? O22 Mn1 O1 Mn2 -29.06(19) . . . . ? O22 Mn1 O1 Mn2 -112.68(17) 2_666 . . . ? N21 Mn1 O1 Mn3 3.5(2) . . . . ? O22 Mn1 O1 Mn3 -178.32(18) . . . . ? O22 Mn1 O1 Mn3 98.06(18) 2_666 . . . ? Mn2 Mn1 O1 Mn3 -149.3(3) . . . . ? O13 Mn3 O1 Mn2 41.0(9) . . . . ? O21 Mn3 O1 Mn2 -153.16(19) . . . . ? N23 Mn3 O1 Mn2 22.5(2) . . . . ? O14 Mn3 O1 Mn2 -65.3(2) . . . . ? O2M Mn3 O1 Mn2 118.02(18) . . . . ? O13 Mn3 O1 Mn1 -169.5(7) . . . . ? O21 Mn3 O1 Mn1 -3.6(2) . . . . ? N23 Mn3 O1 Mn1 172.1(2) . . . . ? O14 Mn3 O1 Mn1 84.3(2) . . . . ? O2M Mn3 O1 Mn1 -92.39(19) . . . . ? Mn2 Mn3 O1 Mn1 149.6(3) . . . . ? N21 Mn1 O11 C71 3.8(3) . . . . ? O22 Mn1 O11 C71 -174.4(3) . . . . ? O22 Mn1 O11 C71 -90.4(3) 2_666 . . . ? Mn2 Mn1 O11 C71 156.2(2) . . . . ? O13 Mn3 O21 N21 178.8(3) . . . . ? O1 Mn3 O21 N21 1.8(3) . . . . ? O14 Mn3 O21 N21 -90.1(3) . . . . ? O2M Mn3 O21 N21 92.5(3) . . . . ? Mn2 Mn3 O21 N21 -14.6(3) . . . . ? Mn3 O21 N21 C81 -171.4(3) . . . . ? O1 Mn1 N21 C81 169.6(4) . . . . ? O22 Mn1 N21 C81 85.3(4) 2_666 . . . ? Mn2 Mn1 N21 C81 -175.0(3) . . . . ? O1 Mn1 N21 O21 -2.3(4) . . . . ? O11 Mn1 N21 O21 -178.0(4) . . . . ? O22 Mn1 N21 O21 -86.6(4) 2_666 . . . ? Mn2 Mn1 N21 O21 13.1(4) . . . . ? C61 C11 C21 C31 -0.6(9) . . . . ? C71 C11 C21 C31 176.8(5) . . . . ? C11 C21 C31 C41 -0.5(10) . . . . ? C21 C31 C41 C51 1.1(11) . . . . ? C31 C41 C51 C61 -0.7(11) . . . . ? C21 C11 C61 C51 1.1(8) . . . . ? C71 C11 C61 C51 -176.4(5) . . . . ? C41 C51 C61 C11 -0.4(9) . . . . ? Mn1 O11 C71 C11 -123.0(3) . . . . ? Mn1 O11 C71 C81 -1.4(5) . . . . ? C21 C11 C71 O11 45.1(6) . . . . ? C61 C11 C71 O11 -137.4(4) . . . . ? C21 C11 C71 C81 -76.3(6) . . . . ? C61 C11 C71 C81 101.1(5) . . . . ? O21 N21 C81 N11 0.0(7) . . . . ? Mn1 N21 C81 N11 -172.5(4) . . . . ? O21 N21 C81 C71 179.3(4) . . . . ? Mn1 N21 C81 C71 6.8(5) . . . . ? O11 C71 C81 N21 -3.5(6) . . . . ? C11 C71 C81 N21 120.0(4) . . . . ? O11 C71 C81 N11 175.8(4) . . . . ? C11 C71 C81 N11 -60.7(6) . . . . ? O1 Mn2 O12 C72 -37.1(8) . . . . ? O23 Mn2 O12 C72 -170.4(3) . . . . ? N22 Mn2 O12 C72 -7.8(3) . . . . ? O24 Mn2 O12 C72 95.1(3) . . . . ? Mn3 Mn2 O12 C72 169.9(3) . . . . ? Mn1 Mn2 O12 C72 -1.7(4) . . . . ? O1 Mn1 O22 N22 30.0(3) . . . . ? O11 Mn1 O22 N22 -154.6(3) . . . . ? O22 Mn1 O22 N22 114.0(3) 2_666 . . . ? Mn2 Mn1 O22 N22 13.8(2) . . . . ? O1 Mn1 O22 Mn1 -84.03(13) . . . 2_666 ? O11 Mn1 O22 Mn1 91.35(13) . . . 2_666 ? O22 Mn1 O22 Mn1 -0.002(2) 2_666 . . 2_666 ? Mn2 Mn1 O22 Mn1 -100.21(11) . . . 2_666 ? Mn1 O22 N22 C82 163.5(3) . . . . ? Mn1 O22 N22 C82 -92.4(4) 2_666 . . . ? Mn1 O22 N22 Mn2 -25.5(4) . . . . ? Mn1 O22 N22 Mn2 78.6(3) 2_666 . . . ? O1 Mn2 N22 C82 177.0(4) . . . . ? O12 Mn2 N22 C82 3.2(3) . . . . ? O23 Mn2 N22 C82 80.7(6) . . . . ? O24 Mn2 N22 C82 -92.3(4) . . . . ? Mn3 Mn2 N22 C82 -176.0(3) . . . . ? Mn1 Mn2 N22 C82 -172.1(4) . . . . ? O1 Mn2 N22 O22 6.1(3) . . . . ? O12 Mn2 N22 O22 -167.7(3) . . . . ? O23 Mn2 N22 O22 -90.1(5) . . . . ? O24 Mn2 N22 O22 96.9(3) . . . . ? Mn3 Mn2 N22 O22 13.2(4) . . . . ? Mn1 Mn2 N22 O22 17.1(3) . . . . ? C62 C12 C22 C32 2.3(8) . . . . ? C72 C12 C22 C32 -178.5(5) . . . . ? C12 C22 C32 C42 -0.9(9) . . . . ? C22 C32 C42 C52 -1.3(10) . . . . ? C32 C42 C52 C62 1.9(11) . . . . ? C22 C12 C62 C52 -1.7(8) . . . . ? C72 C12 C62 C52 179.2(5) . . . . ? C42 C52 C62 C12 -0.4(10) . . . . ? Mn2 O12 C72 C12 -114.0(4) . . . . ? Mn2 O12 C72 C82 10.4(5) . . . . ? C62 C12 C72 O12 -141.5(5) . . . . ? C22 C12 C72 O12 39.4(6) . . . . ? C62 C12 C72 C82 95.3(6) . . . . ? C22 C12 C72 C82 -83.9(6) . . . . ? O22 N22 C82 N12 -4.3(7) . . . . ? Mn2 N22 C82 N12 -175.9(4) . . . . ? O22 N22 C82 C72 173.3(4) . . . . ? Mn2 N22 C82 C72 1.7(5) . . . . ? O12 C72 C82 N22 -7.4(6) . . . . ? C12 C72 C82 N22 118.2(5) . . . . ? O12 C72 C82 N12 170.2(4) . . . . ? C12 C72 C82 N12 -64.1(6) . . . . ? O1 Mn3 O13 C73 -10.9(10) . . . . ? O21 Mn3 O13 C73 -176.7(4) . . . . ? N23 Mn3 O13 C73 7.7(4) . . . . ? O14 Mn3 O13 C73 95.5(4) . . . . ? O2M Mn3 O13 C73 -88.4(4) . . . . ? Mn2 Mn3 O13 C73 20.5(5) . . . . ? O1 Mn2 O23 N23 23.6(3) . . . . ? O12 Mn2 O23 N23 -165.7(3) . . . . ? N22 Mn2 O23 N23 118.8(5) . . . . ? O24 Mn2 O23 N23 -67.9(3) . . . . ? Mn3 Mn2 O23 N23 7.0(3) . . . . ? Mn1 Mn2 O23 N23 23.5(4) . . . . ? Mn2 O23 N23 C83 171.9(4) . . . . ? Mn2 O23 N23 Mn3 -12.9(5) . . . . ? O13 Mn3 N23 C83 -6.2(4) . . . . ? O1 Mn3 N23 C83 170.0(4) . . . . ? O14 Mn3 N23 C83 -97.9(4) . . . . ? O2M Mn3 N23 C83 79.5(4) . . . . ? Mn2 Mn3 N23 C83 -176.2(5) . . . . ? O13 Mn3 N23 O23 178.7(5) . . . . ? O1 Mn3 N23 O23 -5.2(4) . . . . ? O14 Mn3 N23 O23 87.0(4) . . . . ? O2M Mn3 N23 O23 -95.7(4) . . . . ? Mn2 Mn3 N23 O23 8.6(3) . . . . ? C63 C13 C23 C33 1.1(9) . . . . ? C73 C13 C23 C33 -174.5(5) . . . . ? C13 C23 C33 C43 1.3(11) . . . . ? C23 C33 C43 C53 -2.5(12) . . . . ? C33 C43 C53 C63 1.3(11) . . . . ? C23 C13 C63 C53 -2.2(9) . . . . ? C73 C13 C63 C53 173.5(5) . . . . ? C43 C53 C63 C13 0.9(10) . . . . ? Mn3 O13 C73 C83 -7.7(6) . . . . ? Mn3 O13 C73 C13 -128.4(4) . . . . ? C23 C13 C73 O13 24.1(7) . . . . ? C63 C13 C73 O13 -151.7(5) . . . . ? C23 C13 C73 C83 -94.9(6) . . . . ? C63 C13 C73 C83 89.2(6) . . . . ? O23 N23 C83 N13 -3.0(9) . . . . ? Mn3 N23 C83 N13 -178.6(5) . . . . ? O23 N23 C83 C73 179.0(4) . . . . ? Mn3 N23 C83 C73 3.4(7) . . . . ? O13 C73 C83 N23 2.5(7) . . . . ? C13 C73 C83 N23 122.8(5) . . . . ? O13 C73 C83 N13 -175.5(5) . . . . ? C13 C73 C83 N13 -55.1(8) . . . . ? O13 Mn3 O14 C14 -121.6(5) . . . . ? O1 Mn3 O14 C14 46.9(5) . . . . ? O21 Mn3 O14 C14 140.9(5) . . . . ? N23 Mn3 O14 C14 -40.1(5) . . . . ? Mn2 Mn3 O14 C14 17.6(5) . . . . ? O1 Mn2 O24 C14 -46.9(6) . . . . ? O12 Mn2 O24 C14 142.5(6) . . . . ? O23 Mn2 O24 C14 47.3(6) . . . . ? N22 Mn2 O24 C14 -134.9(6) . . . . ? Mn3 Mn2 O24 C14 -17.5(5) . . . . ? Mn1 Mn2 O24 C14 -78.3(6) . . . . ? Mn3 O14 C14 O24 -39.7(10) . . . . ? Mn3 O14 C14 C24 127.6(12) . . . . ? Mn2 O24 C14 O14 41.2(11) . . . . ? Mn2 O24 C14 C24 -125.8(12) . . . . ? O13 Mn3 O2M C2M -5.6(4) . . . . ? O1 Mn3 O2M C2M -173.8(4) . . . . ? O21 Mn3 O2M C2M 92.1(4) . . . . ? N23 Mn3 O2M C2M -86.7(4) . . . . ? Mn2 Mn3 O2M C2M -145.0(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11 H11A O21 0.88 2.07 2.808(5) 140.7 2_566 N11 H11B O13 0.88 2.01 2.751(5) 141.2 2_566 N12 H12B O2M 0.88 2.11 2.974(6) 168.6 2_666 N12 H12A O6M 0.88 2.07 2.873(5) 150.4 . N13 H13B O7M 0.88 2.27 3.066(7) 149.7 . N13 H13A O5M 0.88 2.15 2.938(7) 148.7 . O1M H1M O24 0.84 1.94 2.752(6) 162.3 . O2M H2M O3M 0.84 1.78 2.619(5) 178.0 2_666 O3M H3M O11 0.84 1.86 2.697(5) 175.4 . O4M H4M O12 0.84 1.91 2.733(5) 167.3 . O5M H5M O7M 0.84 1.93 2.760(7) 170.1 2 O6M H6M O14 0.84 2.11 2.877(6) 152.5 1_655 O6M H6M O21 0.84 2.60 3.213(6) 130.7 1_655 O7M H7M O4M 0.84 1.82 2.664(7) 178.2 . _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.30 _refine_diff_density_min -0.82 _refine_diff_density_rms 0.109 # Attachment 'complex_2.cif' data_lm142a _database_code_depnum_ccdc_archive 'CCDC 837607' #TrackingRef 'complex_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66.37 H75.75 Mn8 N16 O22.5, 5.25(C H4 O), 9.45(H2 O)' _chemical_formula_sum 'C71.62 H115.65 Mn8 N16 O38.20' _chemical_formula_weight 2251.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 16.608(5) _cell_length_b 17.907(5) _cell_length_c 19.811(6) _cell_angle_alpha 78.12(4) _cell_angle_beta 65.89(4) _cell_angle_gamma 75.79(3) _cell_volume 5176(3) _cell_formula_units_Z 2 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 12488 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.0 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2326 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(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 'Xcalibur PX KM4CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51148 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.1589 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.03 _reflns_number_total 27840 _reflns_number_gt 13808 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^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 27840 _refine_ls_number_parameters 1284 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1136 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.75271(4) 0.25470(3) 0.64983(3) 0.01367(13) Uani 1 1 d . A . Mn2 Mn 0.80814(4) 0.16798(3) 0.79186(3) 0.01482(13) Uani 1 1 d . A . Mn3 Mn 0.76718(4) 0.36328(3) 0.74926(3) 0.01383(13) Uani 1 1 d . A . Mn4 Mn 0.60875(4) 0.25954(3) 0.83073(3) 0.01460(13) Uani 1 1 d . A . Mn5 Mn 0.60193(4) 0.41359(3) 0.68762(3) 0.01429(13) Uani 1 1 d . . . Mn6 Mn 0.71948(4) 0.27369(3) 0.93032(3) 0.01811(14) Uani 1 1 d . A . Mn7 Mn 0.96093(4) 0.25353(3) 0.66093(3) 0.01977(15) Uani 1 1 d . . . Mn8 Mn 0.66199(4) 0.10490(3) 0.74351(3) 0.01624(14) Uani 1 1 d . A . O1 O 0.71458(15) 0.35291(13) 0.68441(13) 0.0143(6) Uani 1 1 d . A . O2 O 0.70675(16) 0.22338(13) 0.86166(14) 0.0156(6) Uani 1 1 d . . . O3 O 0.84127(15) 0.26223(13) 0.73167(13) 0.0153(6) Uani 1 1 d . A . O4 O 0.67885(16) 0.20604(13) 0.74353(13) 0.0149(6) Uani 1 1 d . . . O21 O 0.76184(16) 0.08613(13) 0.65081(14) 0.0188(6) Uani 1 1 d . . . N11 N 0.7995(2) 0.15272(16) 0.61542(16) 0.0149(7) Uani 1 1 d . A . N21 N 0.9157(2) 0.07937(18) 0.52631(18) 0.0263(9) Uani 1 1 d . A . H1N1 H 0.9672 0.0823 0.4887 0.032 Uiso 1 1 d R . . H2N1 H 0.8987 0.0344 0.5467 0.032 Uiso 1 1 d R . . O11 O 0.86381(16) 0.27572(14) 0.57239(14) 0.0182(6) Uani 1 1 d . . . C81 C 0.8744(2) 0.1447(2) 0.5564(2) 0.0138(8) Uani 1 1 d . . . C71 C 0.9095(2) 0.2195(2) 0.5217(2) 0.0173(9) Uani 1 1 d . A . H71 H 0.9747 0.2096 0.5129 0.021 Uiso 1 1 calc R . . C11 C 0.8997(3) 0.2457(2) 0.4470(2) 0.0235(10) Uani 1 1 d . . . C21 C 0.8205(4) 0.2918(3) 0.4440(3) 0.0595(17) Uani 1 1 d . A . H21 H 0.7735 0.3069 0.4889 0.071 Uiso 1 1 calc R . . C31 C 0.8080(4) 0.3167(4) 0.3767(3) 0.082(2) Uani 1 1 d . . . H31 H 0.7543 0.3499 0.3752 0.098 Uiso 1 1 calc R A . C41 C 0.8765(4) 0.2913(4) 0.3118(3) 0.072(2) Uani 1 1 d . A . H41 H 0.8682 0.3046 0.2658 0.087 Uiso 1 1 calc R . . C51 C 0.9556(4) 0.2475(3) 0.3140(3) 0.0494(15) Uani 1 1 d . . . H51 H 1.0021 0.2310 0.2694 0.059 Uiso 1 1 calc R A . C61 C 0.9687(3) 0.2266(3) 0.3816(2) 0.0369(12) Uani 1 1 d . A . H61 H 1.0252 0.1993 0.3820 0.044 Uiso 1 1 calc R . . O22 O 0.97977(16) 0.14345(14) 0.66082(14) 0.0218(7) Uani 1 1 d . A . N12 N 0.91048(19) 0.11104(17) 0.71800(17) 0.0162(7) Uani 1 1 d . . . N22 N 0.9826(2) -0.01093(18) 0.67838(19) 0.0301(9) Uani 1 1 d . . . H1N2 H 0.9764 -0.0595 0.6837 0.036 Uiso 1 1 d R A . H2N2 H 1.0250 0.0075 0.6389 0.036 Uiso 1 1 d R . . O12 O 0.76838(16) 0.07066(13) 0.81495(14) 0.0187(6) Uani 1 1 d . . . C82 C 0.9146(2) 0.0364(2) 0.7230(2) 0.0176(9) Uani 1 1 d . A . C72 C 0.8347(2) 0.0063(2) 0.7834(2) 0.0171(9) Uani 1 1 d . A . H72 H 0.8088 -0.0209 0.7599 0.021 Uiso 1 1 calc R . . C12 C 0.8611(3) -0.0519(2) 0.8425(2) 0.0221(10) Uani 1 1 d . . . C22 C 0.8696(3) -0.1304(2) 0.8426(2) 0.0310(11) Uani 1 1 d . A . H22 H 0.8584 -0.1481 0.8058 0.037 Uiso 1 1 calc R . . C32 C 0.8942(3) -0.1842(2) 0.8954(3) 0.0365(12) Uani 1 1 d . . . H32 H 0.9014 -0.2381 0.8934 0.044 Uiso 1 1 calc R A . C42 C 0.9080(3) -0.1597(3) 0.9504(3) 0.0393(13) Uani 1 1 d . A . H42 H 0.9256 -0.1963 0.9863 0.047 Uiso 1 1 calc R . . C52 C 0.8960(3) -0.0807(3) 0.9528(3) 0.0434(13) Uani 1 1 d . . . H52 H 0.9037 -0.0632 0.9916 0.052 Uiso 1 1 calc R A . C62 C 0.8728(3) -0.0266(2) 0.8992(3) 0.0379(12) Uani 1 1 d . A . H62 H 0.8650 0.0274 0.9013 0.045 Uiso 1 1 calc R . . O23 O 0.60911(16) 0.48492(13) 0.74558(14) 0.0169(6) Uani 1 1 d . I . N13 N 0.6699(2) 0.45207(16) 0.77946(17) 0.0152(7) Uani 1 1 d . . . N23 N 0.6160(2) 0.55624(17) 0.84943(17) 0.0193(7) Uani 1 1 d . . . H1N3 H 0.6177 0.5758 0.8860 0.023 Uiso 1 1 d R I . H2N3 H 0.5860 0.5788 0.8207 0.023 Uiso 1 1 d R . . O13 O 0.77296(16) 0.37151(14) 0.84291(14) 0.0172(6) Uani 1 1 d . . . C83 C 0.6695(2) 0.4887(2) 0.8302(2) 0.0151(9) Uani 1 1 d . A . C73 C 0.7329(2) 0.4456(2) 0.8693(2) 0.0173(9) Uani 1 1 d . A . H73 H 0.6963 0.4367 0.9238 0.021 Uiso 1 1 calc R . . C13 C 0.8015(3) 0.4952(2) 0.8594(2) 0.0192(9) Uani 1 1 d . . . C23 C 0.8841(3) 0.4895(3) 0.8009(2) 0.0303(11) Uani 1 1 d . A . H23 H 0.9022 0.4511 0.7683 0.036 Uiso 1 1 calc R . . C33 C 0.9403(3) 0.5406(3) 0.7905(2) 0.0361(12) Uani 1 1 d . . . H33 H 0.9974 0.5364 0.7508 0.043 Uiso 1 1 calc R A . C43 C 0.9146(3) 0.5965(3) 0.8362(3) 0.0373(12) Uani 1 1 d . A . H43 H 0.9532 0.6317 0.8276 0.045 Uiso 1 1 calc R . . C53 C 0.8325(3) 0.6022(3) 0.8951(3) 0.0347(12) Uani 1 1 d . . . H53 H 0.8147 0.6409 0.9274 0.042 Uiso 1 1 calc R A . C63 C 0.7769(3) 0.5510(2) 0.9065(2) 0.0255(10) Uani 1 1 d . A . H63 H 0.7208 0.5542 0.9474 0.031 Uiso 1 1 calc R . . O24 O 0.59723(16) 0.32422(14) 0.96296(14) 0.0180(6) Uani 1 1 d . . . N14 N 0.5612(2) 0.32654(17) 0.91030(17) 0.0178(7) Uani 1 1 d . A . N24 N 0.4602(2) 0.43536(17) 0.95973(17) 0.0227(8) Uani 1 1 d . A . H1N4 H 0.4901 0.4328 0.9882 0.027 Uiso 1 1 d R . . H2N4 H 0.4330 0.4826 0.9498 0.027 Uiso 1 1 d R . . O14 O 0.52763(16) 0.33725(13) 0.79529(13) 0.0166(6) Uani 1 1 d . A . C84 C 0.4954(2) 0.3837(2) 0.9095(2) 0.0180(9) Uani 1 1 d . . . C74 C 0.4627(2) 0.3869(2) 0.8478(2) 0.0173(9) Uani 1 1 d . A . H74 H 0.4602 0.4411 0.8220 0.021 Uiso 1 1 calc R . . C14 C 0.3685(2) 0.3679(2) 0.8770(2) 0.0169(9) Uani 1 1 d . . . C24 C 0.2944(3) 0.4263(2) 0.8896(2) 0.0260(10) Uani 1 1 d . A . H24 H 0.3019 0.4786 0.8821 0.031 Uiso 1 1 calc R . . C34 C 0.2090(3) 0.4099(2) 0.9129(2) 0.0318(11) Uani 1 1 d . . . H34 H 0.1584 0.4507 0.9214 0.038 Uiso 1 1 calc R A . C44 C 0.1982(3) 0.3343(3) 0.9237(2) 0.0306(11) Uani 1 1 d . A . H44 H 0.1400 0.3228 0.9387 0.037 Uiso 1 1 calc R . . C54 C 0.2711(3) 0.2749(2) 0.9129(2) 0.0249(10) Uani 1 1 d . . . H54 H 0.2630 0.2226 0.9210 0.030 Uiso 1 1 calc R A . C64 C 0.3567(3) 0.2914(2) 0.8899(2) 0.0230(10) Uani 1 1 d . A . H64 H 0.4070 0.2504 0.8831 0.028 Uiso 1 1 calc R . . O25 O 0.65361(16) 0.27812(14) 0.60242(14) 0.0173(6) Uani 1 1 d . . . N15 N 0.5919(2) 0.34416(17) 0.62764(17) 0.0173(7) Uani 1 1 d . A . N25 N 0.5314(3) 0.3384(2) 0.5420(2) 0.0443(11) Uani 1 1 d . A . H1N5 H 0.5579 0.2911 0.5310 0.053 Uiso 1 1 d R . . H2N5 H 0.4881 0.3579 0.5251 0.053 Uiso 1 1 d R . . O15 O 0.48923(16) 0.46412(14) 0.68182(15) 0.0194(6) Uani 1 1 d . A . C85 C 0.5356(3) 0.3715(2) 0.5957(3) 0.0273(10) Uani 1 1 d . . . C75 C 0.4739(3) 0.4477(2) 0.6194(2) 0.0301(11) Uani 1 1 d . A . H75 H 0.4911 0.4898 0.5772 0.036 Uiso 1 1 calc R . . C15 C 0.3767(3) 0.4449(2) 0.6414(2) 0.0242(10) Uani 1 1 d . . . C25 C 0.3330(3) 0.3965(3) 0.7034(3) 0.0455(14) Uani 1 1 d . A . H25 H 0.3643 0.3668 0.7337 0.055 Uiso 1 1 calc R . . C35 C 0.2457(4) 0.3908(4) 0.7216(3) 0.0569(17) Uani 1 1 d . . . H35 H 0.2161 0.3584 0.7649 0.068 Uiso 1 1 calc R A . C45 C 0.2012(3) 0.4329(4) 0.6760(3) 0.0566(16) Uani 1 1 d . A . H45 H 0.1406 0.4290 0.6884 0.068 Uiso 1 1 calc R . . C55 C 0.2418(3) 0.4790(3) 0.6144(3) 0.0531(15) Uani 1 1 d . . . H55 H 0.2099 0.5077 0.5842 0.064 Uiso 1 1 calc R A . C65 C 0.3318(3) 0.4846(3) 0.5952(3) 0.0410(13) Uani 1 1 d . A . H65 H 0.3617 0.5154 0.5508 0.049 Uiso 1 1 calc R . . O26 O 0.88412(17) 0.16038(14) 0.85975(14) 0.0202(6) Uani 1 1 d . . . N16 N 0.8367(2) 0.20853(19) 0.91516(19) 0.0236(8) Uani 1 1 d . A . N26 N 0.9339(3) 0.1475(3) 0.9757(2) 0.0652(14) Uani 1 1 d . A . H1N6 H 0.9636 0.1156 0.9416 0.078 Uiso 1 1 d R . . H2N6 H 0.9376 0.1533 1.0173 0.078 Uiso 1 1 d R . . O16 O 0.7334(2) 0.29843(17) 1.01024(17) 0.0357(8) Uani 1 1 d . . . C86 C 0.8635(3) 0.1996(3) 0.9700(3) 0.0393(12) Uani 1 1 d . . . C76 C 0.8064(3) 0.2540(3) 1.0293(3) 0.0386(12) Uani 1 1 d . A . H76 H 0.7827 0.2225 1.0788 0.046 Uiso 1 1 calc R . . C16 C 0.8617(3) 0.3071(3) 1.0333(3) 0.0405(12) Uani 1 1 d . . . C26 C 0.8697(3) 0.3102(3) 1.0990(3) 0.0438(13) Uani 1 1 d . A . H26 H 0.8400 0.2785 1.1428 0.053 Uiso 1 1 calc R . . C36 C 0.9211(4) 0.3595(3) 1.1015(3) 0.0538(15) Uani 1 1 d . . . H36 H 0.9264 0.3614 1.1471 0.065 Uiso 1 1 calc R A . C46 C 0.9647(3) 0.4061(3) 1.0376(3) 0.0449(14) Uani 1 1 d . A . H46 H 1.0011 0.4389 1.0388 0.054 Uiso 1 1 calc R . . C56 C 0.9540(4) 0.4040(3) 0.9714(3) 0.0480(14) Uani 1 1 d . . . H56 H 0.9812 0.4370 0.9279 0.058 Uiso 1 1 calc R A . C66 C 0.9040(4) 0.3540(3) 0.9694(3) 0.0547(15) Uani 1 1 d . A . H66 H 0.8984 0.3517 0.9241 0.066 Uiso 1 1 calc R . . O27 O 0.87105(16) 0.41913(13) 0.67273(14) 0.0177(6) Uani 1 1 d . . . N17 N 0.9485(2) 0.36669(17) 0.64346(17) 0.0172(7) Uani 1 1 d . A . N27 N 1.0225(2) 0.47077(17) 0.58466(18) 0.0210(8) Uani 1 1 d . A . H1N7 H 1.0675 0.4863 0.5457 0.025 Uiso 1 1 d R . . H2N7 H 0.9716 0.5041 0.5955 0.025 Uiso 1 1 d R . . O17 O 1.07550(16) 0.25976(14) 0.58764(15) 0.0239(7) Uani 1 1 d . A . C87 C 1.0200(3) 0.3949(2) 0.5982(2) 0.0182(9) Uani 1 1 d . . . C77 C 1.1006(3) 0.3346(2) 0.5635(2) 0.0226(10) Uani 1 1 d . A . H77 H 1.1488 0.3359 0.5810 0.027 Uiso 1 1 calc R . . C17 C 1.1360(3) 0.3500(2) 0.4797(2) 0.0246(10) Uani 1 1 d . . . C27 C 1.0846(3) 0.3455(2) 0.4411(2) 0.0260(10) Uani 1 1 d . A . H27 H 1.0265 0.3329 0.4678 0.031 Uiso 1 1 calc R . . C37 C 1.1166(3) 0.3593(2) 0.3641(2) 0.0313(11) Uani 1 1 d . . . H37 H 1.0807 0.3551 0.3384 0.038 Uiso 1 1 calc R A . C47 C 1.2007(3) 0.3790(2) 0.3241(3) 0.0365(13) Uani 1 1 d . A . H47 H 1.2224 0.3889 0.2713 0.044 Uiso 1 1 calc R . . C57 C 1.2519(3) 0.3838(3) 0.3620(3) 0.0427(15) Uani 1 1 d . . . H57 H 1.3094 0.3975 0.3349 0.051 Uiso 1 1 calc R A . C67 C 1.2214(3) 0.3692(2) 0.4393(2) 0.0328(12) Uani 1 1 d . A . H67 H 1.2581 0.3722 0.4646 0.039 Uiso 1 1 calc R . . O28 O 0.53869(16) 0.16962(13) 0.88528(14) 0.0181(6) Uani 1 1 d . . . N18 N 0.5647(2) 0.11067(16) 0.84134(17) 0.0158(7) Uani 1 1 d . A . N28 N 0.4505(2) 0.05196(18) 0.93335(18) 0.0243(9) Uani 1 1 d . A . H1N8 H 0.4443 0.0849 0.9633 0.029 Uiso 1 1 d R . . H2N8 H 0.4351 0.0068 0.9554 0.029 Uiso 1 1 d R . . O18 O 0.63414(17) 0.00494(13) 0.75740(14) 0.0193(6) Uani 1 1 d . . . C88 C 0.5209(2) 0.0529(2) 0.8688(2) 0.0180(9) Uani 1 1 d . . . C78 C 0.5551(3) -0.0110(2) 0.8188(2) 0.0204(9) Uani 1 1 d . A . H78 H 0.5083 -0.0108 0.7992 0.024 Uiso 1 1 calc R . . C18 C 0.5719(3) -0.0901(2) 0.8613(2) 0.0283(11) Uani 1 1 d . . . C28 C 0.5230(3) -0.1463(2) 0.8693(3) 0.0398(13) Uani 1 1 d . A . H28 H 0.4780 -0.1351 0.8489 0.048 Uiso 1 1 calc R . . C38 C 0.5406(4) -0.2205(3) 0.9082(3) 0.0533(17) Uani 1 1 d . . . H38 H 0.5069 -0.2589 0.9142 0.064 Uiso 1 1 calc R A . C48 C 0.6055(3) -0.2370(2) 0.9370(3) 0.0367(13) Uani 1 1 d . A . H48 H 0.6176 -0.2868 0.9625 0.044 Uiso 1 1 calc R . . C58 C 0.6536(3) -0.1807(3) 0.9288(3) 0.0422(13) Uani 1 1 d . . . H58 H 0.6987 -0.1922 0.9491 0.051 Uiso 1 1 calc R A . C68 C 0.6371(3) -0.1069(2) 0.8911(3) 0.0347(12) Uani 1 1 d . A . H68 H 0.6707 -0.0687 0.8861 0.042 Uiso 1 1 calc R . . O1M O 1.00923(19) 0.23120(17) 0.75588(16) 0.0317(8) Uani 0.674(4) 1 d P A 1 H1M H 0.9728 0.2085 0.7929 0.048 Uiso 0.674(4) 1 d PR A 1 C1M C 1.0372(6) 0.2846(5) 0.7792(4) 0.056(3) Uani 0.674(4) 1 d P A 1 H1M1 H 1.0931 0.2980 0.7405 0.084 Uiso 0.674(4) 1 calc PR A 1 H1M2 H 1.0473 0.2621 0.8252 0.084 Uiso 0.674(4) 1 calc PR A 1 H1M3 H 0.9909 0.3315 0.7885 0.084 Uiso 0.674(4) 1 calc PR A 1 O12M O 1.00923(19) 0.23120(17) 0.75588(16) 0.0317(8) Uani 0.201(12) 1 d P B 2 H12M H 0.9737 0.2551 0.7922 0.048 Uiso 0.201(12) 1 calc PR B 2 C12M C 1.0954(19) 0.2062(17) 0.7616(17) 0.064(11) Uiso 0.201(12) 1 d P B 2 H12A H 1.1426 0.2078 0.7117 0.096 Uiso 0.201(12) 1 calc PR B 2 H12B H 1.0996 0.1530 0.7868 0.096 Uiso 0.201(12) 1 calc PR B 2 H12C H 1.1028 0.2407 0.7904 0.096 Uiso 0.201(12) 1 calc PR B 2 O16W O 1.00923(19) 0.23120(17) 0.75588(16) 0.0317(8) Uani 0.125(12) 1 d P A 5 O2M O 0.57420(17) 0.15875(14) 0.67655(15) 0.0220(7) Uani 1 1 d . . . H2M H 0.6009 0.1968 0.6591 0.033 Uiso 1 1 d R A . C2M C 0.4799(3) 0.1860(3) 0.7136(3) 0.0515(15) Uani 1 1 d . A . H2M1 H 0.4508 0.1422 0.7434 0.077 Uiso 1 1 calc R . . H2M2 H 0.4535 0.2103 0.6765 0.077 Uiso 1 1 calc R . . H2M3 H 0.4710 0.2241 0.7463 0.077 Uiso 1 1 calc R . . O3M O 0.4293(2) 0.60846(18) 0.6998(2) 0.0465(9) Uani 1 1 d . . . H3M H 0.4480 0.5607 0.6974 0.070 Uiso 1 1 calc R . . C3M C 0.3336(3) 0.6225(3) 0.7389(3) 0.0499(14) Uani 1 1 d . . . H3M1 H 0.3195 0.6148 0.7927 0.075 Uiso 1 1 calc R . . H3M2 H 0.3075 0.5864 0.7264 0.075 Uiso 1 1 calc R . . H3M3 H 0.3088 0.6760 0.7242 0.075 Uiso 1 1 calc R . . O4M O 0.7738(2) -0.11361(15) 0.70639(18) 0.0379(9) Uani 1 1 d . . . H4M H 0.7276 -0.0813 0.7260 0.057 Uiso 1 1 calc R . . C4M C 0.7503(4) -0.1878(3) 0.7175(3) 0.0591(18) Uani 1 1 d . . . H4M1 H 0.7103 -0.1854 0.6916 0.089 Uiso 1 1 calc R . . H4M2 H 0.7198 -0.2029 0.7709 0.089 Uiso 1 1 calc R . . H4M3 H 0.8048 -0.2262 0.6975 0.089 Uiso 1 1 calc R . . O5M O 0.8658(5) 0.1009(5) 1.1531(4) 0.067(2) Uani 0.50 1 d P . . H5M H 0.8857 0.0539 1.1466 0.100 Uiso 0.50 1 d PR . . C5M C 0.8716(8) 0.1135(7) 1.2176(6) 0.064(4) Uani 0.50 1 d P . . H5M1 H 0.8240 0.1564 1.2395 0.096 Uiso 0.50 1 calc PR . . H5M2 H 0.9302 0.1268 1.2057 0.096 Uiso 0.50 1 calc PR . . H5M3 H 0.8646 0.0664 1.2533 0.096 Uiso 0.50 1 calc PR . . O6M O 0.4978(3) 0.65754(18) 0.78227(19) 0.0452(9) Uani 0.549(16) 1 d PD C 1 H6M H 0.4806 0.6358 0.7581 0.068 Uiso 0.549(16) 1 calc PR C 1 C6M C 0.5183(9) 0.7345(5) 0.7413(7) 0.068(5) Uiso 0.549(16) 1 d PD C 1 H6M1 H 0.4674 0.7753 0.7626 0.102 Uiso 0.549(16) 1 calc PR C 1 H6M2 H 0.5293 0.7353 0.6886 0.102 Uiso 0.549(16) 1 calc PR C 1 H6M3 H 0.5718 0.7436 0.7455 0.102 Uiso 0.549(16) 1 calc PR C 1 O13M O 0.4978(3) 0.65754(18) 0.78227(19) 0.0452(9) Uani 0.451(16) 1 d PD C 2 H13M H 0.5214 0.6515 0.7369 0.068 Uiso 0.451(16) 1 calc PR C 2 C13M C 0.4474(15) 0.7385(8) 0.7911(16) 0.165(12) Uiso 0.451(16) 1 d PD C 2 H13A H 0.3949 0.7388 0.8379 0.247 Uiso 0.451(16) 1 calc PR C 2 H13B H 0.4279 0.7587 0.7493 0.247 Uiso 0.451(16) 1 calc PR C 2 H13C H 0.4864 0.7712 0.7918 0.247 Uiso 0.451(16) 1 calc PR C 2 O7M O 0.5973(5) 0.1844(4) 0.4842(4) 0.0451(18) Uani 0.50 1 d P D 3 H7M H 0.6170 0.1459 0.5090 0.068 Uiso 0.50 1 calc PR D 3 C7M C 0.6432(11) 0.1822(9) 0.4172(9) 0.112(6) Uiso 0.50 1 d P D 3 H7M1 H 0.6489 0.2350 0.3924 0.169 Uiso 0.50 1 calc PR D 3 H7M2 H 0.6143 0.1582 0.3950 0.169 Uiso 0.50 1 calc PR D 3 H7M3 H 0.7029 0.1515 0.4110 0.169 Uiso 0.50 1 calc PR D 3 O8M O 0.4102(6) 0.2151(4) 0.4981(5) 0.069(2) Uani 0.50 1 d P E 3 H8M H 0.3877 0.2030 0.4717 0.104 Uiso 0.50 1 d PR E 3 C8M C 0.3417(10) 0.2218(7) 0.5753(9) 0.093(5) Uani 0.50 1 d P E 3 H8M1 H 0.3423 0.1706 0.6048 0.139 Uiso 0.50 1 calc PR E 3 H8M2 H 0.2821 0.2415 0.5732 0.139 Uiso 0.50 1 calc PR E 3 H8M3 H 0.3557 0.2576 0.5985 0.139 Uiso 0.50 1 calc PR E 3 O9M O 0.3506(7) 0.1563(6) 0.4197(6) 0.038(3) Uiso 0.30 1 d P F 1 H9M H 0.3537 0.1951 0.3872 0.057 Uiso 0.30 1 calc PR F 1 C9M C 0.2630(11) 0.1561(10) 0.4661(10) 0.052(5) Uiso 0.30 1 d P F 1 H9M1 H 0.2453 0.1917 0.5033 0.078 Uiso 0.30 1 calc PR F 1 H9M2 H 0.2561 0.1036 0.4913 0.078 Uiso 0.30 1 calc PR F 1 H9M3 H 0.2247 0.1729 0.4370 0.078 Uiso 0.30 1 calc PR F 1 O10M O 0.6432(12) 0.1792(10) 1.1960(10) 0.088(6) Uiso 0.25 1 d P G 10 H10M H 0.6437 0.2020 1.1543 0.132 Uiso 0.25 1 d PR G 10 C10M C 0.6889(13) 0.1001(11) 1.1916(12) 0.046(5) Uiso 0.25 1 d P G 10 H10A H 0.7489 0.0960 1.1915 0.069 Uiso 0.25 1 calc PR G 10 H10B H 0.6941 0.0833 1.1457 0.069 Uiso 0.25 1 calc PR G 10 H10C H 0.6549 0.0671 1.2347 0.069 Uiso 0.25 1 calc PR G 10 O11M O 0.6808(7) 0.1593(7) 1.0290(6) 0.128(4) Uiso 0.50 1 d P H 3 H11B H 0.6964 0.1983 1.0342 0.191 Uiso 0.50 1 d PR H 3 C11M C 0.7135(9) 0.0856(8) 1.0771(8) 0.072(4) Uiso 0.50 1 d P H 3 H11C H 0.6787 0.0902 1.1302 0.108 Uiso 0.50 1 calc PR H 3 H11D H 0.7772 0.0822 1.0666 0.108 Uiso 0.50 1 calc PR H 3 H11E H 0.7049 0.0388 1.0645 0.108 Uiso 0.50 1 calc PR H 3 O1W O 0.66640(17) 0.48561(14) 0.57856(14) 0.0227(7) Uani 1 1 d . I 3 H1W1 H 0.6407 0.5319 0.5682 0.034 Uiso 1 1 d R I 3 H2W1 H 0.7237 0.4749 0.5561 0.034 Uiso 1 1 d R I 3 O2W O 0.5935(12) 0.0153(10) 0.3082(10) 0.087(6) Uiso 0.25 1 d P J 4 O3W O 0.6222(2) 0.41708(16) 1.08679(17) 0.0382(8) Uani 1 1 d . . . H1W3 H 0.5776 0.4002 1.1228 0.057 Uiso 1 1 d R . . H2W3 H 0.6613 0.3831 1.0594 0.057 Uiso 1 1 d R . . O4W O 0.84817(16) 0.44117(14) 0.53782(14) 0.0209(6) Uani 1 1 d . . . H1W4 H 0.8538 0.4477 0.5774 0.031 Uiso 1 1 d R . . H2W4 H 0.8612 0.3944 0.5272 0.031 Uiso 1 1 d R . . O5W O 0.89035(18) -0.07852(15) 0.56509(17) 0.0368(9) Uani 1 1 d . . . H1W5 H 0.8750 -0.0970 0.5362 0.055 Uiso 1 1 d R . . H2W5 H 0.8590 -0.0840 0.6121 0.055 Uiso 1 1 d R . . O6W O 0.63954(19) 0.07467(15) 0.96859(16) 0.0330(8) Uani 1 1 d . . . H1W6 H 0.5970 0.1096 0.9615 0.049 Uiso 1 1 d R . . H2W6 H 0.6852 0.0582 0.9308 0.049 Uiso 1 1 d R . . O7W O 0.4343(2) 0.36439(18) 0.44028(19) 0.0490(9) Uani 1 1 d . . . H7W1 H 0.4177 0.3200 0.4526 0.073 Uiso 1 1 d R . . H7W2 H 0.4840 0.3680 0.4029 0.073 Uiso 1 1 d R . . O8W O 0.1764(3) 0.1436(2) 0.5124(3) 0.0439(14) Uani 0.70 1 d P K 2 O9W O 0.7022(3) 0.0686(3) 0.5368(3) 0.0754(18) Uani 0.75 1 d P . . O10W O 0.1723(3) 0.0076(3) 0.5909(3) 0.081(2) Uani 0.75 1 d P . . O11W O 0.4132(5) 0.0155(4) 0.3591(4) 0.060(2) Uani 0.50 1 d P . . O12W O 0.1451(7) 0.0950(6) 0.7111(7) 0.131(4) Uani 0.50 1 d P . . O13W O 0.2519(18) 0.1151(15) 0.8170(15) 0.150(9) Uiso 0.25 1 d P L 6 O14M O 0.730(2) 0.0316(18) 1.0996(18) 0.125(10) Uiso 0.20 1 d PD M 5 H14M H 0.6845 0.0358 1.0889 0.187 Uiso 0.20 1 d PR M 5 C14M C 0.736(4) -0.037(3) 1.153(3) 0.20(3) Uiso 0.20 1 d PD M 5 H14A H 0.6766 -0.0390 1.1928 0.295 Uiso 0.20 1 calc PR M 5 H14B H 0.7791 -0.0354 1.1735 0.295 Uiso 0.20 1 calc PR M 5 H14C H 0.7548 -0.0838 1.1271 0.295 Uiso 0.20 1 calc PR M 5 O14W O 0.9298(6) -0.0301(7) 1.1188(6) 0.101(4) Uani 0.50 1 d P . . O15W O 0.8978(14) -0.0619(11) 1.1456(12) 0.077(6) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0142(3) 0.0106(3) 0.0127(3) -0.0022(2) -0.0009(2) -0.0029(2) Mn2 0.0151(3) 0.0109(3) 0.0151(3) -0.0009(2) -0.0028(2) -0.0022(2) Mn3 0.0138(3) 0.0122(3) 0.0133(3) -0.0021(2) -0.0026(2) -0.0025(2) Mn4 0.0149(3) 0.0117(3) 0.0134(3) -0.0013(2) -0.0016(2) -0.0025(2) Mn5 0.0141(3) 0.0123(3) 0.0151(3) -0.0019(2) -0.0041(2) -0.0022(2) Mn6 0.0184(3) 0.0184(3) 0.0160(3) -0.0043(2) -0.0040(3) -0.0032(3) Mn7 0.0157(3) 0.0136(3) 0.0217(4) -0.0019(2) 0.0015(3) -0.0032(2) Mn8 0.0173(3) 0.0115(3) 0.0159(3) -0.0025(2) -0.0008(2) -0.0044(2) O1 0.0149(14) 0.0122(12) 0.0136(14) -0.0025(10) -0.0024(11) -0.0029(11) O2 0.0138(14) 0.0165(13) 0.0160(14) -0.0022(11) -0.0050(11) -0.0027(11) O3 0.0135(14) 0.0119(12) 0.0152(14) -0.0019(10) -0.0007(11) -0.0011(11) O4 0.0167(14) 0.0112(12) 0.0133(14) -0.0022(10) -0.0011(11) -0.0039(11) O21 0.0198(15) 0.0125(13) 0.0177(15) 0.0002(11) 0.0013(11) -0.0081(11) N11 0.0177(17) 0.0104(15) 0.0127(17) -0.0005(12) -0.0012(13) -0.0045(13) N21 0.027(2) 0.0161(16) 0.023(2) -0.0064(14) 0.0086(15) -0.0090(15) O11 0.0193(14) 0.0155(13) 0.0131(14) -0.0051(11) 0.0038(11) -0.0060(11) C81 0.0132(19) 0.0148(18) 0.013(2) -0.0039(15) -0.0036(15) -0.0026(16) C71 0.015(2) 0.0150(18) 0.018(2) -0.0024(15) -0.0026(16) -0.0025(16) C11 0.026(2) 0.022(2) 0.018(2) -0.0013(17) -0.0027(18) -0.0087(19) C21 0.038(3) 0.103(5) 0.018(3) 0.003(3) -0.004(2) 0.002(3) C31 0.061(4) 0.140(6) 0.028(4) 0.005(4) -0.017(3) -0.001(4) C41 0.076(5) 0.115(6) 0.023(3) 0.003(3) -0.018(3) -0.024(4) C51 0.064(4) 0.045(3) 0.017(3) -0.003(2) 0.003(3) -0.003(3) C61 0.043(3) 0.032(2) 0.020(3) -0.004(2) 0.001(2) -0.002(2) O22 0.0157(14) 0.0164(13) 0.0215(16) -0.0005(11) 0.0042(12) -0.0032(11) N12 0.0145(17) 0.0138(15) 0.0164(18) -0.0010(13) -0.0026(13) -0.0023(13) N22 0.030(2) 0.0141(17) 0.030(2) -0.0049(15) 0.0043(16) -0.0021(15) O12 0.0155(14) 0.0115(13) 0.0226(16) -0.0016(11) -0.0022(11) -0.0005(11) C82 0.018(2) 0.0173(19) 0.019(2) -0.0047(16) -0.0090(17) 0.0002(17) C72 0.015(2) 0.0097(17) 0.024(2) -0.0008(15) -0.0073(17) 0.0008(15) C12 0.020(2) 0.0159(19) 0.025(2) -0.0010(17) -0.0045(18) -0.0022(17) C22 0.045(3) 0.022(2) 0.028(3) -0.0009(19) -0.015(2) -0.007(2) C32 0.054(3) 0.012(2) 0.044(3) 0.003(2) -0.021(3) -0.007(2) C42 0.047(3) 0.026(2) 0.045(3) 0.012(2) -0.025(3) -0.006(2) C52 0.060(4) 0.037(3) 0.048(3) -0.005(2) -0.038(3) -0.004(3) C62 0.053(3) 0.018(2) 0.050(3) -0.006(2) -0.031(3) 0.003(2) O23 0.0164(14) 0.0151(13) 0.0181(15) -0.0042(11) -0.0066(11) 0.0008(11) N13 0.0160(17) 0.0129(15) 0.0157(18) -0.0023(13) -0.0041(14) -0.0040(13) N23 0.0220(18) 0.0188(17) 0.0208(19) -0.0074(14) -0.0112(14) -0.0002(15) O13 0.0170(14) 0.0165(13) 0.0175(15) -0.0031(11) -0.0051(11) -0.0035(11) C83 0.0126(19) 0.0141(18) 0.015(2) -0.0035(15) 0.0015(15) -0.0074(16) C73 0.020(2) 0.0155(19) 0.014(2) -0.0038(15) -0.0023(16) -0.0055(16) C13 0.023(2) 0.019(2) 0.018(2) 0.0001(16) -0.0087(17) -0.0069(17) C23 0.029(3) 0.045(3) 0.021(2) -0.012(2) -0.0036(19) -0.016(2) C33 0.032(3) 0.060(3) 0.021(3) 0.000(2) -0.006(2) -0.027(3) C43 0.045(3) 0.039(3) 0.040(3) 0.003(2) -0.020(2) -0.029(3) C53 0.041(3) 0.030(3) 0.043(3) -0.010(2) -0.020(2) -0.012(2) C63 0.026(2) 0.025(2) 0.029(3) -0.0066(18) -0.0099(19) -0.0077(19) O24 0.0180(14) 0.0229(14) 0.0123(14) -0.0048(11) -0.0030(11) -0.0049(12) N14 0.0170(18) 0.0171(16) 0.0161(18) -0.0026(13) -0.0012(14) -0.0062(14) N24 0.0228(19) 0.0185(17) 0.021(2) -0.0102(14) -0.0003(15) -0.0015(15) O14 0.0149(14) 0.0147(13) 0.0151(14) -0.0004(11) -0.0018(11) -0.0016(11) C84 0.016(2) 0.0168(19) 0.016(2) -0.0024(16) 0.0026(16) -0.0089(17) C74 0.015(2) 0.0123(18) 0.019(2) -0.0028(15) -0.0024(16) 0.0004(16) C14 0.019(2) 0.0183(19) 0.013(2) -0.0022(15) -0.0052(16) -0.0028(17) C24 0.019(2) 0.020(2) 0.031(3) -0.0047(18) -0.0016(18) -0.0031(18) C34 0.018(2) 0.030(2) 0.042(3) -0.008(2) -0.007(2) 0.0017(19) C44 0.015(2) 0.039(3) 0.037(3) -0.004(2) -0.0082(19) -0.006(2) C54 0.021(2) 0.022(2) 0.029(3) -0.0018(18) -0.0056(19) -0.0075(19) C64 0.020(2) 0.020(2) 0.023(2) -0.0009(17) -0.0040(18) -0.0021(18) O25 0.0181(14) 0.0162(13) 0.0167(15) -0.0040(11) -0.0057(11) -0.0012(11) N15 0.0174(18) 0.0162(16) 0.0187(18) -0.0046(13) -0.0073(14) -0.0011(14) N25 0.055(3) 0.036(2) 0.060(3) -0.024(2) -0.044(2) 0.014(2) O15 0.0181(15) 0.0167(13) 0.0251(16) -0.0052(12) -0.0100(12) -0.0006(12) C85 0.027(2) 0.023(2) 0.037(3) -0.010(2) -0.016(2) -0.002(2) C75 0.030(3) 0.032(2) 0.032(3) -0.009(2) -0.014(2) -0.002(2) C15 0.018(2) 0.032(2) 0.022(2) -0.0027(19) -0.0058(18) -0.0064(19) C25 0.048(3) 0.058(3) 0.036(3) -0.002(3) -0.015(3) -0.022(3) C35 0.043(4) 0.092(5) 0.034(3) -0.003(3) -0.003(3) -0.031(3) C45 0.029(3) 0.108(5) 0.038(3) -0.018(3) -0.014(3) -0.013(3) C55 0.028(3) 0.091(4) 0.042(4) 0.004(3) -0.019(3) -0.012(3) C65 0.031(3) 0.056(3) 0.030(3) -0.006(2) -0.008(2) -0.001(2) O26 0.0236(15) 0.0180(14) 0.0187(15) -0.0062(11) -0.0089(12) 0.0016(12) N16 0.025(2) 0.0258(19) 0.023(2) -0.0063(15) -0.0133(16) 0.0027(16) N26 0.077(4) 0.074(3) 0.059(3) -0.042(3) -0.055(3) 0.040(3) O16 0.0356(19) 0.0428(18) 0.0318(19) -0.0179(15) -0.0224(15) 0.0155(15) C86 0.043(3) 0.037(3) 0.041(3) -0.011(2) -0.025(3) 0.009(2) C76 0.044(3) 0.041(3) 0.035(3) -0.013(2) -0.023(2) 0.006(2) C16 0.036(3) 0.051(3) 0.032(3) -0.009(2) -0.017(2) 0.008(2) C26 0.046(3) 0.058(3) 0.033(3) -0.003(3) -0.017(2) -0.017(3) C36 0.052(4) 0.076(4) 0.038(3) -0.003(3) -0.019(3) -0.018(3) C46 0.034(3) 0.046(3) 0.048(4) -0.010(3) -0.012(3) -0.001(2) C56 0.053(4) 0.050(3) 0.041(3) -0.003(3) -0.021(3) -0.006(3) C66 0.069(4) 0.057(4) 0.037(3) -0.006(3) -0.025(3) -0.001(3) O27 0.0145(14) 0.0133(13) 0.0196(15) -0.0042(11) -0.0005(11) -0.0012(11) N17 0.0131(17) 0.0168(16) 0.0188(18) -0.0046(13) -0.0014(14) -0.0037(14) N27 0.0172(18) 0.0168(17) 0.025(2) -0.0007(14) -0.0033(14) -0.0061(14) O17 0.0172(15) 0.0145(13) 0.0289(17) -0.0017(12) 0.0034(12) -0.0056(12) C87 0.018(2) 0.018(2) 0.020(2) -0.0035(16) -0.0078(17) -0.0034(17) C77 0.014(2) 0.017(2) 0.027(2) -0.0014(17) 0.0010(17) -0.0038(17) C17 0.026(2) 0.0148(19) 0.024(2) -0.0029(17) 0.0012(19) -0.0057(18) C27 0.025(2) 0.017(2) 0.026(3) 0.0003(17) -0.0012(19) -0.0042(18) C37 0.038(3) 0.019(2) 0.030(3) -0.0023(19) -0.008(2) -0.003(2) C47 0.046(3) 0.018(2) 0.029(3) -0.0059(19) 0.005(2) -0.009(2) C57 0.041(3) 0.029(3) 0.038(3) -0.005(2) 0.014(2) -0.019(2) C67 0.029(3) 0.029(2) 0.030(3) -0.008(2) 0.005(2) -0.011(2) O28 0.0196(15) 0.0113(12) 0.0187(15) -0.0043(11) -0.0013(11) -0.0029(11) N18 0.0162(17) 0.0120(15) 0.0161(18) -0.0014(13) -0.0027(13) -0.0033(13) N28 0.027(2) 0.0199(17) 0.0198(19) -0.0025(14) 0.0030(15) -0.0139(16) O18 0.0231(15) 0.0128(13) 0.0164(15) -0.0018(11) 0.0009(11) -0.0079(12) C88 0.015(2) 0.0172(19) 0.018(2) 0.0028(16) -0.0066(16) -0.0008(16) C78 0.019(2) 0.020(2) 0.021(2) -0.0021(17) -0.0041(17) -0.0087(17) C18 0.030(3) 0.025(2) 0.024(2) -0.0048(18) -0.001(2) -0.009(2) C28 0.049(3) 0.029(3) 0.038(3) 0.000(2) -0.009(2) -0.018(2) C38 0.064(4) 0.033(3) 0.045(4) -0.001(2) 0.003(3) -0.022(3) C48 0.043(3) 0.021(2) 0.030(3) 0.0030(19) -0.001(2) -0.005(2) C58 0.041(3) 0.036(3) 0.033(3) 0.001(2) -0.007(2) 0.006(2) C68 0.036(3) 0.027(2) 0.032(3) 0.001(2) -0.004(2) -0.008(2) O1M 0.0271(19) 0.0401(19) 0.0313(19) 0.0005(15) -0.0136(14) -0.0115(15) C1M 0.081(7) 0.077(6) 0.039(5) 0.003(4) -0.028(4) -0.066(6) O12M 0.0271(19) 0.0401(19) 0.0313(19) 0.0005(15) -0.0136(14) -0.0115(15) O16W 0.0271(19) 0.0401(19) 0.0313(19) 0.0005(15) -0.0136(14) -0.0115(15) O2M 0.0230(16) 0.0196(14) 0.0256(17) -0.0002(12) -0.0104(13) -0.0079(13) C2M 0.032(3) 0.056(3) 0.057(4) 0.014(3) -0.015(3) -0.011(3) O3M 0.057(2) 0.0305(18) 0.060(3) -0.0180(17) -0.0329(19) 0.0093(17) C3M 0.044(3) 0.051(3) 0.055(4) -0.021(3) -0.024(3) 0.013(3) O4M 0.039(2) 0.0188(15) 0.042(2) -0.0119(14) 0.0036(15) -0.0067(15) C4M 0.066(4) 0.030(3) 0.059(4) -0.022(3) 0.012(3) -0.021(3) O5M 0.056(5) 0.083(6) 0.057(6) 0.014(5) -0.026(4) -0.016(5) C5M 0.087(10) 0.085(9) 0.044(7) 0.029(7) -0.049(7) -0.044(8) O6M 0.056(3) 0.0328(19) 0.049(2) -0.0078(17) -0.025(2) -0.0011(17) O13M 0.056(3) 0.0328(19) 0.049(2) -0.0078(17) -0.025(2) -0.0011(17) O7M 0.062(5) 0.031(4) 0.043(4) -0.023(3) -0.022(4) 0.010(3) O8M 0.110(7) 0.040(4) 0.052(6) 0.003(4) -0.031(5) -0.011(5) C8M 0.109(12) 0.062(9) 0.161(17) -0.026(10) -0.114(12) 0.012(9) O1W 0.0191(15) 0.0208(14) 0.0215(16) 0.0026(12) -0.0041(12) -0.0021(12) O3W 0.044(2) 0.0259(16) 0.035(2) -0.0124(14) -0.0095(15) 0.0075(15) O4W 0.0207(15) 0.0207(14) 0.0193(15) -0.0026(11) -0.0040(12) -0.0064(12) O5W 0.0340(18) 0.0227(16) 0.036(2) -0.0072(13) 0.0081(14) -0.0076(14) O6W 0.0334(18) 0.0248(15) 0.0283(18) 0.0047(13) -0.0023(14) -0.0065(14) O7W 0.056(2) 0.041(2) 0.060(3) -0.0048(18) -0.0378(19) -0.0021(18) O8W 0.023(2) 0.037(3) 0.062(3) -0.037(2) 0.010(2) -0.007(2) O9W 0.054(3) 0.089(4) 0.081(4) -0.052(3) -0.013(3) 0.005(3) O10W 0.043(3) 0.081(4) 0.080(4) -0.010(3) 0.016(3) -0.011(3) O11W 0.077(6) 0.059(5) 0.071(6) -0.044(4) -0.048(4) 0.003(4) O12W 0.085(8) 0.099(8) 0.192(13) -0.016(8) -0.054(8) 0.016(6) O14W 0.045(6) 0.169(11) 0.092(8) -0.050(8) 0.001(5) -0.042(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.886(2) . ? Mn1 O11 1.921(2) . ? Mn1 O4 1.926(2) . ? Mn1 N11 1.946(3) . ? Mn1 O25 2.128(3) . ? Mn1 Mn3 3.1481(13) . ? Mn2 O2 1.891(3) . ? Mn2 O3 1.914(2) . ? Mn2 O12 1.916(2) . ? Mn2 N12 1.950(3) . ? Mn2 O26 2.156(3) . ? Mn2 Mn4 3.1652(16) . ? Mn2 Mn7 3.2264(19) . ? Mn3 O1 1.882(3) . ? Mn3 O3 1.930(2) . ? Mn3 O13 1.934(3) . ? Mn3 N13 1.959(3) . ? Mn3 O27 2.088(2) . ? Mn4 O2 1.892(3) . ? Mn4 O14 1.922(3) . ? Mn4 O4 1.936(3) . ? Mn4 N14 1.961(3) . ? Mn4 O28 2.071(2) . ? Mn5 O1 1.902(3) . ? Mn5 O15 1.907(3) . ? Mn5 O23 1.938(3) . ? Mn5 N15 1.964(3) . ? Mn5 O1W 2.262(3) . ? Mn5 O14 2.328(3) . ? Mn6 O16 1.842(3) . ? Mn6 O2 1.881(3) . ? Mn6 O24 1.904(3) . ? Mn6 N16 1.947(4) . ? Mn6 O13 2.261(3) . ? Mn6 H11B 2.1605 . ? Mn7 O17 1.877(3) . ? Mn7 O3 1.898(2) . ? Mn7 O22 1.919(2) . ? Mn7 N17 1.958(3) . ? Mn7 O1M 2.260(3) . ? Mn8 O18 1.896(2) . ? Mn8 O4 1.899(2) . ? Mn8 O21 1.931(3) . ? Mn8 N18 1.954(3) . ? Mn8 O2M 2.276(3) . ? O21 N11 1.403(3) . ? N11 C81 1.314(4) . ? N21 C81 1.324(4) . ? N21 H1N1 0.8800 . ? N21 H2N1 0.8800 . ? O11 C71 1.420(4) . ? C81 C71 1.512(5) . ? C71 C11 1.519(6) . ? C71 H71 1.0000 . ? C11 C61 1.374(5) . ? C11 C21 1.387(7) . ? C21 C31 1.399(8) . ? C21 H21 0.9500 . ? C31 C41 1.394(8) . ? C31 H31 0.9500 . ? C41 C51 1.368(8) . ? C41 H41 0.9500 . ? C51 C61 1.403(7) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? O22 N12 1.392(3) . ? N12 C82 1.306(4) . ? N22 C82 1.342(5) . ? N22 H1N2 0.8800 . ? N22 H2N2 0.8800 . ? O12 C72 1.429(4) . ? C82 C72 1.507(5) . ? C72 C12 1.530(6) . ? C72 H72 1.0000 . ? C12 C22 1.377(5) . ? C12 C62 1.392(6) . ? C22 C32 1.390(6) . ? C22 H22 0.9500 . ? C32 C42 1.374(6) . ? C32 H32 0.9500 . ? C42 C52 1.388(6) . ? C42 H42 0.9500 . ? C52 C62 1.394(7) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? O23 N13 1.384(4) . ? N13 C83 1.306(4) . ? N23 C83 1.335(4) . ? N23 H1N3 0.8800 . ? N23 H2N3 0.8800 . ? O13 C73 1.431(4) . ? C83 C73 1.524(6) . ? C73 C13 1.538(5) . ? C73 H73 1.0000 . ? C13 C63 1.382(5) . ? C13 C23 1.384(5) . ? C23 C33 1.390(5) . ? C23 H23 0.9500 . ? C33 C43 1.362(6) . ? C33 H33 0.9500 . ? C43 C53 1.382(6) . ? C43 H43 0.9500 . ? C53 C63 1.380(5) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? O24 N14 1.389(4) . ? N14 C84 1.303(5) . ? N24 C84 1.351(4) . ? N24 H1N4 0.8799 . ? N24 H2N4 0.8800 . ? O14 C74 1.425(4) . ? C84 C74 1.514(6) . ? C74 C14 1.529(5) . ? C74 H74 1.0000 . ? C14 C24 1.375(5) . ? C14 C64 1.389(5) . ? C24 C34 1.387(5) . ? C24 H24 0.9500 . ? C34 C44 1.371(5) . ? C34 H34 0.9500 . ? C44 C54 1.375(6) . ? C44 H44 0.9500 . ? C54 C64 1.394(5) . ? C54 H54 0.9500 . ? C64 H64 0.9500 . ? O25 N15 1.389(4) . ? N15 C85 1.283(5) . ? N25 C85 1.352(5) . ? N25 H1N5 0.8800 . ? N25 H2N5 0.8800 . ? O15 C75 1.458(5) . ? C85 C75 1.522(6) . ? C75 C15 1.501(6) . ? C75 H75 1.0000 . ? C15 C25 1.387(6) . ? C15 C65 1.390(6) . ? C25 C35 1.368(7) . ? C25 H25 0.9500 . ? C35 C45 1.388(8) . ? C35 H35 0.9500 . ? C45 C55 1.346(7) . ? C45 H45 0.9500 . ? C55 C65 1.407(6) . ? C55 H55 0.9500 . ? C65 H65 0.9500 . ? O26 N16 1.385(4) . ? N16 C86 1.302(6) . ? N26 C86 1.334(6) . ? N26 H1N6 0.8800 . ? N26 H2N6 0.8800 . ? O16 C76 1.422(6) . ? C86 C76 1.527(6) . ? C76 C16 1.508(6) . ? C76 H76 1.0000 . ? C16 C26 1.375(6) . ? C16 C66 1.388(7) . ? C26 C36 1.392(6) . ? C26 H26 0.9500 . ? C36 C46 1.391(7) . ? C36 H36 0.9500 . ? C46 C56 1.404(7) . ? C46 H46 0.9500 . ? C56 C66 1.377(7) . ? C56 H56 0.9500 . ? C66 H66 0.9500 . ? O27 N17 1.377(4) . ? N17 C87 1.307(4) . ? N27 C87 1.337(4) . ? N27 H1N7 0.8800 . ? N27 H2N7 0.8799 . ? O17 C77 1.430(4) . ? C87 C77 1.507(5) . ? C77 C17 1.508(6) . ? C77 H77 1.0000 . ? C17 C27 1.382(6) . ? C17 C67 1.403(5) . ? C27 C37 1.385(6) . ? C27 H27 0.9500 . ? C37 C47 1.388(6) . ? C37 H37 0.9500 . ? C47 C57 1.371(7) . ? C47 H47 0.9500 . ? C57 C67 1.392(6) . ? C57 H57 0.9500 . ? C67 H67 0.9500 . ? O28 N18 1.381(4) . ? N18 C88 1.308(4) . ? N28 C88 1.335(4) . ? N28 H1N8 0.8800 . ? N28 H2N8 0.8800 . ? O18 C78 1.421(4) . ? C88 C78 1.516(5) . ? C78 C18 1.517(6) . ? C78 H78 1.0000 . ? C18 C68 1.379(7) . ? C18 C28 1.388(5) . ? C28 C38 1.421(7) . ? C28 H28 0.9500 . ? C38 C48 1.359(7) . ? C38 H38 0.9500 . ? C48 C58 1.379(6) . ? C48 H48 0.9500 . ? C58 C68 1.401(6) . ? C58 H58 0.9500 . ? C68 H68 0.9500 . ? O1M C1M 1.385(7) . ? O1M H1M 0.8400 . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? C12M H12A 0.9800 . ? C12M H12B 0.9800 . ? C12M H12C 0.9800 . ? O2M C2M 1.436(5) . ? O2M H2M 0.8400 . ? C2M H2M1 0.9800 . ? C2M H2M2 0.9800 . ? C2M H2M3 0.9800 . ? O3M C3M 1.437(5) . ? O3M H3M 0.8400 . ? C3M H3M1 0.9800 . ? C3M H3M2 0.9800 . ? C3M H3M3 0.9800 . ? O4M C4M 1.425(4) . ? O4M H4M 0.8400 . ? C4M H4M1 0.9800 . ? C4M H4M2 0.9800 . ? C4M H4M3 0.9800 . ? O5M C5M 1.388(12) . ? O5M H5M 0.8400 . ? C5M H5M1 0.9800 . ? C5M H5M2 0.9800 . ? C5M H5M3 0.9800 . ? O6M C6M 1.490(8) . ? O6M H6M 0.8400 . ? C6M H6M1 0.9800 . ? C6M H6M2 0.9800 . ? C6M H6M3 0.9800 . ? C13M H13A 0.9800 . ? C13M H13B 0.9800 . ? C13M H13C 0.9800 . ? O7M C7M 1.236(15) . ? O7M H7M 0.8400 . ? C7M H7M1 0.9800 . ? C7M H7M2 0.9800 . ? C7M H7M3 0.9800 . ? O8M C8M 1.494(16) . ? O8M H8M 0.8400 . ? C8M H8M1 0.9800 . ? C8M H8M2 0.9800 . ? C8M H8M3 0.9800 . ? O9M C9M 1.369(17) . ? O9M H9M 0.8400 . ? C9M H9M1 0.9800 . ? C9M H9M2 0.9800 . ? C9M H9M3 0.9800 . ? O10M C10M 1.43(2) . ? O10M H10M 0.8400 . ? C10M H10A 0.9800 . ? C10M H10B 0.9800 . ? C10M H10C 0.9800 . ? O11M C11M 1.581(16) . ? O11M H11B 0.8400 . ? C11M H11C 0.9800 . ? C11M H11D 0.9800 . ? C11M H11E 0.9800 . ? C11M H14M 1.0567 . ? O1W H1W1 0.8599 . ? O1W H2W1 0.8600 . ? O3W H1W3 0.8599 . ? O3W H2W3 0.8601 . ? O4W H1W4 0.8601 . ? O4W H2W4 0.8599 . ? O5W H1W5 0.8601 . ? O5W H2W5 0.8600 . ? O6W H1W6 0.8600 . ? O6W H2W6 0.8600 . ? O7W H7W1 0.8600 . ? O7W H7W2 0.8600 . ? O14M C14M 1.458(19) . ? O14M H14M 0.8400 . ? C14M H14A 0.9800 . ? C14M H14B 0.9800 . ? C14M H14C 0.9800 . ? O14W O15W 0.827(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O11 96.47(10) . . ? O1 Mn1 O4 92.40(11) . . ? O11 Mn1 O4 155.28(12) . . ? O1 Mn1 N11 176.07(13) . . ? O11 Mn1 N11 81.38(11) . . ? O4 Mn1 N11 88.30(11) . . ? O1 Mn1 O25 91.96(11) . . ? O11 Mn1 O25 108.27(11) . . ? O4 Mn1 O25 94.38(11) . . ? N11 Mn1 O25 91.84(12) . . ? O1 Mn1 Mn3 33.30(8) . . ? O11 Mn1 Mn3 90.67(8) . . ? O4 Mn1 Mn3 84.17(8) . . ? N11 Mn1 Mn3 143.09(10) . . ? O25 Mn1 Mn3 124.69(7) . . ? O2 Mn2 O3 91.53(11) . . ? O2 Mn2 O12 98.18(11) . . ? O3 Mn2 O12 155.87(12) . . ? O2 Mn2 N12 178.20(13) . . ? O3 Mn2 N12 88.30(12) . . ? O12 Mn2 N12 81.31(11) . . ? O2 Mn2 O26 90.18(11) . . ? O3 Mn2 O26 96.21(11) . . ? O12 Mn2 O26 105.74(11) . . ? N12 Mn2 O26 91.62(12) . . ? O2 Mn2 Mn4 33.20(8) . . ? O3 Mn2 Mn4 85.00(8) . . ? O12 Mn2 Mn4 91.09(8) . . ? N12 Mn2 Mn4 145.01(10) . . ? O26 Mn2 Mn4 123.21(8) . . ? O2 Mn2 Mn7 121.99(8) . . ? O3 Mn2 Mn7 32.02(7) . . ? O12 Mn2 Mn7 138.32(8) . . ? N12 Mn2 Mn7 58.19(9) . . ? O26 Mn2 Mn7 86.30(7) . . ? Mn4 Mn2 Mn7 115.76(4) . . ? O1 Mn3 O3 89.83(11) . . ? O1 Mn3 O13 157.13(10) . . ? O3 Mn3 O13 98.88(12) . . ? O1 Mn3 N13 85.78(13) . . ? O3 Mn3 N13 166.85(10) . . ? O13 Mn3 N13 81.00(13) . . ? O1 Mn3 O27 98.91(11) . . ? O3 Mn3 O27 91.95(10) . . ? O13 Mn3 O27 101.86(11) . . ? N13 Mn3 O27 100.97(11) . . ? O1 Mn3 Mn1 33.39(7) . . ? O3 Mn3 Mn1 56.59(8) . . ? O13 Mn3 Mn1 146.58(8) . . ? N13 Mn3 Mn1 117.50(10) . . ? O27 Mn3 Mn1 101.34(8) . . ? O2 Mn4 O14 154.76(10) . . ? O2 Mn4 O4 87.79(11) . . ? O14 Mn4 O4 101.06(12) . . ? O2 Mn4 N14 85.37(13) . . ? O14 Mn4 N14 80.87(13) . . ? O4 Mn4 N14 166.69(11) . . ? O2 Mn4 O28 98.33(11) . . ? O14 Mn4 O28 104.78(11) . . ? O4 Mn4 O28 92.45(10) . . ? N14 Mn4 O28 99.82(11) . . ? O2 Mn4 Mn2 33.18(8) . . ? O14 Mn4 Mn2 145.91(8) . . ? O4 Mn4 Mn2 54.70(9) . . ? N14 Mn4 Mn2 117.30(11) . . ? O28 Mn4 Mn2 100.26(8) . . ? O1 Mn5 O15 171.57(11) . . ? O1 Mn5 O23 91.28(11) . . ? O15 Mn5 O23 97.14(11) . . ? O1 Mn5 N15 90.51(13) . . ? O15 Mn5 N15 81.06(13) . . ? O23 Mn5 N15 178.02(13) . . ? O1 Mn5 O1W 92.22(11) . . ? O15 Mn5 O1W 87.01(11) . . ? O23 Mn5 O1W 92.60(10) . . ? N15 Mn5 O1W 86.50(11) . . ? O1 Mn5 O14 90.71(10) . . ? O15 Mn5 O14 89.50(11) . . ? O23 Mn5 O14 91.37(10) . . ? N15 Mn5 O14 89.43(11) . . ? O1W Mn5 O14 175.01(10) . . ? O16 Mn6 O2 165.68(13) . . ? O16 Mn6 O24 91.82(13) . . ? O2 Mn6 O24 92.63(12) . . ? O16 Mn6 N16 83.20(15) . . ? O2 Mn6 N16 89.91(13) . . ? O24 Mn6 N16 168.71(13) . . ? O16 Mn6 O13 100.24(12) . . ? O2 Mn6 O13 92.84(10) . . ? O24 Mn6 O13 95.77(11) . . ? N16 Mn6 O13 95.09(12) . . ? O16 Mn6 H11B 57.3 . . ? O2 Mn6 H11B 108.9 . . ? O24 Mn6 H11B 91.8 . . ? N16 Mn6 H11B 77.0 . . ? O13 Mn6 H11B 156.6 . . ? O17 Mn7 O3 172.11(11) . . ? O17 Mn7 O22 92.09(11) . . ? O3 Mn7 O22 95.45(11) . . ? O17 Mn7 N17 81.92(12) . . ? O3 Mn7 N17 90.31(12) . . ? O22 Mn7 N17 170.69(13) . . ? O17 Mn7 O1M 93.59(12) . . ? O3 Mn7 O1M 88.90(11) . . ? O22 Mn7 O1M 88.78(12) . . ? N17 Mn7 O1M 98.66(13) . . ? O17 Mn7 Mn2 155.55(8) . . ? O3 Mn7 Mn2 32.33(7) . . ? O22 Mn7 Mn2 65.04(8) . . ? N17 Mn7 Mn2 121.84(9) . . ? O1M Mn7 Mn2 78.15(8) . . ? O18 Mn8 O4 172.05(10) . . ? O18 Mn8 O21 92.66(11) . . ? O4 Mn8 O21 95.10(10) . . ? O18 Mn8 N18 81.65(12) . . ? O4 Mn8 N18 90.49(12) . . ? O21 Mn8 N18 173.09(12) . . ? O18 Mn8 O2M 93.39(11) . . ? O4 Mn8 O2M 88.55(11) . . ? O21 Mn8 O2M 88.31(11) . . ? N18 Mn8 O2M 95.91(12) . . ? Mn3 O1 Mn1 113.31(13) . . ? Mn3 O1 Mn5 121.53(13) . . ? Mn1 O1 Mn5 120.10(13) . . ? Mn6 O2 Mn2 120.70(13) . . ? Mn6 O2 Mn4 120.57(13) . . ? Mn2 O2 Mn4 113.62(13) . . ? Mn7 O3 Mn2 115.65(13) . . ? Mn7 O3 Mn3 120.01(12) . . ? Mn2 O3 Mn3 123.71(12) . . ? Mn8 O4 Mn1 116.32(12) . . ? Mn8 O4 Mn4 119.30(12) . . ? Mn1 O4 Mn4 123.70(12) . . ? N11 O21 Mn8 111.93(19) . . ? C81 N11 O21 117.3(3) . . ? C81 N11 Mn1 117.6(2) . . ? O21 N11 Mn1 125.0(2) . . ? C81 N21 H1N1 114.8 . . ? C81 N21 H2N1 123.0 . . ? H1N1 N21 H2N1 121.3 . . ? C71 O11 Mn1 115.71(19) . . ? N11 C81 N21 125.3(3) . . ? N11 C81 C71 113.6(3) . . ? N21 C81 C71 121.1(3) . . ? O11 C71 C81 108.9(3) . . ? O11 C71 C11 112.8(3) . . ? C81 C71 C11 110.0(3) . . ? O11 C71 H71 108.3 . . ? C81 C71 H71 108.3 . . ? C11 C71 H71 108.3 . . ? C61 C11 C21 118.7(5) . . ? C61 C11 C71 121.5(4) . . ? C21 C11 C71 119.8(4) . . ? C11 C21 C31 121.9(5) . . ? C11 C21 H21 119.1 . . ? C31 C21 H21 119.1 . . ? C41 C31 C21 118.1(6) . . ? C41 C31 H31 121.0 . . ? C21 C31 H31 121.0 . . ? C51 C41 C31 120.4(6) . . ? C51 C41 H41 119.8 . . ? C31 C41 H41 119.8 . . ? C41 C51 C61 120.6(5) . . ? C41 C51 H51 119.7 . . ? C61 C51 H51 119.7 . . ? C11 C61 C51 120.1(5) . . ? C11 C61 H61 120.0 . . ? C51 C61 H61 120.0 . . ? N12 O22 Mn7 111.53(19) . . ? C82 N12 O22 117.5(3) . . ? C82 N12 Mn2 117.3(2) . . ? O22 N12 Mn2 125.2(2) . . ? C82 N22 H1N2 116.9 . . ? C82 N22 H2N2 121.3 . . ? H1N2 N22 H2N2 120.2 . . ? C72 O12 Mn2 116.0(2) . . ? N12 C82 N22 124.2(3) . . ? N12 C82 C72 114.4(3) . . ? N22 C82 C72 121.3(3) . . ? O12 C72 C82 108.9(3) . . ? O12 C72 C12 111.9(3) . . ? C82 C72 C12 111.8(3) . . ? O12 C72 H72 108.0 . . ? C82 C72 H72 108.0 . . ? C12 C72 H72 108.0 . . ? C22 C12 C62 118.6(4) . . ? C22 C12 C72 120.6(4) . . ? C62 C12 C72 120.8(4) . . ? C12 C22 C32 121.5(4) . . ? C12 C22 H22 119.3 . . ? C32 C22 H22 119.3 . . ? C42 C32 C22 120.2(4) . . ? C42 C32 H32 119.9 . . ? C22 C32 H32 119.9 . . ? C32 C42 C52 118.9(5) . . ? C32 C42 H42 120.5 . . ? C52 C42 H42 120.5 . . ? C42 C52 C62 121.0(5) . . ? C42 C52 H52 119.5 . . ? C62 C52 H52 119.5 . . ? C12 C62 C52 119.7(4) . . ? C12 C62 H62 120.1 . . ? C52 C62 H62 120.1 . . ? N13 O23 Mn5 111.50(19) . . ? C83 N13 O23 117.3(3) . . ? C83 N13 Mn3 116.4(3) . . ? O23 N13 Mn3 125.8(2) . . ? C83 N23 H1N3 118.2 . . ? C83 N23 H2N3 115.1 . . ? H1N3 N23 H2N3 126.4 . . ? C73 O13 Mn3 114.5(2) . . ? C73 O13 Mn6 111.9(2) . . ? Mn3 O13 Mn6 111.10(11) . . ? N13 C83 N23 123.9(4) . . ? N13 C83 C73 114.1(3) . . ? N23 C83 C73 122.0(3) . . ? O13 C73 C83 108.9(3) . . ? O13 C73 C13 113.7(3) . . ? C83 C73 C13 110.6(3) . . ? O13 C73 H73 107.8 . . ? C83 C73 H73 107.8 . . ? C13 C73 H73 107.8 . . ? C63 C13 C23 119.4(3) . . ? C63 C13 C73 118.8(3) . . ? C23 C13 C73 121.5(3) . . ? C13 C23 C33 119.2(4) . . ? C13 C23 H23 120.4 . . ? C33 C23 H23 120.4 . . ? C43 C33 C23 121.0(4) . . ? C43 C33 H33 119.5 . . ? C23 C33 H33 119.5 . . ? C33 C43 C53 120.2(4) . . ? C33 C43 H43 119.9 . . ? C53 C43 H43 119.9 . . ? C63 C53 C43 119.3(4) . . ? C63 C53 H53 120.4 . . ? C43 C53 H53 120.4 . . ? C53 C63 C13 120.9(4) . . ? C53 C63 H63 119.5 . . ? C13 C63 H63 119.5 . . ? N14 O24 Mn6 110.9(2) . . ? C84 N14 O24 116.2(3) . . ? C84 N14 Mn4 117.4(3) . . ? O24 N14 Mn4 126.0(2) . . ? C84 N24 H1N4 115.5 . . ? C84 N24 H2N4 121.8 . . ? H1N4 N24 H2N4 113.6 . . ? C74 O14 Mn4 116.1(2) . . ? C74 O14 Mn5 108.68(19) . . ? Mn4 O14 Mn5 112.58(11) . . ? N14 C84 N24 122.3(4) . . ? N14 C84 C74 114.2(3) . . ? N24 C84 C74 123.4(4) . . ? O14 C74 C84 108.2(3) . . ? O14 C74 C14 113.0(3) . . ? C84 C74 C14 112.7(3) . . ? O14 C74 H74 107.6 . . ? C84 C74 H74 107.6 . . ? C14 C74 H74 107.6 . . ? C24 C14 C64 119.1(3) . . ? C24 C14 C74 120.7(3) . . ? C64 C14 C74 120.3(3) . . ? C14 C24 C34 121.1(4) . . ? C14 C24 H24 119.4 . . ? C34 C24 H24 119.4 . . ? C44 C34 C24 119.4(4) . . ? C44 C34 H34 120.3 . . ? C24 C34 H34 120.3 . . ? C34 C44 C54 120.5(4) . . ? C34 C44 H44 119.7 . . ? C54 C44 H44 119.7 . . ? C44 C54 C64 119.9(4) . . ? C44 C54 H54 120.0 . . ? C64 C54 H54 120.0 . . ? C14 C64 C54 119.9(4) . . ? C14 C64 H64 120.1 . . ? C54 C64 H64 120.1 . . ? N15 O25 Mn1 109.8(2) . . ? C85 N15 O25 116.5(3) . . ? C85 N15 Mn5 116.0(3) . . ? O25 N15 Mn5 125.5(2) . . ? C85 N25 H1N5 124.8 . . ? C85 N25 H2N5 119.4 . . ? H1N5 N25 H2N5 113.3 . . ? C75 O15 Mn5 114.8(2) . . ? N15 C85 N25 124.1(4) . . ? N15 C85 C75 115.7(4) . . ? N25 C85 C75 120.2(4) . . ? O15 C75 C15 110.4(3) . . ? O15 C75 C85 106.8(4) . . ? C15 C75 C85 112.8(3) . . ? O15 C75 H75 108.9 . . ? C15 C75 H75 108.9 . . ? C85 C75 H75 108.9 . . ? C25 C15 C65 118.7(4) . . ? C25 C15 C75 121.0(4) . . ? C65 C15 C75 119.9(4) . . ? C35 C25 C15 121.3(5) . . ? C35 C25 H25 119.3 . . ? C15 C25 H25 119.3 . . ? C25 C35 C45 119.0(5) . . ? C25 C35 H35 120.5 . . ? C45 C35 H35 120.5 . . ? C55 C45 C35 121.6(5) . . ? C55 C45 H45 119.2 . . ? C35 C45 H45 119.2 . . ? C45 C55 C65 119.6(5) . . ? C45 C55 H55 120.2 . . ? C65 C55 H55 120.2 . . ? C15 C65 C55 119.8(5) . . ? C15 C65 H65 120.1 . . ? C55 C65 H65 120.1 . . ? N16 O26 Mn2 109.5(2) . . ? C86 N16 O26 117.6(4) . . ? C86 N16 Mn6 115.3(3) . . ? O26 N16 Mn6 125.9(3) . . ? C86 N26 H1N6 119.2 . . ? C86 N26 H2N6 106.0 . . ? H1N6 N26 H2N6 134.7 . . ? C76 O16 Mn6 117.4(3) . . ? N16 C86 N26 124.0(4) . . ? N16 C86 C76 114.1(4) . . ? N26 C86 C76 121.9(5) . . ? O16 C76 C16 110.0(4) . . ? O16 C76 C86 108.5(4) . . ? C16 C76 C86 110.3(4) . . ? O16 C76 H76 109.4 . . ? C16 C76 H76 109.4 . . ? C86 C76 H76 109.4 . . ? C26 C16 C66 120.0(5) . . ? C26 C16 C76 121.1(5) . . ? C66 C16 C76 118.9(5) . . ? C16 C26 C36 120.2(5) . . ? C16 C26 H26 119.9 . . ? C36 C26 H26 119.9 . . ? C46 C36 C26 120.3(5) . . ? C46 C36 H36 119.9 . . ? C26 C36 H36 119.9 . . ? C36 C46 C56 119.0(5) . . ? C36 C46 H46 120.5 . . ? C56 C46 H46 120.5 . . ? C66 C56 C46 120.2(5) . . ? C66 C56 H56 119.9 . . ? C46 C56 H56 119.9 . . ? C56 C66 C16 120.4(5) . . ? C56 C66 H66 119.8 . . ? C16 C66 H66 119.8 . . ? N17 O27 Mn3 111.34(18) . . ? C87 N17 O27 117.1(3) . . ? C87 N17 Mn7 116.7(3) . . ? O27 N17 Mn7 126.1(2) . . ? C87 N27 H1N7 117.4 . . ? C87 N27 H2N7 118.8 . . ? H1N7 N27 H2N7 115.3 . . ? C77 O17 Mn7 117.6(2) . . ? N17 C87 N27 123.0(3) . . ? N17 C87 C77 114.4(3) . . ? N27 C87 C77 122.5(3) . . ? O17 C77 C87 108.8(3) . . ? O17 C77 C17 110.3(3) . . ? C87 C77 C17 111.2(3) . . ? O17 C77 H77 108.9 . . ? C87 C77 H77 108.9 . . ? C17 C77 H77 108.9 . . ? C27 C17 C67 118.7(4) . . ? C27 C17 C77 120.4(4) . . ? C67 C17 C77 120.9(4) . . ? C17 C27 C37 121.0(4) . . ? C17 C27 H27 119.5 . . ? C37 C27 H27 119.5 . . ? C27 C37 C47 120.4(5) . . ? C27 C37 H37 119.8 . . ? C47 C37 H37 119.8 . . ? C57 C47 C37 119.0(4) . . ? C57 C47 H47 120.5 . . ? C37 C47 H47 120.5 . . ? C47 C57 C67 121.4(4) . . ? C47 C57 H57 119.3 . . ? C67 C57 H57 119.3 . . ? C57 C67 C17 119.6(5) . . ? C57 C67 H67 120.2 . . ? C17 C67 H67 120.2 . . ? N18 O28 Mn4 111.43(18) . . ? C88 N18 O28 116.5(3) . . ? C88 N18 Mn8 117.4(3) . . ? O28 N18 Mn8 126.06(19) . . ? C88 N28 H1N8 116.1 . . ? C88 N28 H2N8 117.8 . . ? H1N8 N28 H2N8 115.5 . . ? C78 O18 Mn8 116.9(2) . . ? N18 C88 N28 122.9(3) . . ? N18 C88 C78 113.7(3) . . ? N28 C88 C78 123.4(3) . . ? O18 C78 C88 109.2(3) . . ? O18 C78 C18 111.3(3) . . ? C88 C78 C18 111.5(3) . . ? O18 C78 H78 108.2 . . ? C88 C78 H78 108.2 . . ? C18 C78 H78 108.2 . . ? C68 C18 C28 119.7(4) . . ? C68 C18 C78 119.9(4) . . ? C28 C18 C78 120.4(4) . . ? C18 C28 C38 119.6(5) . . ? C18 C28 H28 120.2 . . ? C38 C28 H28 120.2 . . ? C48 C38 C28 120.4(5) . . ? C48 C38 H38 119.8 . . ? C28 C38 H38 119.8 . . ? C38 C48 C58 119.5(4) . . ? C38 C48 H48 120.3 . . ? C58 C48 H48 120.3 . . ? C48 C58 C68 121.2(5) . . ? C48 C58 H58 119.4 . . ? C68 C58 H58 119.4 . . ? C18 C68 C58 119.5(4) . . ? C18 C68 H68 120.2 . . ? C58 C68 H68 120.2 . . ? C1M O1M Mn7 126.1(4) . . ? C1M O1M H1M 109.5 . . ? Mn7 O1M H1M 108.3 . . ? H12A C12M H12B 109.5 . . ? H12A C12M H12C 109.5 . . ? H12B C12M H12C 109.5 . . ? C2M O2M Mn8 120.5(3) . . ? C2M O2M H2M 109.5 . . ? Mn8 O2M H2M 91.2 . . ? O2M C2M H2M1 109.5 . . ? O2M C2M H2M2 109.5 . . ? H2M1 C2M H2M2 109.5 . . ? O2M C2M H2M3 109.5 . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C3M O3M H3M 109.5 . . ? O3M C3M H3M1 109.5 . . ? O3M C3M H3M2 109.5 . . ? H3M1 C3M H3M2 109.5 . . ? O3M C3M H3M3 109.5 . . ? H3M1 C3M H3M3 109.5 . . ? H3M2 C3M H3M3 109.5 . . ? C4M O4M H4M 109.5 . . ? O4M C4M H4M1 109.5 . . ? O4M C4M H4M2 109.5 . . ? H4M1 C4M H4M2 109.5 . . ? O4M C4M H4M3 109.5 . . ? H4M1 C4M H4M3 109.5 . . ? H4M2 C4M H4M3 109.5 . . ? C5M O5M H5M 109.2 . . ? O5M C5M H5M1 109.5 . . ? O5M C5M H5M2 109.5 . . ? H5M1 C5M H5M2 109.5 . . ? O5M C5M H5M3 109.5 . . ? H5M1 C5M H5M3 109.5 . . ? H5M2 C5M H5M3 109.5 . . ? O6M C6M H6M1 109.5 . . ? O6M C6M H6M2 109.5 . . ? H6M1 C6M H6M2 109.5 . . ? O6M C6M H6M3 109.5 . . ? H6M1 C6M H6M3 109.5 . . ? H6M2 C6M H6M3 109.5 . . ? H13A C13M H13B 109.5 . . ? H13A C13M H13C 109.5 . . ? H13B C13M H13C 109.5 . . ? O7M C7M H7M1 109.5 . . ? O7M C7M H7M2 109.5 . . ? H7M1 C7M H7M2 109.5 . . ? O7M C7M H7M3 109.5 . . ? H7M1 C7M H7M3 109.5 . . ? H7M2 C7M H7M3 109.5 . . ? C8M O8M H8M 109.7 . . ? O8M C8M H8M1 109.5 . . ? O8M C8M H8M2 109.5 . . ? H8M1 C8M H8M2 109.5 . . ? O8M C8M H8M3 109.5 . . ? H8M1 C8M H8M3 109.5 . . ? H8M2 C8M H8M3 109.5 . . ? O9M C9M H9M1 109.5 . . ? O9M C9M H9M2 109.5 . . ? H9M1 C9M H9M2 109.5 . . ? O9M C9M H9M3 109.5 . . ? H9M1 C9M H9M3 109.5 . . ? H9M2 C9M H9M3 109.5 . . ? C10M O10M H10M 112.0 . . ? O10M C10M H10A 109.5 . . ? O10M C10M H10B 109.5 . . ? H10A C10M H10B 109.5 . . ? O10M C10M H10C 109.5 . . ? H10A C10M H10C 109.5 . . ? H10B C10M H10C 109.5 . . ? C11M O11M H11B 109.4 . . ? O11M C11M H11C 109.5 . . ? O11M C11M H11D 109.5 . . ? H11C C11M H11D 109.5 . . ? O11M C11M H11E 109.5 . . ? H11C C11M H11E 109.5 . . ? H11D C11M H11E 109.5 . . ? O11M C11M H14M 118.6 . . ? H11C C11M H14M 83.5 . . ? H11D C11M H14M 122.2 . . ? H11E C11M H14M 26.1 . . ? Mn5 O1W H1W1 121.0 . . ? Mn5 O1W H2W1 118.1 . . ? H1W1 O1W H2W1 116.5 . . ? H1W3 O3W H2W3 115.9 . . ? H1W4 O4W H2W4 117.0 . . ? H1W5 O5W H2W5 117.9 . . ? H1W6 O6W H2W6 119.3 . . ? H7W1 O7W H7W2 116.8 . . ? C14M O14M H14M 110.0 . . ? O14M C14M H14A 109.5 . . ? O14M C14M H14B 109.5 . . ? H14A C14M H14B 109.5 . . ? O14M C14M H14C 109.5 . . ? H14A C14M H14C 109.5 . . ? H14B C14M H14C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N21 H1N1 O5W 0.88 2.15 2.980(4) 156.5 2_756 N21 H2N1 O5W 0.88 2.01 2.861(4) 162.6 . N22 H2N2 O10W 0.88 2.23 2.975(6) 141.8 1_655 N23 H2N3 O6M 0.88 2.04 2.883(5) 159.6 . N23 H2N3 O13M 0.88 2.04 2.883(5) 159.6 . N24 H2N4 O3W 0.88 1.95 2.821(5) 171.5 2_667 N25 H1N5 O7M 0.88 2.13 2.984(7) 162.2 . N25 H2N5 O7W 0.88 2.17 2.962(5) 148.6 . N26 H1N6 O14W 0.88 2.15 2.978(11) 157.7 2_757 N26 H1N6 O15W 0.88 2.36 3.14(2) 148.4 2_757 N26 H2N6 O5M 0.88 2.54 3.214(9) 134.6 . N27 H1N7 O4W 0.88 2.12 2.970(4) 161.6 2_766 N28 H2N8 O6W 0.88 2.10 2.938(4) 159.9 2_657 O1M H1M O26 0.84 1.80 2.624(4) 168.6 . O1M H1M N16 0.84 2.55 3.315(5) 152.1 . O2M H2M O25 0.84 1.82 2.641(3) 166.7 . O2M H2M N15 0.84 2.57 3.312(4) 148.7 . O3M H3M O15 0.84 1.74 2.574(4) 173.6 . O4M H4M O18 0.84 1.90 2.731(4) 169.8 . O5M H5M O14W 0.84 1.60 2.435(14) 169.9 . O5M H5M O15W 0.84 2.04 2.86(2) 164.2 . O6M H6M O3M 0.84 1.88 2.707(5) 167.8 . O7M H7M O9W 0.84 1.89 2.690(10) 158.4 . O1W H1W1 O7W 0.86 1.98 2.836(4) 170.9 2_666 O1W H2W1 O4W 0.86 1.91 2.737(4) 161.9 . O3W H1W3 O6M 0.86 2.02 2.854(5) 162.8 2_667 O3W H1W3 O13M 0.86 2.02 2.854(5) 162.8 2_667 O3W H2W3 O16 0.86 1.86 2.708(4) 170.6 . O4W H1W4 O27 0.86 1.97 2.787(4) 157.9 . O4W H1W4 N17 0.86 2.46 3.090(5) 130.1 . O4W H2W4 O11 0.86 2.13 2.872(3) 144.7 . O5W H1W5 O8W 0.86 1.92 2.776(6) 169.8 2_656 O5W H2W5 O4M 0.86 1.89 2.725(4) 163.2 . O6W H1W6 O28 0.86 2.09 2.850(4) 146.4 . O6W H2W6 O12 0.86 2.14 2.923(4) 151.3 . O7W H7W1 O8M 0.86 1.92 2.740(7) 159.1 . O7W H7W2 O3M 0.86 1.99 2.814(5) 161.2 2_666 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.93 _refine_diff_density_min -0.61 _refine_diff_density_rms 0.100