# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email roubeau@unizar.es _publ_contact_author_name 'Olivier Roubeau' loop_ _publ_author_name 'G. Aromi' L.Barrios J.Sanchez G.Craig 'O. Roubeau' S.Teat 'F. Luis' 'M. Evangelisti' 'A. Camon' data_jsc52 _database_code_depnum_ccdc_archive 'CCDC 827222' #TrackingRef 'jsc52.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C194 H150 Mn14 N40 O38, 2(C2 H3 O2), 4(C H4 O), C H4 O, 2(O H2)' _chemical_formula_sum 'C203 H180 Mn14 N40 O49' _chemical_formula_weight 4733.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0018 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0036 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0066 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Mn Mn 0.2253 0.7864 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.784(3) _cell_length_b 19.250(4) _cell_length_c 20.841(4) _cell_angle_alpha 63.51(3) _cell_angle_beta 87.10(3) _cell_angle_gamma 72.53(3) _cell_volume 5380(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 81195 _cell_measurement_theta_min 0.99 _cell_measurement_theta_max 27.85 _exptl_crystal_description rhomb _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2420 _exptl_absorpt_coefficient_mu 0.965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 'HKL2000, Otwinoski, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.73830 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'ESRF BM16' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'phi rotation at various kappa' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 21761 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.11 _reflns_number_total 21761 _reflns_number_gt 17234 _reflns_threshold_expression >2sigma(I) _computing_data_collection MxCube _computing_cell_refinement 'HKL-2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL-2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-hydrogens were refined anisotropically. Hydrogens were placed geometrically at calculated positions on their carrier atom and refined with a riding model, except those of the coordinated water molecules (O9, O15, O19) and hydroxo group (O18), which were found in a difference Fourier map and refined with distance restrains and their thermal parameter 1.5 times that of their carrier oxygen. Hydrogens of the partial water (O1W and O2W) and methanol (O3S, C3S) could not be found and were omitted in the final structural model. At the end of the refinement, large voids remained in the structure containing only diffuse electron density that could not be modeled satisfactorily. These voids were thus analyzed and taken into account by PLATON/SQUEEZE that recovered a total of 30 electrons per cell mostly in one void occupying c.a. 420 cubic angstroms, resulting in a significant improvement both in R1 and wR2 factors. The derived figures (electrons/volume) would reasonably account for one diffuse methanol molecule. Bond valence sum analysis indicate that Mn1 is a Mn(II) ion, while the rest of Mn sites are Mn(III). Electroneutrality considerations then implies that the lattice moiety O20-O21-C100-C101 is a deprotonated acetate anion. ; _vrf_PLAT029_jsc52 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: The low completeness is likely due both to poor diffraction of the crystal that showed rapid damage even in oil and to geometrical limitations of the single-axis goniometer set-up on BM16, with a best resolution of 0.79 angstroms and important blind area. In the present case two full-sphere datasets were collected for two kappa positions of the crystal. ; _vrf_PLAT415_jsc52 ; PROBLEM: Short Inter D-H..H-X H11B .. H19B .. 1.70 Ang. RESPONSE: Hydrogens on the coordinated water oxygens O15 and O19 were found in difference Fourier maps and refined only with soft distance restraints. They may thus have ill-defined positions, which is likely at the origin of a short H H contact, as well as the absence of an acceptor for some of them. ; _vrf_PLAT420_jsc52 ; PROBLEM: D-H Without Acceptor RESPONSE: Hydrogens on the coordinated water oxygens O15 and O19 were found in difference Fourier maps and refined only with soft distance restraints. They may thus have ill-defined positions, which is likely at the origin of a short H H contact, as well as the absence of an acceptor for some of them. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 418.9 28.1 2 0.064 0.370 0.465 21.0 1.3 3 0.220 0.745 0.664 8.9 0.8 4 0.303 0.302 0.874 17.9 1.4 5 0.697 0.698 0.126 18.0 1.4 6 0.780 0.255 0.336 8.8 0.8 7 0.936 0.630 0.535 21.0 1.3 _platon_squeeze_details ; ? ; _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^)+(0.1511P)^2^+0.9730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0133(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 21761 _refine_ls_number_parameters 1499 _refine_ls_number_restraints 320 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.2123 _refine_ls_wR_factor_gt 0.2015 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.087 _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 0.30866(4) -0.03147(3) 0.24496(3) 0.05806(16) Uani 1 1 d . A . Mn2 Mn 0.21218(4) 0.12470(3) 0.31633(3) 0.05156(15) Uani 1 1 d . . . Mn3 Mn 0.23626(3) 0.30414(3) 0.20210(3) 0.05185(15) Uani 1 1 d . . . Mn4 Mn 0.11619(4) 0.10861(3) 0.16997(3) 0.06178(16) Uani 1 1 d D . . Mn5 Mn 0.03899(4) 0.26489(3) 0.22786(3) 0.05541(15) Uani 1 1 d . . . Mn6 Mn 0.19535(4) 0.46301(3) 0.26471(3) 0.05283(15) Uani 1 1 d . . . Mn7 Mn 0.33019(4) 0.46522(3) 0.39865(3) 0.05493(15) Uani 1 1 d D . . O1 O 0.4001(4) -0.0262(3) -0.0143(2) 0.1258(15) Uani 1 1 d U . . H1B H 0.3711 0.0045 -0.0549 0.189 Uiso 1 1 calc R . . O2 O 0.18081(17) 0.14598(15) 0.39505(12) 0.0590(6) Uani 1 1 d . . . O3 O 0.16563(19) -0.00741(16) 0.20888(14) 0.0648(6) Uani 1 1 d . . . O4 O 0.13249(19) 0.57529(16) 0.23653(14) 0.0643(6) Uani 1 1 d . . . O5 O -0.08382(18) 0.29984(16) 0.19914(15) 0.0671(6) Uani 1 1 d . . . O6 O 0.42877(19) 0.49336(16) 0.41497(13) 0.0618(6) Uani 1 1 d . . . O7 O 0.27697(19) 0.47585(16) 0.47928(13) 0.0626(6) Uani 1 1 d . . . O8 O 0.69162(17) -0.36117(14) 0.85796(12) 0.0587(6) Uani 1 1 d . . . O9 O 0.44421(19) -0.03851(18) 0.26909(14) 0.0665(6) Uani 1 1 d D . . H9A H 0.484(3) -0.052(3) 0.242(2) 0.100 Uiso 1 1 d D . . H9B H 0.467(3) -0.052(3) 0.3120(15) 0.100 Uiso 1 1 d D . . O10 O 0.23442(17) 0.10034(14) 0.23437(12) 0.0555(5) Uani 1 1 d . . . O11 O 0.3135(2) 0.05325(16) 0.12689(14) 0.0680(7) Uani 1 1 d . . . O12 O 0.1741(2) 0.13175(18) 0.08184(14) 0.0748(8) Uani 1 1 d . . . O13 O 0.16152(16) 0.24015(14) 0.25479(12) 0.0537(5) Uani 1 1 d . . . O14 O 0.22156(19) 0.26539(15) 0.11557(12) 0.0624(6) Uani 1 1 d . . . O15 O -0.0015(2) 0.1095(2) 0.1190(2) 0.0879(9) Uani 1 1 d D . . H15A H -0.005(3) 0.101(4) 0.080(2) 0.132 Uiso 1 1 d D . . H15B H -0.037(3) 0.078(3) 0.1444(18) 0.132 Uiso 1 1 d D . . O16 O 0.07215(18) 0.22441(15) 0.14163(13) 0.0610(6) Uani 1 1 d . . . O17 O 0.24274(16) 0.35113(14) 0.28491(12) 0.0546(5) Uani 1 1 d . . . O18 O 0.22935(18) 0.44604(16) 0.37145(13) 0.0606(6) Uani 1 1 d D . . H18 H 0.196(3) 0.432(3) 0.410(2) 0.091 Uiso 1 1 d D . . O19 O 0.2352(4) 0.6047(3) 0.3256(3) 0.1267(15) Uani 1 1 d D . . H19C H 0.226(5) 0.6262(19) 0.3598(17) 0.190 Uiso 1 1 d D . . H19B H 0.276(2) 0.6336(17) 0.299(3) 0.190 Uiso 1 1 d D . . N1 N 0.3931(3) -0.1022(2) 0.12656(18) 0.0711(9) Uani 1 1 d . . . H1A H 0.3885 -0.0532 0.0917 0.085 Uiso 1 1 calc R . . N2 N 0.3674(3) -0.1157(2) 0.19251(18) 0.0714(9) Uani 1 1 d . A . N3 N 0.3341(3) -0.1702(2) 0.32614(19) 0.0787(10) Uani 1 1 d . . . N4 N 0.2672(2) -0.04722(17) 0.35442(15) 0.0571(7) Uani 1 1 d . . . N5 N 0.2349(2) 0.00798(17) 0.38008(14) 0.0552(6) Uani 1 1 d . A . N6 N 0.0595(2) 0.08925(19) 0.26012(17) 0.0604(7) Uani 1 1 d . . . N7 N 0.0388(2) 0.14662(19) 0.28508(17) 0.0600(7) Uani 1 1 d . . . N8 N -0.0094(2) 0.2412(2) 0.34875(17) 0.0614(7) Uani 1 1 d . . . N9 N 0.0707(2) 0.36743(18) 0.32024(15) 0.0569(7) Uani 1 1 d . . . H9 H 0.1150 0.3225 0.3298 0.068 Uiso 1 1 calc R . . N10 N 0.0765(2) 0.44431(18) 0.28395(15) 0.0556(6) Uani 1 1 d . . . N11 N 0.03903(19) 0.37891(17) 0.17232(15) 0.0543(6) Uani 1 1 d . . . N12 N 0.11693(19) 0.39800(17) 0.15656(14) 0.0531(6) Uani 1 1 d . . . N13 N 0.2172(2) 0.51031(17) 0.14242(14) 0.0537(6) Uani 1 1 d . . . N14 N 0.3134(2) 0.48768(18) 0.25178(15) 0.0549(6) Uani 1 1 d . . . N15 N 0.3712(2) 0.48032(18) 0.30293(15) 0.0566(7) Uani 1 1 d . . . N16 N 0.3829(2) 0.33274(18) 0.47861(15) 0.0581(7) Uani 1 1 d . . . N17 N 0.4480(2) 0.27156(17) 0.47526(15) 0.0567(7) Uani 1 1 d . . . H17A H 0.4885 0.2785 0.4443 0.068 Uiso 1 1 calc R . . N18 N 0.5139(2) 0.05252(17) 0.59208(15) 0.0562(7) Uani 1 1 d . . . N19 N 0.6599(2) -0.14381(16) 0.68988(14) 0.0531(6) Uani 1 1 d . . . N20 N 0.65411(19) -0.21057(16) 0.74972(14) 0.0526(6) Uani 1 1 d . . . C1 C 0.4495(4) -0.0995(4) -0.0123(3) 0.0992(17) Uani 1 1 d . . . C2 C 0.4874(6) -0.1020(4) -0.0726(3) 0.118(2) Uani 1 1 d . . . H2A H 0.4810 -0.0526 -0.1152 0.142 Uiso 1 1 calc R . . C3 C 0.5335(6) -0.1740(4) -0.0713(4) 0.119(2) Uani 1 1 d . . . H3A H 0.5620 -0.1752 -0.1123 0.143 Uiso 1 1 calc R . . C4 C 0.5392(5) -0.2461(4) -0.0104(4) 0.118(2) Uani 1 1 d . . . H4A H 0.5663 -0.2968 -0.0113 0.142 Uiso 1 1 calc R . . C5 C 0.5056(5) -0.2447(4) 0.0520(3) 0.1022(17) Uani 1 1 d . . . H5A H 0.5126 -0.2943 0.0946 0.123 Uiso 1 1 calc R . . C6 C 0.4613(4) -0.1698(3) 0.0520(3) 0.0812(12) Uani 1 1 d . . . C7 C 0.4265(4) -0.1706(3) 0.1192(3) 0.0795(12) Uani 1 1 d . . . C8 C 0.4216(5) -0.2322(3) 0.1836(3) 0.1065(18) Uani 1 1 d U A . H8A H 0.4384 -0.2886 0.1958 0.128 Uiso 1 1 calc R . . C9 C 0.3868(4) -0.1958(3) 0.2283(3) 0.0907(13) Uani 1 1 d U . . C10 C 0.3874(9) -0.2262(7) 0.3095(6) 0.087(2) Uani 0.50 1 d PU A 1 C11 C 0.4300(9) -0.3081(6) 0.3609(6) 0.099(2) Uani 0.50 1 d PU A 1 H11A H 0.4630 -0.3471 0.3454 0.119 Uiso 0.50 1 calc PR A 1 C12 C 0.4236(9) -0.3302(6) 0.4309(6) 0.098(2) Uani 0.50 1 d PU A 1 H12A H 0.4532 -0.3845 0.4657 0.118 Uiso 0.50 1 calc PR A 1 C13 C 0.3720(8) -0.2715(5) 0.4527(5) 0.086(2) Uani 0.50 1 d PU A 1 H13A H 0.3727 -0.2827 0.5020 0.104 Uiso 0.50 1 calc PR A 1 C10B C 0.3443(8) -0.2269(6) 0.2994(6) 0.076(2) Uani 0.50 1 d PU A 2 C11B C 0.3452(7) -0.3046(5) 0.3413(5) 0.0751(16) Uani 0.50 1 d PU A 2 H11B H 0.3617 -0.3438 0.3232 0.090 Uiso 0.50 1 calc PR A 2 C12B C 0.3219(7) -0.3262(5) 0.4107(5) 0.0753(17) Uani 0.50 1 d PU A 2 H12B H 0.3206 -0.3803 0.4403 0.090 Uiso 0.50 1 calc PR A 2 C13B C 0.3002(7) -0.2691(4) 0.4373(4) 0.0710(17) Uani 0.50 1 d PU A 2 H13B H 0.2759 -0.2808 0.4823 0.085 Uiso 0.50 1 calc PR A 2 C14 C 0.3158(5) -0.1902(3) 0.3942(3) 0.0976(18) Uani 1 1 d . A . C15 C 0.2800(3) -0.1212(2) 0.4099(2) 0.0673(10) Uani 1 1 d . A . C16 C 0.2547(3) -0.1144(2) 0.4727(2) 0.0654(9) Uani 1 1 d . . . H16A H 0.2564 -0.1576 0.5193 0.078 Uiso 1 1 calc R A . C17 C 0.2267(2) -0.0312(2) 0.45263(18) 0.0564(8) Uani 1 1 d . A . C18 C 0.2015(3) 0.0119(2) 0.49584(19) 0.0604(8) Uani 1 1 d . . . C19 C 0.2045(3) -0.0320(3) 0.57101(19) 0.0649(9) Uani 1 1 d . A . H19A H 0.2137 -0.0891 0.5918 0.078 Uiso 1 1 calc R . . C20 C 0.1945(3) 0.0047(3) 0.6158(2) 0.0749(11) Uani 1 1 d . . . H20A H 0.1965 -0.0267 0.6665 0.090 Uiso 1 1 calc R A . C21 C 0.1815(3) 0.0882(3) 0.5858(2) 0.0752(11) Uani 1 1 d . A . H21A H 0.1770 0.1140 0.6160 0.090 Uiso 1 1 calc R . . C22 C 0.1752(3) 0.1334(3) 0.5118(2) 0.0669(9) Uani 1 1 d . . . H22A H 0.1638 0.1908 0.4917 0.080 Uiso 1 1 calc R A . C23 C 0.1852(3) 0.0969(2) 0.46584(18) 0.0595(8) Uani 1 1 d . A . C24 C 0.1205(3) -0.0610(3) 0.2478(2) 0.0709(10) Uani 1 1 d . . . C25 C 0.1374(4) -0.1317(3) 0.2382(3) 0.0869(13) Uani 1 1 d . . . H25A H 0.1758 -0.1387 0.2035 0.104 Uiso 1 1 calc R . . C26 C 0.0987(4) -0.1907(4) 0.2787(4) 0.1046(18) Uani 1 1 d . . . H26A H 0.1112 -0.2383 0.2720 0.126 Uiso 1 1 calc R . . C27 C 0.0417(4) -0.1819(3) 0.3290(4) 0.1027(18) Uani 1 1 d . . . H27A H 0.0147 -0.2227 0.3562 0.123 Uiso 1 1 calc R . . C28 C 0.0245(4) -0.1127(3) 0.3394(3) 0.0883(14) Uani 1 1 d . . . H28A H -0.0135 -0.1066 0.3746 0.106 Uiso 1 1 calc R . . C29 C 0.0638(3) -0.0508(3) 0.2972(2) 0.0709(10) Uani 1 1 d . . . C30 C 0.0424(3) 0.0223(2) 0.3091(2) 0.0628(9) Uani 1 1 d . . . C31 C 0.0062(3) 0.0371(2) 0.3666(2) 0.0676(9) Uani 1 1 d . . . H31A H -0.0135 0.0010 0.4084 0.081 Uiso 1 1 calc R . . C32 C 0.0056(3) 0.1147(2) 0.3490(2) 0.0606(8) Uani 1 1 d . . . C33 C -0.0240(3) 0.1676(2) 0.3840(2) 0.0608(8) Uani 1 1 d . . . C34 C -0.0640(3) 0.1459(3) 0.4479(2) 0.0733(11) Uani 1 1 d . . . H34A H -0.0732 0.0940 0.4716 0.088 Uiso 1 1 calc R . . C35 C -0.0905(3) 0.2005(3) 0.4770(2) 0.0771(11) Uani 1 1 d . . . H35A H -0.1179 0.1863 0.5208 0.093 Uiso 1 1 calc R . . C36 C -0.0767(3) 0.2756(3) 0.4415(2) 0.0727(10) Uani 1 1 d . . . H36A H -0.0955 0.3144 0.4599 0.087 Uiso 1 1 calc R . . C37 C -0.0349(3) 0.2933(2) 0.3785(2) 0.0623(8) Uani 1 1 d . . . C38 C -0.0130(3) 0.3697(2) 0.3397(2) 0.0618(8) Uani 1 1 d . . . C39 C -0.0632(3) 0.4504(2) 0.3158(2) 0.0629(8) Uani 1 1 d . . . H39A H -0.1240 0.4712 0.3221 0.075 Uiso 1 1 calc R . . C40 C -0.0049(3) 0.4959(2) 0.27983(19) 0.0589(8) Uani 1 1 d . . . C41 C -0.0235(3) 0.5836(2) 0.24028(19) 0.0633(9) Uani 1 1 d . . . C42 C -0.1124(3) 0.6347(3) 0.2211(2) 0.0789(11) Uani 1 1 d . . . H42A H -0.1592 0.6110 0.2355 0.095 Uiso 1 1 calc R . . C43 C -0.1333(4) 0.7187(3) 0.1818(3) 0.0947(15) Uani 1 1 d . . . H43A H -0.1936 0.7529 0.1707 0.114 Uiso 1 1 calc R . . C44 C -0.0630(4) 0.7520(3) 0.1587(3) 0.0972(16) Uani 1 1 d . . . H44A H -0.0761 0.8092 0.1299 0.117 Uiso 1 1 calc R . . C45 C 0.0250(3) 0.7030(3) 0.1769(3) 0.0819(12) Uani 1 1 d . . . H45A H 0.0712 0.7273 0.1609 0.098 Uiso 1 1 calc R . . C46 C 0.0473(3) 0.6179(2) 0.2186(2) 0.0637(9) Uani 1 1 d . . . C47 C -0.1458(3) 0.3732(2) 0.17673(18) 0.0604(8) Uani 1 1 d . . . C48 C -0.2351(3) 0.3772(3) 0.1796(2) 0.0685(9) Uani 1 1 d . . . H48A H -0.2500 0.3279 0.1993 0.082 Uiso 1 1 calc R . . C49 C -0.3021(3) 0.4498(3) 0.1551(2) 0.0771(11) Uani 1 1 d . . . H49A H -0.3627 0.4509 0.1560 0.092 Uiso 1 1 calc R . . C50 C -0.2803(3) 0.5233(3) 0.1282(2) 0.0785(12) Uani 1 1 d . . . H50A H -0.3262 0.5742 0.1121 0.094 Uiso 1 1 calc R . . C51 C -0.1926(3) 0.5205(2) 0.1256(2) 0.0651(9) Uani 1 1 d . . . H51A H -0.1783 0.5700 0.1085 0.078 Uiso 1 1 calc R . . C52 C -0.1233(2) 0.4468(2) 0.14753(17) 0.0567(8) Uani 1 1 d . . . C53 C -0.0310(2) 0.4472(2) 0.13915(17) 0.0552(7) Uani 1 1 d . . . C54 C 0.0021(2) 0.5124(2) 0.09988(17) 0.0558(8) Uani 1 1 d . . . H54A H -0.0312 0.5678 0.0707 0.067 Uiso 1 1 calc R . . C55 C 0.0940(2) 0.4787(2) 0.11276(17) 0.0526(7) Uani 1 1 d . . . C56 C 0.1624(2) 0.5206(2) 0.08891(17) 0.0542(7) Uani 1 1 d . . . C57 C 0.1704(3) 0.5682(2) 0.01628(18) 0.0584(8) Uani 1 1 d . . . H57A H 0.1323 0.5734 -0.0205 0.070 Uiso 1 1 calc R . . C58 C 0.2336(3) 0.6070(2) -0.00082(19) 0.0618(9) Uani 1 1 d . . . H58A H 0.2380 0.6420 -0.0496 0.074 Uiso 1 1 calc R . . C59 C 0.2918(3) 0.5949(2) 0.05390(18) 0.0580(8) Uani 1 1 d . . . H59A H 0.3374 0.6202 0.0429 0.070 Uiso 1 1 calc R . . C60 C 0.2822(2) 0.5457(2) 0.12418(18) 0.0553(7) Uani 1 1 d . . . C61 C 0.3401(3) 0.5260(2) 0.18663(18) 0.0571(8) Uani 1 1 d . . . C62 C 0.4179(3) 0.5432(2) 0.1947(2) 0.0608(8) Uani 1 1 d . . . H62A H 0.4517 0.5692 0.1578 0.073 Uiso 1 1 calc R . . C63 C 0.4348(2) 0.5139(2) 0.26846(19) 0.0593(8) Uani 1 1 d . B . C64 C 0.5053(3) 0.5182(3) 0.3074(2) 0.0738(11) Uani 1 1 d . . . C65 C 0.5715(8) 0.5539(7) 0.2633(6) 0.074(2) Uani 0.50 1 d PU B 2 H65A H 0.5714 0.5653 0.2140 0.089 Uiso 0.50 1 calc PR B 2 C66 C 0.6345(6) 0.5707(7) 0.2944(5) 0.0774(17) Uani 0.50 1 d PU B 2 H66A H 0.6814 0.5883 0.2684 0.093 Uiso 0.50 1 calc PR B 2 C67 C 0.6265(6) 0.5609(7) 0.3655(5) 0.0764(16) Uani 0.50 1 d PU B 2 H67A H 0.6686 0.5723 0.3872 0.092 Uiso 0.50 1 calc PR B 2 C68 C 0.5586(8) 0.5349(7) 0.4044(6) 0.0720(19) Uani 0.50 1 d PU B 2 H68A H 0.5511 0.5360 0.4495 0.086 Uiso 0.50 1 calc PR B 2 C65B C 0.5893(8) 0.5146(7) 0.2832(6) 0.077(2) Uani 0.50 1 d PU B 1 H65B H 0.5987 0.5143 0.2379 0.092 Uiso 0.50 1 calc PR B 1 C66B C 0.6585(7) 0.5116(7) 0.3213(5) 0.0793(17) Uani 0.50 1 d PU B 1 H66B H 0.7118 0.5170 0.2992 0.095 Uiso 0.50 1 calc PR B 1 C67B C 0.6535(7) 0.5009(7) 0.3899(5) 0.0787(17) Uani 0.50 1 d PU B 1 H67B H 0.7033 0.4979 0.4159 0.094 Uiso 0.50 1 calc PR B 1 C68B C 0.5763(8) 0.4944(7) 0.4216(6) 0.0728(19) Uani 0.50 1 d PU B 1 H68B H 0.5737 0.4822 0.4710 0.087 Uiso 0.50 1 calc PR B 1 C69 C 0.4987(3) 0.5063(3) 0.3794(2) 0.0708(10) Uani 1 1 d . B . C70 C 0.2260(3) 0.4322(2) 0.5198(2) 0.0633(9) Uani 1 1 d . . . C71 C 0.1447(3) 0.4720(3) 0.5365(2) 0.0724(10) Uani 1 1 d . . . H71A H 0.1259 0.5298 0.5169 0.087 Uiso 1 1 calc R . . C72 C 0.0909(3) 0.4291(3) 0.5811(3) 0.0830(12) Uani 1 1 d . . . H72A H 0.0362 0.4578 0.5918 0.100 Uiso 1 1 calc R . . C73 C 0.1161(3) 0.3449(3) 0.6101(3) 0.0848(13) Uani 1 1 d . . . H73A H 0.0798 0.3152 0.6412 0.102 Uiso 1 1 calc R . . C74 C 0.1955(3) 0.3047(3) 0.5928(3) 0.0788(12) Uani 1 1 d . . . H74A H 0.2127 0.2469 0.6123 0.095 Uiso 1 1 calc R . . C75 C 0.2515(3) 0.3459(2) 0.5475(2) 0.0641(9) Uani 1 1 d . . . C76 C 0.3337(3) 0.2983(2) 0.5311(2) 0.0639(9) Uani 1 1 d . . . C77 C 0.3733(3) 0.2118(2) 0.5627(2) 0.0645(9) Uani 1 1 d . . . H77A H 0.3538 0.1722 0.6019 0.077 Uiso 1 1 calc R . . C78 C 0.4443(3) 0.1972(2) 0.52552(18) 0.0577(8) Uani 1 1 d . . . C79 C 0.5026(2) 0.1207(2) 0.52832(18) 0.0561(8) Uani 1 1 d . . . C80 C 0.5406(3) 0.1180(2) 0.46753(19) 0.0593(8) Uani 1 1 d . . . H80A H 0.5318 0.1668 0.4238 0.071 Uiso 1 1 calc R . . C81 C 0.5914(2) 0.0440(2) 0.47148(19) 0.0589(8) Uani 1 1 d . . . H81A H 0.6176 0.0406 0.4305 0.071 Uiso 1 1 calc R . . C82 C 0.6033(2) -0.0256(2) 0.53666(19) 0.0578(8) Uani 1 1 d . . . H82A H 0.6384 -0.0774 0.5410 0.069 Uiso 1 1 calc R . . C83 C 0.5637(2) -0.0189(2) 0.59524(18) 0.0562(8) Uani 1 1 d . . . C84 C 0.5759(2) -0.0942(2) 0.66401(18) 0.0551(7) Uani 1 1 d . . . C85 C 0.5163(3) -0.1285(2) 0.70696(19) 0.0604(8) Uani 1 1 d . . . H85A H 0.4531 -0.1058 0.7014 0.072 Uiso 1 1 calc R . . C86 C 0.5676(2) -0.2036(2) 0.76039(18) 0.0556(8) Uani 1 1 d . . . C87 C 0.5410(3) -0.2692(2) 0.81924(19) 0.0626(9) Uani 1 1 d . . . C88 C 0.4498(3) -0.2574(3) 0.8305(3) 0.0784(12) Uani 1 1 d . . . H88A H 0.4068 -0.2081 0.7984 0.094 Uiso 1 1 calc R . . C89 C 0.4220(3) -0.3147(3) 0.8858(3) 0.0969(17) Uani 1 1 d . . . H89A H 0.3605 -0.3049 0.8932 0.116 Uiso 1 1 calc R . . C90 C 0.4856(3) -0.3888(3) 0.9320(3) 0.0817(13) Uani 1 1 d . . . H90A H 0.4667 -0.4301 0.9698 0.098 Uiso 1 1 calc R . . C91 C 0.5742(3) -0.4015(2) 0.9228(2) 0.0684(10) Uani 1 1 d . . . H91A H 0.6165 -0.4509 0.9557 0.082 Uiso 1 1 calc R . . C92 C 0.6044(2) -0.3422(2) 0.86493(18) 0.0577(8) Uani 1 1 d . . . C93 C 0.2573(3) 0.1030(2) 0.0761(2) 0.0697(10) Uani 1 1 d . . . C94 C 0.2833(4) 0.1356(3) 0.0000(2) 0.0962(16) Uani 1 1 d . . . H94A H 0.3479 0.1256 0.0010 0.144 Uiso 1 1 calc R . . H94B H 0.2525 0.1944 -0.0260 0.144 Uiso 1 1 calc R . . H94C H 0.2662 0.1079 -0.0245 0.144 Uiso 1 1 calc R . . C95 C 0.2159(4) 0.3238(3) 0.0410(2) 0.0780(12) Uani 1 1 d . . . H95A H 0.2012 0.3019 0.0101 0.117 Uiso 1 1 calc R . . H95B H 0.2733 0.3341 0.0302 0.117 Uiso 1 1 calc R . . H95C H 0.1693 0.3749 0.0320 0.117 Uiso 1 1 calc R . . C96 C 0.0173(3) 0.2761(3) 0.0749(2) 0.0761(11) Uani 1 1 d . . . H96A H 0.0427 0.2595 0.0381 0.114 Uiso 1 1 calc R . . H96B H 0.0146 0.3329 0.0597 0.114 Uiso 1 1 calc R . . H96C H -0.0430 0.2714 0.0812 0.114 Uiso 1 1 calc R . . C97 C 0.3092(3) 0.2979(2) 0.3443(2) 0.0734(11) Uani 1 1 d . . . H97A H 0.2968 0.3142 0.3830 0.110 Uiso 1 1 calc R . . H97B H 0.3681 0.3012 0.3287 0.110 Uiso 1 1 calc R . . H97C H 0.3082 0.2417 0.3619 0.110 Uiso 1 1 calc R . . O1S O 0.4088(5) 0.1358(4) 0.7615(3) 0.157(2) Uani 1 1 d U . . H1S H 0.3843 0.1152 0.7991 0.235 Uiso 1 1 calc R . . C1S C 0.3872(6) 0.2221(6) 0.7378(5) 0.149(3) Uani 1 1 d U . . H1S1 H 0.4095 0.2315 0.7753 0.224 Uiso 1 1 calc R . . H1S2 H 0.3223 0.2473 0.7284 0.224 Uiso 1 1 calc R . . H1S3 H 0.4150 0.2462 0.6935 0.224 Uiso 1 1 calc R . . O2S O 0.5818(3) 0.3082(2) 0.3825(2) 0.1102(13) Uani 1 1 d U . . H2S H 0.5999 0.3466 0.3785 0.165 Uiso 1 1 calc R . . C2S C 0.5789(6) 0.3078(5) 0.3135(4) 0.140(2) Uani 1 1 d U . . H2S1 H 0.5200 0.3068 0.3020 0.211 Uiso 1 1 calc R . . H2S2 H 0.6248 0.2593 0.3155 0.211 Uiso 1 1 calc R . . H2S3 H 0.5900 0.3570 0.2763 0.211 Uiso 1 1 calc R . . O3S O -0.1844(8) 0.1795(7) 0.2409(7) 0.158(4) Uani 0.50 1 d PU . . C3S C -0.1497(12) 0.1884(11) 0.1705(11) 0.146(4) Uani 0.50 1 d PU . . O1W O 0.2276(7) 0.6233(6) 0.4844(6) 0.126(3) Uani 0.50 1 d PU C 2 O2W O 0.7041(7) 0.3746(6) 0.3853(5) 0.123(3) Uani 0.50 1 d PU D 2 O20 O 0.3087(4) 0.0717(3) 0.8599(3) 0.1312(15) Uani 1 1 d U . . O21 O 0.2061(6) 0.0077(6) 0.8797(5) 0.248(4) Uani 1 1 d U . . C100 C 0.2483(8) 0.0540(8) 0.8386(6) 0.178(3) Uani 1 1 d U . . C101 C 0.2194(9) 0.0935(8) 0.7634(6) 0.214(4) Uani 1 1 d U . . H10A H 0.1574 0.0959 0.7569 0.321 Uiso 1 1 calc R . . H10B H 0.2574 0.0627 0.7402 0.321 Uiso 1 1 calc R . . H10C H 0.2236 0.1490 0.7416 0.321 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0686(3) 0.0471(3) 0.0505(3) -0.0180(2) 0.0047(2) -0.0137(3) Mn2 0.0579(3) 0.0447(3) 0.0454(3) -0.0149(2) 0.0047(2) -0.0157(2) Mn3 0.0548(3) 0.0425(3) 0.0466(3) -0.0121(2) 0.0040(2) -0.0120(2) Mn4 0.0696(4) 0.0527(3) 0.0565(3) -0.0215(2) -0.0019(2) -0.0140(3) Mn5 0.0570(3) 0.0471(3) 0.0544(3) -0.0171(2) 0.0029(2) -0.0147(2) Mn6 0.0574(3) 0.0472(3) 0.0488(3) -0.0173(2) 0.0035(2) -0.0161(2) Mn7 0.0689(3) 0.0451(3) 0.0469(3) -0.0154(2) 0.0019(2) -0.0205(2) O1 0.167(4) 0.103(3) 0.090(2) -0.049(2) 0.028(2) -0.013(3) O2 0.0659(15) 0.0567(13) 0.0503(12) -0.0197(10) 0.0054(10) -0.0204(12) O3 0.0701(16) 0.0549(14) 0.0661(15) -0.0263(12) 0.0039(12) -0.0162(13) O4 0.0685(16) 0.0523(13) 0.0679(15) -0.0237(12) 0.0031(12) -0.0181(12) O5 0.0638(15) 0.0575(14) 0.0726(16) -0.0222(12) 0.0022(12) -0.0193(12) O6 0.0746(16) 0.0582(14) 0.0545(13) -0.0221(11) 0.0048(11) -0.0285(13) O7 0.0739(16) 0.0557(13) 0.0572(13) -0.0234(11) 0.0025(11) -0.0212(13) O8 0.0624(14) 0.0453(12) 0.0510(12) -0.0100(10) 0.0067(10) -0.0123(11) O9 0.0706(17) 0.0658(16) 0.0565(14) -0.0234(12) 0.0063(12) -0.0190(14) O10 0.0646(14) 0.0469(12) 0.0485(11) -0.0178(10) 0.0047(10) -0.0143(11) O11 0.0860(18) 0.0541(14) 0.0533(13) -0.0191(11) 0.0104(12) -0.0160(14) O12 0.090(2) 0.0657(16) 0.0558(14) -0.0235(12) -0.0025(13) -0.0119(16) O13 0.0586(13) 0.0461(11) 0.0475(11) -0.0153(9) 0.0042(9) -0.0135(10) O14 0.0747(16) 0.0535(13) 0.0472(12) -0.0169(10) 0.0049(11) -0.0133(12) O15 0.084(2) 0.085(2) 0.095(2) -0.0422(19) -0.0141(17) -0.0201(17) O16 0.0655(15) 0.0531(13) 0.0507(12) -0.0172(10) -0.0057(10) -0.0082(12) O17 0.0589(13) 0.0498(12) 0.0479(11) -0.0171(10) 0.0019(9) -0.0146(11) O18 0.0670(15) 0.0611(14) 0.0519(13) -0.0233(11) 0.0065(11) -0.0213(12) O19 0.150(4) 0.080(2) 0.131(4) -0.036(2) 0.022(3) -0.030(3) N1 0.087(2) 0.0605(18) 0.0615(18) -0.0297(15) 0.0103(16) -0.0142(18) N2 0.087(2) 0.0631(19) 0.0621(18) -0.0283(15) 0.0105(16) -0.0215(18) N3 0.114(3) 0.0499(17) 0.0626(19) -0.0190(15) 0.0094(18) -0.0222(19) N4 0.0686(18) 0.0450(14) 0.0508(14) -0.0164(12) 0.0072(12) -0.0169(13) N5 0.0660(17) 0.0499(14) 0.0449(13) -0.0155(11) 0.0052(12) -0.0206(14) N6 0.0609(17) 0.0524(15) 0.0665(17) -0.0250(14) 0.0023(13) -0.0180(14) N7 0.0634(18) 0.0528(15) 0.0607(16) -0.0224(13) 0.0076(13) -0.0191(14) N8 0.0600(17) 0.0613(17) 0.0617(17) -0.0248(14) 0.0082(13) -0.0224(15) N9 0.0606(17) 0.0527(15) 0.0572(15) -0.0240(13) 0.0116(12) -0.0196(14) N10 0.0625(17) 0.0493(14) 0.0486(14) -0.0165(12) 0.0054(12) -0.0176(13) N11 0.0554(15) 0.0501(15) 0.0493(14) -0.0174(12) 0.0015(11) -0.0128(13) N12 0.0565(15) 0.0469(14) 0.0492(14) -0.0167(11) 0.0040(11) -0.0148(13) N13 0.0591(16) 0.0461(14) 0.0461(13) -0.0157(11) 0.0017(11) -0.0108(13) N14 0.0622(17) 0.0500(14) 0.0474(13) -0.0171(11) 0.0027(12) -0.0179(13) N15 0.0589(16) 0.0543(15) 0.0542(15) -0.0222(12) 0.0000(12) -0.0172(13) N16 0.0644(17) 0.0489(15) 0.0511(14) -0.0129(12) 0.0012(12) -0.0190(14) N17 0.0614(17) 0.0446(14) 0.0540(15) -0.0133(12) 0.0041(12) -0.0169(13) N18 0.0595(16) 0.0448(14) 0.0528(14) -0.0114(11) 0.0017(12) -0.0168(13) N19 0.0592(16) 0.0410(13) 0.0461(13) -0.0090(11) 0.0021(11) -0.0146(12) N20 0.0564(15) 0.0419(13) 0.0490(14) -0.0135(11) 0.0056(11) -0.0124(12) C1 0.124(5) 0.085(3) 0.089(3) -0.050(3) 0.028(3) -0.020(3) C2 0.174(7) 0.099(4) 0.085(3) -0.049(3) 0.039(4) -0.041(5) C3 0.167(7) 0.109(5) 0.104(4) -0.065(4) 0.058(4) -0.055(5) C4 0.151(6) 0.104(4) 0.121(5) -0.075(4) 0.033(4) -0.033(4) C5 0.129(5) 0.079(3) 0.104(4) -0.054(3) 0.033(3) -0.022(3) C6 0.089(3) 0.081(3) 0.085(3) -0.050(2) 0.016(2) -0.024(3) C7 0.094(3) 0.067(2) 0.079(3) -0.041(2) 0.010(2) -0.015(2) C8 0.168(5) 0.059(2) 0.088(3) -0.039(2) 0.031(3) -0.023(3) C9 0.138(4) 0.0508(19) 0.074(2) -0.0274(15) 0.023(2) -0.020(2) C10 0.126(5) 0.047(3) 0.075(2) -0.024(2) 0.015(4) -0.015(4) C11 0.131(5) 0.052(3) 0.087(3) -0.018(2) 0.012(4) -0.011(4) C12 0.123(5) 0.054(3) 0.086(3) -0.012(3) 0.011(4) -0.015(4) C13 0.114(5) 0.054(3) 0.073(4) -0.013(3) 0.008(4) -0.026(4) C10B 0.106(5) 0.046(3) 0.071(3) -0.023(2) 0.011(3) -0.021(3) C11B 0.103(4) 0.043(2) 0.074(3) -0.025(2) 0.012(3) -0.018(3) C12B 0.102(4) 0.041(3) 0.071(3) -0.017(2) 0.009(3) -0.018(3) C13B 0.093(5) 0.043(3) 0.064(3) -0.017(2) 0.011(3) -0.017(3) C14 0.159(5) 0.045(2) 0.066(2) -0.0151(18) 0.026(3) -0.019(3) C15 0.086(3) 0.0527(19) 0.0547(19) -0.0144(15) 0.0104(17) -0.0266(19) C16 0.080(2) 0.0501(18) 0.0549(18) -0.0123(15) 0.0106(17) -0.0241(18) C17 0.0616(19) 0.0521(18) 0.0497(16) -0.0148(14) 0.0065(14) -0.0233(16) C18 0.064(2) 0.066(2) 0.0502(17) -0.0202(15) 0.0103(14) -0.0284(18) C19 0.073(2) 0.074(2) 0.0502(17) -0.0232(16) 0.0102(16) -0.034(2) C20 0.085(3) 0.090(3) 0.055(2) -0.031(2) 0.0172(18) -0.039(2) C21 0.089(3) 0.095(3) 0.059(2) -0.040(2) 0.0194(19) -0.045(3) C22 0.075(2) 0.071(2) 0.059(2) -0.0289(18) 0.0114(17) -0.031(2) C23 0.063(2) 0.068(2) 0.0498(17) -0.0244(15) 0.0110(14) -0.0264(18) C24 0.067(2) 0.062(2) 0.084(3) -0.034(2) 0.0004(19) -0.019(2) C25 0.091(3) 0.074(3) 0.113(4) -0.053(3) 0.013(3) -0.031(3) C26 0.103(4) 0.084(3) 0.153(6) -0.072(4) 0.020(4) -0.038(3) C27 0.104(4) 0.075(3) 0.145(5) -0.053(3) 0.033(4) -0.048(3) C28 0.087(3) 0.063(2) 0.119(4) -0.041(3) 0.019(3) -0.032(2) C29 0.070(2) 0.059(2) 0.085(3) -0.033(2) 0.004(2) -0.022(2) C30 0.061(2) 0.0524(18) 0.069(2) -0.0224(16) 0.0039(16) -0.0175(17) C31 0.065(2) 0.060(2) 0.070(2) -0.0202(18) 0.0084(17) -0.0240(18) C32 0.061(2) 0.0578(19) 0.0573(18) -0.0197(15) 0.0056(15) -0.0210(17) C33 0.059(2) 0.0587(19) 0.064(2) -0.0251(16) 0.0125(16) -0.0227(17) C34 0.079(3) 0.073(2) 0.071(2) -0.025(2) 0.018(2) -0.040(2) C35 0.086(3) 0.087(3) 0.073(2) -0.039(2) 0.029(2) -0.046(3) C36 0.082(3) 0.077(3) 0.068(2) -0.034(2) 0.024(2) -0.038(2) C37 0.061(2) 0.063(2) 0.067(2) -0.0300(17) 0.0131(16) -0.0232(18) C38 0.066(2) 0.066(2) 0.0590(19) -0.0297(17) 0.0145(16) -0.0271(19) C39 0.061(2) 0.063(2) 0.062(2) -0.0273(17) 0.0099(16) -0.0180(18) C40 0.062(2) 0.0594(19) 0.0553(18) -0.0258(15) 0.0044(15) -0.0185(17) C41 0.074(2) 0.0559(19) 0.0536(18) -0.0228(15) 0.0054(16) -0.0143(18) C42 0.076(3) 0.071(3) 0.070(2) -0.020(2) -0.002(2) -0.014(2) C43 0.086(3) 0.068(3) 0.095(3) -0.019(2) -0.012(3) 0.000(3) C44 0.103(4) 0.058(2) 0.094(3) -0.009(2) -0.006(3) -0.014(3) C45 0.087(3) 0.056(2) 0.082(3) -0.017(2) 0.008(2) -0.018(2) C46 0.075(2) 0.0537(19) 0.0552(18) -0.0207(15) 0.0010(16) -0.0162(18) C47 0.061(2) 0.066(2) 0.0497(17) -0.0222(15) 0.0035(14) -0.0188(17) C48 0.067(2) 0.074(2) 0.066(2) -0.0324(19) 0.0099(17) -0.025(2) C49 0.062(2) 0.088(3) 0.073(2) -0.030(2) 0.0099(18) -0.022(2) C50 0.067(2) 0.070(2) 0.073(2) -0.022(2) 0.0089(19) -0.004(2) C51 0.065(2) 0.060(2) 0.0554(19) -0.0188(16) 0.0084(16) -0.0113(18) C52 0.0597(19) 0.0571(19) 0.0459(16) -0.0195(14) 0.0053(13) -0.0139(16) C53 0.0594(19) 0.0523(17) 0.0454(15) -0.0170(13) 0.0009(13) -0.0131(15) C54 0.0616(20) 0.0498(17) 0.0477(16) -0.0172(13) -0.0002(14) -0.0129(15) C55 0.0590(18) 0.0460(16) 0.0450(15) -0.0173(13) 0.0016(13) -0.0107(15) C56 0.0600(19) 0.0423(15) 0.0505(16) -0.0160(13) 0.0011(14) -0.0097(15) C57 0.068(2) 0.0505(17) 0.0451(16) -0.0151(14) -0.0035(14) -0.0124(16) C58 0.072(2) 0.0524(18) 0.0497(17) -0.0137(14) 0.0071(15) -0.0189(17) C59 0.068(2) 0.0476(17) 0.0492(16) -0.0131(14) 0.0051(14) -0.0193(16) C60 0.0621(19) 0.0468(16) 0.0496(16) -0.0156(13) 0.0042(14) -0.0168(15) C61 0.063(2) 0.0495(17) 0.0517(17) -0.0174(14) 0.0064(14) -0.0171(16) C62 0.066(2) 0.060(2) 0.0558(18) -0.0238(16) 0.0089(15) -0.0234(18) C63 0.060(2) 0.063(2) 0.0578(18) -0.0279(16) 0.0075(15) -0.0207(17) C64 0.069(2) 0.099(3) 0.074(2) -0.051(2) 0.0140(19) -0.036(2) C65 0.074(4) 0.099(5) 0.057(4) -0.036(4) 0.009(3) -0.038(4) C66 0.071(4) 0.104(4) 0.064(3) -0.035(3) 0.011(3) -0.043(4) C67 0.077(3) 0.098(4) 0.065(3) -0.035(3) 0.003(3) -0.044(3) C68 0.075(4) 0.091(5) 0.061(4) -0.037(4) 0.008(3) -0.035(4) C65B 0.076(4) 0.102(5) 0.064(4) -0.041(4) 0.014(3) -0.038(4) C66B 0.072(3) 0.102(4) 0.070(3) -0.040(3) 0.012(3) -0.035(4) C67B 0.077(4) 0.096(4) 0.071(3) -0.041(3) 0.004(3) -0.032(4) C68B 0.077(4) 0.087(5) 0.065(4) -0.040(4) 0.006(3) -0.031(4) C69 0.072(2) 0.089(3) 0.068(2) -0.044(2) 0.0118(18) -0.033(2) C70 0.069(2) 0.066(2) 0.0557(18) -0.0285(17) 0.0046(16) -0.0201(19) C71 0.082(3) 0.073(2) 0.070(2) -0.039(2) 0.0070(19) -0.022(2) C72 0.081(3) 0.091(3) 0.087(3) -0.050(3) 0.017(2) -0.026(3) C73 0.085(3) 0.088(3) 0.087(3) -0.041(3) 0.026(2) -0.037(3) C74 0.090(3) 0.069(2) 0.078(3) -0.030(2) 0.020(2) -0.033(2) C75 0.070(2) 0.060(2) 0.0593(19) -0.0247(16) 0.0047(16) -0.0184(18) C76 0.075(2) 0.0563(19) 0.0536(18) -0.0171(15) 0.0047(16) -0.0236(18) C77 0.075(2) 0.0495(18) 0.0556(18) -0.0120(15) 0.0069(16) -0.0206(18) C78 0.065(2) 0.0460(16) 0.0489(16) -0.0095(13) -0.0021(14) -0.0170(16) C79 0.0611(19) 0.0483(17) 0.0511(16) -0.0135(14) -0.0005(14) -0.0196(15) C80 0.064(2) 0.0477(17) 0.0511(17) -0.0081(14) -0.0006(14) -0.0191(16) C81 0.0581(19) 0.0584(19) 0.0511(17) -0.0152(15) 0.0016(14) -0.0203(16) C82 0.0565(19) 0.0526(18) 0.0559(18) -0.0165(15) 0.0046(14) -0.0183(16) C83 0.0567(18) 0.0485(17) 0.0536(17) -0.0136(14) 0.0018(14) -0.0176(15) C84 0.0584(19) 0.0459(16) 0.0509(16) -0.0161(14) 0.0019(14) -0.0113(15) C85 0.060(2) 0.0509(18) 0.0550(18) -0.0129(15) 0.0041(15) -0.0144(16) C86 0.0555(18) 0.0473(16) 0.0517(17) -0.0138(14) 0.0055(14) -0.0129(15) C87 0.065(2) 0.0547(19) 0.0551(18) -0.0137(15) 0.0116(15) -0.0189(17) C88 0.062(2) 0.061(2) 0.084(3) -0.012(2) 0.011(2) -0.0156(19) C89 0.069(3) 0.074(3) 0.101(3) -0.003(3) 0.023(2) -0.021(2) C90 0.078(3) 0.055(2) 0.085(3) -0.010(2) 0.028(2) -0.022(2) C91 0.073(2) 0.0462(18) 0.063(2) -0.0099(16) 0.0163(18) -0.0135(18) C92 0.062(2) 0.0497(17) 0.0535(17) -0.0168(14) 0.0122(14) -0.0181(16) C93 0.094(3) 0.0531(19) 0.0506(18) -0.0214(16) 0.0041(18) -0.009(2) C94 0.123(4) 0.082(3) 0.053(2) -0.020(2) 0.011(2) -0.008(3) C95 0.102(3) 0.073(3) 0.0506(19) -0.0202(18) 0.0118(19) -0.029(2) C96 0.083(3) 0.062(2) 0.062(2) -0.0213(18) -0.0126(19) -0.003(2) C97 0.093(3) 0.055(2) 0.058(2) -0.0207(17) -0.0122(19) -0.009(2) O1S 0.146(4) 0.139(4) 0.142(5) -0.047(4) 0.036(4) -0.017(4) C1S 0.142(6) 0.150(4) 0.153(6) -0.081(5) -0.010(5) -0.017(6) O2S 0.127(3) 0.074(2) 0.116(3) -0.0284(19) 0.058(2) -0.043(2) C2S 0.179(6) 0.108(4) 0.133(4) -0.052(4) 0.062(4) -0.053(4) O3S 0.131(6) 0.137(6) 0.168(7) -0.031(5) 0.010(5) -0.051(5) C3S 0.134(8) 0.138(8) 0.182(7) -0.097(7) -0.018(6) -0.018(6) O1W 0.126(6) 0.096(5) 0.151(6) -0.063(5) 0.043(5) -0.023(5) O2W 0.141(6) 0.109(5) 0.120(6) -0.045(4) 0.010(5) -0.052(5) O20 0.146(4) 0.145(4) 0.108(3) -0.062(3) 0.020(3) -0.047(3) O21 0.218(6) 0.235(7) 0.237(6) -0.024(5) 0.005(5) -0.128(5) C100 0.188(6) 0.185(6) 0.154(4) -0.044(4) -0.008(4) -0.095(4) C101 0.246(8) 0.229(8) 0.164(4) -0.070(5) -0.037(5) -0.089(6) _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 O9 2.173(3) . ? Mn1 N4 2.253(3) . ? Mn1 O3 2.261(3) . ? Mn1 O11 2.280(3) . ? Mn1 N2 2.293(4) . ? Mn1 N3 2.356(3) . ? Mn1 O10 2.367(3) . ? Mn2 O2 1.871(3) . ? Mn2 O13 1.928(2) . ? Mn2 O10 1.953(2) . ? Mn2 N5 1.960(3) . ? Mn2 N19 2.146(3) 2_656 ? Mn2 Mn5 3.1300(18) . ? Mn3 O8 1.857(2) 2_656 ? Mn3 O13 1.910(2) . ? Mn3 N20 1.984(3) 2_656 ? Mn3 N12 2.079(3) . ? Mn3 O14 2.282(3) . ? Mn3 O17 2.296(2) . ? Mn4 O3 1.912(3) . ? Mn4 O16 1.933(3) . ? Mn4 O12 1.937(3) . ? Mn4 N6 1.968(3) . ? Mn4 O15 2.178(3) . ? Mn4 O10 2.279(3) . ? Mn5 O5 1.883(3) . ? Mn5 O13 1.897(3) . ? Mn5 N11 1.973(3) . ? Mn5 N7 2.046(3) . ? Mn5 O16 2.241(3) . ? Mn5 N8 2.476(3) . ? Mn6 O17 1.906(3) . ? Mn6 O4 1.908(3) . ? Mn6 N10 2.002(3) . ? Mn6 N14 2.033(3) . ? Mn6 O18 2.171(3) . ? Mn6 N13 2.339(3) . ? Mn7 O6 1.885(3) . ? Mn7 O18 1.903(3) . ? Mn7 O7 1.906(3) . ? Mn7 N15 1.987(3) . ? Mn7 N16 2.247(3) . ? Mn7 O19 2.438(5) . ? O1 C1 1.375(7) . ? O1 H1B 0.8400 . ? O2 C23 1.342(4) . ? O3 C24 1.365(5) . ? O4 C46 1.317(5) . ? O5 C47 1.341(5) . ? O6 C69 1.322(5) . ? O7 C70 1.331(5) . ? O8 C92 1.332(4) . ? O8 Mn3 1.857(2) 2_656 ? O9 H9A 0.88(5) . ? O9 H9B 0.88(5) . ? O11 C93 1.227(5) . ? O12 C93 1.285(6) . ? O14 C95 1.443(4) . ? O15 H15A 0.91(5) . ? O15 H15B 0.92(5) . ? O16 C96 1.430(4) . ? O17 C97 1.427(5) . ? O18 H18 0.91(2) . ? O19 H19C 0.96(2) . ? O19 H19B 0.97(2) . ? N1 C7 1.338(6) . ? N1 N2 1.345(5) . ? N1 H1A 0.8800 . ? N2 C9 1.320(5) . ? N3 C10 1.323(13) . ? N3 C14 1.336(6) . ? N3 C10B 1.399(12) . ? N4 C15 1.338(4) . ? N4 N5 1.352(4) . ? N5 C17 1.376(4) . ? N6 C30 1.336(5) . ? N6 N7 1.369(4) . ? N7 C32 1.349(5) . ? N8 C37 1.355(5) . ? N8 C33 1.360(5) . ? N9 C38 1.356(5) . ? N9 N10 1.359(4) . ? N9 H9 0.8800 . ? N10 C40 1.347(5) . ? N11 C53 1.350(4) . ? N11 N12 1.370(4) . ? N12 C55 1.344(4) . ? N13 C60 1.346(5) . ? N13 C56 1.352(4) . ? N14 C61 1.343(4) . ? N14 N15 1.370(4) . ? N15 C63 1.358(5) . ? N16 N17 1.338(4) . ? N16 C76 1.348(5) . ? N17 C78 1.363(4) . ? N17 H17A 0.8800 . ? N18 C83 1.338(5) . ? N18 C79 1.359(4) . ? N19 C84 1.348(5) . ? N19 N20 1.358(4) . ? N19 Mn2 2.146(3) 2_656 ? N20 C86 1.349(4) . ? N20 Mn3 1.984(3) 2_656 ? C1 C2 1.378(7) . ? C1 C6 1.385(8) . ? C2 C3 1.348(9) . ? C2 H2A 0.9500 . ? C3 C4 1.382(9) . ? C3 H3A 0.9500 . ? C4 C5 1.390(8) . ? C4 H4A 0.9500 . ? C5 C6 1.399(7) . ? C5 H5A 0.9500 . ? C6 C7 1.474(6) . ? C7 C8 1.355(7) . ? C8 C9 1.399(7) . ? C8 H8A 0.9500 . ? C9 C10 1.524(13) . ? C9 C10B 1.534(12) . ? C10 C11 1.419(14) . ? C11 C12 1.333(15) . ? C11 H11A 0.9500 . ? C12 C13 1.420(15) . ? C12 H12A 0.9500 . ? C13 C14 1.515(10) . ? C13 H13A 0.9500 . ? C10B C11B 1.350(12) . ? C11B C12B 1.379(12) . ? C11B H11B 0.9500 . ? C12B C13B 1.392(12) . ? C12B H12B 0.9500 . ? C13B C14 1.470(9) . ? C13B H13B 0.9500 . ? C14 C15 1.451(6) . ? C15 C16 1.399(6) . ? C16 C17 1.389(5) . ? C16 H16A 0.9500 . ? C17 C18 1.446(5) . ? C18 C19 1.405(5) . ? C18 C23 1.409(5) . ? C19 C20 1.379(6) . ? C19 H19A 0.9500 . ? C20 C21 1.392(7) . ? C20 H20A 0.9500 . ? C21 C22 1.383(5) . ? C21 H21A 0.9500 . ? C22 C23 1.399(5) . ? C22 H22A 0.9500 . ? C24 C29 1.372(6) . ? C24 C25 1.409(6) . ? C25 C26 1.372(8) . ? C25 H25A 0.9500 . ? C26 C27 1.381(8) . ? C26 H26A 0.9500 . ? C27 C28 1.389(7) . ? C27 H27A 0.9500 . ? C28 C29 1.425(6) . ? C28 H28A 0.9500 . ? C29 C30 1.474(6) . ? C30 C31 1.407(6) . ? C31 C32 1.367(6) . ? C31 H31A 0.9500 . ? C32 C33 1.460(6) . ? C33 C34 1.388(5) . ? C34 C35 1.387(6) . ? C34 H34A 0.9500 . ? C35 C36 1.380(6) . ? C35 H35A 0.9500 . ? C36 C37 1.388(5) . ? C36 H36A 0.9500 . ? C37 C38 1.467(5) . ? C38 C39 1.379(6) . ? C39 C40 1.414(5) . ? C39 H39A 0.9500 . ? C40 C41 1.451(5) . ? C41 C42 1.404(6) . ? C41 C46 1.419(6) . ? C42 C43 1.387(7) . ? C42 H42A 0.9500 . ? C43 C44 1.405(8) . ? C43 H43A 0.9500 . ? C44 C45 1.382(7) . ? C44 H44A 0.9500 . ? C45 C46 1.407(6) . ? C45 H45A 0.9500 . ? C47 C48 1.389(5) . ? C47 C52 1.419(5) . ? C48 C49 1.364(6) . ? C48 H48A 0.9500 . ? C49 C50 1.415(7) . ? C49 H49A 0.9500 . ? C50 C51 1.369(6) . ? C50 H50A 0.9500 . ? C51 C52 1.399(5) . ? C51 H51A 0.9500 . ? C52 C53 1.460(5) . ? C53 C54 1.397(5) . ? C54 C55 1.384(5) . ? C54 H54A 0.9500 . ? C55 C56 1.475(5) . ? C56 C57 1.400(5) . ? C57 C58 1.361(5) . ? C57 H57A 0.9500 . ? C58 C59 1.392(5) . ? C58 H58A 0.9500 . ? C59 C60 1.375(4) . ? C59 H59A 0.9500 . ? C60 C61 1.465(5) . ? C61 C62 1.399(5) . ? C62 C63 1.390(5) . ? C62 H62A 0.9500 . ? C63 C64 1.454(6) . ? C64 C65B 1.388(13) . ? C64 C69 1.416(6) . ? C64 C65 1.476(12) . ? C65 C66 1.400(14) . ? C65 H65A 0.9500 . ? C66 C67 1.411(12) . ? C66 H66A 0.9500 . ? C67 C68 1.389(14) . ? C67 H67A 0.9500 . ? C68 C69 1.444(12) . ? C68 H68A 0.9500 . ? C65B C66B 1.354(15) . ? C65B H65B 0.9500 . ? C66B C67B 1.353(13) . ? C66B H66B 0.9500 . ? C67B C68B 1.369(15) . ? C67B H67B 0.9500 . ? C68B C69 1.443(12) . ? C68B H68B 0.9500 . ? C70 C71 1.398(6) . ? C70 C75 1.422(6) . ? C71 C72 1.387(7) . ? C71 H71A 0.9500 . ? C72 C73 1.384(7) . ? C72 H72A 0.9500 . ? C73 C74 1.386(7) . ? C73 H73A 0.9500 . ? C74 C75 1.404(6) . ? C74 H74A 0.9500 . ? C75 C76 1.469(6) . ? C76 C77 1.427(5) . ? C77 C78 1.362(5) . ? C77 H77A 0.9500 . ? C78 C79 1.461(5) . ? C79 C80 1.389(5) . ? C80 C81 1.377(5) . ? C80 H80A 0.9500 . ? C81 C82 1.388(5) . ? C81 H81A 0.9500 . ? C82 C83 1.383(5) . ? C82 H82A 0.9500 . ? C83 C84 1.483(5) . ? C84 C85 1.373(5) . ? C85 C86 1.392(5) . ? C85 H85A 0.9500 . ? C86 C87 1.469(5) . ? C87 C92 1.393(5) . ? C87 C88 1.413(6) . ? C88 C89 1.357(6) . ? C88 H88A 0.9500 . ? C89 C90 1.408(7) . ? C89 H89A 0.9500 . ? C90 C91 1.364(6) . ? C90 H90A 0.9500 . ? C91 C92 1.423(5) . ? C91 H91A 0.9500 . ? C93 C94 1.510(6) . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? O1S C1S 1.436(10) . ? O1S H1S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O2S C2S 1.443(9) . ? O2S H2S 0.8400 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? O3S C3S 1.50(2) . ? O20 C100 1.262(11) . ? O21 C100 1.261(12) . ? C100 C101 1.430(14) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 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 O9 Mn1 N4 94.17(11) . . ? O9 Mn1 O3 172.57(10) . . ? N4 Mn1 O3 89.17(11) . . ? O9 Mn1 O11 90.00(11) . . ? N4 Mn1 O11 149.01(10) . . ? O3 Mn1 O11 83.75(11) . . ? O9 Mn1 N2 87.90(13) . . ? N4 Mn1 N2 136.27(12) . . ? O3 Mn1 N2 94.28(12) . . ? O11 Mn1 N2 74.49(11) . . ? O9 Mn1 N3 91.89(14) . . ? N4 Mn1 N3 68.58(12) . . ? O3 Mn1 N3 95.51(14) . . ? O11 Mn1 N3 142.04(12) . . ? N2 Mn1 N3 67.70(13) . . ? O9 Mn1 O10 98.45(11) . . ? N4 Mn1 O10 72.69(10) . . ? O3 Mn1 O10 76.19(10) . . ? O11 Mn1 O10 76.32(10) . . ? N2 Mn1 O10 150.11(10) . . ? N3 Mn1 O10 140.49(11) . . ? O2 Mn2 O13 87.91(11) . . ? O2 Mn2 O10 174.66(11) . . ? O13 Mn2 O10 92.50(10) . . ? O2 Mn2 N5 89.14(12) . . ? O13 Mn2 N5 166.81(12) . . ? O10 Mn2 N5 89.26(11) . . ? O2 Mn2 N19 96.45(12) . 2_656 ? O13 Mn2 N19 87.73(11) . 2_656 ? O10 Mn2 N19 88.89(11) . 2_656 ? N5 Mn2 N19 105.38(12) . 2_656 ? O2 Mn2 Mn5 88.49(9) . . ? O13 Mn2 Mn5 34.78(8) . . ? O10 Mn2 Mn5 88.81(8) . . ? N5 Mn2 Mn5 132.29(10) . . ? N19 Mn2 Mn5 122.23(8) 2_656 . ? O8 Mn3 O13 172.37(11) 2_656 . ? O8 Mn3 N20 87.89(11) 2_656 2_656 ? O13 Mn3 N20 91.81(11) . 2_656 ? O8 Mn3 N12 95.72(11) 2_656 . ? O13 Mn3 N12 84.66(11) . . ? N20 Mn3 N12 176.37(11) 2_656 . ? O8 Mn3 O14 86.12(11) 2_656 . ? O13 Mn3 O14 86.28(10) . . ? N20 Mn3 O14 92.35(11) 2_656 . ? N12 Mn3 O14 88.28(11) . . ? O8 Mn3 O17 93.70(10) 2_656 . ? O13 Mn3 O17 93.93(9) . . ? N20 Mn3 O17 91.64(11) 2_656 . ? N12 Mn3 O17 87.77(11) . . ? O14 Mn3 O17 176.00(9) . . ? O3 Mn4 O16 172.93(11) . . ? O3 Mn4 O12 95.02(13) . . ? O16 Mn4 O12 89.16(12) . . ? O3 Mn4 N6 86.93(13) . . ? O16 Mn4 N6 88.68(12) . . ? O12 Mn4 N6 177.05(13) . . ? O3 Mn4 O15 92.11(13) . . ? O16 Mn4 O15 93.50(13) . . ? O12 Mn4 O15 91.15(14) . . ? N6 Mn4 O15 90.99(14) . . ? O3 Mn4 O10 85.44(11) . . ? O16 Mn4 O10 88.56(11) . . ? O12 Mn4 O10 94.42(12) . . ? N6 Mn4 O10 83.51(11) . . ? O15 Mn4 O10 174.09(12) . . ? O5 Mn5 O13 174.51(11) . . ? O5 Mn5 N11 88.90(13) . . ? O13 Mn5 N11 85.98(12) . . ? O5 Mn5 N7 90.99(13) . . ? O13 Mn5 N7 94.14(12) . . ? N11 Mn5 N7 179.76(13) . . ? O5 Mn5 O16 91.01(12) . . ? O13 Mn5 O16 91.71(10) . . ? N11 Mn5 O16 98.76(11) . . ? N7 Mn5 O16 81.03(11) . . ? O5 Mn5 N8 84.71(12) . . ? O13 Mn5 N8 95.19(11) . . ? N11 Mn5 N8 110.04(12) . . ? N7 Mn5 N8 70.16(12) . . ? O16 Mn5 N8 150.76(10) . . ? O5 Mn5 Mn2 149.66(9) . . ? O13 Mn5 Mn2 35.42(7) . . ? N11 Mn5 Mn2 121.40(9) . . ? N7 Mn5 Mn2 58.72(10) . . ? O16 Mn5 Mn2 86.08(7) . . ? N8 Mn5 Mn2 83.31(8) . . ? O17 Mn6 O4 171.01(11) . . ? O17 Mn6 N10 87.06(12) . . ? O4 Mn6 N10 86.18(12) . . ? O17 Mn6 N14 96.87(12) . . ? O4 Mn6 N14 90.33(12) . . ? N10 Mn6 N14 174.17(12) . . ? O17 Mn6 O18 96.69(11) . . ? O4 Mn6 O18 89.95(12) . . ? N10 Mn6 O18 96.43(11) . . ? N14 Mn6 O18 78.87(11) . . ? O17 Mn6 N13 93.40(10) . . ? O4 Mn6 N13 83.60(12) . . ? N10 Mn6 N13 111.61(12) . . ? N14 Mn6 N13 72.57(11) . . ? O18 Mn6 N13 150.64(10) . . ? O6 Mn7 O18 173.62(11) . . ? O6 Mn7 O7 91.77(12) . . ? O18 Mn7 O7 92.14(11) . . ? O6 Mn7 N15 87.81(12) . . ? O18 Mn7 N15 87.27(12) . . ? O7 Mn7 N15 167.32(12) . . ? O6 Mn7 N16 95.64(12) . . ? O18 Mn7 N16 89.83(12) . . ? O7 Mn7 N16 83.09(12) . . ? N15 Mn7 N16 109.56(13) . . ? O6 Mn7 O19 96.14(16) . . ? O18 Mn7 O19 79.09(16) . . ? O7 Mn7 O19 86.40(15) . . ? N15 Mn7 O19 81.05(16) . . ? N16 Mn7 O19 164.44(15) . . ? C1 O1 H1B 109.5 . . ? C23 O2 Mn2 132.5(2) . . ? C24 O3 Mn4 124.1(3) . . ? C24 O3 Mn1 120.5(2) . . ? Mn4 O3 Mn1 103.23(13) . . ? C46 O4 Mn6 132.4(2) . . ? C47 O5 Mn5 131.2(2) . . ? C69 O6 Mn7 133.5(2) . . ? C70 O7 Mn7 124.3(2) . . ? C92 O8 Mn3 133.9(2) . 2_656 ? Mn1 O9 H9A 115(3) . . ? Mn1 O9 H9B 125(3) . . ? H9A O9 H9B 114(4) . . ? Mn2 O10 Mn4 118.72(12) . . ? Mn2 O10 Mn1 123.94(11) . . ? Mn4 O10 Mn1 89.74(9) . . ? C93 O11 Mn1 134.8(3) . . ? C93 O12 Mn4 127.0(3) . . ? Mn5 O13 Mn3 125.26(12) . . ? Mn5 O13 Mn2 109.81(12) . . ? Mn3 O13 Mn2 120.49(13) . . ? C95 O14 Mn3 118.4(2) . . ? Mn4 O15 H15A 127(2) . . ? Mn4 O15 H15B 122(2) . . ? H15A O15 H15B 94(3) . . ? C96 O16 Mn4 117.7(3) . . ? C96 O16 Mn5 115.1(2) . . ? Mn4 O16 Mn5 118.41(12) . . ? C97 O17 Mn6 118.4(2) . . ? C97 O17 Mn3 114.9(2) . . ? Mn6 O17 Mn3 123.71(11) . . ? Mn7 O18 Mn6 125.12(13) . . ? Mn7 O18 H18 109(3) . . ? Mn6 O18 H18 126(3) . . ? Mn7 O19 H19C 101.6(16) . . ? Mn7 O19 H19B 104.5(17) . . ? H19C O19 H19B 97(4) . . ? C7 N1 N2 113.3(4) . . ? C7 N1 H1A 123.4 . . ? N2 N1 H1A 123.4 . . ? C9 N2 N1 104.3(4) . . ? C9 N2 Mn1 122.4(3) . . ? N1 N2 Mn1 133.2(3) . . ? C10 N3 C14 120.0(6) . . ? C14 N3 C10B 119.5(5) . . ? C10 N3 Mn1 118.5(5) . . ? C14 N3 Mn1 118.9(3) . . ? C10B N3 Mn1 119.4(5) . . ? C15 N4 N5 107.1(3) . . ? C15 N4 Mn1 121.6(3) . . ? N5 N4 Mn1 131.1(2) . . ? N4 N5 C17 110.1(3) . . ? N4 N5 Mn2 120.2(2) . . ? C17 N5 Mn2 129.6(2) . . ? C30 N6 N7 108.7(3) . . ? C30 N6 Mn4 130.1(3) . . ? N7 N6 Mn4 120.9(2) . . ? C32 N7 N6 107.3(3) . . ? C32 N7 Mn5 126.4(3) . . ? N6 N7 Mn5 125.6(2) . . ? C37 N8 C33 117.6(3) . . ? C37 N8 Mn5 130.1(2) . . ? C33 N8 Mn5 111.4(2) . . ? C38 N9 N10 110.5(3) . . ? C38 N9 H9 124.8 . . ? N10 N9 H9 124.8 . . ? C40 N10 N9 106.8(3) . . ? C40 N10 Mn6 131.1(2) . . ? N9 N10 Mn6 120.8(2) . . ? C53 N11 N12 109.5(3) . . ? C53 N11 Mn5 128.7(2) . . ? N12 N11 Mn5 121.6(2) . . ? C55 N12 N11 106.7(3) . . ? C55 N12 Mn3 135.4(2) . . ? N11 N12 Mn3 117.8(2) . . ? C60 N13 C56 118.1(3) . . ? C60 N13 Mn6 112.9(2) . . ? C56 N13 Mn6 127.4(2) . . ? C61 N14 N15 108.6(3) . . ? C61 N14 Mn6 122.5(2) . . ? N15 N14 Mn6 128.3(2) . . ? C63 N15 N14 107.7(3) . . ? C63 N15 Mn7 128.8(2) . . ? N14 N15 Mn7 119.0(2) . . ? N17 N16 C76 106.8(3) . . ? N17 N16 Mn7 130.4(2) . . ? C76 N16 Mn7 120.6(3) . . ? N16 N17 C78 111.9(3) . . ? N16 N17 H17A 124.0 . . ? C78 N17 H17A 124.0 . . ? C83 N18 C79 117.8(3) . . ? C84 N19 N20 106.9(3) . . ? C84 N19 Mn2 134.2(2) . 2_656 ? N20 N19 Mn2 114.4(2) . 2_656 ? C86 N20 N19 109.6(3) . . ? C86 N20 Mn3 130.6(2) . 2_656 ? N19 N20 Mn3 119.2(2) . 2_656 ? O1 C1 C2 120.3(5) . . ? O1 C1 C6 118.2(5) . . ? C2 C1 C6 121.4(5) . . ? C3 C2 C1 120.4(6) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 119.9(6) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 120.4(6) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C4 C5 C6 119.8(6) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C1 C6 C5 117.7(5) . . ? C1 C6 C7 123.9(5) . . ? C5 C6 C7 118.4(5) . . ? N1 C7 C8 105.7(4) . . ? N1 C7 C6 122.2(4) . . ? C8 C7 C6 132.2(4) . . ? C7 C8 C9 106.1(4) . . ? C7 C8 H8A 127.0 . . ? C9 C8 H8A 127.0 . . ? N2 C9 C8 110.6(4) . . ? N2 C9 C10 112.7(5) . . ? C8 C9 C10 134.7(6) . . ? N2 C9 C10B 115.1(5) . . ? C8 C9 C10B 131.7(6) . . ? N3 C10 C11 123.6(10) . . ? N3 C10 C9 111.9(8) . . ? C11 C10 C9 124.0(10) . . ? C12 C11 C10 119.9(11) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 119.2(9) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C12 C13 C14 117.3(9) . . ? C12 C13 H13A 121.4 . . ? C14 C13 H13A 121.4 . . ? C11B C10B N3 122.8(9) . . ? C11B C10B C9 126.4(9) . . ? N3 C10B C9 107.1(7) . . ? C10B C11B C12B 119.0(9) . . ? C10B C11B H11B 120.5 . . ? C12B C11B H11B 120.5 . . ? C11B C12B C13B 120.2(7) . . ? C11B C12B H12B 119.9 . . ? C13B C12B H12B 119.9 . . ? C12B C13B C14 118.4(7) . . ? C12B C13B H13B 120.8 . . ? C14 C13B H13B 120.8 . . ? N3 C14 C15 114.6(4) . . ? N3 C14 C13B 118.7(5) . . ? C15 C14 C13B 122.4(5) . . ? N3 C14 C13 118.1(6) . . ? C15 C14 C13 119.7(6) . . ? C13B C14 C13 46.4(5) . . ? N4 C15 C16 110.4(4) . . ? N4 C15 C14 116.2(4) . . ? C16 C15 C14 133.4(4) . . ? C17 C16 C15 105.5(3) . . ? C17 C16 H16A 127.3 . . ? C15 C16 H16A 127.3 . . ? N5 C17 C16 106.9(3) . . ? N5 C17 C18 122.3(3) . . ? C16 C17 C18 130.4(3) . . ? C19 C18 C23 118.0(4) . . ? C19 C18 C17 119.9(4) . . ? C23 C18 C17 121.5(3) . . ? C20 C19 C18 122.4(4) . . ? C20 C19 H19A 118.8 . . ? C18 C19 H19A 118.8 . . ? C19 C20 C21 119.1(4) . . ? C19 C20 H20A 120.5 . . ? C21 C20 H20A 120.5 . . ? C22 C21 C20 119.7(4) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C21 C22 C23 121.7(4) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? O2 C23 C22 116.9(3) . . ? O2 C23 C18 124.1(3) . . ? C22 C23 C18 119.0(3) . . ? O3 C24 C29 123.3(4) . . ? O3 C24 C25 117.2(4) . . ? C29 C24 C25 119.4(4) . . ? C26 C25 C24 120.5(5) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C27 121.1(5) . . ? C25 C26 H26A 119.4 . . ? C27 C26 H26A 119.4 . . ? C26 C27 C28 119.3(5) . . ? C26 C27 H27A 120.3 . . ? C28 C27 H27A 120.3 . . ? C27 C28 C29 120.0(5) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C24 C29 C28 119.7(4) . . ? C24 C29 C30 122.1(4) . . ? C28 C29 C30 118.2(4) . . ? N6 C30 C31 108.7(3) . . ? N6 C30 C29 119.7(4) . . ? C31 C30 C29 131.6(4) . . ? C32 C31 C30 105.0(3) . . ? C32 C31 H31A 127.5 . . ? C30 C31 H31A 127.5 . . ? N7 C32 C31 110.2(4) . . ? N7 C32 C33 116.2(3) . . ? C31 C32 C33 133.6(4) . . ? N8 C33 C34 121.9(4) . . ? N8 C33 C32 114.6(3) . . ? C34 C33 C32 123.5(4) . . ? C35 C34 C33 119.5(4) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C36 C35 C34 119.2(4) . . ? C36 C35 H35A 120.4 . . ? C34 C35 H35A 120.4 . . ? C35 C36 C37 118.6(4) . . ? C35 C36 H36A 120.7 . . ? C37 C36 H36A 120.7 . . ? N8 C37 C36 123.1(4) . . ? N8 C37 C38 114.8(3) . . ? C36 C37 C38 122.1(4) . . ? N9 C38 C39 107.8(3) . . ? N9 C38 C37 119.8(4) . . ? C39 C38 C37 132.4(4) . . ? C38 C39 C40 105.4(3) . . ? C38 C39 H39A 127.3 . . ? C40 C39 H39A 127.3 . . ? N10 C40 C39 109.4(3) . . ? N10 C40 C41 121.1(3) . . ? C39 C40 C41 129.4(4) . . ? C42 C41 C46 119.9(4) . . ? C42 C41 C40 119.5(4) . . ? C46 C41 C40 120.6(4) . . ? C43 C42 C41 121.5(5) . . ? C43 C42 H42A 119.2 . . ? C41 C42 H42A 119.2 . . ? C42 C43 C44 118.2(5) . . ? C42 C43 H43A 120.9 . . ? C44 C43 H43A 120.9 . . ? C45 C44 C43 121.3(4) . . ? C45 C44 H44A 119.4 . . ? C43 C44 H44A 119.4 . . ? C44 C45 C46 121.2(5) . . ? C44 C45 H45A 119.4 . . ? C46 C45 H45A 119.4 . . ? O4 C46 C45 118.0(4) . . ? O4 C46 C41 124.1(3) . . ? C45 C46 C41 117.9(4) . . ? O5 C47 C48 118.6(4) . . ? O5 C47 C52 122.3(3) . . ? C48 C47 C52 119.1(4) . . ? C49 C48 C47 122.0(4) . . ? C49 C48 H48A 119.0 . . ? C47 C48 H48A 119.0 . . ? C48 C49 C50 119.3(4) . . ? C48 C49 H49A 120.3 . . ? C50 C49 H49A 120.3 . . ? C51 C50 C49 119.4(4) . . ? C51 C50 H50A 120.3 . . ? C49 C50 H50A 120.3 . . ? C50 C51 C52 121.9(4) . . ? C50 C51 H51A 119.1 . . ? C52 C51 H51A 119.1 . . ? C51 C52 C47 118.1(4) . . ? C51 C52 C53 120.0(3) . . ? C47 C52 C53 121.8(3) . . ? N11 C53 C54 108.1(3) . . ? N11 C53 C52 122.3(3) . . ? C54 C53 C52 129.5(3) . . ? C55 C54 C53 105.1(3) . . ? C55 C54 H54A 127.4 . . ? C53 C54 H54A 127.4 . . ? N12 C55 C54 110.5(3) . . ? N12 C55 C56 120.9(3) . . ? C54 C55 C56 128.4(3) . . ? N13 C56 C57 121.9(3) . . ? N13 C56 C55 115.2(3) . . ? C57 C56 C55 122.9(3) . . ? C58 C57 C56 119.0(3) . . ? C58 C57 H57A 120.5 . . ? C56 C57 H57A 120.5 . . ? C57 C58 C59 119.3(3) . . ? C57 C58 H58A 120.3 . . ? C59 C58 H58A 120.3 . . ? C60 C59 C58 119.0(3) . . ? C60 C59 H59A 120.5 . . ? C58 C59 H59A 120.5 . . ? N13 C60 C59 122.5(3) . . ? N13 C60 C61 112.9(3) . . ? C59 C60 C61 124.7(3) . . ? N14 C61 C62 109.4(3) . . ? N14 C61 C60 116.7(3) . . ? C62 C61 C60 133.8(3) . . ? C63 C62 C61 104.9(3) . . ? C63 C62 H62A 127.6 . . ? C61 C62 H62A 127.6 . . ? N15 C63 C62 109.5(3) . . ? N15 C63 C64 121.7(3) . . ? C62 C63 C64 128.8(4) . . ? C65B C64 C69 116.0(6) . . ? C65B C64 C63 121.4(6) . . ? C69 C64 C63 120.9(4) . . ? C69 C64 C65 121.8(6) . . ? C63 C64 C65 115.8(5) . . ? C66 C65 C64 119.7(8) . . ? C66 C65 H65A 120.1 . . ? C64 C65 H65A 120.1 . . ? C65 C66 C67 118.2(8) . . ? C65 C66 H66A 120.9 . . ? C67 C66 H66A 120.9 . . ? C68 C67 C66 121.6(8) . . ? C68 C67 H67A 119.2 . . ? C66 C67 H67A 119.2 . . ? C67 C68 C69 122.9(9) . . ? C67 C68 H68A 118.6 . . ? C69 C68 H68A 118.6 . . ? C66B C65B C64 122.8(10) . . ? C66B C65B H65B 118.6 . . ? C64 C65B H65B 118.6 . . ? C67B C66B C65B 121.7(9) . . ? C67B C66B H66B 119.2 . . ? C65B C66B H66B 119.2 . . ? C66B C67B C68B 119.5(9) . . ? C66B C67B H67B 120.2 . . ? C68B C67B H67B 120.2 . . ? C67B C68B C69 119.6(9) . . ? C67B C68B H68B 120.2 . . ? C69 C68B H68B 120.2 . . ? O6 C69 C64 123.6(4) . . ? O6 C69 C68B 116.0(6) . . ? C64 C69 C68B 119.6(6) . . ? O6 C69 C68 118.7(6) . . ? C64 C69 C68 114.9(6) . . ? O7 C70 C71 119.3(4) . . ? O7 C70 C75 122.2(4) . . ? C71 C70 C75 118.5(4) . . ? C72 C71 C70 121.7(4) . . ? C72 C71 H71A 119.2 . . ? C70 C71 H71A 119.2 . . ? C73 C72 C71 120.5(5) . . ? C73 C72 H72A 119.7 . . ? C71 C72 H72A 119.7 . . ? C72 C73 C74 118.5(4) . . ? C72 C73 H73A 120.8 . . ? C74 C73 H73A 120.8 . . ? C73 C74 C75 122.7(4) . . ? C73 C74 H74A 118.7 . . ? C75 C74 H74A 118.7 . . ? C74 C75 C70 118.1(4) . . ? C74 C75 C76 118.8(4) . . ? C70 C75 C76 123.0(4) . . ? N16 C76 C77 108.2(4) . . ? N16 C76 C75 123.0(3) . . ? C77 C76 C75 128.6(3) . . ? C78 C77 C76 106.6(3) . . ? C78 C77 H77A 126.7 . . ? C76 C77 H77A 126.7 . . ? C77 C78 N17 106.4(3) . . ? C77 C78 C79 130.7(3) . . ? N17 C78 C79 122.5(3) . . ? N18 C79 C80 122.3(3) . . ? N18 C79 C78 116.6(3) . . ? C80 C79 C78 121.0(3) . . ? C81 C80 C79 119.2(3) . . ? C81 C80 H80A 120.4 . . ? C79 C80 H80A 120.4 . . ? C80 C81 C82 118.5(4) . . ? C80 C81 H81A 120.7 . . ? C82 C81 H81A 120.7 . . ? C83 C82 C81 119.5(4) . . ? C83 C82 H82A 120.3 . . ? C81 C82 H82A 120.3 . . ? N18 C83 C82 122.6(3) . . ? N18 C83 C84 118.7(3) . . ? C82 C83 C84 118.7(3) . . ? N19 C84 C85 110.0(3) . . ? N19 C84 C83 117.4(3) . . ? C85 C84 C83 132.4(3) . . ? C84 C85 C86 105.7(3) . . ? C84 C85 H85A 127.2 . . ? C86 C85 H85A 127.2 . . ? N20 C86 C85 107.7(3) . . ? N20 C86 C87 121.5(3) . . ? C85 C86 C87 130.8(3) . . ? C92 C87 C88 119.5(3) . . ? C92 C87 C86 121.1(3) . . ? C88 C87 C86 119.4(3) . . ? C89 C88 C87 121.8(4) . . ? C89 C88 H88A 119.1 . . ? C87 C88 H88A 119.1 . . ? C88 C89 C90 119.0(4) . . ? C88 C89 H89A 120.5 . . ? C90 C89 H89A 120.5 . . ? C91 C90 C89 120.4(4) . . ? C91 C90 H90A 119.8 . . ? C89 C90 H90A 119.8 . . ? C90 C91 C92 121.2(4) . . ? C90 C91 H91A 119.4 . . ? C92 C91 H91A 119.4 . . ? O8 C92 C87 124.7(3) . . ? O8 C92 C91 117.3(3) . . ? C87 C92 C91 118.0(3) . . ? O11 C93 O12 124.7(4) . . ? O11 C93 C94 120.6(4) . . ? O12 C93 C94 114.7(4) . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? O14 C95 H95A 109.5 . . ? O14 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? O14 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? O16 C96 H96A 109.5 . . ? O16 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? O16 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? O17 C97 H97A 109.5 . . ? O17 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? O17 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O21 C100 O20 124.5(11) . . ? O21 C100 C101 116.3(11) . . ? O20 C100 C101 119.0(11) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 1.451 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.099