# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kwong, H.L.' _publ_contact_author_email bhhoik@cityu.edu.hk _publ_section_title ; New binuclear double-stranded manganese helicates as catalysts for alkene epoxidation ; loop_ _publ_author_name K.-C.Sham H.-L.Yeung S.-M.Yiu T.-C.Lau H.L.Kwong # Attachment '- 0331a.cif' data_0331a _database_code_depnum_ccdc_archive 'CCDC 775970' #TrackingRef '- 0331a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H99.50 Cl4 Mn2 N9.50 O18.50' _chemical_formula_weight 1958.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.5520(6) _cell_length_b 12.3483(4) _cell_length_c 25.6368(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.533(4) _cell_angle_gamma 90.00 _cell_volume 5072.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 27743 _cell_measurement_theta_min 3.5497 _cell_measurement_theta_max 71.6465 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 3.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54055 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69145 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 67.00 _reflns_number_total 17982 _reflns_number_gt 15605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep-3 _computing_publication_material wingx _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(5) _chemical_absolute_configuration rmad _refine_ls_number_reflns 17982 _refine_ls_number_parameters 1208 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2375 _refine_ls_wR_factor_gt 0.2249 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _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 O2A O 0.6032(6) 0.8863(9) 0.7725(5) 0.065(3) Uiso 0.50 1 d PD A 1 H2OA H 0.6311 0.9436 0.7829 0.079 Uiso 0.50 1 d PR A 1 C96A C 0.5203(9) 0.9253(15) 0.7538(7) 0.082(4) Uiso 0.50 1 d PD A 1 H96A H 0.5212 0.9973 0.7379 0.124 Uiso 0.50 1 calc PR A 1 H96B H 0.4941 0.9298 0.7840 0.124 Uiso 0.50 1 calc PR A 1 H96C H 0.4882 0.8757 0.7265 0.124 Uiso 0.50 1 calc PR A 1 O2B O 0.5809(6) 0.8780(8) 0.7514(5) 0.060(2) Uiso 0.50 1 d PD A 2 H2OB H 0.5521 0.8274 0.7603 0.072 Uiso 0.50 1 d PR A 2 C96B C 0.5780(18) 0.967(2) 0.7873(11) 0.129(8) Uiso 0.50 1 d PD A 2 H96D H 0.6185 0.9548 0.8219 0.193 Uiso 0.50 1 calc PR A 2 H96E H 0.5219 0.9726 0.7931 0.193 Uiso 0.50 1 calc PR A 2 H96F H 0.5917 1.0346 0.7713 0.193 Uiso 0.50 1 calc PR A 2 O1E O 0.3139(4) 0.7787(6) 0.6566(3) 0.0505(17) Uiso 0.50 1 d PD B 3 C1E C 0.2499(9) 0.6271(11) 0.6016(6) 0.069(3) Uiso 0.50 1 d PD B 3 H1E1 H 0.3001 0.5828 0.6051 0.103 Uiso 0.50 1 calc PR B 3 H1E2 H 0.2100 0.6111 0.5672 0.103 Uiso 0.50 1 calc PR B 3 H1E3 H 0.2245 0.6106 0.6313 0.103 Uiso 0.50 1 calc PR B 3 C2E C 0.2730(9) 0.7442(11) 0.6034(5) 0.071(3) Uiso 0.50 1 d PD B 3 H2E1 H 0.3103 0.7569 0.5793 0.085 Uiso 0.50 1 calc PR B 3 H2E2 H 0.2219 0.7880 0.5900 0.085 Uiso 0.50 1 calc PR B 3 C3E C 0.3374(12) 0.8874(12) 0.6548(7) 0.087(5) Uiso 0.50 1 d PD B 3 H3E1 H 0.2868 0.9297 0.6379 0.104 Uiso 0.50 1 calc PR B 3 H3E2 H 0.3756 0.8925 0.6307 0.104 Uiso 0.50 1 calc PR B 3 C4E C 0.379(2) 0.941(3) 0.7077(11) 0.156(11) Uiso 0.50 1 d PD B 3 H4E1 H 0.3517 0.9189 0.7355 0.234 Uiso 0.50 1 calc PR B 3 H4E2 H 0.3757 1.0201 0.7033 0.234 Uiso 0.50 1 calc PR B 3 H4E3 H 0.4383 0.9196 0.7184 0.234 Uiso 0.50 1 calc PR B 3 Mn1 Mn 1.14648(4) 0.81131(6) 0.76546(3) 0.03791(19) Uani 1 1 d . . . Mn2 Mn 0.68326(5) 0.79914(6) 0.72494(3) 0.0424(2) Uani 1 1 d . . . Cl1 Cl 1.27993(10) 1.01395(15) 0.84549(7) 0.0659(4) Uani 1 1 d . . . O1 O 1.2458(2) 0.7227(4) 0.74076(17) 0.0562(10) Uani 1 1 d . . . H1OA H 1.2491 0.7392 0.7092 0.067 Uiso 1 1 d R . . H1OB H 1.2416 0.6545 0.7436 0.067 Uiso 1 1 d R . . O3 O 1.2574(2) 0.9199(4) 0.80858(17) 0.0580(10) Uani 1 1 d . . . O4 O 1.2315(4) 1.1049(6) 0.8225(3) 0.102(2) Uani 1 1 d . . . O5 O 1.3655(4) 1.0358(7) 0.8535(3) 0.102(2) Uani 1 1 d . . . O6 O 1.2635(4) 0.9875(8) 0.8943(2) 0.107(2) Uani 1 1 d . . . Cl2 Cl 0.05837(9) 0.78081(10) 0.06111(5) 0.0486(3) Uani 1 1 d . . . O7 O 0.0814(3) 0.7826(3) 0.11794(15) 0.0622(11) Uani 1 1 d . . . O8 O 0.1206(5) 0.7233(6) 0.0436(2) 0.108(2) Uani 1 1 d . . . O9 O 0.0524(3) 0.8892(4) 0.04040(18) 0.0648(11) Uani 1 1 d . . . O10 O -0.0191(5) 0.7263(7) 0.0436(3) 0.130(4) Uani 1 1 d . . . Cl3 Cl 0.13549(11) 0.82397(12) 0.46286(6) 0.0606(4) Uani 1 1 d . . . O11 O 0.1981(6) 0.8923(8) 0.4895(3) 0.133(3) Uani 1 1 d . . . O12 O 0.1114(4) 0.8352(5) 0.4057(2) 0.0828(15) Uani 1 1 d . . . O13 O 0.0567(5) 0.8658(7) 0.4761(3) 0.113(2) Uani 1 1 d . . . O14 O 0.1375(7) 0.7145(6) 0.4795(3) 0.129(3) Uani 1 1 d . . . Cl4A Cl 0.4614(3) 0.7759(4) 0.3112(2) 0.0840(11) Uiso 0.55 1 d PD C 1 O15A O 0.4229(10) 0.8296(15) 0.2609(7) 0.123(5) Uiso 0.55 1 d PD C 1 O16A O 0.5370(8) 0.8306(13) 0.3313(6) 0.109(4) Uiso 0.55 1 d PD C 1 O17A O 0.4712(10) 0.6610(11) 0.3087(7) 0.107(4) Uiso 0.55 1 d PD C 1 O18A O 0.4080(7) 0.7917(10) 0.3415(5) 0.086(3) Uiso 0.55 1 d PD C 1 Cl4B Cl 0.4588(3) 0.7565(5) 0.2902(3) 0.0881(14) Uiso 0.45 1 d PD D 2 O15B O 0.4317(15) 0.787(2) 0.2399(8) 0.144(8) Uiso 0.45 1 d PD D 2 O16B O 0.5414(8) 0.7865(15) 0.3077(7) 0.103(4) Uiso 0.45 1 d PD D 2 O17B O 0.445(2) 0.6450(16) 0.2835(14) 0.177(11) Uiso 0.45 1 d PD D 2 O18B O 0.3989(11) 0.8170(16) 0.3105(9) 0.120(5) Uiso 0.45 1 d PD D 2 N1 N 1.1593(3) 0.6969(4) 0.83329(17) 0.0429(9) Uani 1 1 d . . . N2 N 1.0792(2) 0.8913(3) 0.82426(16) 0.0353(8) Uani 1 1 d . . . N3 N 0.7547(2) 0.6566(4) 0.69523(19) 0.0437(10) Uani 1 1 d . A . N4 N 0.6991(2) 0.6736(3) 0.78665(18) 0.0414(9) Uani 1 1 d . A . N5 N 1.1332(3) 0.9176(4) 0.69482(16) 0.0398(9) Uani 1 1 d . . . N6 N 1.0568(2) 0.7209(3) 0.69176(16) 0.0364(8) Uani 1 1 d . . . N7 N 0.7610(3) 0.9496(3) 0.75642(18) 0.0426(9) Uani 1 1 d . A . N8 N 0.6578(2) 0.9125(3) 0.65758(17) 0.0398(9) Uani 1 1 d . A . C1 C 1.3372(6) 0.2888(8) 0.9358(4) 0.089(3) Uani 1 1 d . . . H1A H 1.3771 0.2967 0.9135 0.133 Uiso 1 1 calc R . . H1B H 1.2988 0.2291 0.9219 0.133 Uiso 1 1 calc R . . H1C H 1.3676 0.2732 0.9730 0.133 Uiso 1 1 calc R . . C2 C 1.3472(4) 0.4849(7) 0.9570(3) 0.076(2) Uani 1 1 d . . . H2A H 1.3783 0.4662 0.9936 0.114 Uiso 1 1 calc R . . H2B H 1.3159 0.5520 0.9578 0.114 Uiso 1 1 calc R . . H2C H 1.3863 0.4954 0.9343 0.114 Uiso 1 1 calc R . . C3 C 1.2874(4) 0.3946(6) 0.9341(3) 0.0670(18) Uani 1 1 d . . . C4 C 1.2091(4) 0.3775(6) 0.9561(3) 0.0651(17) Uani 1 1 d . . . H4 H 1.2159 0.3225 0.9856 0.078 Uiso 1 1 calc R . . C5 C 1.1634(5) 0.3372(6) 0.9005(3) 0.0727(19) Uani 1 1 d . . . H5A H 1.1042 0.3598 0.8890 0.087 Uiso 1 1 calc R . . H5B H 1.1697 0.2586 0.8949 0.087 Uiso 1 1 calc R . . C6 C 1.2241(5) 0.4097(5) 0.8787(3) 0.0648(17) Uani 1 1 d . . . H6 H 1.2413 0.3828 0.8463 0.078 Uiso 1 1 calc R . . C7 C 1.1918(4) 0.5245(5) 0.8766(3) 0.0522(13) Uani 1 1 d . . . C8 C 1.1655(3) 0.5620(5) 0.9209(2) 0.0473(12) Uani 1 1 d . . . C9 C 1.1721(4) 0.4850(6) 0.9676(3) 0.0590(15) Uani 1 1 d . . . H9A H 1.1160 0.4727 0.9735 0.071 Uiso 1 1 calc R . . H9B H 1.2078 0.5173 1.0007 0.071 Uiso 1 1 calc R . . C10 C 1.1873(4) 0.5959(5) 0.8342(2) 0.0498(12) Uani 1 1 d . . . H10 H 1.2055 0.5711 0.8040 0.060 Uiso 1 1 calc R . . C11 C 1.1338(3) 0.7333(4) 0.8761(2) 0.0399(10) Uani 1 1 d . . . C12 C 1.1367(3) 0.6667(5) 0.9203(2) 0.0456(11) Uani 1 1 d . . . H12 H 1.1188 0.6936 0.9503 0.055 Uiso 1 1 calc R . . C13 C 1.1017(3) 0.8449(4) 0.87391(18) 0.0364(9) Uani 1 1 d . . . C14 C 1.0932(3) 0.8972(5) 0.9199(2) 0.0468(12) Uani 1 1 d . . . H14 H 1.1085 0.8617 0.9538 0.056 Uiso 1 1 calc R . . C15 C 1.0624(4) 1.0013(5) 0.9160(2) 0.0516(13) Uani 1 1 d . . . H15 H 1.0578 1.0391 0.9474 0.062 Uiso 1 1 calc R . . C16 C 1.0385(3) 1.0501(5) 0.8661(2) 0.0462(11) Uani 1 1 d . . . H16 H 1.0177 1.1222 0.8627 0.055 Uiso 1 1 calc R . . C17 C 1.0450(3) 0.9928(4) 0.8209(2) 0.0371(10) Uani 1 1 d . . . C18 C 1.0070(3) 1.0367(4) 0.7665(2) 0.0399(10) Uani 1 1 d . . . C19 C 1.0047(4) 1.1488(5) 0.7550(2) 0.0517(13) Uani 1 1 d . . . H19 H 1.0333 1.1993 0.7812 0.062 Uiso 1 1 calc R . . C20 C 0.9599(4) 1.1829(4) 0.7051(3) 0.0573(14) Uani 1 1 d . . . H20 H 0.9584 1.2583 0.6975 0.069 Uiso 1 1 calc R . . C21 C 0.9174(4) 1.1143(5) 0.6656(2) 0.0548(14) Uani 1 1 d . . . H21 H 0.8871 1.1421 0.6318 0.066 Uiso 1 1 calc R . . C22 C 0.9191(3) 1.0018(4) 0.6758(2) 0.0389(10) Uani 1 1 d . . . C23 C 0.9655(3) 0.9666(4) 0.72732(19) 0.0367(9) Uani 1 1 d . . . H23 H 0.9679 0.8913 0.7350 0.044 Uiso 1 1 calc R . . C24 C 0.8716(3) 0.9232(5) 0.6377(2) 0.0453(11) Uani 1 1 d . . . C25 C 0.8554(3) 0.9364(6) 0.5818(2) 0.0538(14) Uani 1 1 d . . . H25 H 0.8738 0.9996 0.5672 0.065 Uiso 1 1 calc R . . C26 C 0.8123(4) 0.8567(7) 0.5482(2) 0.0626(18) Uani 1 1 d . A . H26 H 0.8001 0.8674 0.5103 0.075 Uiso 1 1 calc R . . C28 C 0.8009(3) 0.7487(5) 0.6238(2) 0.0480(13) Uani 1 1 d . A . C29 C 0.8425(3) 0.8290(4) 0.65658(19) 0.0385(10) Uani 1 1 d . . . H29 H 0.8520 0.8199 0.6944 0.046 Uiso 1 1 calc R . . C30 C 0.7782(3) 0.6472(5) 0.6484(3) 0.0508(14) Uani 1 1 d . . . C31 C 0.7866(4) 0.5472(6) 0.6257(3) 0.0628(18) Uani 1 1 d . A . H31 H 0.8029 0.5429 0.5928 0.075 Uiso 1 1 calc R . . C32 C 0.7714(5) 0.4559(6) 0.6507(4) 0.077(2) Uani 1 1 d . . . H32 H 0.7755 0.3869 0.6351 0.093 Uiso 1 1 calc R A . C33 C 0.7497(4) 0.4643(5) 0.6999(4) 0.073(2) Uani 1 1 d . A . H33 H 0.7391 0.4014 0.7185 0.088 Uiso 1 1 calc R . . C34 C 0.7440(3) 0.5655(5) 0.7206(3) 0.0526(14) Uani 1 1 d . . . C35 C 0.7249(3) 0.5759(4) 0.7747(3) 0.0469(12) Uani 1 1 d . A . C36 C 0.7332(4) 0.4903(5) 0.8086(4) 0.069(2) Uani 1 1 d . . . H36 H 0.7508 0.4221 0.7984 0.083 Uiso 1 1 calc R A . C37 C 0.7157(4) 0.5026(5) 0.8588(3) 0.0601(16) Uani 1 1 d . A . C38 C 0.6896(3) 0.6036(5) 0.8722(2) 0.0497(13) Uani 1 1 d . . . C39 C 0.6824(3) 0.6869(5) 0.8349(2) 0.0468(12) Uani 1 1 d . A . H39 H 0.6650 0.7563 0.8440 0.056 Uiso 1 1 calc R . . C40 C 0.7209(6) 0.4087(7) 0.8971(5) 0.100(3) Uani 1 1 d . . . H40A H 0.7781 0.3783 0.9061 0.120 Uiso 1 1 calc R A . H40B H 0.6817 0.3510 0.8799 0.120 Uiso 1 1 calc R . . C41 C 0.6987(4) 0.4477(7) 0.9492(4) 0.080(2) Uani 1 1 d . A . H41 H 0.7032 0.3920 0.9781 0.097 Uiso 1 1 calc R . . C42 C 0.7461(4) 0.5570(8) 0.9672(4) 0.085(3) Uani 1 1 d . . . H42A H 0.8005 0.5627 0.9580 0.102 Uiso 1 1 calc R A . H42B H 0.7510 0.5764 1.0053 0.102 Uiso 1 1 calc R . . C43 C 0.6723(4) 0.6152(5) 0.9261(3) 0.0557(14) Uani 1 1 d . A . H43 H 0.6562 0.6889 0.9362 0.067 Uiso 1 1 calc R . . C44 C 0.6154(4) 0.5160(6) 0.9352(3) 0.0627(16) Uani 1 1 d . . . C45 C 0.5459(4) 0.4800(7) 0.8895(3) 0.0684(17) Uani 1 1 d . A . H45A H 0.5654 0.4772 0.8565 0.103 Uiso 1 1 calc R . . H45B H 0.4994 0.5312 0.8847 0.103 Uiso 1 1 calc R . . H45C H 0.5271 0.4078 0.8973 0.103 Uiso 1 1 calc R . . C46 C 0.5814(4) 0.5329(7) 0.9852(3) 0.0688(18) Uani 1 1 d . A . H46A H 0.5364 0.5867 0.9771 0.103 Uiso 1 1 calc R . . H46B H 0.6263 0.5588 1.0152 0.103 Uiso 1 1 calc R . . H46C H 0.5597 0.4642 0.9952 0.103 Uiso 1 1 calc R . . C47 C 1.2732(4) 1.1521(8) 0.5965(3) 0.076(2) Uani 1 1 d . . . H47A H 1.2895 1.1754 0.5640 0.114 Uiso 1 1 calc R . . H47B H 1.2463 1.0810 0.5902 0.114 Uiso 1 1 calc R . . H47C H 1.3229 1.1474 0.6267 0.114 Uiso 1 1 calc R . . C48 C 1.2124(4) 1.2341(6) 0.6098(3) 0.0636(17) Uani 1 1 d . . . C49 C 1.2541(5) 1.3473(7) 0.6175(4) 0.084(2) Uani 1 1 d . . . H49A H 1.3078 1.3427 0.6443 0.126 Uiso 1 1 calc R . . H49B H 1.2177 1.3985 0.6300 0.126 Uiso 1 1 calc R . . H49C H 1.2630 1.3725 0.5832 0.126 Uiso 1 1 calc R . . C50 C 1.1707(4) 1.2050(5) 0.6559(3) 0.0571(14) Uani 1 1 d . . . H50 H 1.1987 1.2338 0.6924 0.069 Uiso 1 1 calc R . . C51 C 1.0930(4) 1.2697(6) 0.6236(3) 0.0664(17) Uani 1 1 d . . . H51A H 1.0957 1.3486 0.6308 0.080 Uiso 1 1 calc R . . H51B H 1.0387 1.2389 0.6256 0.080 Uiso 1 1 calc R . . C52 C 1.1221(4) 1.2352(6) 0.5723(3) 0.0658(18) Uani 1 1 d . . . H52 H 1.1123 1.2905 0.5429 0.079 Uiso 1 1 calc R . . C53 C 1.0882(4) 1.1261(6) 0.5552(3) 0.0613(16) Uani 1 1 d . . . H53A H 1.1155 1.0970 0.5280 0.074 Uiso 1 1 calc R . . H53B H 1.0276 1.1317 0.5384 0.074 Uiso 1 1 calc R . . C54 C 1.1028(3) 1.0491(5) 0.6031(2) 0.0440(11) Uani 1 1 d . . . C55 C 1.1460(3) 1.0892(4) 0.6536(2) 0.0446(11) Uani 1 1 d . . . C56 C 1.1582(3) 1.0201(4) 0.6975(2) 0.0410(10) Uani 1 1 d . . . H56 H 1.1861 1.0480 0.7318 0.049 Uiso 1 1 calc R . . C57 C 1.0928(3) 0.8775(4) 0.64624(19) 0.0370(10) Uani 1 1 d . . . C58 C 1.0768(3) 0.9407(5) 0.6006(2) 0.0479(12) Uani 1 1 d . . . H58 H 1.0477 0.9106 0.5670 0.058 Uiso 1 1 calc R . . C59 C 1.0642(3) 0.7640(5) 0.6447(2) 0.0426(11) Uani 1 1 d . . . C60 C 1.0440(4) 0.7064(6) 0.5959(3) 0.0565(14) Uani 1 1 d . . . H60 H 1.0487 0.7390 0.5633 0.068 Uiso 1 1 calc R . . C61 C 1.0171(4) 0.6009(5) 0.5969(3) 0.0561(14) Uani 1 1 d . . . H61 H 1.0054 0.5586 0.5649 0.067 Uiso 1 1 calc R . . C62 C 1.0069(3) 0.5562(5) 0.6447(3) 0.0509(13) Uani 1 1 d . . . H62 H 0.9877 0.4839 0.6453 0.061 Uiso 1 1 calc R . . C63 C 1.0250(3) 0.6175(4) 0.6909(2) 0.0405(10) Uani 1 1 d . . . C64 C 1.0044(3) 0.5784(4) 0.7403(2) 0.0391(10) Uani 1 1 d . . . C65 C 0.7865(3) 0.7626(7) 0.5676(2) 0.0610(18) Uani 1 1 d . . . H65 H 0.7594 0.7076 0.5436 0.073 Uiso 1 1 calc R A . C66 C 1.0079(3) 0.4692(4) 0.7536(3) 0.0506(13) Uani 1 1 d . . . H66 H 1.0286 0.4179 0.7325 0.061 Uiso 1 1 calc R . . C67 C 0.9804(4) 0.4357(5) 0.7984(3) 0.0547(14) Uani 1 1 d . . . H67 H 0.9830 0.3612 0.8080 0.066 Uiso 1 1 calc R . . C68 C 0.9496(3) 0.5092(4) 0.8288(2) 0.0461(11) Uani 1 1 d . . . H68 H 0.9309 0.4849 0.8589 0.055 Uiso 1 1 calc R . . C69 C 0.9455(3) 0.6173(4) 0.8162(2) 0.0370(10) Uani 1 1 d . . . C70 C 0.9738(3) 0.6504(4) 0.7716(2) 0.0370(9) Uani 1 1 d . . . H70 H 0.9717 0.7252 0.7626 0.044 Uiso 1 1 calc R . . C71 C 0.9096(3) 0.7009(4) 0.84564(19) 0.0363(10) Uani 1 1 d . . . C72 C 0.9135(3) 0.6951(5) 0.9001(2) 0.0478(12) Uani 1 1 d . . . H72 H 0.9380 0.6339 0.9204 0.057 Uiso 1 1 calc R . . C73 C 0.8817(3) 0.7790(7) 0.9249(2) 0.0585(16) Uani 1 1 d . . . H73 H 0.8858 0.7749 0.9625 0.070 Uiso 1 1 calc R . . C74 C 0.8446(3) 0.8671(5) 0.8967(2) 0.0512(13) Uani 1 1 d . . . H74 H 0.8236 0.9237 0.9147 0.061 Uiso 1 1 calc R . . C75 C 0.8374(3) 0.8738(4) 0.8411(2) 0.0426(11) Uani 1 1 d . A . C76 C 0.8703(3) 0.7889(4) 0.81705(19) 0.0353(9) Uani 1 1 d . . . H76 H 0.8654 0.7917 0.7793 0.042 Uiso 1 1 calc R . . C77 C 0.8018(3) 0.9689(4) 0.8074(2) 0.0454(12) Uani 1 1 d . . . C78 C 0.8168(5) 1.0724(6) 0.8282(3) 0.075(2) Uani 1 1 d . A . H78 H 0.8465 1.0831 0.8647 0.090 Uiso 1 1 calc R . . C79 C 0.7884(6) 1.1590(6) 0.7957(4) 0.096(3) Uani 1 1 d . . . H79 H 0.7944 1.2304 0.8099 0.115 Uiso 1 1 calc R A . C80 C 0.7507(5) 1.1410(5) 0.7416(4) 0.084(3) Uani 1 1 d . A . H80 H 0.7352 1.2002 0.7175 0.100 Uiso 1 1 calc R . . C81 C 0.7362(3) 1.0367(5) 0.7236(3) 0.0536(14) Uani 1 1 d . . . C82 C 0.6896(3) 1.0121(5) 0.6669(2) 0.0508(13) Uani 1 1 d . A . C83 C 0.6805(4) 1.0889(5) 0.6264(3) 0.0625(16) Uani 1 1 d . . . H83 H 0.7047 1.1587 0.6341 0.075 Uiso 1 1 calc R A . C84 C 0.6356(4) 1.0631(6) 0.5742(3) 0.0579(15) Uani 1 1 d . A . C85 C 0.6001(4) 0.9614(6) 0.5659(2) 0.0573(15) Uani 1 1 d . . . C86 C 0.6128(4) 0.8901(5) 0.6072(2) 0.0503(12) Uani 1 1 d . A . H86 H 0.5886 0.8201 0.6002 0.060 Uiso 1 1 calc R . . C87 C 0.5479(5) 0.9383(7) 0.5094(3) 0.079(2) Uani 1 1 d . A . H87 H 0.5227 0.8645 0.5023 0.094 Uiso 1 1 calc R . . C88 C 0.6016(7) 0.9790(11) 0.4711(4) 0.109(4) Uani 1 1 d . . . H88A H 0.6626 0.9715 0.4862 0.130 Uiso 1 1 calc R A . H88B H 0.5842 0.9493 0.4341 0.130 Uiso 1 1 calc R . . C89 C 0.5679(5) 1.0929(8) 0.4769(4) 0.089(3) Uani 1 1 d . A . H89 H 0.5566 1.1386 0.4437 0.107 Uiso 1 1 calc R . . C90 C 0.6221(5) 1.1446(8) 0.5271(4) 0.085(2) Uani 1 1 d . . . H90A H 0.5947 1.2108 0.5361 0.102 Uiso 1 1 calc R A . H90B H 0.6765 1.1654 0.5207 0.102 Uiso 1 1 calc R . . C91 C 0.4897(5) 1.0370(8) 0.4888(3) 0.079(2) Uani 1 1 d . . . C92 C 0.4451(5) 1.0913(8) 0.5272(4) 0.087(3) Uani 1 1 d . A . H92A H 0.4855 1.1073 0.5614 0.130 Uiso 1 1 calc R . . H92B H 0.4019 1.0428 0.5338 0.130 Uiso 1 1 calc R . . H92C H 0.4193 1.1589 0.5111 0.130 Uiso 1 1 calc R . . C93 C 0.4241(8) 1.0081(11) 0.4361(4) 0.116(4) Uani 1 1 d . A . H93A H 0.3756 0.9742 0.4449 0.174 Uiso 1 1 calc R . . H93B H 0.4486 0.9577 0.4149 0.174 Uiso 1 1 calc R . . H93C H 0.4064 1.0742 0.4152 0.174 Uiso 1 1 calc R . . N1S N 0.6898(10) 0.9854(14) 0.2422(7) 0.104(6) Uani 0.50 1 d P . . C1S C 0.6655(9) 0.9001(13) 0.2326(6) 0.067(3) Uani 0.50 1 d P . . C2S C 0.6307(10) 0.7946(13) 0.2182(7) 0.073(4) Uani 0.50 1 d P . . H2S1 H 0.6188 0.7600 0.2499 0.110 Uiso 0.50 1 calc PR . . H2S2 H 0.6706 0.7503 0.2051 0.110 Uiso 0.50 1 calc PR . . H2S3 H 0.5789 0.8015 0.1898 0.110 Uiso 0.50 1 calc PR . . N9 N 0.5678(3) 0.6969(5) 0.6810(3) 0.0680(15) Uani 1 1 d . A . C94 C 0.5213(5) 0.6438(8) 0.6932(4) 0.090(3) Uani 1 1 d D . . C95A C 0.4676(13) 0.5814(19) 0.7202(10) 0.100(6) Uiso 0.50 1 d PD A 1 H95A H 0.5023 0.5343 0.7477 0.150 Uiso 0.50 1 calc PR A 1 H95B H 0.4286 0.5370 0.6936 0.150 Uiso 0.50 1 calc PR A 1 H95C H 0.4361 0.6313 0.7374 0.150 Uiso 0.50 1 calc PR A 1 C95B C 0.4709(16) 0.5447(19) 0.6950(13) 0.121(8) Uiso 0.50 1 d PD A 2 H95D H 0.4120 0.5600 0.6784 0.181 Uiso 0.50 1 calc PR A 2 H95E H 0.4776 0.5227 0.7326 0.181 Uiso 0.50 1 calc PR A 2 H95F H 0.4901 0.4862 0.6752 0.181 Uiso 0.50 1 calc PR A 2 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 0.0439(4) 0.0413(4) 0.0316(4) 0.0041(3) 0.0151(3) 0.0055(3) Mn2 0.0442(4) 0.0416(4) 0.0410(4) -0.0033(3) 0.0101(3) 0.0076(3) Cl1 0.0610(8) 0.0752(10) 0.0598(9) 0.0007(7) 0.0122(7) -0.0037(7) O1 0.061(2) 0.059(2) 0.057(2) 0.0126(19) 0.0302(19) 0.0162(19) O3 0.051(2) 0.075(3) 0.047(2) 0.001(2) 0.0087(17) 0.0046(19) O4 0.117(5) 0.085(4) 0.088(4) -0.017(3) -0.002(3) 0.030(4) O5 0.079(3) 0.120(5) 0.104(5) -0.009(4) 0.019(3) -0.029(4) O6 0.099(4) 0.166(7) 0.059(3) -0.008(4) 0.023(3) -0.040(4) Cl2 0.0671(7) 0.0420(6) 0.0338(6) 0.0002(5) 0.0073(5) -0.0021(5) O7 0.106(3) 0.048(2) 0.0281(18) 0.0012(16) 0.0078(19) 0.018(2) O8 0.180(7) 0.086(4) 0.068(4) -0.007(3) 0.050(4) 0.045(4) O9 0.095(3) 0.045(2) 0.054(3) 0.0157(19) 0.017(2) -0.003(2) O10 0.117(5) 0.136(6) 0.098(5) 0.069(5) -0.048(4) -0.066(5) Cl3 0.0940(10) 0.0484(7) 0.0456(7) -0.0034(6) 0.0292(7) -0.0147(7) O11 0.142(6) 0.150(7) 0.094(5) -0.001(5) 0.005(4) -0.074(6) O12 0.112(4) 0.085(4) 0.053(3) 0.007(2) 0.024(3) -0.025(3) O13 0.141(6) 0.133(6) 0.074(4) -0.011(4) 0.045(4) -0.001(5) O14 0.200(9) 0.072(4) 0.099(5) 0.019(4) 0.011(5) -0.009(5) N1 0.048(2) 0.046(2) 0.037(2) 0.0089(18) 0.0163(17) 0.0083(17) N2 0.0351(17) 0.039(2) 0.032(2) -0.0002(15) 0.0094(15) 0.0020(15) N3 0.0348(18) 0.047(2) 0.050(3) -0.0183(19) 0.0122(17) -0.0008(16) N4 0.0376(18) 0.036(2) 0.050(2) -0.0059(18) 0.0098(17) 0.0021(16) N5 0.045(2) 0.044(2) 0.034(2) 0.0035(17) 0.0174(17) 0.0023(17) N6 0.0425(19) 0.037(2) 0.034(2) -0.0001(16) 0.0163(16) 0.0037(15) N7 0.043(2) 0.036(2) 0.047(2) -0.0087(18) 0.0072(17) 0.0094(16) N8 0.0402(19) 0.039(2) 0.041(2) -0.0007(17) 0.0105(16) 0.0065(16) C1 0.093(5) 0.086(6) 0.097(6) 0.037(5) 0.043(5) 0.045(5) C2 0.050(3) 0.092(5) 0.086(5) 0.024(4) 0.018(3) 0.017(3) C3 0.064(3) 0.076(4) 0.069(4) 0.033(3) 0.030(3) 0.024(3) C4 0.061(3) 0.060(4) 0.079(5) 0.033(3) 0.027(3) 0.019(3) C5 0.082(4) 0.048(4) 0.085(5) 0.015(3) 0.015(4) 0.011(3) C6 0.081(4) 0.053(4) 0.065(4) 0.017(3) 0.027(3) 0.023(3) C7 0.054(3) 0.051(3) 0.055(3) 0.015(3) 0.019(2) 0.014(2) C8 0.046(2) 0.050(3) 0.049(3) 0.015(2) 0.017(2) 0.010(2) C9 0.059(3) 0.070(4) 0.055(3) 0.027(3) 0.028(3) 0.012(3) C10 0.061(3) 0.050(3) 0.043(3) 0.006(2) 0.020(2) 0.016(2) C11 0.034(2) 0.051(3) 0.036(2) 0.003(2) 0.0115(18) 0.0030(19) C12 0.047(3) 0.059(3) 0.034(3) 0.005(2) 0.016(2) 0.004(2) C13 0.041(2) 0.045(3) 0.025(2) -0.0019(18) 0.0119(17) -0.0027(18) C14 0.058(3) 0.049(3) 0.031(3) -0.004(2) 0.007(2) 0.001(2) C15 0.063(3) 0.055(3) 0.038(3) -0.013(2) 0.014(2) 0.000(3) C16 0.055(3) 0.044(3) 0.042(3) -0.008(2) 0.016(2) 0.001(2) C17 0.043(2) 0.035(2) 0.037(2) -0.0082(19) 0.0173(19) -0.0014(18) C18 0.059(3) 0.029(2) 0.037(3) 0.0002(18) 0.023(2) 0.0048(19) C19 0.077(4) 0.036(3) 0.045(3) 0.001(2) 0.021(3) 0.004(2) C20 0.088(4) 0.028(2) 0.061(4) 0.004(2) 0.027(3) 0.005(2) C21 0.082(4) 0.043(3) 0.042(3) 0.013(2) 0.020(3) 0.021(3) C22 0.051(3) 0.031(2) 0.038(3) 0.0086(19) 0.018(2) 0.0104(19) C23 0.046(2) 0.036(2) 0.033(2) 0.0038(18) 0.0180(19) 0.0046(18) C24 0.053(3) 0.053(3) 0.030(2) 0.001(2) 0.011(2) 0.017(2) C25 0.053(3) 0.076(4) 0.036(3) 0.008(3) 0.020(2) 0.017(3) C26 0.051(3) 0.109(6) 0.027(3) -0.008(3) 0.008(2) 0.013(3) C28 0.038(2) 0.070(4) 0.037(3) -0.019(2) 0.011(2) 0.009(2) C29 0.045(2) 0.044(3) 0.028(2) -0.0041(19) 0.0107(18) 0.0050(19) C30 0.032(2) 0.054(3) 0.066(4) -0.028(3) 0.010(2) -0.002(2) C31 0.049(3) 0.073(4) 0.071(4) -0.043(4) 0.024(3) -0.009(3) C32 0.080(4) 0.052(4) 0.113(6) -0.052(4) 0.048(4) -0.022(3) C33 0.074(4) 0.036(3) 0.123(6) -0.024(3) 0.050(4) -0.014(3) C34 0.040(2) 0.039(3) 0.085(4) -0.020(3) 0.028(3) 0.000(2) C35 0.036(2) 0.040(3) 0.067(4) -0.008(2) 0.017(2) 0.0007(19) C36 0.048(3) 0.045(3) 0.124(6) 0.013(3) 0.042(4) 0.008(2) C37 0.049(3) 0.052(3) 0.084(5) 0.018(3) 0.026(3) 0.011(2) C38 0.037(2) 0.051(3) 0.058(3) 0.009(3) 0.006(2) -0.003(2) C39 0.045(2) 0.046(3) 0.050(3) -0.004(2) 0.012(2) 0.001(2) C40 0.091(5) 0.072(5) 0.157(9) 0.063(6) 0.072(6) 0.038(4) C41 0.058(4) 0.084(5) 0.103(6) 0.048(5) 0.028(4) 0.007(3) C42 0.044(3) 0.127(7) 0.076(5) 0.040(5) 0.002(3) -0.018(4) C43 0.052(3) 0.059(3) 0.052(3) 0.014(3) 0.006(2) -0.007(3) C44 0.048(3) 0.066(4) 0.075(4) 0.008(3) 0.018(3) -0.011(3) C45 0.064(4) 0.074(4) 0.071(4) -0.008(3) 0.023(3) -0.018(3) C46 0.058(3) 0.083(5) 0.066(4) 0.002(3) 0.018(3) -0.015(3) C47 0.061(3) 0.103(6) 0.073(5) 0.018(4) 0.033(3) -0.004(4) C48 0.057(3) 0.078(4) 0.054(4) 0.024(3) 0.011(3) -0.015(3) C49 0.086(5) 0.079(5) 0.088(5) 0.032(4) 0.023(4) -0.025(4) C50 0.067(3) 0.058(3) 0.048(3) 0.008(3) 0.018(3) -0.008(3) C51 0.069(4) 0.060(4) 0.074(4) 0.028(3) 0.024(3) 0.001(3) C52 0.062(3) 0.080(5) 0.055(4) 0.034(3) 0.015(3) -0.005(3) C53 0.060(3) 0.077(4) 0.050(3) 0.024(3) 0.019(3) -0.003(3) C54 0.051(3) 0.053(3) 0.031(3) 0.010(2) 0.015(2) -0.006(2) C55 0.052(3) 0.048(3) 0.039(3) 0.007(2) 0.021(2) -0.001(2) C56 0.048(2) 0.042(3) 0.036(3) -0.002(2) 0.015(2) -0.004(2) C57 0.040(2) 0.042(2) 0.033(2) -0.0033(19) 0.0167(18) -0.0028(18) C58 0.052(3) 0.065(3) 0.029(2) 0.001(2) 0.013(2) -0.001(2) C59 0.046(2) 0.053(3) 0.033(2) -0.006(2) 0.018(2) 0.006(2) C60 0.064(3) 0.065(4) 0.046(3) -0.014(3) 0.024(3) -0.009(3) C61 0.067(3) 0.059(3) 0.047(3) -0.016(3) 0.023(3) -0.001(3) C62 0.049(3) 0.049(3) 0.059(4) -0.013(3) 0.022(2) 0.000(2) C63 0.039(2) 0.042(3) 0.045(3) -0.007(2) 0.020(2) 0.0048(19) C64 0.037(2) 0.030(2) 0.050(3) -0.0018(19) 0.012(2) 0.0082(17) C65 0.041(2) 0.102(5) 0.038(3) -0.030(3) 0.005(2) 0.002(3) C66 0.053(3) 0.035(3) 0.071(4) -0.003(2) 0.028(3) 0.008(2) C67 0.057(3) 0.034(3) 0.075(4) 0.005(3) 0.020(3) 0.003(2) C68 0.044(2) 0.039(3) 0.055(3) 0.009(2) 0.013(2) 0.002(2) C69 0.036(2) 0.034(2) 0.041(3) 0.0041(19) 0.0092(18) 0.0007(17) C70 0.045(2) 0.032(2) 0.037(2) 0.0024(18) 0.0154(19) 0.0040(18) C71 0.033(2) 0.043(3) 0.035(2) -0.0002(19) 0.0128(18) -0.0005(18) C72 0.037(2) 0.064(3) 0.043(3) 0.011(2) 0.012(2) 0.005(2) C73 0.046(3) 0.101(5) 0.029(2) -0.004(3) 0.010(2) 0.007(3) C74 0.047(3) 0.069(4) 0.037(3) -0.015(3) 0.010(2) 0.008(2) C75 0.038(2) 0.045(3) 0.042(3) -0.015(2) 0.0037(19) 0.0073(19) C76 0.0324(18) 0.040(2) 0.035(2) -0.0038(19) 0.0107(16) 0.0022(17) C77 0.043(2) 0.043(3) 0.045(3) -0.015(2) 0.002(2) 0.011(2) C78 0.078(4) 0.055(4) 0.071(4) -0.031(3) -0.019(3) 0.026(3) C79 0.105(5) 0.038(3) 0.110(7) -0.031(4) -0.041(5) 0.024(4) C80 0.093(5) 0.028(3) 0.102(6) -0.004(3) -0.028(4) 0.022(3) C81 0.051(3) 0.040(3) 0.061(4) -0.010(2) -0.003(2) 0.010(2) C82 0.048(3) 0.046(3) 0.054(3) -0.007(2) 0.004(2) 0.009(2) C83 0.053(3) 0.044(3) 0.085(5) 0.010(3) 0.007(3) 0.009(2) C84 0.054(3) 0.062(4) 0.057(4) 0.013(3) 0.012(3) 0.018(3) C85 0.055(3) 0.068(4) 0.047(3) -0.005(3) 0.009(2) 0.022(3) C86 0.056(3) 0.049(3) 0.041(3) -0.005(2) 0.002(2) 0.006(2) C87 0.094(5) 0.082(5) 0.046(4) -0.006(3) -0.009(3) 0.023(4) C88 0.103(6) 0.171(11) 0.052(4) 0.016(6) 0.020(4) 0.046(7) C89 0.087(5) 0.110(7) 0.069(5) 0.040(5) 0.017(4) 0.033(5) C90 0.072(4) 0.092(6) 0.088(6) 0.033(5) 0.012(4) 0.019(4) C91 0.068(4) 0.094(6) 0.066(5) 0.019(4) -0.002(3) 0.017(4) C92 0.058(4) 0.106(6) 0.092(6) 0.021(5) 0.012(4) 0.033(4) C93 0.131(8) 0.124(9) 0.068(6) 0.026(6) -0.025(5) 0.018(7) N1S 0.119(11) 0.104(11) 0.126(13) -0.063(10) 0.099(11) -0.052(9) C1S 0.074(8) 0.073(9) 0.068(9) -0.006(7) 0.047(7) -0.005(7) C2S 0.080(8) 0.062(8) 0.076(9) -0.006(7) 0.017(7) -0.024(7) N9 0.044(2) 0.070(4) 0.085(4) 0.021(3) 0.007(3) -0.008(2) C94 0.063(4) 0.092(6) 0.097(6) 0.005(5) -0.012(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2A C96A 1.420(14) . ? O2A Mn2 2.283(11) . ? O2A H2OA 0.8500 . ? O2A H2OB 1.1001 . ? C96A H96A 0.9800 . ? C96A H96B 0.9800 . ? C96A H96C 0.9800 . ? C96A H2OB 1.3125 . ? O2B C96B 1.443(17) . ? O2B Mn2 2.204(9) . ? O2B H2OA 1.2889 . ? O2B H2OB 0.8499 . ? C96B H2OA 0.9582 . ? C96B H96D 0.9800 . ? C96B H96E 0.9800 . ? C96B H96F 0.9800 . ? O1E C3E 1.402(15) . ? O1E C2E 1.427(13) . ? C1E C2E 1.493(15) . ? C1E H1E1 0.9800 . ? C1E H1E2 0.9800 . ? C1E H1E3 0.9800 . ? C2E H2E1 0.9900 . ? C2E H2E2 0.9900 . ? C3E C4E 1.513(18) . ? C3E H3E1 0.9900 . ? C3E H3E2 0.9900 . ? C4E H4E1 0.9800 . ? C4E H4E2 0.9800 . ? C4E H4E3 0.9800 . ? Mn1 O1 2.197(4) . ? Mn1 N5 2.202(4) . ? Mn1 N1 2.209(4) . ? Mn1 N2 2.309(4) . ? Mn1 O3 2.318(4) . ? Mn1 N6 2.369(4) . ? Mn2 N8 2.181(4) . ? Mn2 N4 2.184(5) . ? Mn2 N7 2.288(4) . ? Mn2 N9 2.331(6) . ? Mn2 N3 2.351(4) . ? Cl1 O6 1.385(6) . ? Cl1 O5 1.405(6) . ? Cl1 O4 1.419(6) . ? Cl1 O3 1.485(5) . ? O1 H1OA 0.8499 . ? O1 H1OB 0.8499 . ? Cl2 O7 1.411(4) . ? Cl2 O8 1.414(7) . ? Cl2 O10 1.418(6) . ? Cl2 O9 1.434(4) . ? Cl3 O11 1.377(7) . ? Cl3 O14 1.416(7) . ? Cl3 O12 1.427(5) . ? Cl3 O13 1.518(8) . ? Cl4A O18A 1.330(11) . ? Cl4A O16A 1.402(12) . ? Cl4A O17A 1.431(13) . ? Cl4A O15A 1.446(14) . ? Cl4B O15B 1.309(16) . ? Cl4B O16B 1.380(13) . ? Cl4B O17B 1.398(18) . ? Cl4B O18B 1.438(15) . ? N1 C10 1.329(7) . ? N1 C11 1.348(7) . ? N2 C13 1.360(6) . ? N2 C17 1.370(6) . ? N3 C34 1.334(8) . ? N3 C30 1.357(8) . ? N4 C35 1.340(7) . ? N4 C39 1.345(7) . ? N5 C56 1.328(7) . ? N5 C57 1.351(6) . ? N6 C59 1.352(7) . ? N6 C63 1.378(7) . ? N7 C77 1.333(7) . ? N7 C81 1.363(8) . ? N8 C82 1.335(7) . ? N8 C86 1.349(7) . ? C1 C3 1.540(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.508(12) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C6 1.551(10) . ? C3 C4 1.552(9) . ? C4 C5 1.520(12) . ? C4 C9 1.522(10) . ? C4 H4 1.0000 . ? C5 C6 1.551(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.511(8) . ? C6 H6 1.0000 . ? C7 C10 1.387(8) . ? C7 C8 1.393(8) . ? C8 C12 1.376(8) . ? C8 C9 1.512(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10 0.9500 . ? C11 C12 1.391(7) . ? C11 C13 1.473(7) . ? C12 H12 0.9500 . ? C13 C14 1.381(7) . ? C14 C15 1.378(9) . ? C14 H14 0.9500 . ? C15 C16 1.380(8) . ? C15 H15 0.9500 . ? C16 C17 1.384(7) . ? C16 H16 0.9500 . ? C17 C18 1.480(7) . ? C18 C23 1.372(7) . ? C18 C19 1.415(7) . ? C19 C20 1.374(9) . ? C19 H19 0.9500 . ? C20 C21 1.373(9) . ? C20 H20 0.9500 . ? C21 C22 1.412(7) . ? C21 H21 0.9500 . ? C22 C23 1.420(7) . ? C22 C24 1.459(8) . ? C23 H23 0.9500 . ? C24 C29 1.390(8) . ? C24 C25 1.400(7) . ? C25 C26 1.383(10) . ? C25 H25 0.9500 . ? C26 C65 1.375(11) . ? C26 H26 0.9500 . ? C28 C29 1.369(7) . ? C28 C65 1.410(8) . ? C28 C30 1.493(9) . ? C29 H29 0.9500 . ? C30 C31 1.386(8) . ? C31 C32 1.351(12) . ? C31 H31 0.9500 . ? C32 C33 1.399(11) . ? C32 H32 0.9500 . ? C33 C34 1.371(8) . ? C33 H33 0.9500 . ? C34 C35 1.503(9) . ? C35 C36 1.355(9) . ? C36 C37 1.396(11) . ? C36 H36 0.9500 . ? C37 C38 1.391(9) . ? C37 C40 1.508(9) . ? C38 C39 1.388(8) . ? C38 C43 1.487(9) . ? C39 H39 0.9500 . ? C40 C41 1.549(14) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.571(13) . ? C41 C44 1.578(10) . ? C41 H41 1.0000 . ? C42 C43 1.573(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.598(8) . ? C43 H43 1.0000 . ? C44 C45 1.489(10) . ? C44 C46 1.539(10) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.525(12) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.550(10) . ? C48 C50 1.554(9) . ? C48 C52 1.560(9) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C55 1.483(8) . ? C50 C51 1.562(9) . ? C50 H50 1.0000 . ? C51 C52 1.569(11) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.483(11) . ? C52 H52 1.0000 . ? C53 C54 1.524(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.402(8) . ? C54 C58 1.402(8) . ? C55 C56 1.388(7) . ? C56 H56 0.9500 . ? C57 C58 1.377(7) . ? C57 C59 1.476(7) . ? C58 H58 0.9500 . ? C59 C60 1.405(8) . ? C60 C61 1.379(9) . ? C60 H60 0.9500 . ? C61 C62 1.390(9) . ? C61 H61 0.9500 . ? C62 C63 1.374(8) . ? C62 H62 0.9500 . ? C63 C64 1.473(7) . ? C64 C70 1.377(7) . ? C64 C66 1.389(7) . ? C65 H65 0.9500 . ? C66 C67 1.402(9) . ? C66 H66 0.9500 . ? C67 C68 1.375(9) . ? C67 H67 0.9500 . ? C68 C69 1.371(7) . ? C68 H68 0.9500 . ? C69 C70 1.400(7) . ? C69 C71 1.489(7) . ? C70 H70 0.9500 . ? C71 C76 1.379(7) . ? C71 C72 1.382(7) . ? C72 C73 1.387(9) . ? C72 H72 0.9500 . ? C73 C74 1.364(9) . ? C73 H73 0.9500 . ? C74 C75 1.404(8) . ? C74 H74 0.9500 . ? C75 C76 1.394(7) . ? C75 C77 1.489(8) . ? C76 H76 0.9500 . ? C77 C78 1.383(8) . ? C78 C79 1.364(11) . ? C78 H78 0.9500 . ? C79 C80 1.388(12) . ? C79 H79 0.9500 . ? C80 C81 1.370(9) . ? C80 H80 0.9500 . ? C81 C82 1.495(8) . ? C82 C83 1.388(9) . ? C83 C84 1.393(10) . ? C83 H83 0.9500 . ? C84 C85 1.380(10) . ? C84 C90 1.545(10) . ? C85 C86 1.352(9) . ? C85 C87 1.516(9) . ? C86 H86 0.9500 . ? C87 C91 1.561(11) . ? C87 C88 1.564(14) . ? C87 H87 1.0000 . ? C88 C89 1.533(15) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.513(14) . ? C89 C91 1.563(13) . ? C89 H89 1.0000 . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.525(13) . ? C91 C93 1.548(12) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? N1S C1S 1.13(2) . ? C1S C2S 1.44(2) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? N9 C94 1.114(11) . ? C94 C95A 1.475(16) . ? C94 C95B 1.488(17) . ? C95A H95A 0.9800 . ? C95A H95B 0.9800 . ? C95A H95C 0.9800 . ? C95B H95D 0.9800 . ? C95B H95E 0.9800 . ? C95B H95F 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 C96A O2A Mn2 128.4(11) . . ? C96A O2A H2OA 103.0 . . ? Mn2 O2A H2OA 102.6 . . ? C96A O2A H2OB 61.2 . . ? Mn2 O2A H2OB 92.5 . . ? H2OA O2A H2OB 163.2 . . ? O2A C96A H2OB 47.3 . . ? H96A C96A H2OB 147.2 . . ? H96B C96A H2OB 101.2 . . ? H96C C96A H2OB 69.1 . . ? C96B O2B Mn2 133.1(14) . . ? C96B O2B H2OA 40.6 . . ? Mn2 O2B H2OA 92.6 . . ? C96B O2B H2OB 106.3 . . ? Mn2 O2B H2OB 106.5 . . ? H2OA O2B H2OB 127.7 . . ? O2B C96B H2OA 61.0 . . ? O2B C96B H96D 109.5 . . ? O2B C96B H96E 109.5 . . ? H96D C96B H96E 109.5 . . ? O2B C96B H96F 109.5 . . ? H96D C96B H96F 109.5 . . ? H96E C96B H96F 109.5 . . ? C3E O1E C2E 108.8(11) . . ? O1E C2E C1E 112.0(12) . . ? O1E C2E H2E1 109.2 . . ? C1E C2E H2E1 109.2 . . ? O1E C2E H2E2 109.2 . . ? C1E C2E H2E2 109.2 . . ? H2E1 C2E H2E2 107.9 . . ? O1E C3E C4E 117.4(19) . . ? O1E C3E H3E1 108.0 . . ? C4E C3E H3E1 108.0 . . ? O1E C3E H3E2 108.0 . . ? C4E C3E H3E2 108.0 . . ? H3E1 C3E H3E2 107.2 . . ? O1 Mn1 N5 89.26(15) . . ? O1 Mn1 N1 88.72(16) . . ? N5 Mn1 N1 176.82(17) . . ? O1 Mn1 N2 156.92(15) . . ? N5 Mn1 N2 108.49(15) . . ? N1 Mn1 N2 74.11(15) . . ? O1 Mn1 O3 82.23(17) . . ? N5 Mn1 O3 87.19(16) . . ? N1 Mn1 O3 94.97(17) . . ? N2 Mn1 O3 83.99(15) . . ? O1 Mn1 N6 84.27(15) . . ? N5 Mn1 N6 73.24(15) . . ? N1 Mn1 N6 104.10(16) . . ? N2 Mn1 N6 114.45(13) . . ? O3 Mn1 N6 156.32(15) . . ? N8 Mn2 N4 173.70(16) . . ? N8 Mn2 O2B 87.1(3) . . ? N4 Mn2 O2B 93.0(3) . . ? N8 Mn2 O2A 95.6(3) . . ? N4 Mn2 O2A 85.9(3) . . ? O2B Mn2 O2A 14.8(3) . . ? N8 Mn2 N7 74.79(16) . . ? N4 Mn2 N7 111.51(16) . . ? O2B Mn2 N7 86.6(3) . . ? O2A Mn2 N7 77.2(3) . . ? N8 Mn2 N9 89.61(18) . . ? N4 Mn2 N9 84.26(18) . . ? O2B Mn2 N9 77.7(3) . . ? O2A Mn2 N9 89.9(3) . . ? N7 Mn2 N9 158.45(18) . . ? N8 Mn2 N3 103.71(17) . . ? N4 Mn2 N3 74.01(17) . . ? O2B Mn2 N3 156.7(3) . . ? O2A Mn2 N3 158.8(3) . . ? N7 Mn2 N3 116.00(14) . . ? N9 Mn2 N3 81.73(19) . . ? O6 Cl1 O5 109.4(4) . . ? O6 Cl1 O4 110.1(5) . . ? O5 Cl1 O4 110.6(5) . . ? O6 Cl1 O3 108.5(4) . . ? O5 Cl1 O3 109.0(4) . . ? O4 Cl1 O3 109.2(3) . . ? Mn1 O1 H1OA 112.8 . . ? Mn1 O1 H1OB 112.6 . . ? H1OA O1 H1OB 110.2 . . ? Cl1 O3 Mn1 143.0(3) . . ? O7 Cl2 O8 107.9(3) . . ? O7 Cl2 O10 108.8(4) . . ? O8 Cl2 O10 109.5(6) . . ? O7 Cl2 O9 110.1(3) . . ? O8 Cl2 O9 109.8(4) . . ? O10 Cl2 O9 110.7(4) . . ? O11 Cl3 O14 118.6(6) . . ? O11 Cl3 O12 115.5(4) . . ? O14 Cl3 O12 112.5(4) . . ? O11 Cl3 O13 105.2(6) . . ? O14 Cl3 O13 102.3(6) . . ? O12 Cl3 O13 99.3(4) . . ? O18A Cl4A O16A 112.1(9) . . ? O18A Cl4A O17A 105.8(9) . . ? O16A Cl4A O17A 113.1(10) . . ? O18A Cl4A O15A 104.2(10) . . ? O16A Cl4A O15A 105.0(9) . . ? O17A Cl4A O15A 116.4(11) . . ? O15B Cl4B O16B 108.1(14) . . ? O15B Cl4B O17B 99(2) . . ? O16B Cl4B O17B 115.0(16) . . ? O15B Cl4B O18B 96.3(15) . . ? O16B Cl4B O18B 117.3(12) . . ? O17B Cl4B O18B 116.7(16) . . ? C10 N1 C11 118.5(5) . . ? C10 N1 Mn1 125.3(4) . . ? C11 N1 Mn1 116.1(3) . . ? C13 N2 C17 117.2(4) . . ? C13 N2 Mn1 111.5(3) . . ? C17 N2 Mn1 127.6(3) . . ? C34 N3 C30 117.5(5) . . ? C34 N3 Mn2 109.5(3) . . ? C30 N3 Mn2 129.1(4) . . ? C35 N4 C39 118.2(5) . . ? C35 N4 Mn2 117.4(4) . . ? C39 N4 Mn2 124.4(3) . . ? C56 N5 C57 118.2(4) . . ? C56 N5 Mn1 124.0(4) . . ? C57 N5 Mn1 117.6(3) . . ? C59 N6 C63 118.0(4) . . ? C59 N6 Mn1 110.3(3) . . ? C63 N6 Mn1 127.5(3) . . ? C77 N7 C81 117.6(5) . . ? C77 N7 Mn2 126.3(4) . . ? C81 N7 Mn2 111.6(3) . . ? C82 N8 C86 117.4(5) . . ? C82 N8 Mn2 117.4(4) . . ? C86 N8 Mn2 125.3(4) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C3 C1 108.8(6) . . ? C2 C3 C6 119.6(6) . . ? C1 C3 C6 111.2(7) . . ? C2 C3 C4 119.1(7) . . ? C1 C3 C4 111.3(6) . . ? C6 C3 C4 85.2(5) . . ? C5 C4 C9 109.7(5) . . ? C5 C4 C3 88.2(6) . . ? C9 C4 C3 111.4(6) . . ? C5 C4 H4 114.9 . . ? C9 C4 H4 114.9 . . ? C3 C4 H4 114.9 . . ? C4 C5 C6 86.3(6) . . ? C4 C5 H5A 114.3 . . ? C6 C5 H5A 114.3 . . ? C4 C5 H5B 114.3 . . ? C6 C5 H5B 114.3 . . ? H5A C5 H5B 111.4 . . ? C7 C6 C5 107.4(5) . . ? C7 C6 C3 107.2(6) . . ? C5 C6 C3 87.1(5) . . ? C7 C6 H6 117.0 . . ? C5 C6 H6 117.0 . . ? C3 C6 H6 117.0 . . ? C10 C7 C8 117.4(5) . . ? C10 C7 C6 124.9(6) . . ? C8 C7 C6 117.7(5) . . ? C12 C8 C7 118.9(5) . . ? C12 C8 C9 123.7(5) . . ? C7 C8 C9 117.4(5) . . ? C8 C9 C4 110.4(5) . . ? C8 C9 H9A 109.6 . . ? C4 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C4 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N1 C10 C7 124.1(5) . . ? N1 C10 H10 118.0 . . ? C7 C10 H10 118.0 . . ? N1 C11 C12 120.8(5) . . ? N1 C11 C13 117.6(4) . . ? C12 C11 C13 121.6(5) . . ? C8 C12 C11 120.3(5) . . ? C8 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? N2 C13 C14 122.6(5) . . ? N2 C13 C11 116.2(4) . . ? C14 C13 C11 121.2(5) . . ? C15 C14 C13 119.4(5) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.3(5) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C17 119.3(5) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? N2 C17 C16 122.2(5) . . ? N2 C17 C18 117.7(4) . . ? C16 C17 C18 119.8(5) . . ? C23 C18 C19 118.8(5) . . ? C23 C18 C17 118.4(4) . . ? C19 C18 C17 122.5(5) . . ? C20 C19 C18 118.3(5) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C21 C20 C19 123.7(5) . . ? C21 C20 H20 118.1 . . ? C19 C20 H20 118.1 . . ? C20 C21 C22 119.2(5) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C22 C23 117.0(5) . . ? C21 C22 C24 123.3(5) . . ? C23 C22 C24 119.5(4) . . ? C18 C23 C22 122.9(4) . . ? C18 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C29 C24 C25 117.3(5) . . ? C29 C24 C22 120.0(4) . . ? C25 C24 C22 122.6(5) . . ? C26 C25 C24 119.5(6) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C65 C26 C25 122.2(5) . . ? C65 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C29 C28 C65 118.0(6) . . ? C29 C28 C30 119.3(5) . . ? C65 C28 C30 122.5(5) . . ? C28 C29 C24 123.8(5) . . ? C28 C29 H29 118.1 . . ? C24 C29 H29 118.1 . . ? N3 C30 C31 121.9(6) . . ? N3 C30 C28 117.4(4) . . ? C31 C30 C28 120.6(6) . . ? C32 C31 C30 119.7(6) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.0(5) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C34 C33 C32 118.4(7) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? N3 C34 C33 123.3(6) . . ? N3 C34 C35 117.5(4) . . ? C33 C34 C35 119.1(6) . . ? N4 C35 C36 122.8(6) . . ? N4 C35 C34 116.2(5) . . ? C36 C35 C34 121.0(5) . . ? C35 C36 C37 119.8(6) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 118.3(6) . . ? C38 C37 C40 120.0(7) . . ? C36 C37 C40 121.7(7) . . ? C39 C38 C37 118.3(6) . . ? C39 C38 C43 124.4(6) . . ? C37 C38 C43 117.3(5) . . ? N4 C39 C38 122.7(5) . . ? N4 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C37 C40 C41 109.6(7) . . ? C37 C40 H40A 109.8 . . ? C41 C40 H40A 109.8 . . ? C37 C40 H40B 109.8 . . ? C41 C40 H40B 109.8 . . ? H40A C40 H40B 108.2 . . ? C40 C41 C42 108.1(6) . . ? C40 C41 C44 110.6(6) . . ? C42 C41 C44 87.2(6) . . ? C40 C41 H41 115.8 . . ? C42 C41 H41 115.8 . . ? C44 C41 H41 115.8 . . ? C41 C42 C43 87.1(5) . . ? C41 C42 H42A 114.1 . . ? C43 C42 H42A 114.1 . . ? C41 C42 H42B 114.1 . . ? C43 C42 H42B 114.1 . . ? H42A C42 H42B 111.3 . . ? C38 C43 C42 106.3(6) . . ? C38 C43 C44 108.7(5) . . ? C42 C43 C44 86.4(5) . . ? C38 C43 H43 117.0 . . ? C42 C43 H43 117.0 . . ? C44 C43 H43 117.0 . . ? C45 C44 C46 108.9(5) . . ? C45 C44 C41 118.6(7) . . ? C46 C44 C41 111.4(6) . . ? C45 C44 C43 118.7(6) . . ? C46 C44 C43 111.7(6) . . ? C41 C44 C43 86.0(5) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C47 C48 C49 109.3(6) . . ? C47 C48 C50 117.5(6) . . ? C49 C48 C50 112.3(7) . . ? C47 C48 C52 116.9(7) . . ? C49 C48 C52 113.4(6) . . ? C50 C48 C52 86.0(5) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C55 C50 C48 111.3(6) . . ? C55 C50 C51 106.9(5) . . ? C48 C50 C51 86.7(5) . . ? C55 C50 H50 116.1 . . ? C48 C50 H50 116.1 . . ? C51 C50 H50 116.1 . . ? C50 C51 C52 85.4(5) . . ? C50 C51 H51A 114.4 . . ? C52 C51 H51A 114.4 . . ? C50 C51 H51B 114.4 . . ? C52 C51 H51B 114.4 . . ? H51A C51 H51B 111.5 . . ? C53 C52 C48 114.0(6) . . ? C53 C52 C51 108.7(5) . . ? C48 C52 C51 86.2(5) . . ? C53 C52 H52 114.8 . . ? C48 C52 H52 114.8 . . ? C51 C52 H52 114.8 . . ? C52 C53 C54 110.9(5) . . ? C52 C53 H53A 109.5 . . ? C54 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 108.0 . . ? C55 C54 C58 117.4(5) . . ? C55 C54 C53 117.6(5) . . ? C58 C54 C53 125.0(5) . . ? C56 C55 C54 117.9(5) . . ? C56 C55 C50 125.3(5) . . ? C54 C55 C50 116.7(5) . . ? N5 C56 C55 124.3(5) . . ? N5 C56 H56 117.8 . . ? C55 C56 H56 117.8 . . ? N5 C57 C58 121.4(5) . . ? N5 C57 C59 117.0(4) . . ? C58 C57 C59 121.6(5) . . ? C57 C58 C54 120.7(5) . . ? C57 C58 H58 119.7 . . ? C54 C58 H58 119.7 . . ? N6 C59 C60 122.7(5) . . ? N6 C59 C57 116.8(4) . . ? C60 C59 C57 120.5(5) . . ? C61 C60 C59 117.9(6) . . ? C61 C60 H60 121.0 . . ? C59 C60 H60 121.0 . . ? C60 C61 C62 120.1(6) . . ? C60 C61 H61 119.9 . . ? C62 C61 H61 119.9 . . ? C63 C62 C61 119.5(6) . . ? C63 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? C62 C63 N6 121.6(5) . . ? C62 C63 C64 120.9(5) . . ? N6 C63 C64 117.3(4) . . ? C70 C64 C66 118.9(5) . . ? C70 C64 C63 119.2(4) . . ? C66 C64 C63 121.7(5) . . ? C26 C65 C28 119.0(6) . . ? C26 C65 H65 120.5 . . ? C28 C65 H65 120.5 . . ? C64 C66 C67 119.1(5) . . ? C64 C66 H66 120.5 . . ? C67 C66 H66 120.5 . . ? C68 C67 C66 120.8(5) . . ? C68 C67 H67 119.6 . . ? C66 C67 H67 119.6 . . ? C69 C68 C67 120.8(5) . . ? C69 C68 H68 119.6 . . ? C67 C68 H68 119.6 . . ? C68 C69 C70 118.1(5) . . ? C68 C69 C71 123.8(5) . . ? C70 C69 C71 118.0(4) . . ? C64 C70 C69 122.3(5) . . ? C64 C70 H70 118.9 . . ? C69 C70 H70 118.9 . . ? C76 C71 C72 118.2(5) . . ? C76 C71 C69 118.2(4) . . ? C72 C71 C69 123.6(5) . . ? C71 C72 C73 119.9(5) . . ? C71 C72 H72 120.1 . . ? C73 C72 H72 120.1 . . ? C74 C73 C72 121.6(5) . . ? C74 C73 H73 119.2 . . ? C72 C73 H73 119.2 . . ? C73 C74 C75 119.8(5) . . ? C73 C74 H74 120.1 . . ? C75 C74 H74 120.1 . . ? C76 C75 C74 117.5(5) . . ? C76 C75 C77 118.6(5) . . ? C74 C75 C77 123.8(5) . . ? C71 C76 C75 122.8(4) . . ? C71 C76 H76 118.6 . . ? C75 C76 H76 118.6 . . ? N7 C77 C78 122.8(6) . . ? N7 C77 C75 117.2(4) . . ? C78 C77 C75 119.9(5) . . ? C79 C78 C77 119.2(6) . . ? C79 C78 H78 120.4 . . ? C77 C78 H78 120.4 . . ? C78 C79 C80 119.0(6) . . ? C78 C79 H79 120.5 . . ? C80 C79 H79 120.5 . . ? C81 C80 C79 119.0(7) . . ? C81 C80 H80 120.5 . . ? C79 C80 H80 120.5 . . ? N7 C81 C80 122.2(6) . . ? N7 C81 C82 116.2(5) . . ? C80 C81 C82 121.5(6) . . ? N8 C82 C83 122.1(5) . . ? N8 C82 C81 116.5(5) . . ? C83 C82 C81 121.5(6) . . ? C82 C83 C84 119.6(6) . . ? C82 C83 H83 120.2 . . ? C84 C83 H83 120.2 . . ? C85 C84 C83 117.4(6) . . ? C85 C84 C90 119.9(7) . . ? C83 C84 C90 122.6(7) . . ? C86 C85 C84 119.7(6) . . ? C86 C85 C87 124.3(7) . . ? C84 C85 C87 116.0(6) . . ? N8 C86 C85 123.7(6) . . ? N8 C86 H86 118.1 . . ? C85 C86 H86 118.1 . . ? C85 C87 C91 109.4(6) . . ? C85 C87 C88 105.2(7) . . ? C91 C87 C88 86.4(7) . . ? C85 C87 H87 117.2 . . ? C91 C87 H87 117.2 . . ? C88 C87 H87 117.2 . . ? C89 C88 C87 87.4(7) . . ? C89 C88 H88A 114.1 . . ? C87 C88 H88A 114.1 . . ? C89 C88 H88B 114.1 . . ? C87 C88 H88B 114.1 . . ? H88A C88 H88B 111.3 . . ? C90 C89 C88 108.5(7) . . ? C90 C89 C91 111.3(7) . . ? C88 C89 C91 87.4(8) . . ? C90 C89 H89 115.5 . . ? C88 C89 H89 115.5 . . ? C91 C89 H89 115.5 . . ? C89 C90 C84 109.2(8) . . ? C89 C90 H90A 109.8 . . ? C84 C90 H90A 109.8 . . ? C89 C90 H90B 109.8 . . ? C84 C90 H90B 109.8 . . ? H90A C90 H90B 108.3 . . ? C92 C91 C93 108.5(8) . . ? C92 C91 C87 118.9(7) . . ? C93 C91 C87 110.7(8) . . ? C92 C91 C89 119.3(8) . . ? C93 C91 C89 111.4(8) . . ? C87 C91 C89 86.5(6) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? N1S C1S C2S 177(2) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C94 N9 Mn2 136.4(7) . . ? N9 C94 C95A 168.5(14) . . ? N9 C94 C95B 157.7(16) . . ? C95A C94 C95B 31.4(13) . . ? C94 C95A H95A 109.5 . . ? C94 C95A H95B 109.5 . . ? C94 C95A H95C 109.5 . . ? C94 C95B H95D 109.5 . . ? C94 C95B H95E 109.5 . . ? H95D C95B H95E 109.5 . . ? C94 C95B H95F 109.5 . . ? H95D C95B H95F 109.5 . . ? H95E C95B H95F 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 C3E O1E C2E C1E 177.0(13) . . . . ? C2E O1E C3E C4E 177.9(19) . . . . ? C96B O2B Mn2 N8 -91.5(19) . . . . ? C96B O2B Mn2 N4 94.8(19) . . . . ? C96B O2B Mn2 O2A 34(2) . . . . ? C96B O2B Mn2 N7 -16.5(19) . . . . ? C96B O2B Mn2 N9 178.3(19) . . . . ? C96B O2B Mn2 N3 149.7(17) . . . . ? C96A O2A Mn2 N8 47.7(13) . . . . ? C96A O2A Mn2 N4 -126.1(13) . . . . ? C96A O2A Mn2 O2B -7.5(15) . . . . ? C96A O2A Mn2 N7 120.7(13) . . . . ? C96A O2A Mn2 N9 -41.8(13) . . . . ? C96A O2A Mn2 N3 -108.0(13) . . . . ? O6 Cl1 O3 Mn1 61.8(6) . . . . ? O5 Cl1 O3 Mn1 -179.1(5) . . . . ? O4 Cl1 O3 Mn1 -58.2(6) . . . . ? O1 Mn1 O3 Cl1 -175.2(5) . . . . ? N5 Mn1 O3 Cl1 95.2(5) . . . . ? N1 Mn1 O3 Cl1 -87.1(5) . . . . ? N2 Mn1 O3 Cl1 -13.7(4) . . . . ? N6 Mn1 O3 Cl1 129.0(4) . . . . ? O1 Mn1 N1 C10 -26.0(5) . . . . ? N5 Mn1 N1 C10 24(3) . . . . ? N2 Mn1 N1 C10 169.6(5) . . . . ? O3 Mn1 N1 C10 -108.1(5) . . . . ? N6 Mn1 N1 C10 57.7(5) . . . . ? O1 Mn1 N1 C11 156.1(4) . . . . ? N5 Mn1 N1 C11 -153(3) . . . . ? N2 Mn1 N1 C11 -8.3(3) . . . . ? O3 Mn1 N1 C11 74.0(4) . . . . ? N6 Mn1 N1 C11 -120.1(3) . . . . ? O1 Mn1 N2 C13 -26.3(6) . . . . ? N5 Mn1 N2 C13 -164.9(3) . . . . ? N1 Mn1 N2 C13 17.1(3) . . . . ? O3 Mn1 N2 C13 -79.9(3) . . . . ? N6 Mn1 N2 C13 115.6(3) . . . . ? O1 Mn1 N2 C17 131.1(4) . . . . ? N5 Mn1 N2 C17 -7.5(4) . . . . ? N1 Mn1 N2 C17 174.4(4) . . . . ? O3 Mn1 N2 C17 77.5(4) . . . . ? N6 Mn1 N2 C17 -87.0(4) . . . . ? N8 Mn2 N3 C34 -154.4(4) . . . . ? N4 Mn2 N3 C34 19.5(4) . . . . ? O2B Mn2 N3 C34 -38.6(9) . . . . ? O2A Mn2 N3 C34 0.7(10) . . . . ? N7 Mn2 N3 C34 126.0(4) . . . . ? N9 Mn2 N3 C34 -66.9(4) . . . . ? N8 Mn2 N3 C30 2.4(4) . . . . ? N4 Mn2 N3 C30 176.3(4) . . . . ? O2B Mn2 N3 C30 118.2(9) . . . . ? O2A Mn2 N3 C30 157.5(9) . . . . ? N7 Mn2 N3 C30 -77.1(4) . . . . ? N9 Mn2 N3 C30 90.0(4) . . . . ? N8 Mn2 N4 C35 58.0(15) . . . . ? O2B Mn2 N4 C35 148.7(4) . . . . ? O2A Mn2 N4 C35 161.7(5) . . . . ? N7 Mn2 N4 C35 -123.8(3) . . . . ? N9 Mn2 N4 C35 71.4(4) . . . . ? N3 Mn2 N4 C35 -11.6(3) . . . . ? N8 Mn2 N4 C39 -120.1(14) . . . . ? O2B Mn2 N4 C39 -29.3(5) . . . . ? O2A Mn2 N4 C39 -16.4(5) . . . . ? N7 Mn2 N4 C39 58.2(4) . . . . ? N9 Mn2 N4 C39 -106.6(4) . . . . ? N3 Mn2 N4 C39 170.3(4) . . . . ? O1 Mn1 N5 C56 -107.7(4) . . . . ? N1 Mn1 N5 C56 -158(3) . . . . ? N2 Mn1 N5 C56 57.3(4) . . . . ? O3 Mn1 N5 C56 -25.4(4) . . . . ? N6 Mn1 N5 C56 168.1(4) . . . . ? O1 Mn1 N5 C57 76.3(4) . . . . ? N1 Mn1 N5 C57 26(3) . . . . ? N2 Mn1 N5 C57 -118.7(3) . . . . ? O3 Mn1 N5 C57 158.6(3) . . . . ? N6 Mn1 N5 C57 -7.9(3) . . . . ? O1 Mn1 N6 C59 -73.3(3) . . . . ? N5 Mn1 N6 C59 17.7(3) . . . . ? N1 Mn1 N6 C59 -160.5(3) . . . . ? N2 Mn1 N6 C59 120.8(3) . . . . ? O3 Mn1 N6 C59 -17.8(6) . . . . ? O1 Mn1 N6 C63 83.1(4) . . . . ? N5 Mn1 N6 C63 174.0(4) . . . . ? N1 Mn1 N6 C63 -4.2(4) . . . . ? N2 Mn1 N6 C63 -82.9(4) . . . . ? O3 Mn1 N6 C63 138.5(4) . . . . ? N8 Mn2 N7 C77 170.4(4) . . . . ? N4 Mn2 N7 C77 -9.4(4) . . . . ? O2B Mn2 N7 C77 82.4(5) . . . . ? O2A Mn2 N7 C77 70.9(5) . . . . ? N9 Mn2 N7 C77 125.4(6) . . . . ? N3 Mn2 N7 C77 -91.5(4) . . . . ? N8 Mn2 N7 C81 14.9(4) . . . . ? N4 Mn2 N7 C81 -164.9(4) . . . . ? O2B Mn2 N7 C81 -73.0(5) . . . . ? O2A Mn2 N7 C81 -84.6(5) . . . . ? N9 Mn2 N7 C81 -30.1(7) . . . . ? N3 Mn2 N7 C81 113.0(4) . . . . ? N4 Mn2 N8 C82 172.0(13) . . . . ? O2B Mn2 N8 C82 81.0(5) . . . . ? O2A Mn2 N8 C82 68.8(5) . . . . ? N7 Mn2 N8 C82 -6.3(4) . . . . ? N9 Mn2 N8 C82 158.7(4) . . . . ? N3 Mn2 N8 C82 -119.9(4) . . . . ? N4 Mn2 N8 C86 -8.3(16) . . . . ? O2B Mn2 N8 C86 -99.4(5) . . . . ? O2A Mn2 N8 C86 -111.5(5) . . . . ? N7 Mn2 N8 C86 173.4(4) . . . . ? N9 Mn2 N8 C86 -21.6(4) . . . . ? N3 Mn2 N8 C86 59.8(4) . . . . ? C2 C3 C4 C5 148.6(6) . . . . ? C1 C3 C4 C5 -83.6(7) . . . . ? C6 C3 C4 C5 27.2(5) . . . . ? C2 C3 C4 C9 38.1(8) . . . . ? C1 C3 C4 C9 165.9(7) . . . . ? C6 C3 C4 C9 -83.2(7) . . . . ? C9 C4 C5 C6 84.9(6) . . . . ? C3 C4 C5 C6 -27.2(5) . . . . ? C4 C5 C6 C7 -79.9(6) . . . . ? C4 C5 C6 C3 27.2(5) . . . . ? C2 C3 C6 C7 -40.2(8) . . . . ? C1 C3 C6 C7 -168.3(6) . . . . ? C4 C3 C6 C7 80.7(6) . . . . ? C2 C3 C6 C5 -147.5(6) . . . . ? C1 C3 C6 C5 84.4(7) . . . . ? C4 C3 C6 C5 -26.6(5) . . . . ? C5 C6 C7 C10 -136.4(7) . . . . ? C3 C6 C7 C10 131.2(7) . . . . ? C5 C6 C7 C8 44.4(8) . . . . ? C3 C6 C7 C8 -48.0(8) . . . . ? C10 C7 C8 C12 0.0(8) . . . . ? C6 C7 C8 C12 179.3(6) . . . . ? C10 C7 C8 C9 -178.8(6) . . . . ? C6 C7 C8 C9 0.5(8) . . . . ? C12 C8 C9 C4 -177.9(6) . . . . ? C7 C8 C9 C4 0.8(8) . . . . ? C5 C4 C9 C8 -49.4(7) . . . . ? C3 C4 C9 C8 46.5(8) . . . . ? C11 N1 C10 C7 0.3(9) . . . . ? Mn1 N1 C10 C7 -177.5(5) . . . . ? C8 C7 C10 N1 -0.3(9) . . . . ? C6 C7 C10 N1 -179.5(6) . . . . ? C10 N1 C11 C12 0.0(7) . . . . ? Mn1 N1 C11 C12 178.1(4) . . . . ? C10 N1 C11 C13 -179.1(5) . . . . ? Mn1 N1 C11 C13 -1.1(5) . . . . ? C7 C8 C12 C11 0.3(8) . . . . ? C9 C8 C12 C11 179.0(5) . . . . ? N1 C11 C12 C8 -0.3(8) . . . . ? C13 C11 C12 C8 178.8(5) . . . . ? C17 N2 C13 C14 -1.7(7) . . . . ? Mn1 N2 C13 C14 158.3(4) . . . . ? C17 N2 C13 C11 176.5(4) . . . . ? Mn1 N2 C13 C11 -23.5(5) . . . . ? N1 C11 C13 N2 17.5(6) . . . . ? C12 C11 C13 N2 -161.7(5) . . . . ? N1 C11 C13 C14 -164.3(5) . . . . ? C12 C11 C13 C14 16.5(7) . . . . ? N2 C13 C14 C15 -1.4(8) . . . . ? C11 C13 C14 C15 -179.5(5) . . . . ? C13 C14 C15 C16 1.9(8) . . . . ? C14 C15 C16 C17 0.7(8) . . . . ? C13 N2 C17 C16 4.4(7) . . . . ? Mn1 N2 C17 C16 -151.9(4) . . . . ? C13 N2 C17 C18 -169.7(4) . . . . ? Mn1 N2 C17 C18 33.9(6) . . . . ? C15 C16 C17 N2 -4.0(8) . . . . ? C15 C16 C17 C18 170.0(5) . . . . ? N2 C17 C18 C23 36.2(6) . . . . ? C16 C17 C18 C23 -138.1(5) . . . . ? N2 C17 C18 C19 -150.4(5) . . . . ? C16 C17 C18 C19 35.3(7) . . . . ? C23 C18 C19 C20 0.7(8) . . . . ? C17 C18 C19 C20 -172.7(5) . . . . ? C18 C19 C20 C21 -0.1(10) . . . . ? C19 C20 C21 C22 -0.4(10) . . . . ? C20 C21 C22 C23 0.2(8) . . . . ? C20 C21 C22 C24 175.9(6) . . . . ? C19 C18 C23 C22 -0.9(7) . . . . ? C17 C18 C23 C22 172.8(4) . . . . ? C21 C22 C23 C18 0.4(7) . . . . ? C24 C22 C23 C18 -175.4(5) . . . . ? C21 C22 C24 C29 -148.8(5) . . . . ? C23 C22 C24 C29 26.7(7) . . . . ? C21 C22 C24 C25 33.1(8) . . . . ? C23 C22 C24 C25 -151.3(5) . . . . ? C29 C24 C25 C26 -0.3(7) . . . . ? C22 C24 C25 C26 177.8(5) . . . . ? C24 C25 C26 C65 -1.9(9) . . . . ? C65 C28 C29 C24 -0.2(7) . . . . ? C30 C28 C29 C24 175.3(4) . . . . ? C25 C24 C29 C28 1.4(7) . . . . ? C22 C24 C29 C28 -176.8(5) . . . . ? C34 N3 C30 C31 3.5(7) . . . . ? Mn2 N3 C30 C31 -151.8(4) . . . . ? C34 N3 C30 C28 -172.3(5) . . . . ? Mn2 N3 C30 C28 32.5(6) . . . . ? C29 C28 C30 N3 36.9(7) . . . . ? C65 C28 C30 N3 -147.8(5) . . . . ? C29 C28 C30 C31 -138.9(5) . . . . ? C65 C28 C30 C31 36.4(7) . . . . ? N3 C30 C31 C32 -0.3(9) . . . . ? C28 C30 C31 C32 175.3(6) . . . . ? C30 C31 C32 C33 -1.7(11) . . . . ? C31 C32 C33 C34 0.5(11) . . . . ? C30 N3 C34 C33 -4.8(8) . . . . ? Mn2 N3 C34 C33 155.0(5) . . . . ? C30 N3 C34 C35 175.0(4) . . . . ? Mn2 N3 C34 C35 -25.1(6) . . . . ? C32 C33 C34 N3 2.9(10) . . . . ? C32 C33 C34 C35 -177.0(6) . . . . ? C39 N4 C35 C36 1.4(8) . . . . ? Mn2 N4 C35 C36 -176.8(4) . . . . ? C39 N4 C35 C34 -179.1(4) . . . . ? Mn2 N4 C35 C34 2.7(6) . . . . ? N3 C34 C35 N4 16.7(7) . . . . ? C33 C34 C35 N4 -163.4(6) . . . . ? N3 C34 C35 C36 -163.7(5) . . . . ? C33 C34 C35 C36 16.1(9) . . . . ? N4 C35 C36 C37 -1.0(9) . . . . ? C34 C35 C36 C37 179.5(5) . . . . ? C35 C36 C37 C38 0.3(9) . . . . ? C35 C36 C37 C40 177.7(7) . . . . ? C36 C37 C38 C39 -0.1(8) . . . . ? C40 C37 C38 C39 -177.5(7) . . . . ? C36 C37 C38 C43 -179.3(5) . . . . ? C40 C37 C38 C43 3.3(9) . . . . ? C35 N4 C39 C38 -1.1(7) . . . . ? Mn2 N4 C39 C38 176.9(4) . . . . ? C37 C38 C39 N4 0.5(8) . . . . ? C43 C38 C39 N4 179.6(5) . . . . ? C38 C37 C40 C41 -3.1(10) . . . . ? C36 C37 C40 C41 179.6(6) . . . . ? C37 C40 C41 C42 -45.2(9) . . . . ? C37 C40 C41 C44 48.7(9) . . . . ? C40 C41 C42 C43 83.5(6) . . . . ? C44 C41 C42 C43 -27.3(5) . . . . ? C39 C38 C43 C42 -134.9(6) . . . . ? C37 C38 C43 C42 44.3(7) . . . . ? C39 C38 C43 C44 133.3(6) . . . . ? C37 C38 C43 C44 -47.5(7) . . . . ? C41 C42 C43 C38 -81.4(6) . . . . ? C41 C42 C43 C44 27.0(6) . . . . ? C40 C41 C44 C45 39.3(9) . . . . ? C42 C41 C44 C45 147.6(7) . . . . ? C40 C41 C44 C46 166.8(6) . . . . ? C42 C41 C44 C46 -84.9(6) . . . . ? C40 C41 C44 C43 -81.4(7) . . . . ? C42 C41 C44 C43 26.9(5) . . . . ? C38 C43 C44 C45 -41.5(8) . . . . ? C42 C43 C44 C45 -147.4(7) . . . . ? C38 C43 C44 C46 -169.5(5) . . . . ? C42 C43 C44 C46 84.6(7) . . . . ? C38 C43 C44 C41 79.1(6) . . . . ? C42 C43 C44 C41 -26.9(6) . . . . ? C47 C48 C50 C55 -40.8(8) . . . . ? C49 C48 C50 C55 -168.9(6) . . . . ? C52 C48 C50 C55 77.5(6) . . . . ? C47 C48 C50 C51 -147.7(7) . . . . ? C49 C48 C50 C51 84.3(6) . . . . ? C52 C48 C50 C51 -29.4(5) . . . . ? C55 C50 C51 C52 -82.0(5) . . . . ? C48 C50 C51 C52 29.3(5) . . . . ? C47 C48 C52 C53 39.3(8) . . . . ? C49 C48 C52 C53 167.8(6) . . . . ? C50 C48 C52 C53 -79.6(6) . . . . ? C47 C48 C52 C51 148.1(6) . . . . ? C49 C48 C52 C51 -83.3(7) . . . . ? C50 C48 C52 C51 29.3(5) . . . . ? C50 C51 C52 C53 85.0(5) . . . . ? C50 C51 C52 C48 -29.1(5) . . . . ? C48 C52 C53 C54 47.1(7) . . . . ? C51 C52 C53 C54 -47.3(7) . . . . ? C52 C53 C54 C55 -1.6(8) . . . . ? C52 C53 C54 C58 178.7(5) . . . . ? C58 C54 C55 C56 -1.5(7) . . . . ? C53 C54 C55 C56 178.8(5) . . . . ? C58 C54 C55 C50 -178.0(5) . . . . ? C53 C54 C55 C50 2.3(7) . . . . ? C48 C50 C55 C56 136.3(6) . . . . ? C51 C50 C55 C56 -130.6(6) . . . . ? C48 C50 C55 C54 -47.6(7) . . . . ? C51 C50 C55 C54 45.5(7) . . . . ? C57 N5 C56 C55 -0.5(7) . . . . ? Mn1 N5 C56 C55 -176.4(4) . . . . ? C54 C55 C56 N5 1.6(8) . . . . ? C50 C55 C56 N5 177.7(5) . . . . ? C56 N5 C57 C58 -0.7(7) . . . . ? Mn1 N5 C57 C58 175.5(4) . . . . ? C56 N5 C57 C59 -178.7(4) . . . . ? Mn1 N5 C57 C59 -2.4(5) . . . . ? N5 C57 C58 C54 0.6(8) . . . . ? C59 C57 C58 C54 178.5(5) . . . . ? C55 C54 C58 C57 0.5(8) . . . . ? C53 C54 C58 C57 -179.8(5) . . . . ? C63 N6 C59 C60 -2.5(7) . . . . ? Mn1 N6 C59 C60 156.4(4) . . . . ? C63 N6 C59 C57 175.9(4) . . . . ? Mn1 N6 C59 C57 -25.3(5) . . . . ? N5 C57 C59 N6 20.0(6) . . . . ? C58 C57 C59 N6 -158.0(5) . . . . ? N5 C57 C59 C60 -161.6(5) . . . . ? C58 C57 C59 C60 20.5(7) . . . . ? N6 C59 C60 C61 -1.2(8) . . . . ? C57 C59 C60 C61 -179.6(5) . . . . ? C59 C60 C61 C62 2.9(9) . . . . ? C60 C61 C62 C63 -0.9(9) . . . . ? C61 C62 C63 N6 -3.1(8) . . . . ? C61 C62 C63 C64 171.7(5) . . . . ? C59 N6 C63 C62 4.7(7) . . . . ? Mn1 N6 C63 C62 -150.1(4) . . . . ? C59 N6 C63 C64 -170.2(4) . . . . ? Mn1 N6 C63 C64 35.0(6) . . . . ? C62 C63 C64 C70 -140.1(5) . . . . ? N6 C63 C64 C70 34.8(6) . . . . ? C62 C63 C64 C66 33.9(7) . . . . ? N6 C63 C64 C66 -151.2(5) . . . . ? C25 C26 C65 C28 3.1(9) . . . . ? C29 C28 C65 C26 -2.0(8) . . . . ? C30 C28 C65 C26 -177.3(5) . . . . ? C70 C64 C66 C67 -0.2(8) . . . . ? C63 C64 C66 C67 -174.2(5) . . . . ? C64 C66 C67 C68 0.5(9) . . . . ? C66 C67 C68 C69 -0.4(9) . . . . ? C67 C68 C69 C70 -0.1(8) . . . . ? C67 C68 C69 C71 177.2(5) . . . . ? C66 C64 C70 C69 -0.3(8) . . . . ? C63 C64 C70 C69 173.9(4) . . . . ? C68 C69 C70 C64 0.5(7) . . . . ? C71 C69 C70 C64 -177.0(4) . . . . ? C68 C69 C71 C76 -147.6(5) . . . . ? C70 C69 C71 C76 29.7(6) . . . . ? C68 C69 C71 C72 32.4(7) . . . . ? C70 C69 C71 C72 -150.3(5) . . . . ? C76 C71 C72 C73 -2.8(7) . . . . ? C69 C71 C72 C73 177.1(5) . . . . ? C71 C72 C73 C74 1.4(9) . . . . ? C72 C73 C74 C75 0.5(9) . . . . ? C73 C74 C75 C76 -0.8(8) . . . . ? C73 C74 C75 C77 -176.9(5) . . . . ? C72 C71 C76 C75 2.6(7) . . . . ? C69 C71 C76 C75 -177.4(4) . . . . ? C74 C75 C76 C71 -0.8(7) . . . . ? C77 C75 C76 C71 175.6(4) . . . . ? C81 N7 C77 C78 2.5(9) . . . . ? Mn2 N7 C77 C78 -151.7(6) . . . . ? C81 N7 C77 C75 -172.8(5) . . . . ? Mn2 N7 C77 C75 33.0(6) . . . . ? C76 C75 C77 N7 36.4(7) . . . . ? C74 C75 C77 N7 -147.5(5) . . . . ? C76 C75 C77 C78 -139.1(7) . . . . ? C74 C75 C77 C78 37.0(9) . . . . ? N7 C77 C78 C79 0.5(12) . . . . ? C75 C77 C78 C79 175.6(8) . . . . ? C77 C78 C79 C80 -4.7(15) . . . . ? C78 C79 C80 C81 5.9(16) . . . . ? C77 N7 C81 C80 -1.2(10) . . . . ? Mn2 N7 C81 C80 156.6(7) . . . . ? C77 N7 C81 C82 -179.2(5) . . . . ? Mn2 N7 C81 C82 -21.3(6) . . . . ? C79 C80 C81 N7 -3.0(13) . . . . ? C79 C80 C81 C82 174.9(8) . . . . ? C86 N8 C82 C83 -2.8(8) . . . . ? Mn2 N8 C82 C83 176.9(4) . . . . ? C86 N8 C82 C81 177.5(5) . . . . ? Mn2 N8 C82 C81 -2.8(6) . . . . ? N7 C81 C82 N8 17.0(8) . . . . ? C80 C81 C82 N8 -161.0(7) . . . . ? N7 C81 C82 C83 -162.7(6) . . . . ? C80 C81 C82 C83 19.3(10) . . . . ? N8 C82 C83 C84 1.2(9) . . . . ? C81 C82 C83 C84 -179.2(6) . . . . ? C82 C83 C84 C85 1.7(9) . . . . ? C82 C83 C84 C90 179.4(6) . . . . ? C83 C84 C85 C86 -2.8(9) . . . . ? C90 C84 C85 C86 179.4(6) . . . . ? C83 C84 C85 C87 176.8(6) . . . . ? C90 C84 C85 C87 -1.0(9) . . . . ? C82 N8 C86 C85 1.6(8) . . . . ? Mn2 N8 C86 C85 -178.0(4) . . . . ? C84 C85 C86 N8 1.2(9) . . . . ? C87 C85 C86 N8 -178.4(6) . . . . ? C86 C85 C87 C91 134.6(7) . . . . ? C84 C85 C87 C91 -45.0(9) . . . . ? C86 C85 C87 C88 -133.9(8) . . . . ? C84 C85 C87 C88 46.6(8) . . . . ? C85 C87 C88 C89 -82.9(7) . . . . ? C91 C87 C88 C89 26.2(6) . . . . ? C87 C88 C89 C90 85.5(8) . . . . ? C87 C88 C89 C91 -26.1(6) . . . . ? C88 C89 C90 C84 -47.1(9) . . . . ? C91 C89 C90 C84 47.4(9) . . . . ? C85 C84 C90 C89 0.2(9) . . . . ? C83 C84 C90 C89 -177.5(7) . . . . ? C85 C87 C91 C92 -42.7(11) . . . . ? C88 C87 C91 C92 -147.5(9) . . . . ? C85 C87 C91 C93 -169.3(8) . . . . ? C88 C87 C91 C93 85.9(9) . . . . ? C85 C87 C91 C89 79.1(8) . . . . ? C88 C87 C91 C89 -25.7(7) . . . . ? C90 C89 C91 C92 38.8(9) . . . . ? C88 C89 C91 C92 147.6(7) . . . . ? C90 C89 C91 C93 166.5(8) . . . . ? C88 C89 C91 C93 -84.7(8) . . . . ? C90 C89 C91 C87 -82.6(7) . . . . ? C88 C89 C91 C87 26.2(6) . . . . ? N8 Mn2 N9 C94 -149.6(9) . . . . ? N4 Mn2 N9 C94 31.8(9) . . . . ? O2B Mn2 N9 C94 -62.5(10) . . . . ? O2A Mn2 N9 C94 -54.0(10) . . . . ? N7 Mn2 N9 C94 -106.6(10) . . . . ? N3 Mn2 N9 C94 106.5(10) . . . . ? Mn2 N9 C94 C95A 8(7) . . . . ? Mn2 N9 C94 C95B -127(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.087 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.132 # start Validation Reply Form _vrf_PLAT432_0331a ; PROBLEM: Short Inter X...Y Contact C4E .. C96A .. 2.35 Ang. RESPONSE: These coordinated and non-coordinated solvent molecules are not fully occupied. ; _vrf_PLAT601_0331a ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 416.00 A**3 RESPONSE: Some of the cocrystallized solvents are easily lost even the x-ray analysis was done at low temp and they are too weak to be located using the difference map. ; _vrf_PLAT770_0331a ; PROBLEM: Suspect C-H Bond in CIF: C96A -- H2OB .. 1.31 Ang. RESPONSE: These coordinated solvent molecules are not fully occupied. ; _vrf_PLAT222_0331a ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.59 Ratio RESPONSE: It is due to the relatively large temperature factors of terminal methyl groups. ; _vrf_PLAT230_0331a ; PROBLEM: Hirshfeld Test Diff for N9 -- C94 .. 9.33 su RESPONSE: The coordinated acetonitrile molecule was disordered and has been fixed by split model. ; # end Validation Reply Form # Attachment '- 091609a.cif' data_091609a _database_code_depnum_ccdc_archive 'CCDC 775971' #TrackingRef '- 091609a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H103.50 Cl4 Mn2 N8 O21.75' _chemical_formula_weight 2065.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 18.81287(15) _cell_length_b 22.75489(19) _cell_length_c 23.7655(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10173.64(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15520 _cell_measurement_theta_min 3.5689 _cell_measurement_theta_max 71.3667 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4302 _exptl_absorpt_coefficient_mu 3.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.34874 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31704 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 66.99 _reflns_number_total 16631 _reflns_number_gt 12495 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep-3 _computing_publication_material wingx _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^)+(0.1213P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(5) _chemical_absolute_configuration rmad _refine_ls_number_reflns 16631 _refine_ls_number_parameters 1265 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1799 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.35850(4) -0.15933(3) 0.61858(3) 0.04096(18) Uani 1 1 d . . . Mn2 Mn 0.07584(4) 0.16518(3) 0.62220(3) 0.04133(19) Uani 1 1 d . . . O1 O 0.3750(2) -0.23193(18) 0.6791(2) 0.0698(12) Uani 1 1 d . . . H1OA H 0.3735 -0.2658 0.6640 0.084 Uiso 1 1 d R . . H1OB H 0.3475 -0.2302 0.7073 0.084 Uiso 1 1 d R . . O2 O 0.4501(2) -0.20106(18) 0.57297(17) 0.0605(10) Uani 1 1 d . . . H2OA H 0.4416 -0.2043 0.5380 0.073 Uiso 1 1 d R . . H2OB H 0.4599 -0.2347 0.5864 0.073 Uiso 1 1 d R . . O3 O -0.0101(2) 0.20373(17) 0.56904(17) 0.0576(10) Uani 1 1 d . . . H3OA H 0.0022 0.2021 0.5347 0.069 Uiso 1 1 d R . . H3OB H -0.0159 0.2396 0.5778 0.069 Uiso 1 1 d R . . O4 O 0.0544(2) 0.23618(16) 0.68387(18) 0.0641(11) Uani 1 1 d . . . H4OA H 0.0430 0.2685 0.6684 0.077 Uiso 1 1 d R . . H4OB H 0.0884 0.2414 0.7069 0.077 Uiso 1 1 d R . . Cl1 Cl 0.46517(9) 0.81274(7) 0.41031(8) 0.0713(4) Uani 1 1 d . . . O5 O 0.3945(3) 0.8229(4) 0.3990(3) 0.150(3) Uani 1 1 d . . . O6 O 0.4999(8) 0.8668(4) 0.4210(6) 0.242(6) Uani 1 1 d . . . O7 O 0.5008(4) 0.7897(3) 0.3643(3) 0.129(3) Uani 1 1 d . . . O8 O 0.4732(4) 0.7728(3) 0.4561(3) 0.116(2) Uani 1 1 d . . . Cl2 Cl -0.00174(8) 0.21104(6) 0.40965(7) 0.0614(4) Uani 1 1 d D . . O17 O -0.0105(4) 0.1598(3) 0.4399(4) 0.145(3) Uani 1 1 d . A . O18 O -0.0573(2) 0.2204(2) 0.3703(2) 0.0809(14) Uani 1 1 d . A . O19A O -0.0164(6) 0.2489(5) 0.4577(4) 0.082(3) Uiso 0.50 1 d PD A 1 O20A O 0.0658(6) 0.2225(5) 0.3878(5) 0.089(3) Uiso 0.50 1 d PD A 1 O19B O 0.0116(6) 0.2653(5) 0.4413(5) 0.086(3) Uiso 0.50 1 d PD A 2 O20B O 0.0604(6) 0.1934(6) 0.3778(6) 0.099(4) Uiso 0.50 1 d PD A 2 Cl3A Cl 0.95319(18) 0.35463(13) 0.61798(14) 0.0688(8) Uiso 0.60 1 d PD B 1 O9A O 0.9210(6) 0.4081(4) 0.6178(6) 0.110(4) Uiso 0.60 1 d PD B 1 O10A O 0.9986(7) 0.3568(6) 0.5657(5) 0.144(5) Uiso 0.60 1 d PD B 1 O11A O 1.0145(7) 0.3581(7) 0.6573(6) 0.162(6) Uiso 0.60 1 d PD B 1 O12A O 0.9183(6) 0.3044(4) 0.6184(5) 0.128(4) Uiso 0.60 1 d PD B 1 Cl3B Cl 0.9783(2) 0.36475(17) 0.61567(18) 0.0563(9) Uiso 0.40 1 d PD C 2 O9B O 0.9023(6) 0.3951(5) 0.6233(6) 0.065(3) Uiso 0.40 1 d PD C 2 O10B O 0.9671(10) 0.3269(7) 0.5721(6) 0.135(6) Uiso 0.40 1 d PD C 2 O11B O 0.9821(6) 0.3411(5) 0.6710(4) 0.067(3) Uiso 0.40 1 d PD C 2 O12B O 1.0258(9) 0.4075(8) 0.6090(9) 0.173(9) Uiso 0.40 1 d PD C 2 Cl4A Cl 0.5062(3) 0.6576(2) 0.6560(2) 0.0795(13) Uiso 0.40 1 d PD D 1 O13A O 0.4554(11) 0.6503(10) 0.6072(8) 0.180(9) Uiso 0.40 1 d PD D 1 O14A O 0.4602(10) 0.6479(9) 0.7015(7) 0.155(7) Uiso 0.40 1 d PD D 1 O15A O 0.5543(8) 0.6123(7) 0.6548(8) 0.133(6) Uiso 0.40 1 d PD D 1 O16A O 0.5337(12) 0.7119(7) 0.6505(11) 0.198(11) Uiso 0.40 1 d PD D 1 Cl4B Cl 0.4864(2) 0.64383(15) 0.64050(16) 0.0792(9) Uiso 0.60 1 d PD E 2 O13B O 0.5058(8) 0.5928(5) 0.6144(6) 0.149(5) Uiso 0.60 1 d PD E 2 O14B O 0.4221(6) 0.6527(5) 0.6600(6) 0.133(4) Uiso 0.60 1 d PD E 2 O15B O 0.5117(6) 0.6964(4) 0.6119(5) 0.115(3) Uiso 0.60 1 d PD E 2 O16B O 0.5347(10) 0.6498(10) 0.6926(7) 0.271(11) Uiso 0.60 1 d PD E 2 N1 N 0.4413(2) -0.10624(18) 0.65955(19) 0.0451(10) Uani 1 1 d . . . N2 N 0.3783(2) -0.07701(17) 0.55846(18) 0.0411(9) Uani 1 1 d . . . N3 N 0.1810(2) 0.15673(17) 0.67388(17) 0.0398(9) Uani 1 1 d . . . N4 N 0.1554(2) 0.22163(19) 0.57982(19) 0.0477(10) Uani 1 1 d . . . N5 N -0.0097(2) 0.11407(17) 0.66339(18) 0.0424(9) Uani 1 1 d . . . N6 N 0.0540(2) 0.08334(17) 0.56419(17) 0.0401(9) Uani 1 1 d . . . N7 N 0.2498(2) -0.15599(16) 0.66647(17) 0.0397(9) Uani 1 1 d . . . N8 N 0.2838(2) -0.21251(19) 0.56848(19) 0.0472(10) Uani 1 1 d . F . C1 C 0.6670(4) -0.1117(4) 0.7558(4) 0.092(2) Uani 1 1 d . . . H1A H 0.6510 -0.1016 0.7187 0.138 Uiso 1 1 calc R . . H1B H 0.6610 -0.1532 0.7618 0.138 Uiso 1 1 calc R . . H1C H 0.7164 -0.1018 0.7596 0.138 Uiso 1 1 calc R . . C2 C 0.6242(3) -0.0782(3) 0.7988(3) 0.0670(17) Uani 1 1 d . . . C3 C 0.6534(5) -0.0937(4) 0.8575(4) 0.102(3) Uani 1 1 d . . . H3A H 0.6417 -0.1338 0.8663 0.154 Uiso 1 1 calc R . . H3B H 0.6325 -0.0681 0.8850 0.154 Uiso 1 1 calc R . . H3C H 0.7041 -0.0889 0.8577 0.154 Uiso 1 1 calc R . . C4 C 0.5410(3) -0.0835(3) 0.7965(3) 0.0687(17) Uani 1 1 d . . . H4 H 0.5189 -0.1142 0.8196 0.082 Uiso 1 1 calc R . . C5 C 0.5392(4) -0.0206(4) 0.8196(4) 0.095(3) Uani 1 1 d . . . H5A H 0.5020 0.0037 0.8036 0.113 Uiso 1 1 calc R . . H5B H 0.5397 -0.0182 0.8603 0.113 Uiso 1 1 calc R . . C6 C 0.6119(4) -0.0121(3) 0.7923(3) 0.077(2) Uani 1 1 d . . . H6 H 0.6449 0.0128 0.8135 0.093 Uiso 1 1 calc R . . C7 C 0.6010(4) 0.0057(3) 0.7321(3) 0.077(2) Uani 1 1 d . . . H7A H 0.6456 0.0027 0.7118 0.092 Uiso 1 1 calc R . . H7B H 0.5853 0.0463 0.7305 0.092 Uiso 1 1 calc R . . C8 C 0.4662(3) -0.1132(2) 0.7120(2) 0.0498(12) Uani 1 1 d . . . H8 H 0.4475 -0.1438 0.7334 0.060 Uiso 1 1 calc R . . C9 C 0.5170(3) -0.0786(2) 0.7365(2) 0.0516(13) Uani 1 1 d . . . C10 C 0.5455(3) -0.0339(2) 0.7046(3) 0.0524(13) Uani 1 1 d . . . C11 C 0.5233(3) -0.0273(2) 0.6499(3) 0.0577(15) Uani 1 1 d . . . H11 H 0.5444 0.0011 0.6272 0.069 Uiso 1 1 calc R . . C12 C 0.4699(3) -0.0625(2) 0.6283(2) 0.0458(12) Uani 1 1 d . . . C13 C 0.4416(3) -0.0525(2) 0.5711(2) 0.0447(11) Uani 1 1 d . . . C14 C 0.4775(4) -0.0189(3) 0.5329(3) 0.0687(17) Uani 1 1 d . . . H14 H 0.5227 -0.0051 0.5417 0.082 Uiso 1 1 calc R . . C15 C 0.4479(4) -0.0050(3) 0.4819(3) 0.081(2) Uani 1 1 d . . . H15 H 0.4719 0.0187 0.4562 0.097 Uiso 1 1 calc R . . C16 C 0.3813(4) -0.0273(3) 0.4696(3) 0.0651(16) Uani 1 1 d . . . H16 H 0.3592 -0.0182 0.4357 0.078 Uiso 1 1 calc R . . C17 C 0.3477(3) -0.0633(2) 0.5083(2) 0.0462(12) Uani 1 1 d . . . C18 C 0.2749(3) -0.0840(2) 0.4965(2) 0.0469(12) Uani 1 1 d . . . C19 C 0.2541(3) -0.1000(3) 0.4419(3) 0.0621(15) Uani 1 1 d . . . H19A H 0.2874 -0.1001 0.4130 0.074 Uiso 1 1 calc R . . C20 C 0.1854(4) -0.1155(3) 0.4308(3) 0.073(2) Uani 1 1 d . . . H20A H 0.1723 -0.1263 0.3945 0.088 Uiso 1 1 calc R . . C21 C 0.1355(3) -0.1151(3) 0.4732(3) 0.0621(15) Uani 1 1 d . . . H21 H 0.0889 -0.1256 0.4650 0.075 Uiso 1 1 calc R . . C22 C 0.1534(3) -0.0994(2) 0.5280(2) 0.0484(12) Uani 1 1 d . . . C23 C 0.2237(3) -0.0841(2) 0.5381(2) 0.0450(12) Uani 1 1 d . . . H23 H 0.2369 -0.0735 0.5744 0.054 Uiso 1 1 calc R . . C24 C 0.1004(2) -0.0973(2) 0.5745(2) 0.0449(12) Uani 1 1 d . . . C25 C 0.0411(3) -0.1330(3) 0.5761(3) 0.0597(15) Uani 1 1 d . . . H25 H 0.0319 -0.1593 0.5470 0.072 Uiso 1 1 calc R . . C26 C -0.0044(3) -0.1290(2) 0.6215(3) 0.0667(16) Uani 1 1 d . . . H26 H -0.0443 -0.1532 0.6226 0.080 Uiso 1 1 calc R . . C27 C 0.0072(3) -0.0905(2) 0.6649(3) 0.0574(14) Uani 1 1 d . . . H27 H -0.0243 -0.0894 0.6950 0.069 Uiso 1 1 calc R . . C28 C 0.0655(3) -0.0532(2) 0.6646(2) 0.0469(12) Uani 1 1 d . . . C29 C 0.1116(2) -0.0582(2) 0.6183(2) 0.0439(11) Uani 1 1 d . . . H29 H 0.1515 -0.0341 0.6170 0.053 Uiso 1 1 calc R . . C30 C 0.0820(3) -0.0099(2) 0.7092(2) 0.0454(12) Uani 1 1 d . . . C31 C 0.0593(3) -0.0173(3) 0.7650(3) 0.0593(15) Uani 1 1 d . . . H31 H 0.0328 -0.0503 0.7745 0.071 Uiso 1 1 calc R . . C32 C 0.0752(4) 0.0233(3) 0.8058(2) 0.0648(16) Uani 1 1 d . . . H32 H 0.0577 0.0182 0.8420 0.078 Uiso 1 1 calc R . . C33 C 0.1173(3) 0.0720(3) 0.7934(2) 0.0567(14) Uani 1 1 d . . . H33 H 0.1296 0.0987 0.8214 0.068 Uiso 1 1 calc R . . C34 C 0.1406(3) 0.0801(2) 0.7383(2) 0.0429(11) Uani 1 1 d . . . C35 C 0.1225(3) 0.0392(2) 0.6974(2) 0.0410(11) Uani 1 1 d . . . H35 H 0.1382 0.0451 0.6607 0.049 Uiso 1 1 calc R . . C36 C 0.1893(3) 0.1295(2) 0.7244(2) 0.0416(11) Uani 1 1 d . . . C37 C 0.2442(3) 0.1431(2) 0.7603(2) 0.0522(13) Uani 1 1 d . . . H37 H 0.2478 0.1248 0.7951 0.063 Uiso 1 1 calc R . . C38 C 0.2948(3) 0.1849(3) 0.7436(3) 0.0643(16) Uani 1 1 d . . . H38 H 0.3333 0.1936 0.7667 0.077 Uiso 1 1 calc R . . C39 C 0.2870(3) 0.2121(2) 0.6940(3) 0.0540(13) Uani 1 1 d . . . H39 H 0.3196 0.2405 0.6827 0.065 Uiso 1 1 calc R . . C40 C 0.2293(2) 0.1974(2) 0.6591(2) 0.0435(11) Uani 1 1 d . . . C41 C 0.2188(2) 0.2276(2) 0.6043(2) 0.0415(11) Uani 1 1 d . . . C42 C 0.2724(3) 0.2605(2) 0.5789(3) 0.0539(13) Uani 1 1 d . . . H42 H 0.3169 0.2631 0.5959 0.065 Uiso 1 1 calc R . . C43 C 0.2601(3) 0.2894(2) 0.5287(2) 0.0526(13) Uani 1 1 d . . . C44 C 0.1931(3) 0.2843(3) 0.5040(3) 0.0579(15) Uani 1 1 d . . . C45 C 0.1441(3) 0.2499(3) 0.5312(2) 0.0597(15) Uani 1 1 d . . . H45 H 0.0996 0.2459 0.5146 0.072 Uiso 1 1 calc R . . C46 C 0.3137(4) 0.3273(4) 0.5000(4) 0.096(3) Uani 1 1 d . . . H46A H 0.3558 0.3042 0.4916 0.115 Uiso 1 1 calc R . . H46B H 0.3276 0.3591 0.5249 0.115 Uiso 1 1 calc R . . C47 C 0.2833(4) 0.3528(4) 0.4455(3) 0.092(3) Uani 1 1 d . . . H47 H 0.3163 0.3770 0.4236 0.110 Uiso 1 1 calc R . . C48 C 0.2481(5) 0.3030(4) 0.4130(3) 0.102(3) Uani 1 1 d . . . H48A H 0.2691 0.2646 0.4193 0.122 Uiso 1 1 calc R . . H48B H 0.2413 0.3108 0.3732 0.122 Uiso 1 1 calc R . . C49 C 0.1819(4) 0.3166(4) 0.4505(3) 0.081(2) Uani 1 1 d . . . H49 H 0.1354 0.3117 0.4326 0.097 Uiso 1 1 calc R . . C50 C 0.2096(5) 0.3797(3) 0.4551(3) 0.083(2) Uani 1 1 d . . . C51 C 0.1864(6) 0.4183(5) 0.4055(5) 0.132(4) Uani 1 1 d . . . H51A H 0.2242 0.4205 0.3785 0.199 Uiso 1 1 calc R . . H51B H 0.1752 0.4570 0.4188 0.199 Uiso 1 1 calc R . . H51C H 0.1451 0.4014 0.3881 0.199 Uiso 1 1 calc R . . C52 C 0.1948(8) 0.4137(4) 0.5101(5) 0.147(5) Uani 1 1 d . . . H52A H 0.2141 0.4526 0.5073 0.221 Uiso 1 1 calc R . . H52B H 0.2166 0.3935 0.5411 0.221 Uiso 1 1 calc R . . H52C H 0.1444 0.4161 0.5162 0.221 Uiso 1 1 calc R . . C53 C -0.2288(4) 0.1158(4) 0.8564(4) 0.105(3) Uani 1 1 d . . . H53A H -0.2253 0.1577 0.8604 0.157 Uiso 1 1 calc R . . H53B H -0.2018 0.0971 0.8856 0.157 Uiso 1 1 calc R . . H53C H -0.2777 0.1041 0.8592 0.157 Uiso 1 1 calc R . . C54 C -0.2373(4) 0.1289(4) 0.7524(4) 0.086(2) Uani 1 1 d . . . H54A H -0.2179 0.1170 0.7168 0.129 Uiso 1 1 calc R . . H54B H -0.2313 0.1705 0.7569 0.129 Uiso 1 1 calc R . . H54C H -0.2870 0.1194 0.7536 0.129 Uiso 1 1 calc R . . C55 C -0.1994(4) 0.0974(3) 0.7988(3) 0.0709(19) Uani 1 1 d . . . C56 C -0.1162(3) 0.0990(3) 0.7986(3) 0.0634(16) Uani 1 1 d . . . H56 H -0.0937 0.1298 0.8212 0.076 Uiso 1 1 calc R . . C57 C -0.1187(4) 0.0365(4) 0.8250(3) 0.084(2) Uani 1 1 d . . . H57A H -0.0824 0.0098 0.8112 0.101 Uiso 1 1 calc R . . H57B H -0.1212 0.0361 0.8658 0.101 Uiso 1 1 calc R . . C58 C -0.1896(4) 0.0307(3) 0.7959(3) 0.0722(19) Uani 1 1 d . . . H58 H -0.2252 0.0080 0.8167 0.087 Uiso 1 1 calc R . . C59 C -0.1761(4) 0.0094(3) 0.7356(3) 0.0716(19) Uani 1 1 d . . . H59A H -0.1617 -0.0315 0.7362 0.086 Uiso 1 1 calc R . . H59B H -0.2196 0.0124 0.7139 0.086 Uiso 1 1 calc R . . C60 C -0.0360(3) 0.1236(2) 0.7151(2) 0.0481(12) Uani 1 1 d . . . H60 H -0.0169 0.1546 0.7357 0.058 Uiso 1 1 calc R . . C61 C -0.0887(3) 0.0912(2) 0.7398(2) 0.0511(13) Uani 1 1 d . . . C62 C -0.1191(3) 0.0458(2) 0.7085(3) 0.0542(14) Uani 1 1 d . . . C63 C -0.0940(3) 0.0360(2) 0.6550(2) 0.0494(13) Uani 1 1 d . . . H63 H -0.1141 0.0065 0.6331 0.059 Uiso 1 1 calc R . . C64 C -0.0393(2) 0.0697(2) 0.6334(2) 0.0395(10) Uani 1 1 d . . . C65 C -0.0088(3) 0.0580(2) 0.5763(2) 0.0431(11) Uani 1 1 d . . . C66 C -0.0433(3) 0.0215(3) 0.5384(3) 0.0578(14) Uani 1 1 d . . . H66 H -0.0875 0.0057 0.5473 0.069 Uiso 1 1 calc R . . C67 C -0.0122(3) 0.0089(3) 0.4883(3) 0.0638(16) Uani 1 1 d . . . H67 H -0.0343 -0.0163 0.4629 0.077 Uiso 1 1 calc R . . C68 C 0.0527(3) 0.0338(3) 0.4753(2) 0.0568(14) Uani 1 1 d . . . H68 H 0.0745 0.0256 0.4411 0.068 Uiso 1 1 calc R . . C69 C 0.0848(3) 0.0706(2) 0.5132(2) 0.0438(11) Uani 1 1 d . . . C70 C 0.1567(3) 0.0934(2) 0.5026(2) 0.0432(11) Uani 1 1 d . . . C71 C 0.1767(3) 0.1145(3) 0.4496(2) 0.0555(14) Uani 1 1 d . . . H71 H 0.1437 0.1165 0.4206 0.067 Uiso 1 1 calc R . . C72 C 0.2465(4) 0.1326(3) 0.4410(3) 0.0666(16) Uani 1 1 d . . . H72 H 0.2594 0.1481 0.4062 0.080 Uiso 1 1 calc R . . C73 C 0.2964(3) 0.1280(3) 0.4825(3) 0.0584(14) Uani 1 1 d . . . H73 H 0.3431 0.1392 0.4754 0.070 Uiso 1 1 calc R . . C74 C 0.2776(3) 0.1063(2) 0.5362(2) 0.0480(12) Uani 1 1 d . . . C75 C 0.2077(3) 0.0900(2) 0.5444(2) 0.0438(11) Uani 1 1 d . . . H75 H 0.1943 0.0761 0.5797 0.053 Uiso 1 1 calc R . . C76 C 0.3309(3) 0.1004(2) 0.5822(2) 0.0490(12) Uani 1 1 d . . . C77 C 0.3923(3) 0.1337(3) 0.5863(3) 0.0633(16) Uani 1 1 d . . . H77 H 0.4037 0.1602 0.5579 0.076 Uiso 1 1 calc R . . C78 C 0.4369(3) 0.1278(3) 0.6321(3) 0.0708(18) Uani 1 1 d . . . H78 H 0.4782 0.1502 0.6339 0.085 Uiso 1 1 calc R . . C79 C 0.4215(3) 0.0896(2) 0.6748(3) 0.0641(16) Uani 1 1 d . . . H79 H 0.4512 0.0874 0.7060 0.077 Uiso 1 1 calc R . . C80 C 0.3610(3) 0.0536(2) 0.6717(2) 0.0468(12) Uani 1 1 d . . . C81 C 0.3175(3) 0.0597(2) 0.6248(2) 0.0451(11) Uani 1 1 d . . . H81 H 0.2777 0.0357 0.6217 0.054 Uiso 1 1 calc R . . C82 C 0.3419(3) 0.0096(2) 0.7147(2) 0.0490(13) Uani 1 1 d . . . C83 C 0.3570(4) 0.0162(3) 0.7712(3) 0.0645(16) Uani 1 1 d . . . H83 H 0.3819 0.0493 0.7832 0.077 Uiso 1 1 calc R . . C84 C 0.3364(4) -0.0243(3) 0.8095(3) 0.079(2) Uani 1 1 d . . . H84 H 0.3479 -0.0190 0.8472 0.094 Uiso 1 1 calc R . . C85 C 0.2978(4) -0.0744(3) 0.7931(3) 0.0694(18) Uani 1 1 d . . . H85 H 0.2837 -0.1019 0.8198 0.083 Uiso 1 1 calc R . . C86 C 0.2809(3) -0.0824(2) 0.7372(2) 0.0462(12) Uani 1 1 d . . . C87 C 0.3042(3) -0.0404(2) 0.6985(2) 0.0431(11) Uani 1 1 d . . . H87 H 0.2942 -0.0460 0.6605 0.052 Uiso 1 1 calc R . . C88 C 0.2372(3) -0.1319(2) 0.7177(2) 0.0434(11) Uani 1 1 d . . . C89 C 0.1800(3) -0.1503(2) 0.7508(2) 0.0552(14) Uani 1 1 d . . . H89 H 0.1724 -0.1338 0.7861 0.066 Uiso 1 1 calc R . . C90 C 0.1350(3) -0.1929(3) 0.7305(3) 0.0660(16) Uani 1 1 d . . . H90 H 0.0967 -0.2055 0.7520 0.079 Uiso 1 1 calc R . . C91 C 0.1469(3) -0.2168(2) 0.6780(3) 0.0575(14) Uani 1 1 d . . . H91 H 0.1166 -0.2454 0.6636 0.069 Uiso 1 1 calc R . . C92 C 0.2051(3) -0.1975(2) 0.6467(2) 0.0439(11) Uani 1 1 d . . . C93 C 0.2191(2) -0.22228(19) 0.5908(2) 0.0420(11) Uani 1 1 d . . . C94 C 0.1698(3) -0.2555(3) 0.5609(3) 0.0605(16) Uani 1 1 d . F . H94 H 0.1247 -0.2618 0.5758 0.073 Uiso 1 1 calc R . . C95 C 0.1871(3) -0.2791(3) 0.5096(3) 0.0582(15) Uani 1 1 d . . . C96 C 0.2537(3) -0.2691(3) 0.4872(2) 0.0551(14) Uani 1 1 d . F . C97 C 0.2996(3) -0.2351(3) 0.5179(2) 0.0563(14) Uani 1 1 d . . . H97 H 0.3441 -0.2271 0.5028 0.068 Uiso 1 1 calc R F . C98A C 0.1315(17) -0.3083(13) 0.4713(14) 0.087(9) Uani 0.55 1 d PU F 1 H98A H 0.0988 -0.2790 0.4568 0.105 Uiso 0.55 1 calc PR F 1 H98B H 0.1046 -0.3373 0.4923 0.105 Uiso 0.55 1 calc PR F 1 C98B C 0.1412(15) -0.3279(14) 0.482(2) 0.087(11) Uani 0.45 1 d PU F 2 H98C H 0.0919 -0.3155 0.4797 0.104 Uiso 0.45 1 calc PR F 2 H98D H 0.1435 -0.3637 0.5042 0.104 Uiso 0.45 1 calc PR F 2 C99 C 0.1725(4) -0.3387(4) 0.4215(4) 0.095(3) Uani 1 1 d . . . H99 H 0.1430 -0.3630 0.3968 0.115 Uiso 1 1 calc R F 1 C100 C 0.2064(5) -0.2845(4) 0.3930(3) 0.103(3) Uani 1 1 d . F . H10A H 0.2162 -0.2894 0.3532 0.124 Uiso 1 1 calc R . . H10B H 0.1821 -0.2477 0.4004 0.124 Uiso 1 1 calc R . . C101 C 0.2705(4) -0.2964(3) 0.4316(3) 0.0696(17) Uani 1 1 d . . . H101 H 0.3175 -0.2875 0.4158 0.084 Uiso 1 1 calc R F . C102 C 0.2482(4) -0.3620(3) 0.4317(3) 0.078(2) Uani 1 1 d . F . C103 C 0.2768(5) -0.3938(4) 0.3809(4) 0.104(3) Uani 1 1 d . . . H10C H 0.3273 -0.3985 0.3846 0.155 Uiso 1 1 calc R F . H10D H 0.2665 -0.3715 0.3476 0.155 Uiso 1 1 calc R . . H10E H 0.2547 -0.4318 0.3781 0.155 Uiso 1 1 calc R . . C104 C 0.2639(7) -0.3966(4) 0.4831(4) 0.121(4) Uani 1 1 d . . . H10F H 0.2363 -0.4321 0.4829 0.182 Uiso 1 1 calc R F . H10G H 0.2520 -0.3738 0.5158 0.182 Uiso 1 1 calc R . . H10H H 0.3136 -0.4063 0.4840 0.182 Uiso 1 1 calc R . . O1W O 0.1202(5) 0.2569(4) 0.7841(3) 0.158(3) Uani 1 1 d . . . H1WA H 0.1570 0.2353 0.7856 0.189 Uiso 1 1 d R . . H1WB H 0.0925 0.2462 0.8104 0.189 Uiso 1 1 d R . . O2W O 0.4050(14) 0.7369(11) 0.7822(11) 0.109(7) Uiso 0.25 1 d P G 1 O2WA O 0.3409(9) 0.7698(7) 0.7934(7) 0.137(5) Uiso 0.50 1 d P H 2 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 0.0402(4) 0.0409(4) 0.0417(4) -0.0004(4) 0.0002(3) -0.0059(3) Mn2 0.0411(4) 0.0423(4) 0.0405(4) 0.0042(4) -0.0013(4) -0.0072(3) O1 0.079(3) 0.057(2) 0.073(3) 0.018(2) 0.009(2) 0.010(2) O2 0.059(2) 0.070(2) 0.053(2) 0.003(2) 0.0028(19) 0.0096(19) O3 0.060(2) 0.054(2) 0.059(2) 0.0095(18) -0.0047(19) 0.0022(18) O4 0.078(3) 0.046(2) 0.068(3) -0.0048(19) -0.009(2) 0.0060(19) Cl1 0.0668(8) 0.0736(9) 0.0736(10) 0.0074(8) 0.0148(8) 0.0224(7) O5 0.078(4) 0.202(8) 0.169(7) 0.108(6) 0.041(4) 0.057(4) O6 0.323(15) 0.120(7) 0.283(14) -0.063(8) -0.040(13) -0.039(9) O7 0.133(5) 0.148(6) 0.105(5) 0.020(4) 0.064(4) 0.049(5) O8 0.121(5) 0.141(5) 0.087(4) 0.037(4) 0.015(4) 0.039(4) Cl2 0.0556(7) 0.0616(8) 0.0671(9) 0.0062(7) -0.0087(7) 0.0071(6) O17 0.141(6) 0.112(5) 0.183(7) 0.083(5) -0.041(5) -0.010(4) O18 0.067(3) 0.090(3) 0.085(3) 0.001(3) -0.031(3) 0.011(2) N1 0.041(2) 0.047(2) 0.048(3) 0.0036(19) 0.0004(19) -0.0071(17) N2 0.039(2) 0.043(2) 0.042(2) 0.0049(18) 0.0003(18) 0.0011(16) N3 0.045(2) 0.0372(19) 0.037(2) 0.0000(18) -0.0053(18) -0.0006(17) N4 0.042(2) 0.052(2) 0.049(3) 0.010(2) -0.008(2) -0.0099(18) N5 0.042(2) 0.043(2) 0.042(2) -0.0026(18) -0.0004(19) -0.0038(17) N6 0.043(2) 0.0383(19) 0.039(2) -0.0036(17) -0.0044(18) 0.0028(16) N7 0.0407(19) 0.0358(19) 0.043(2) 0.0027(18) 0.0001(18) 0.0016(16) N8 0.049(2) 0.043(2) 0.049(3) -0.005(2) 0.003(2) -0.0081(18) C1 0.073(4) 0.096(6) 0.108(7) 0.001(5) -0.026(5) 0.004(4) C2 0.064(4) 0.079(4) 0.058(4) 0.015(3) -0.026(3) -0.017(3) C3 0.091(5) 0.124(7) 0.093(6) 0.027(5) -0.044(5) -0.029(5) C4 0.064(4) 0.096(5) 0.046(3) 0.001(3) -0.002(3) -0.025(3) C5 0.074(4) 0.133(7) 0.077(5) -0.034(5) -0.014(4) -0.004(5) C6 0.074(4) 0.077(4) 0.081(5) -0.012(4) -0.034(4) -0.015(3) C7 0.074(4) 0.069(4) 0.086(5) 0.017(4) -0.038(4) -0.024(3) C8 0.050(3) 0.059(3) 0.041(3) 0.014(2) -0.004(2) -0.014(2) C9 0.042(3) 0.058(3) 0.055(3) 0.002(3) -0.006(2) -0.007(2) C10 0.046(3) 0.053(3) 0.057(3) 0.006(3) -0.008(3) -0.008(2) C11 0.055(3) 0.049(3) 0.069(4) 0.016(3) -0.016(3) -0.016(2) C12 0.046(2) 0.039(2) 0.053(3) 0.008(2) -0.001(2) -0.007(2) C13 0.046(3) 0.049(3) 0.039(3) 0.009(2) 0.002(2) -0.003(2) C14 0.070(4) 0.083(4) 0.053(4) 0.017(3) -0.005(3) -0.025(3) C15 0.086(5) 0.088(5) 0.069(5) 0.029(4) 0.001(4) -0.025(4) C16 0.079(4) 0.074(4) 0.042(3) 0.017(3) 0.000(3) 0.002(3) C17 0.051(3) 0.050(3) 0.038(3) -0.001(2) 0.000(2) 0.008(2) C18 0.052(3) 0.050(3) 0.039(3) 0.002(2) -0.002(2) 0.008(2) C19 0.062(3) 0.079(4) 0.045(3) -0.011(3) -0.009(3) 0.013(3) C20 0.075(4) 0.108(5) 0.038(3) -0.028(3) -0.016(3) 0.018(4) C21 0.056(3) 0.072(4) 0.058(4) -0.018(3) -0.017(3) 0.000(3) C22 0.052(3) 0.041(3) 0.052(3) -0.008(2) -0.003(2) 0.004(2) C23 0.053(3) 0.039(2) 0.043(3) -0.002(2) -0.008(2) 0.006(2) C24 0.039(2) 0.040(2) 0.056(3) -0.001(2) -0.007(2) 0.0010(19) C25 0.053(3) 0.057(3) 0.069(4) -0.014(3) -0.002(3) -0.004(3) C26 0.057(3) 0.051(3) 0.091(5) -0.007(3) -0.001(4) -0.013(3) C27 0.049(3) 0.050(3) 0.073(4) 0.001(3) 0.007(3) -0.005(2) C28 0.050(3) 0.039(2) 0.051(3) 0.010(2) 0.002(3) 0.003(2) C29 0.042(2) 0.038(2) 0.052(3) -0.001(2) 0.003(3) 0.0026(19) C30 0.050(3) 0.041(2) 0.045(3) 0.006(2) 0.005(2) 0.008(2) C31 0.064(3) 0.058(3) 0.056(4) 0.024(3) 0.011(3) 0.000(3) C32 0.084(4) 0.073(4) 0.037(3) 0.005(3) 0.012(3) -0.014(3) C33 0.069(4) 0.055(3) 0.046(3) 0.002(3) 0.003(3) 0.004(3) C34 0.049(3) 0.044(2) 0.035(3) 0.006(2) -0.001(2) 0.005(2) C35 0.047(3) 0.041(2) 0.035(3) 0.006(2) 0.007(2) 0.002(2) C36 0.050(3) 0.040(2) 0.034(3) -0.005(2) -0.004(2) 0.007(2) C37 0.064(3) 0.054(3) 0.038(3) 0.002(2) -0.012(3) -0.001(3) C38 0.064(3) 0.064(3) 0.065(4) -0.002(3) -0.023(3) -0.016(3) C39 0.056(3) 0.049(3) 0.057(3) 0.001(3) -0.018(3) -0.009(2) C40 0.038(2) 0.039(2) 0.053(3) -0.004(2) -0.007(2) -0.0044(19) C41 0.040(2) 0.040(2) 0.045(3) 0.003(2) -0.007(2) -0.0042(19) C42 0.045(3) 0.055(3) 0.062(4) 0.005(3) -0.006(3) -0.007(2) C43 0.053(3) 0.054(3) 0.050(3) 0.011(3) 0.001(3) -0.016(2) C44 0.061(3) 0.061(3) 0.052(3) 0.014(3) -0.009(3) -0.017(3) C45 0.055(3) 0.079(4) 0.046(3) 0.021(3) -0.016(3) -0.021(3) C46 0.068(4) 0.125(7) 0.094(6) 0.054(5) -0.012(4) -0.037(4) C47 0.091(5) 0.108(6) 0.076(5) 0.040(5) -0.006(4) -0.048(5) C48 0.132(7) 0.124(7) 0.049(4) 0.013(4) 0.015(5) -0.025(6) C49 0.077(4) 0.106(5) 0.059(4) 0.038(4) -0.015(4) -0.034(4) C50 0.104(6) 0.072(4) 0.073(5) 0.032(4) -0.005(4) -0.007(4) C51 0.133(8) 0.140(9) 0.124(9) 0.085(8) 0.002(7) 0.011(7) C52 0.231(14) 0.079(6) 0.131(10) 0.037(6) 0.013(10) 0.013(8) C53 0.090(5) 0.135(7) 0.090(6) -0.049(6) 0.042(5) -0.040(5) C54 0.061(4) 0.095(5) 0.101(6) -0.007(5) 0.012(4) 0.006(4) C55 0.064(4) 0.082(4) 0.067(4) -0.026(4) 0.023(3) -0.018(3) C56 0.060(3) 0.085(4) 0.045(3) -0.006(3) 0.002(3) -0.026(3) C57 0.082(5) 0.110(6) 0.060(4) 0.024(4) 0.010(4) -0.021(4) C58 0.065(4) 0.082(4) 0.070(4) 0.000(4) 0.022(3) -0.024(3) C59 0.073(4) 0.067(4) 0.075(4) -0.015(3) 0.030(4) -0.026(3) C60 0.053(3) 0.050(3) 0.041(3) -0.004(2) -0.001(2) -0.007(2) C61 0.050(3) 0.056(3) 0.048(3) -0.002(3) 0.000(2) -0.008(2) C62 0.051(3) 0.050(3) 0.061(4) -0.007(3) 0.007(3) -0.007(2) C63 0.053(3) 0.042(3) 0.053(3) -0.011(2) 0.011(3) -0.011(2) C64 0.035(2) 0.040(2) 0.044(3) -0.006(2) 0.000(2) -0.0003(18) C65 0.051(3) 0.039(2) 0.040(3) 0.001(2) -0.001(2) 0.002(2) C66 0.054(3) 0.066(3) 0.053(3) -0.006(3) -0.001(3) -0.012(3) C67 0.065(4) 0.074(4) 0.052(4) -0.015(3) -0.008(3) -0.007(3) C68 0.068(4) 0.067(3) 0.035(3) -0.003(3) 0.002(3) 0.003(3) C69 0.051(3) 0.041(2) 0.039(3) 0.003(2) 0.001(2) 0.005(2) C70 0.045(3) 0.045(3) 0.040(3) 0.004(2) 0.001(2) 0.009(2) C71 0.070(3) 0.059(3) 0.037(3) 0.006(3) 0.001(3) 0.003(3) C72 0.072(4) 0.081(4) 0.047(3) 0.019(3) 0.012(3) -0.004(3) C73 0.061(3) 0.063(3) 0.051(3) 0.009(3) 0.010(3) -0.009(3) C74 0.055(3) 0.040(3) 0.049(3) 0.005(2) -0.001(3) 0.007(2) C75 0.045(3) 0.047(3) 0.039(3) 0.005(2) 0.003(2) 0.004(2) C76 0.052(3) 0.040(3) 0.055(3) -0.001(2) 0.002(3) 0.001(2) C77 0.053(3) 0.053(3) 0.083(5) 0.014(3) -0.001(3) -0.010(3) C78 0.052(3) 0.061(3) 0.099(5) 0.007(4) -0.016(4) -0.014(3) C79 0.066(4) 0.050(3) 0.077(4) -0.006(3) -0.019(3) -0.005(3) C80 0.049(3) 0.037(2) 0.055(3) -0.006(2) -0.008(3) 0.002(2) C81 0.051(3) 0.037(2) 0.047(3) 0.003(2) -0.006(3) -0.0041(19) C82 0.050(3) 0.038(2) 0.059(4) -0.007(2) -0.014(3) 0.002(2) C83 0.090(4) 0.052(3) 0.051(4) -0.004(3) -0.022(3) -0.004(3) C84 0.121(6) 0.078(4) 0.037(3) -0.004(3) -0.026(4) -0.010(4) C85 0.105(5) 0.054(3) 0.049(3) -0.001(3) -0.009(4) -0.013(3) C86 0.058(3) 0.046(3) 0.035(3) 0.001(2) -0.007(2) 0.002(2) C87 0.048(3) 0.042(2) 0.040(3) -0.001(2) -0.007(2) 0.003(2) C88 0.051(3) 0.042(2) 0.038(3) 0.005(2) -0.004(2) 0.005(2) C89 0.065(3) 0.055(3) 0.045(3) -0.002(3) 0.009(3) -0.006(3) C90 0.067(4) 0.069(4) 0.063(4) 0.000(3) 0.024(3) -0.010(3) C91 0.051(3) 0.049(3) 0.073(4) -0.007(3) 0.009(3) -0.012(2) C92 0.044(2) 0.036(2) 0.052(3) 0.002(2) 0.002(2) 0.001(2) C93 0.042(2) 0.033(2) 0.050(3) -0.005(2) 0.001(2) -0.0011(19) C94 0.038(3) 0.070(4) 0.074(4) -0.021(3) 0.003(3) -0.004(2) C95 0.048(3) 0.055(3) 0.072(4) -0.019(3) -0.009(3) -0.002(2) C96 0.065(3) 0.056(3) 0.044(3) -0.007(3) -0.006(3) -0.007(3) C97 0.060(3) 0.061(3) 0.047(3) -0.009(3) 0.008(3) -0.018(3) C98A 0.087(17) 0.097(19) 0.079(12) -0.042(13) -0.003(10) -0.016(12) C98B 0.031(7) 0.079(17) 0.15(3) -0.057(17) -0.005(11) -0.013(11) C99 0.079(5) 0.113(6) 0.094(6) -0.058(5) -0.006(4) -0.019(5) C100 0.140(8) 0.115(7) 0.054(4) -0.018(4) -0.024(5) 0.017(6) C101 0.074(4) 0.082(4) 0.054(4) -0.017(3) 0.005(3) -0.019(3) C102 0.094(5) 0.072(4) 0.067(4) -0.033(4) 0.011(4) -0.026(4) C103 0.102(6) 0.100(6) 0.108(7) -0.058(5) 0.011(5) -0.004(5) C104 0.199(11) 0.073(5) 0.092(7) -0.011(5) 0.002(7) 0.024(6) O1W 0.191(8) 0.186(8) 0.097(5) -0.030(5) -0.036(5) 0.057(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 N1 2.199(4) . ? Mn1 N8 2.203(4) . ? Mn1 O1 2.212(4) . ? Mn1 O2 2.247(4) . ? Mn1 N7 2.342(4) . ? Mn1 N2 2.385(4) . ? Mn2 N4 2.214(4) . ? Mn2 N5 2.214(4) . ? Mn2 O4 2.218(4) . ? Mn2 O3 2.232(4) . ? Mn2 N3 2.336(4) . ? Mn2 N6 2.353(4) . ? O1 H1OA 0.8502 . ? O1 H1OB 0.8494 . ? O2 H2OA 0.8499 . ? O2 H2OB 0.8498 . ? O3 H3OA 0.8497 . ? O3 H3OB 0.8502 . ? O4 H4OA 0.8501 . ? O4 H4OB 0.8498 . ? Cl1 O5 1.376(6) . ? Cl1 O7 1.385(6) . ? Cl1 O6 1.416(10) . ? Cl1 O8 1.425(6) . ? Cl2 O17 1.380(6) . ? Cl2 O20A 1.397(10) . ? Cl2 O18 1.419(4) . ? Cl2 O20B 1.450(11) . ? Cl2 O19A 1.456(10) . ? Cl2 O19B 1.467(10) . ? Cl3A O12A 1.318(9) . ? Cl3A O9A 1.359(9) . ? Cl3A O11A 1.486(11) . ? Cl3A O10A 1.508(10) . ? Cl3B O12B 1.330(12) . ? Cl3B O10B 1.364(12) . ? Cl3B O11B 1.422(10) . ? Cl3B O9B 1.598(10) . ? Cl4A O16A 1.345(13) . ? Cl4A O15A 1.373(12) . ? Cl4A O14A 1.404(13) . ? Cl4A O13A 1.511(13) . ? Cl4B O14B 1.311(10) . ? Cl4B O13B 1.367(10) . ? Cl4B O15B 1.456(9) . ? Cl4B O16B 1.541(12) . ? N1 C8 1.342(7) . ? N1 C12 1.354(6) . ? N2 C13 1.350(6) . ? N2 C17 1.359(7) . ? N3 C40 1.345(6) . ? N3 C36 1.360(6) . ? N4 C41 1.335(6) . ? N4 C45 1.339(7) . ? N5 C60 1.341(7) . ? N5 C64 1.356(6) . ? N6 C65 1.345(6) . ? N6 C69 1.374(6) . ? N7 C92 1.349(6) . ? N7 C88 1.357(6) . ? N8 C97 1.339(7) . ? N8 C93 1.347(6) . ? C1 C2 1.507(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C6 1.531(10) . ? C2 C3 1.540(10) . ? C2 C4 1.572(9) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C9 1.502(8) . ? C4 C5 1.533(11) . ? C4 H4 0.9800 . ? C5 C6 1.526(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.501(10) . ? C6 H6 0.9800 . ? C7 C10 1.527(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.368(7) . ? C8 H8 0.9300 . ? C9 C10 1.378(8) . ? C10 C11 1.373(8) . ? C11 C12 1.385(7) . ? C11 H11 0.9300 . ? C12 C13 1.477(7) . ? C13 C14 1.365(8) . ? C14 C15 1.372(9) . ? C14 H14 0.9300 . ? C15 C16 1.383(10) . ? C15 H15 0.9300 . ? C16 C17 1.385(8) . ? C16 H16 0.9300 . ? C17 C18 1.476(8) . ? C18 C23 1.380(8) . ? C18 C19 1.404(8) . ? C19 C20 1.364(9) . ? C19 H19A 0.9300 . ? C20 C21 1.377(9) . ? C20 H20A 0.9300 . ? C21 C22 1.392(8) . ? C21 H21 0.9300 . ? C22 C23 1.388(7) . ? C22 C24 1.490(8) . ? C23 H23 0.9300 . ? C24 C25 1.381(7) . ? C24 C29 1.384(7) . ? C25 C26 1.380(9) . ? C25 H25 0.9300 . ? C26 C27 1.372(9) . ? C26 H26 0.9300 . ? C27 C28 1.386(7) . ? C27 H27 0.9300 . ? C28 C29 1.405(7) . ? C28 C30 1.480(8) . ? C29 H29 0.9300 . ? C30 C35 1.382(7) . ? C30 C31 1.404(8) . ? C31 C32 1.371(9) . ? C31 H31 0.9300 . ? C32 C33 1.394(8) . ? C32 H32 0.9300 . ? C33 C34 1.393(8) . ? C33 H33 0.9300 . ? C34 C35 1.388(7) . ? C34 C36 1.488(7) . ? C35 H35 0.9300 . ? C36 C37 1.374(7) . ? C37 C38 1.402(8) . ? C37 H37 0.9300 . ? C38 C39 1.340(9) . ? C38 H38 0.9300 . ? C39 C40 1.406(7) . ? C39 H39 0.9300 . ? C40 C41 1.484(7) . ? C41 C42 1.395(7) . ? C42 C43 1.382(8) . ? C42 H42 0.9300 . ? C43 C44 1.394(8) . ? C43 C46 1.492(8) . ? C44 C45 1.371(8) . ? C44 C49 1.484(9) . ? C45 H45 0.9300 . ? C46 C47 1.531(10) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.521(11) . ? C47 C50 1.534(12) . ? C47 H47 0.9800 . ? C48 C49 1.562(12) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.531(11) . ? C49 H49 0.9800 . ? C50 C51 1.533(11) . ? C50 C52 1.544(14) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C55 1.533(9) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.496(11) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C58 1.531(10) . ? C55 C56 1.566(9) . ? C56 C61 1.500(8) . ? C56 C57 1.556(10) . ? C56 H56 0.9800 . ? C57 C58 1.509(10) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.534(10) . ? C58 H58 0.9800 . ? C59 C62 1.502(8) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.368(7) . ? C60 H60 0.9300 . ? C61 C62 1.396(8) . ? C62 C63 1.374(8) . ? C63 C64 1.382(7) . ? C63 H63 0.9300 . ? C64 C65 1.495(7) . ? C65 C66 1.387(7) . ? C66 C67 1.358(8) . ? C66 H66 0.9300 . ? C67 C68 1.380(9) . ? C67 H67 0.9300 . ? C68 C69 1.370(8) . ? C68 H68 0.9300 . ? C69 C70 1.471(7) . ? C70 C75 1.384(7) . ? C70 C71 1.399(8) . ? C71 C72 1.391(9) . ? C71 H71 0.9300 . ? C72 C73 1.366(9) . ? C72 H72 0.9300 . ? C73 C74 1.413(8) . ? C73 H73 0.9300 . ? C74 C75 1.380(7) . ? C74 C76 1.490(8) . ? C75 H75 0.9300 . ? C76 C77 1.385(7) . ? C76 C81 1.395(7) . ? C77 C78 1.380(9) . ? C77 H77 0.9300 . ? C78 C79 1.368(9) . ? C78 H78 0.9300 . ? C79 C80 1.402(8) . ? C79 H79 0.9300 . ? C80 C81 1.391(7) . ? C80 C82 1.475(8) . ? C81 H81 0.9300 . ? C82 C83 1.382(8) . ? C82 C87 1.395(7) . ? C83 C84 1.353(9) . ? C83 H83 0.9300 . ? C84 C85 1.406(9) . ? C84 H84 0.9300 . ? C85 C86 1.377(8) . ? C85 H85 0.9300 . ? C86 C87 1.397(7) . ? C86 C88 1.471(7) . ? C87 H87 0.9300 . ? C88 C89 1.396(7) . ? C89 C90 1.374(8) . ? C89 H89 0.9300 . ? C90 C91 1.380(9) . ? C90 H90 0.9300 . ? C91 C92 1.394(7) . ? C91 H91 0.9300 . ? C92 C93 1.466(7) . ? C93 C94 1.393(7) . ? C94 C95 1.371(9) . ? C94 H94 0.9300 . ? C95 C96 1.381(8) . ? C95 C98A 1.54(3) . ? C95 C98B 1.55(3) . ? C96 C97 1.371(8) . ? C96 C101 1.494(9) . ? C97 H97 0.9300 . ? C98A C99 1.57(3) . ? C98A H98A 0.9700 . ? C98A H98B 0.9700 . ? C98B C99 1.58(4) . ? C98B H98C 0.9700 . ? C98B H98D 0.9700 . ? C99 C102 1.539(11) . ? C99 C100 1.546(13) . ? C99 H99 0.9800 . ? C100 C101 1.538(11) . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C101 C102 1.552(9) . ? C101 H101 0.9800 . ? C102 C104 1.485(12) . ? C102 C103 1.506(10) . ? C103 H10C 0.9600 . ? C103 H10D 0.9600 . ? C103 H10E 0.9600 . ? C104 H10F 0.9600 . ? C104 H10G 0.9600 . ? C104 H10H 0.9600 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? 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 N1 Mn1 N8 173.07(17) . . ? N1 Mn1 O1 91.33(17) . . ? N8 Mn1 O1 91.75(17) . . ? N1 Mn1 O2 84.39(16) . . ? N8 Mn1 O2 89.78(16) . . ? O1 Mn1 O2 83.68(16) . . ? N1 Mn1 N7 112.69(15) . . ? N8 Mn1 N7 73.97(15) . . ? O1 Mn1 N7 80.28(15) . . ? O2 Mn1 N7 156.67(15) . . ? N1 Mn1 N2 73.94(15) . . ? N8 Mn1 N2 101.94(15) . . ? O1 Mn1 N2 162.56(15) . . ? O2 Mn1 N2 85.60(14) . . ? N7 Mn1 N2 113.69(13) . . ? N4 Mn2 N5 175.63(16) . . ? N4 Mn2 O4 90.07(17) . . ? N5 Mn2 O4 87.60(16) . . ? N4 Mn2 O3 90.23(15) . . ? N5 Mn2 O3 85.98(15) . . ? O4 Mn2 O3 87.47(16) . . ? N4 Mn2 N3 73.43(15) . . ? N5 Mn2 N3 109.88(15) . . ? O4 Mn2 N3 82.35(15) . . ? O3 Mn2 N3 160.64(14) . . ? N4 Mn2 N6 108.10(16) . . ? N5 Mn2 N6 73.51(15) . . ? O4 Mn2 N6 158.67(16) . . ? O3 Mn2 N6 81.52(14) . . ? N3 Mn2 N6 113.01(14) . . ? Mn1 O1 H1OA 113.5 . . ? Mn1 O1 H1OB 113.2 . . ? H1OA O1 H1OB 110.8 . . ? Mn1 O2 H2OA 111.3 . . ? Mn1 O2 H2OB 111.5 . . ? H2OA O2 H2OB 109.4 . . ? Mn2 O3 H3OA 109.3 . . ? Mn2 O3 H3OB 109.4 . . ? H3OA O3 H3OB 108.1 . . ? Mn2 O4 H4OA 112.9 . . ? Mn2 O4 H4OB 112.9 . . ? H4OA O4 H4OB 110.4 . . ? O5 Cl1 O7 112.1(5) . . ? O5 Cl1 O6 109.6(7) . . ? O7 Cl1 O6 104.3(7) . . ? O5 Cl1 O8 111.0(4) . . ? O7 Cl1 O8 108.0(4) . . ? O6 Cl1 O8 111.6(6) . . ? O17 Cl2 O20A 117.4(6) . . ? O17 Cl2 O18 112.5(4) . . ? O20A Cl2 O18 113.3(5) . . ? O17 Cl2 O20B 97.7(7) . . ? O20A Cl2 O20B 28.8(6) . . ? O18 Cl2 O20B 106.9(6) . . ? O17 Cl2 O19A 94.0(6) . . ? O20A Cl2 O19A 110.7(7) . . ? O18 Cl2 O19A 106.8(5) . . ? O20B Cl2 O19A 136.5(7) . . ? O17 Cl2 O19B 117.7(6) . . ? O20A Cl2 O19B 83.1(7) . . ? O18 Cl2 O19B 109.7(5) . . ? O20B Cl2 O19B 111.3(7) . . ? O19A Cl2 O19B 29.9(5) . . ? O12A Cl3A O9A 123.7(7) . . ? O12A Cl3A O11A 115.3(8) . . ? O9A Cl3A O11A 107.5(8) . . ? O12A Cl3A O10A 108.4(7) . . ? O9A Cl3A O10A 102.7(7) . . ? O11A Cl3A O10A 94.4(7) . . ? O12B Cl3B O10B 118.3(11) . . ? O12B Cl3B O11B 110.6(10) . . ? O10B Cl3B O11B 118.1(9) . . ? O12B Cl3B O9B 107.5(9) . . ? O10B Cl3B O9B 102.7(8) . . ? O11B Cl3B O9B 96.0(7) . . ? O16A Cl4A O15A 115.8(11) . . ? O16A Cl4A O14A 117.1(12) . . ? O15A Cl4A O14A 107.7(10) . . ? O16A Cl4A O13A 105.6(11) . . ? O15A Cl4A O13A 108.6(11) . . ? O14A Cl4A O13A 100.5(10) . . ? O14B Cl4B O13B 122.5(8) . . ? O14B Cl4B O15B 109.9(7) . . ? O13B Cl4B O15B 113.5(7) . . ? O14B Cl4B O16B 104.2(9) . . ? O13B Cl4B O16B 106.4(9) . . ? O15B Cl4B O16B 96.3(9) . . ? C8 N1 C12 117.3(4) . . ? C8 N1 Mn1 126.4(3) . . ? C12 N1 Mn1 116.2(3) . . ? C13 N2 C17 118.3(4) . . ? C13 N2 Mn1 109.2(3) . . ? C17 N2 Mn1 129.7(3) . . ? C40 N3 C36 117.8(4) . . ? C40 N3 Mn2 112.2(3) . . ? C36 N3 Mn2 126.8(3) . . ? C41 N4 C45 118.0(4) . . ? C41 N4 Mn2 117.7(3) . . ? C45 N4 Mn2 124.3(3) . . ? C60 N5 C64 116.8(4) . . ? C60 N5 Mn2 126.0(3) . . ? C64 N5 Mn2 117.2(3) . . ? C65 N6 C69 118.0(4) . . ? C65 N6 Mn2 111.5(3) . . ? C69 N6 Mn2 127.5(3) . . ? C92 N7 C88 119.2(4) . . ? C92 N7 Mn1 110.6(3) . . ? C88 N7 Mn1 127.0(3) . . ? C97 N8 C93 119.3(5) . . ? C97 N8 Mn1 123.7(4) . . ? C93 N8 Mn1 117.0(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C6 120.6(6) . . ? C1 C2 C3 107.9(7) . . ? C6 C2 C3 111.8(6) . . ? C1 C2 C4 118.1(6) . . ? C6 C2 C4 85.5(5) . . ? C3 C2 C4 111.6(6) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 105.3(6) . . ? C9 C4 C2 109.1(5) . . ? C5 C4 C2 86.4(5) . . ? C9 C4 H4 117.2 . . ? C5 C4 H4 117.2 . . ? C2 C4 H4 117.2 . . ? C6 C5 C4 87.0(6) . . ? C6 C5 H5A 114.2 . . ? C4 C5 H5A 114.2 . . ? C6 C5 H5B 114.2 . . ? C4 C5 H5B 114.2 . . ? H5A C5 H5B 111.3 . . ? C7 C6 C5 108.5(6) . . ? C7 C6 C2 112.5(6) . . ? C5 C6 C2 88.1(6) . . ? C7 C6 H6 114.9 . . ? C5 C6 H6 114.9 . . ? C2 C6 H6 114.9 . . ? C6 C7 C10 110.0(5) . . ? C6 C7 H7A 109.7 . . ? C10 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? C10 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N1 C8 C9 124.7(5) . . ? N1 C8 H8 117.6 . . ? C9 C8 H8 117.6 . . ? C8 C9 C10 117.7(5) . . ? C8 C9 C4 124.8(5) . . ? C10 C9 C4 117.4(5) . . ? C11 C10 C9 118.9(5) . . ? C11 C10 C7 123.2(5) . . ? C9 C10 C7 117.9(5) . . ? C10 C11 C12 120.6(5) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? N1 C12 C11 120.7(5) . . ? N1 C12 C13 118.4(4) . . ? C11 C12 C13 121.0(5) . . ? N2 C13 C14 121.4(5) . . ? N2 C13 C12 117.3(4) . . ? C14 C13 C12 121.3(5) . . ? C13 C14 C15 121.0(6) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 118.0(6) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C15 C16 C17 119.4(6) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? N2 C17 C16 121.7(5) . . ? N2 C17 C18 119.1(5) . . ? C16 C17 C18 119.0(5) . . ? C23 C18 C19 117.9(5) . . ? C23 C18 C17 120.7(5) . . ? C19 C18 C17 121.2(5) . . ? C20 C19 C18 120.6(6) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C21 120.2(6) . . ? C19 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 . . ? C20 C21 C22 121.3(5) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 117.2(5) . . ? C23 C22 C24 120.1(5) . . ? C21 C22 C24 122.7(5) . . ? C18 C23 C22 122.7(5) . . ? C18 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C25 C24 C29 118.7(5) . . ? C25 C24 C22 122.9(5) . . ? C29 C24 C22 118.4(4) . . ? C26 C25 C24 118.9(5) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C27 C26 C25 122.1(5) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 120.8(6) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C29 116.3(5) . . ? C27 C28 C30 124.7(5) . . ? C29 C28 C30 119.0(5) . . ? C24 C29 C28 123.1(5) . . ? C24 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? C35 C30 C31 117.1(5) . . ? C35 C30 C28 120.6(5) . . ? C31 C30 C28 122.3(5) . . ? C32 C31 C30 121.4(5) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 120.7(5) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 118.8(6) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C35 C34 C33 119.6(5) . . ? C35 C34 C36 120.2(4) . . ? C33 C34 C36 120.1(5) . . ? C30 C35 C34 122.4(5) . . ? C30 C35 H35 118.8 . . ? C34 C35 H35 118.8 . . ? N3 C36 C37 122.1(5) . . ? N3 C36 C34 118.0(4) . . ? C37 C36 C34 119.7(5) . . ? C36 C37 C38 119.2(5) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 119.2(5) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 119.6(5) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? N3 C40 C39 122.1(5) . . ? N3 C40 C41 117.2(4) . . ? C39 C40 C41 120.7(4) . . ? N4 C41 C42 120.8(5) . . ? N4 C41 C40 117.1(4) . . ? C42 C41 C40 122.1(4) . . ? C43 C42 C41 120.5(5) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 118.4(5) . . ? C42 C43 C46 123.7(5) . . ? C44 C43 C46 117.9(5) . . ? C45 C44 C43 117.2(5) . . ? C45 C44 C49 126.3(5) . . ? C43 C44 C49 116.5(5) . . ? N4 C45 C44 125.0(5) . . ? N4 C45 H45 117.5 . . ? C44 C45 H45 117.5 . . ? C43 C46 C47 110.6(6) . . ? C43 C46 H46A 109.5 . . ? C47 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C48 C47 C46 108.1(7) . . ? C48 C47 C50 88.9(6) . . ? C46 C47 C50 111.3(7) . . ? C48 C47 H47 115.2 . . ? C46 C47 H47 115.2 . . ? C50 C47 H47 115.2 . . ? C47 C48 C49 84.8(6) . . ? C47 C48 H48A 114.5 . . ? C49 C48 H48A 114.5 . . ? C47 C48 H48B 114.5 . . ? C49 C48 H48B 114.5 . . ? H48A C48 H48B 111.6 . . ? C44 C49 C50 110.9(6) . . ? C44 C49 C48 106.1(6) . . ? C50 C49 C48 87.5(6) . . ? C44 C49 H49 116.2 . . ? C50 C49 H49 116.2 . . ? C48 C49 H49 116.2 . . ? C49 C50 C51 112.6(8) . . ? C49 C50 C47 85.5(6) . . ? C51 C50 C47 111.8(7) . . ? C49 C50 C52 117.9(7) . . ? C51 C50 C52 108.3(8) . . ? C47 C50 C52 119.4(9) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C55 C53 H53A 109.5 . . ? C55 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C55 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C54 C55 C58 119.9(6) . . ? C54 C55 C53 110.9(7) . . ? C58 C55 C53 110.7(7) . . ? C54 C55 C56 117.6(6) . . ? C58 C55 C56 84.4(5) . . ? C53 C55 C56 111.0(6) . . ? C61 C56 C57 106.2(6) . . ? C61 C56 C55 110.2(5) . . ? C57 C56 C55 87.0(5) . . ? C61 C56 H56 116.5 . . ? C57 C56 H56 116.5 . . ? C55 C56 H56 116.5 . . ? C58 C57 C56 85.4(5) . . ? C58 C57 H57A 114.4 . . ? C56 C57 H57A 114.4 . . ? C58 C57 H57B 114.4 . . ? C56 C57 H57B 114.4 . . ? H57A C57 H57B 111.5 . . ? C57 C58 C55 90.0(6) . . ? C57 C58 C59 108.0(6) . . ? C55 C58 C59 112.1(6) . . ? C57 C58 H58 114.7 . . ? C55 C58 H58 114.7 . . ? C59 C58 H58 114.7 . . ? C62 C59 C58 110.2(5) . . ? C62 C59 H59A 109.6 . . ? C58 C59 H59A 109.6 . . ? C62 C59 H59B 109.6 . . ? C58 C59 H59B 109.6 . . ? H59A C59 H59B 108.1 . . ? N5 C60 C61 125.0(5) . . ? N5 C60 H60 117.5 . . ? C61 C60 H60 117.5 . . ? C60 C61 C62 117.8(5) . . ? C60 C61 C56 126.0(5) . . ? C62 C61 C56 116.3(5) . . ? C63 C62 C61 118.2(5) . . ? C63 C62 C59 123.6(5) . . ? C61 C62 C59 118.1(5) . . ? C62 C63 C64 120.6(5) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? N5 C64 C63 121.5(5) . . ? N5 C64 C65 116.9(4) . . ? C63 C64 C65 121.6(4) . . ? N6 C65 C66 121.8(5) . . ? N6 C65 C64 117.1(4) . . ? C66 C65 C64 121.1(5) . . ? C67 C66 C65 119.7(5) . . ? C67 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? C66 C67 C68 119.3(6) . . ? C66 C67 H67 120.3 . . ? C68 C67 H67 120.3 . . ? C69 C68 C67 119.6(5) . . ? C69 C68 H68 120.2 . . ? C67 C68 H68 120.2 . . ? C68 C69 N6 121.5(5) . . ? C68 C69 C70 120.6(5) . . ? N6 C69 C70 117.7(4) . . ? C75 C70 C71 118.6(5) . . ? C75 C70 C69 119.7(5) . . ? C71 C70 C69 121.5(5) . . ? C72 C71 C70 119.2(6) . . ? C72 C71 H71 120.4 . . ? C70 C71 H71 120.4 . . ? C73 C72 C71 121.3(6) . . ? C73 C72 H72 119.3 . . ? C71 C72 H72 119.3 . . ? C72 C73 C74 120.4(5) . . ? C72 C73 H73 119.8 . . ? C74 C73 H73 119.8 . . ? C75 C74 C73 117.5(5) . . ? C75 C74 C76 120.9(5) . . ? C73 C74 C76 121.7(5) . . ? C74 C75 C70 122.9(5) . . ? C74 C75 H75 118.5 . . ? C70 C75 H75 118.5 . . ? C77 C76 C81 117.6(5) . . ? C77 C76 C74 124.4(5) . . ? C81 C76 C74 118.0(5) . . ? C78 C77 C76 120.6(6) . . ? C78 C77 H77 119.7 . . ? C76 C77 H77 119.7 . . ? C79 C78 C77 121.2(5) . . ? C79 C78 H78 119.4 . . ? C77 C78 H78 119.4 . . ? C78 C79 C80 120.3(6) . . ? C78 C79 H79 119.9 . . ? C80 C79 H79 119.9 . . ? C81 C80 C79 117.5(5) . . ? C81 C80 C82 118.6(4) . . ? C79 C80 C82 123.9(5) . . ? C80 C81 C76 122.8(5) . . ? C80 C81 H81 118.6 . . ? C76 C81 H81 118.6 . . ? C83 C82 C87 117.6(5) . . ? C83 C82 C80 123.2(5) . . ? C87 C82 C80 119.2(5) . . ? C84 C83 C82 121.3(6) . . ? C84 C83 H83 119.3 . . ? C82 C83 H83 119.3 . . ? C83 C84 C85 121.0(6) . . ? C83 C84 H84 119.5 . . ? C85 C84 H84 119.5 . . ? C86 C85 C84 119.5(6) . . ? C86 C85 H85 120.2 . . ? C84 C85 H85 120.2 . . ? C85 C86 C87 118.3(5) . . ? C85 C86 C88 122.2(5) . . ? C87 C86 C88 119.4(5) . . ? C82 C87 C86 122.3(5) . . ? C82 C87 H87 118.9 . . ? C86 C87 H87 118.9 . . ? N7 C88 C89 121.3(5) . . ? N7 C88 C86 119.7(4) . . ? C89 C88 C86 118.9(5) . . ? C90 C89 C88 119.2(5) . . ? C90 C89 H89 120.4 . . ? C88 C89 H89 120.4 . . ? C89 C90 C91 119.8(5) . . ? C89 C90 H90 120.1 . . ? C91 C90 H90 120.1 . . ? C90 C91 C92 119.0(5) . . ? C90 C91 H91 120.5 . . ? C92 C91 H91 120.5 . . ? N7 C92 C91 121.6(5) . . ? N7 C92 C93 118.3(4) . . ? C91 C92 C93 120.2(5) . . ? N8 C93 C94 119.4(5) . . ? N8 C93 C92 117.1(4) . . ? C94 C93 C92 123.5(5) . . ? C95 C94 C93 120.6(5) . . ? C95 C94 H94 119.7 . . ? C93 C94 H94 119.7 . . ? C94 C95 C96 119.5(5) . . ? C94 C95 C98A 122.3(13) . . ? C96 C95 C98A 117.4(14) . . ? C94 C95 C98B 121.5(17) . . ? C96 C95 C98B 117.5(15) . . ? C98A C95 C98B 20(2) . . ? C97 C96 C95 117.3(5) . . ? C97 C96 C101 125.0(6) . . ? C95 C96 C101 117.7(5) . . ? N8 C97 C96 123.8(5) . . ? N8 C97 H97 118.1 . . ? C96 C97 H97 118.1 . . ? C95 C98A C99 107.6(19) . . ? C95 C98A H98A 110.2 . . ? C99 C98A H98A 110.2 . . ? C95 C98A H98B 110.2 . . ? C99 C98A H98B 110.2 . . ? H98A C98A H98B 108.5 . . ? C95 C98B C99 107(2) . . ? C95 C98B H98C 110.4 . . ? C99 C98B H98C 110.4 . . ? C95 C98B H98D 110.4 . . ? C99 C98B H98D 110.4 . . ? H98C C98B H98D 108.6 . . ? C102 C99 C100 87.8(6) . . ? C102 C99 C98A 119.2(13) . . ? C100 C99 C98A 100.5(13) . . ? C102 C99 C98B 104.9(13) . . ? C100 C99 C98B 115.6(13) . . ? C98A C99 C98B 20(2) . . ? C102 C99 H99 115.0 . . ? C100 C99 H99 115.0 . . ? C98A C99 H99 115.0 . . ? C98B C99 H99 115.1 . . ? C101 C100 C99 85.5(6) . . ? C101 C100 H10A 114.4 . . ? C99 C100 H10A 114.4 . . ? C101 C100 H10B 114.4 . . ? C99 C100 H10B 114.4 . . ? H10A C100 H10B 111.5 . . ? C96 C101 C100 106.8(6) . . ? C96 C101 C102 109.9(6) . . ? C100 C101 C102 87.6(6) . . ? C96 C101 H101 116.3 . . ? C100 C101 H101 116.3 . . ? C102 C101 H101 116.3 . . ? C104 C102 C103 109.5(8) . . ? C104 C102 C99 119.8(8) . . ? C103 C102 C99 111.8(7) . . ? C104 C102 C101 117.2(6) . . ? C103 C102 C101 111.4(7) . . ? C99 C102 C101 85.3(6) . . ? C102 C103 H10C 109.5 . . ? C102 C103 H10D 109.5 . . ? H10C C103 H10D 109.5 . . ? C102 C103 H10E 109.5 . . ? H10C C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C102 C104 H10F 109.5 . . ? C102 C104 H10G 109.5 . . ? H10F C104 H10G 109.5 . . ? C102 C104 H10H 109.5 . . ? H10F C104 H10H 109.5 . . ? H10G C104 H10H 109.5 . . ? H1WA O1W H1WB 107.6 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 66.99 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.767 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.065 # start Validation Reply Form _vrf_PLAT222_091609a ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.51 Ratio RESPONSE: It is due to the relatively large temperature factors of terminal methyl groups. ; _vrf_PLAT420_091609a ; PROBLEM: D-H Without Acceptor O1W - H1WA ... ? RESPONSE: The surrounding environment of O1W has been checked and found no suitable acceptor for H1WA. ; # end Validation Reply Form