# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H56 Mn3 N4 O19' _chemical_formula_weight 1446.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.643(9) _cell_length_b 10.850(5) _cell_length_c 34.239(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.091(11) _cell_angle_gamma 90.00 _cell_volume 8647(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 22.41 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2972 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6337 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details 'Sheldrick, G. M. (2008). SADABS' _exptl_special_details ; The value of Theta(max) in compound 1 is relatively low. This is mainly caused by very weak diffraction intensity of data 1. Then less high Theta(max) reflection data were collected for refinement. ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15843 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 22.41 _reflns_number_total 5415 _reflns_number_gt 3427 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1554P)^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_number_reflns 5415 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.2520 _refine_ls_wR_factor_gt 0.2307 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.75329(14) 0.2613(3) 1.00091(9) 0.0429(5) Uiso 0.50 1 d P . . Mn2 Mn 1.17615(5) 1.02132(9) 0.99911(3) 0.0794(5) Uani 1 1 d . . . N1 N 1.1083(3) 0.9785(6) 1.03428(17) 0.099(2) Uani 1 1 d . . . N2 N 1.1312(4) 1.1954(7) 1.00618(18) 0.112(3) Uani 1 1 d . . . C1 C 0.9226(3) 0.5118(7) 0.78020(19) 0.082(2) Uani 1 1 d . . . C2 C 0.9559(4) 0.6096(7) 0.80444(18) 0.095(2) Uani 1 1 d . . . H2A H 0.9812 0.6513 0.7892 0.115 Uiso 1 1 calc R . . H2B H 0.9302 0.6700 0.8128 0.115 Uiso 1 1 calc R . . C3 C 0.8823(4) 0.4492(8) 0.8043(2) 0.114(3) Uani 1 1 d . . . H3A H 0.8586 0.3887 0.7882 0.137 Uiso 1 1 calc R . . H3B H 0.9042 0.4078 0.8272 0.137 Uiso 1 1 calc R . . C4 C 0.8870(4) 0.5764(7) 0.74500(18) 0.092(2) Uani 1 1 d . . . H4A H 0.8602 0.6335 0.7538 0.111 Uiso 1 1 calc R . . H4B H 0.9116 0.6219 0.7302 0.111 Uiso 1 1 calc R . . C5 C 0.9623(3) 0.4204(7) 0.76815(19) 0.086(2) Uani 1 1 d . . . H5A H 0.9826 0.3768 0.7911 0.103 Uiso 1 1 calc R . . H5B H 0.9415 0.3611 0.7498 0.103 Uiso 1 1 calc R . . C6 C 1.0209(4) 0.6196(10) 0.8640(2) 0.102(3) Uani 1 1 d . . . C7 C 1.0277(4) 0.7459(9) 0.8616(2) 0.109(3) Uani 1 1 d . . . H7A H 1.0079 0.7884 0.8399 0.131 Uiso 1 1 calc R . . C8 C 1.0636(4) 0.8099(9) 0.8910(2) 0.105(3) Uani 1 1 d . . . H8A H 1.0687 0.8947 0.8898 0.126 Uiso 1 1 calc R . . C9 C 1.0918(3) 0.7383(13) 0.9229(2) 0.105(3) Uani 1 1 d . . . C10 C 1.0848(5) 0.6135(13) 0.9229(3) 0.135(4) Uani 1 1 d . . . H10A H 1.1054 0.5676 0.9435 0.162 Uiso 1 1 calc R . . C11 C 1.0503(5) 0.5565(11) 0.8950(3) 0.127(3) Uani 1 1 d . . . H11A H 1.0459 0.4715 0.8963 0.153 Uiso 1 1 calc R . . C12 C 1.1281(5) 0.8106(18) 0.9530(3) 0.152(6) Uani 1 1 d . . . C13 C 0.8246(5) 0.5252(10) 0.8490(3) 0.140(4) Uani 1 1 d . . . C14 C 0.8046(6) 0.6275(10) 0.8642(4) 0.188(6) Uani 1 1 d . . . H14A H 0.8067 0.7025 0.8514 0.225 Uiso 1 1 calc R . . C15 C 0.7823(6) 0.6239(8) 0.8970(4) 0.186(7) Uani 1 1 d . . . H15A H 0.7701 0.6957 0.9078 0.223 Uiso 1 1 calc R . . C16 C 0.7774(5) 0.5126(7) 0.9145(2) 0.111(3) Uani 1 1 d . . . C17 C 0.8004(4) 0.4129(7) 0.9012(2) 0.094(2) Uani 1 1 d . . . H17A H 0.8005 0.3394 0.9153 0.113 Uiso 1 1 calc R . . C18 C 0.8237(4) 0.4154(7) 0.8676(2) 0.099(3) Uani 1 1 d . . . H18A H 0.8385 0.3445 0.8578 0.119 Uiso 1 1 calc R . . C19 C 0.7496(5) 0.5132(8) 0.9496(3) 0.122(4) Uani 1 1 d . . . C20 C 0.8329(4) 0.5093(8) 0.6847(2) 0.097(3) Uani 1 1 d . . . C21 C 0.8129(5) 0.4132(8) 0.6627(3) 0.151(5) Uani 1 1 d . . . H21A H 0.8179 0.3343 0.6734 0.181 Uiso 1 1 calc R . . C22 C 0.7856(5) 0.4280(8) 0.6251(3) 0.137(4) Uani 1 1 d . . . H22A H 0.7703 0.3597 0.6105 0.164 Uiso 1 1 calc R . . C23 C 0.7801(3) 0.5424(7) 0.6080(2) 0.083(2) Uani 1 1 d . . . C24 C 0.8008(3) 0.6382(7) 0.63041(19) 0.0783(19) Uani 1 1 d . . . H24A H 0.7967 0.7167 0.6193 0.094 Uiso 1 1 calc R . . C25 C 0.8280(3) 0.6263(7) 0.6690(2) 0.089(2) Uani 1 1 d . . . H25A H 0.8425 0.6944 0.6839 0.107 Uiso 1 1 calc R . . C26 C 0.7498(4) 0.5554(8) 0.5672(2) 0.089(2) Uani 1 1 d . . . C27 C 1.0935(5) 0.8652(9) 1.0446(3) 0.118(3) Uani 1 1 d . . . H27A H 1.1186 0.8008 1.0420 0.142 Uiso 1 1 calc R . . C28 C 1.0446(7) 0.8376(13) 1.0587(4) 0.163(5) Uani 1 1 d . . . H28A H 1.0372 0.7578 1.0663 0.196 Uiso 1 1 calc R . . C29 C 1.0059(6) 0.9333(19) 1.0613(4) 0.172(5) Uani 1 1 d . . . H29A H 0.9717 0.9194 1.0706 0.207 Uiso 1 1 calc R . . C30 C 1.0201(6) 1.0477(16) 1.0498(4) 0.157(5) Uani 1 1 d . . . H30A H 0.9945 1.1125 1.0503 0.189 Uiso 1 1 calc R . . C31 C 1.0710(5) 1.0689(10) 1.0375(2) 0.113(3) Uani 1 1 d . . . C32 C 1.1494(6) 1.3038(9) 0.9954(3) 0.144(4) Uani 1 1 d . . . H32A H 1.1790 1.3048 0.9808 0.173 Uiso 1 1 calc R . . C33 C 1.1273(9) 1.4131(12) 1.0044(4) 0.179(7) Uani 1 1 d . . . H33A H 1.1410 1.4878 0.9966 0.215 Uiso 1 1 calc R . . C34 C 1.0858(11) 1.4071(15) 1.0248(5) 0.215(10) Uani 1 1 d . . . H34A H 1.0701 1.4811 1.0316 0.258 Uiso 1 1 calc R . . C35 C 1.0627(7) 1.2974(14) 1.0373(3) 0.184(7) Uani 1 1 d . . . H35A H 1.0326 1.2954 1.0515 0.221 Uiso 1 1 calc R . . C36 C 1.0901(4) 1.1909(8) 1.0262(3) 0.104(3) Uani 1 1 d . . . O1 O 0.9880(3) 0.5504(5) 0.83754(16) 0.120(2) Uani 1 1 d . . . O2 O 0.8483(3) 0.5410(7) 0.81632(19) 0.155(3) Uani 1 1 d . . . O3 O 0.8574(3) 0.4831(5) 0.72147(17) 0.124(2) Uani 1 1 d . . . O4 O 1.0000 0.4873(7) 0.7500 0.107(2) Uani 1 2 d S . . O5 O 1.1249(3) 0.9218(9) 0.95388(18) 0.135(3) Uani 1 1 d . . . O6 O 1.1610(3) 0.7447(7) 0.97951(18) 0.138(3) Uani 1 1 d . . . O7 O 0.7540(3) 0.4171(5) 0.97003(14) 0.118(2) Uani 1 1 d . . . O8 O 0.7196(4) 0.5987(5) 0.95633(19) 0.150(3) Uani 1 1 d . . . O9 O 0.7411(3) 0.6582(5) 0.55356(13) 0.1039(18) Uani 1 1 d . . . O10 O 0.7335(3) 0.4583(5) 0.54878(15) 0.1053(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn2 0.1059(10) 0.0762(7) 0.0603(6) 0.0163(5) 0.0263(6) 0.0355(6) N1 0.133(6) 0.093(4) 0.076(4) 0.011(3) 0.034(4) 0.034(4) N2 0.170(8) 0.104(5) 0.068(4) 0.012(4) 0.037(4) 0.064(5) C1 0.094(5) 0.100(5) 0.056(4) 0.003(4) 0.027(4) 0.007(4) C2 0.122(7) 0.116(6) 0.050(4) 0.012(4) 0.019(4) 0.038(5) C3 0.137(8) 0.137(7) 0.078(5) 0.039(5) 0.047(5) 0.018(6) C4 0.102(6) 0.125(6) 0.054(4) 0.020(4) 0.025(4) 0.004(5) C5 0.103(6) 0.096(5) 0.063(4) 0.012(4) 0.031(4) 0.002(4) C6 0.110(7) 0.132(8) 0.061(5) 0.016(5) 0.008(4) 0.051(6) C7 0.121(8) 0.139(8) 0.058(5) 0.001(5) -0.009(5) 0.058(6) C8 0.090(6) 0.156(7) 0.064(5) -0.008(5) 0.002(4) 0.045(5) C9 0.063(5) 0.209(11) 0.040(4) -0.010(5) 0.000(4) 0.031(6) C10 0.135(10) 0.164(11) 0.099(8) 0.031(7) 0.002(7) 0.049(8) C11 0.134(9) 0.158(8) 0.082(6) 0.025(6) -0.004(6) 0.041(7) C12 0.094(8) 0.296(17) 0.071(7) 0.002(10) 0.031(6) 0.090(11) C13 0.155(10) 0.165(9) 0.124(7) 0.083(7) 0.093(7) 0.059(7) C14 0.252(15) 0.120(8) 0.237(13) 0.108(8) 0.168(12) 0.100(9) C15 0.313(17) 0.098(6) 0.204(11) 0.077(7) 0.207(12) 0.072(8) C16 0.178(10) 0.072(5) 0.103(6) 0.037(4) 0.079(6) 0.029(5) C17 0.138(7) 0.073(5) 0.080(5) 0.025(4) 0.043(5) 0.008(4) C18 0.131(7) 0.099(5) 0.082(5) 0.033(4) 0.058(5) 0.011(5) C19 0.189(11) 0.081(6) 0.119(7) 0.014(5) 0.090(7) 0.004(6) C20 0.104(6) 0.109(6) 0.076(5) 0.043(5) 0.010(4) -0.021(5) C21 0.238(13) 0.083(6) 0.105(7) 0.039(5) -0.046(7) -0.055(7) C22 0.206(11) 0.075(5) 0.108(7) 0.030(5) -0.033(7) -0.035(6) C23 0.089(6) 0.085(5) 0.073(4) 0.012(4) 0.006(4) -0.013(4) C24 0.083(5) 0.085(5) 0.069(4) 0.027(4) 0.019(4) 0.003(4) C25 0.099(6) 0.089(5) 0.077(5) 0.014(4) 0.009(4) -0.002(4) C26 0.117(7) 0.093(6) 0.061(4) 0.020(4) 0.030(4) 0.022(5) C27 0.144(9) 0.111(7) 0.117(7) 0.006(5) 0.071(6) 0.027(6) C28 0.164(13) 0.186(12) 0.161(10) 0.031(8) 0.089(10) 0.013(10) C29 0.141(12) 0.239(16) 0.160(11) 0.027(11) 0.088(9) 0.023(12) C30 0.124(10) 0.219(14) 0.142(9) 0.000(9) 0.061(8) 0.062(10) C31 0.123(8) 0.143(8) 0.079(5) 0.005(5) 0.030(5) 0.066(7) C32 0.245(14) 0.083(6) 0.099(6) 0.031(5) 0.018(7) 0.047(7) C33 0.32(2) 0.090(8) 0.136(11) 0.008(7) 0.050(11) 0.055(10) C34 0.34(3) 0.113(11) 0.164(14) -0.021(10) -0.024(13) 0.123(15) C35 0.294(19) 0.150(10) 0.112(8) -0.020(8) 0.049(9) 0.121(12) C36 0.116(8) 0.105(7) 0.092(6) 0.010(5) 0.017(5) 0.061(6) O1 0.153(6) 0.121(4) 0.072(3) 0.011(3) -0.023(4) 0.043(4) O2 0.168(6) 0.184(6) 0.142(5) 0.103(5) 0.113(5) 0.087(5) O3 0.149(6) 0.122(4) 0.087(4) 0.042(3) -0.020(4) -0.049(4) O4 0.110(6) 0.113(5) 0.114(6) 0.000 0.068(5) 0.000 O5 0.079(4) 0.241(8) 0.077(4) -0.036(5) -0.011(3) 0.049(5) O6 0.078(4) 0.244(8) 0.086(4) 0.040(4) 0.000(3) 0.011(4) O7 0.207(7) 0.077(3) 0.080(3) 0.018(3) 0.056(4) -0.004(3) O8 0.254(9) 0.081(4) 0.149(6) 0.011(3) 0.131(6) 0.020(5) O9 0.171(6) 0.089(3) 0.057(3) 0.016(2) 0.038(3) 0.036(3) O10 0.149(5) 0.081(3) 0.082(3) 0.009(3) 0.007(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 Mn1 0.292(6) 7_657 ? Mn1 O7 1.995(6) . ? Mn1 O6 2.021(7) 5_767 ? Mn1 O9 2.068(6) 6_566 ? Mn1 O6 2.185(7) 3_445 ? Mn1 O7 2.197(6) 7_657 ? Mn1 O9 2.199(6) 4_646 ? Mn2 O10 1.993(6) 8_566 ? Mn2 O5 2.092(7) . ? Mn2 O8 2.106(6) 3 ? Mn2 N2 2.201(6) . ? Mn2 N1 2.217(7) . ? Mn2 O7 2.510(6) 3 ? Mn2 C19 2.633(10) 3 ? N1 C31 1.336(10) . ? N1 C27 1.342(10) . ? N2 C36 1.286(12) . ? N2 C32 1.327(12) . ? C1 C5 1.473(10) . ? C1 C2 1.485(10) . ? C1 C4 1.515(9) . ? C1 C3 1.525(10) . ? C2 O1 1.404(8) . ? C3 O2 1.386(10) . ? C4 O3 1.402(9) . ? C5 O4 1.380(7) . ? C6 O1 1.320(10) . ? C6 C11 1.349(11) . ? C6 C7 1.383(11) . ? C7 C8 1.383(12) . ? C8 C9 1.409(12) . ? C9 C10 1.364(13) . ? C9 C12 1.452(17) . ? C10 C11 1.298(14) . ? C12 O5 1.209(16) . ? C12 O6 1.301(12) . ? C13 O2 1.347(9) . ? C13 C14 1.347(13) . ? C13 C18 1.354(11) . ? C14 C15 1.321(12) . ? C15 C16 1.362(10) . ? C16 C17 1.326(10) . ? C16 C19 1.466(11) . ? C17 C18 1.362(9) . ? C19 O8 1.215(10) . ? C19 O7 1.250(9) . ? C19 Mn2 2.633(10) 3_445 ? C20 O3 1.321(9) . ? C20 C21 1.325(11) . ? C20 C25 1.375(9) . ? C21 C22 1.345(11) . ? C22 C23 1.368(10) . ? C23 C24 1.334(9) . ? C23 C26 1.461(10) . ? C24 C25 1.369(9) . ? C26 O9 1.214(8) . ? C26 O10 1.254(9) . ? C27 C28 1.362(15) . ? C28 C29 1.398(18) . ? C29 C30 1.362(18) . ? C30 C31 1.363(16) . ? C31 C36 1.471(14) . ? C32 C33 1.353(15) . ? C33 C34 1.30(2) . ? C34 C35 1.41(2) . ? C35 C36 1.409(13) . ? O4 C5 1.380(7) 2_756 ? O6 Mn1 2.021(7) 5_767 ? O6 Mn1 2.185(7) 3 ? O7 Mn1 2.197(6) 7_657 ? O7 Mn2 2.510(6) 3_445 ? O8 Mn2 2.106(5) 3_445 ? O9 Mn1 2.068(6) 6_565 ? O9 Mn1 2.199(6) 4_656 ? O10 Mn2 1.993(6) 8_465 ? 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 Mn1 Mn1 O7 130.8(14) 7_657 . ? Mn1 Mn1 O6 120.6(14) 7_657 5_767 ? O7 Mn1 O6 95.9(3) . 5_767 ? Mn1 Mn1 O9 113.1(13) 7_657 6_566 ? O7 Mn1 O9 96.9(2) . 6_566 ? O6 Mn1 O9 90.5(3) 5_767 6_566 ? Mn1 Mn1 O6 52.8(13) 7_657 3_445 ? O7 Mn1 O6 89.6(3) . 3_445 ? O6 Mn1 O6 173.40(16) 5_767 3_445 ? O9 Mn1 O6 92.5(3) 6_566 3_445 ? Mn1 Mn1 O7 43.4(12) 7_657 7_657 ? O7 Mn1 O7 174.23(17) . 7_657 ? O6 Mn1 O7 88.6(3) 5_767 7_657 ? O9 Mn1 O7 86.7(2) 6_566 7_657 ? O6 Mn1 O7 85.8(3) 3_445 7_657 ? Mn1 Mn1 O9 59.9(13) 7_657 4_646 ? O7 Mn1 O9 88.5(2) . 4_646 ? O6 Mn1 O9 93.4(3) 5_767 4_646 ? O9 Mn1 O9 172.98(15) 6_566 4_646 ? O6 Mn1 O9 83.0(3) 3_445 4_646 ? O7 Mn1 O9 87.5(2) 7_657 4_646 ? O10 Mn2 O5 155.3(3) 8_566 . ? O10 Mn2 O8 102.0(3) 8_566 3 ? O5 Mn2 O8 88.9(3) . 3 ? O10 Mn2 N2 94.6(2) 8_566 . ? O5 Mn2 N2 107.3(3) . . ? O8 Mn2 N2 92.2(3) 3 . ? O10 Mn2 N1 90.5(3) 8_566 . ? O5 Mn2 N1 85.0(3) . . ? O8 Mn2 N1 161.6(3) 3 . ? N2 Mn2 N1 73.2(3) . . ? O10 Mn2 O7 87.2(2) 8_566 3 ? O5 Mn2 O7 81.0(2) . 3 ? O8 Mn2 O7 54.7(2) 3 3 ? N2 Mn2 O7 146.3(3) . 3 ? N1 Mn2 O7 140.5(2) . 3 ? O10 Mn2 C19 97.3(3) 8_566 3 ? O5 Mn2 C19 82.4(3) . 3 ? O8 Mn2 C19 26.9(2) 3 3 ? N2 Mn2 C19 119.0(3) . 3 ? N1 Mn2 C19 164.7(3) . 3 ? O7 Mn2 C19 28.0(2) 3 3 ? C31 N1 C27 116.4(9) . . ? C31 N1 Mn2 116.2(6) . . ? C27 N1 Mn2 125.6(5) . . ? C36 N2 C32 119.6(8) . . ? C36 N2 Mn2 116.8(6) . . ? C32 N2 Mn2 123.0(8) . . ? C5 C1 C2 109.6(7) . . ? C5 C1 C4 112.4(6) . . ? C2 C1 C4 106.2(6) . . ? C5 C1 C3 109.9(6) . . ? C2 C1 C3 109.6(6) . . ? C4 C1 C3 108.9(7) . . ? O1 C2 C1 106.4(6) . . ? O2 C3 C1 106.9(7) . . ? O3 C4 C1 105.9(6) . . ? O4 C5 C1 105.4(6) . . ? O1 C6 C11 114.3(10) . . ? O1 C6 C7 125.7(7) . . ? C11 C6 C7 120.0(10) . . ? C6 C7 C8 121.1(8) . . ? C7 C8 C9 115.6(9) . . ? C10 C9 C8 120.4(9) . . ? C10 C9 C12 126.4(11) . . ? C8 C9 C12 113.1(12) . . ? C11 C10 C9 122.2(10) . . ? C10 C11 C6 120.5(11) . . ? O5 C12 O6 124.2(14) . . ? O5 C12 C9 121.7(11) . . ? O6 C12 C9 114.0(14) . . ? O2 C13 C14 116.3(9) . . ? O2 C13 C18 123.1(9) . . ? C14 C13 C18 120.5(8) . . ? C15 C14 C13 121.6(8) . . ? C14 C15 C16 118.5(9) . . ? C17 C16 C15 120.0(7) . . ? C17 C16 C19 123.6(7) . . ? C15 C16 C19 116.2(7) . . ? C16 C17 C18 121.6(6) . . ? C13 C18 C17 117.3(8) . . ? O8 C19 O7 121.6(8) . . ? O8 C19 C16 121.3(8) . . ? O7 C19 C16 116.8(8) . . ? O8 C19 Mn2 51.6(4) . 3_445 ? O7 C19 Mn2 70.5(5) . 3_445 ? C16 C19 Mn2 165.5(9) . 3_445 ? O3 C20 C21 115.2(7) . . ? O3 C20 C25 124.4(8) . . ? C21 C20 C25 120.4(7) . . ? C20 C21 C22 120.9(8) . . ? C21 C22 C23 120.8(8) . . ? C24 C23 C22 117.6(7) . . ? C24 C23 C26 122.9(7) . . ? C22 C23 C26 119.4(8) . . ? C23 C24 C25 122.9(6) . . ? C24 C25 C20 117.3(7) . . ? O9 C26 O10 124.2(7) . . ? O9 C26 C23 118.6(8) . . ? O10 C26 C23 117.2(7) . . ? N1 C27 C28 124.8(10) . . ? C27 C28 C29 117.8(13) . . ? C30 C29 C28 117.4(13) . . ? C29 C30 C31 121.3(12) . . ? N1 C31 C30 122.2(11) . . ? N1 C31 C36 113.7(9) . . ? C30 C31 C36 124.1(10) . . ? N2 C32 C33 123.8(13) . . ? C34 C33 C32 115.9(15) . . ? C33 C34 C35 125.0(13) . . ? C34 C35 C36 113.0(14) . . ? N2 C36 C35 122.6(12) . . ? N2 C36 C31 118.0(7) . . ? C35 C36 C31 119.4(12) . . ? C6 O1 C2 117.6(7) . . ? C13 O2 C3 120.2(7) . . ? C20 O3 C4 118.9(6) . . ? C5 O4 C5 116.5(8) 2_756 . ? C12 O5 Mn2 120.2(8) . . ? C12 O6 Mn1 133.7(8) . 5_767 ? C12 O6 Mn1 128.9(9) . 3 ? Mn1 O6 Mn1 6.60(16) 5_767 3 ? C19 O7 Mn1 174.7(8) . . ? C19 O7 Mn1 169.5(7) . 7_657 ? Mn1 O7 Mn1 5.77(17) . 7_657 ? C19 O7 Mn2 81.5(5) . 3_445 ? Mn1 O7 Mn2 95.5(2) . 3_445 ? Mn1 O7 Mn2 95.5(2) 7_657 3_445 ? C19 O8 Mn2 101.5(5) . 3_445 ? C26 O9 Mn1 133.1(4) . 6_565 ? C26 O9 Mn1 139.8(4) . 4_656 ? Mn1 O9 Mn1 7.02(15) 6_565 4_656 ? C26 O10 Mn2 116.1(5) . 8_465 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 22.41 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.521 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.139 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 _platon_squeeze_void_content 1 0.166 -0.085 0.250 1509 502 ' ' 2 0.160 -0.010 0.750 1509 503 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 950525' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H50 Mn3 N4 O19' _chemical_formula_weight 1343.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.960(7) _cell_length_b 20.191(5) _cell_length_c 16.386(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.129(4) _cell_angle_gamma 90.00 _cell_volume 9307(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 25.96 _exptl_crystal_description brick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2756 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6337 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details 'Sheldrick, G. M. (2008). SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24906 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.96 _reflns_number_total 9037 _reflns_number_gt 4599 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1863P)^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_number_reflns 9037 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1427 _refine_ls_R_factor_gt 0.0977 _refine_ls_wR_factor_ref 0.3136 _refine_ls_wR_factor_gt 0.2750 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.7500 0.2500 1.0000 0.0284(3) Uani 1 2 d S . . Mn2 Mn 0.76663(3) 0.08717(4) 1.04034(6) 0.0516(3) Uani 1 1 d . . . N1 N 0.7632(2) -0.0140(3) 1.0797(4) 0.0660(15) Uani 1 1 d . . . N2 N 0.7559(2) -0.1228(3) 1.0697(4) 0.0625(14) Uani 1 1 d . . . O1 O 1.0000 0.3203(3) 0.7500 0.0717(18) Uani 1 2 d S . . O2 O 0.98073(16) 0.2884(3) 0.9397(4) 0.0820(15) Uani 1 1 d . . . O3 O 1.09240(16) 0.3040(2) 1.0496(3) 0.0665(12) Uani 1 1 d . . . O4 O 1.12066(16) 0.3275(2) 0.8741(3) 0.0711(13) Uani 1 1 d . . . O5 O 0.83277(19) 0.0928(3) 1.0133(4) 0.0911(17) Uani 1 1 d . . . O6 O 0.81261(13) 0.1861(2) 1.0564(3) 0.0610(11) Uani 1 1 d . . . O7 O 1.21843(17) 0.3441(2) 1.4421(3) 0.0670(12) Uani 1 1 d . . . O8 O 1.2209(2) 0.4454(3) 1.3997(3) 0.0815(15) Uani 1 1 d . . . O9 O 1.22870(15) 0.2732(2) 0.6078(3) 0.0556(11) Uani 1 1 d . . . O10 O 1.24279(16) 0.3804(2) 0.6383(3) 0.0675(12) Uani 1 1 d . . . C1 C 1.04737(19) 0.3109(3) 0.8984(4) 0.0502(14) Uani 1 1 d . . . C2 C 1.0146(2) 0.2564(3) 0.9108(4) 0.0600(16) Uani 1 1 d . . . H2A H 1.0326 0.2251 0.9536 0.072 Uiso 1 1 d R . . H2B H 0.9994 0.2335 0.8570 0.072 Uiso 1 1 d R . . C3 C 1.0690(2) 0.3495(3) 0.9827(4) 0.0571(16) Uani 1 1 d . . . H3A H 1.0443 0.3719 0.9969 0.068 Uiso 1 1 d R . . H3B H 1.0909 0.3820 0.9759 0.068 Uiso 1 1 d R . . C4 C 1.0881(2) 0.2765(4) 0.8743(4) 0.0646(18) Uani 1 1 d . . . H4A H 1.0754 0.2561 0.8181 0.077 Uiso 1 1 d R . . H4B H 1.1031 0.2431 0.9165 0.077 Uiso 1 1 d R . . C5 C 1.0208(2) 0.3571(3) 0.8261(4) 0.0615(17) Uani 1 1 d . . . H5A H 1.0420 0.3896 0.8168 0.074 Uiso 1 1 d R . . H5B H 0.9964 0.3796 0.8409 0.074 Uiso 1 1 d R . . C6 C 0.9480(2) 0.2505(4) 0.9593(5) 0.0681(18) Uani 1 1 d . . . C7 C 0.9419(3) 0.1840(4) 0.9446(6) 0.081(2) Uani 1 1 d . . . H7A H 0.9603 0.1605 0.9190 0.097 Uiso 1 1 calc R . . C8 C 0.9063(2) 0.1516(4) 0.9697(5) 0.080(2) Uani 1 1 d . . . H8A H 0.9020 0.1061 0.9617 0.096 Uiso 1 1 calc R . . C9 C 0.8779(2) 0.1868(4) 1.0057(4) 0.0636(17) Uani 1 1 d . . . C10 C 0.8857(2) 0.2542(4) 1.0200(5) 0.071(2) Uani 1 1 d . . . H10A H 0.8667 0.2786 1.0435 0.085 Uiso 1 1 calc R . . C11 C 0.9204(3) 0.2841(4) 0.9999(6) 0.083(2) Uani 1 1 d . . . H11A H 0.9264 0.3287 1.0133 0.100 Uiso 1 1 calc R . . C12 C 0.8397(2) 0.1531(4) 1.0266(4) 0.0611(17) Uani 1 1 d . . . C13 C 1.1187(2) 0.3279(3) 1.1284(4) 0.0597(17) Uani 1 1 d . . . C14 C 1.1415(3) 0.2789(4) 1.1911(4) 0.0698(19) Uani 1 1 d . . . H14A H 1.1381 0.2341 1.1774 0.084 Uiso 1 1 calc R . . C15 C 1.1685(2) 0.3002(4) 1.2723(4) 0.0684(18) Uani 1 1 d . . . H15A H 1.1826 0.2687 1.3147 0.082 Uiso 1 1 calc R . . C16 C 1.1757(2) 0.3656(3) 1.2938(4) 0.0539(15) Uani 1 1 d . . . C17 C 1.1547(3) 0.4120(4) 1.2327(4) 0.079(2) Uani 1 1 d . . . H17A H 1.1601 0.4566 1.2463 0.095 Uiso 1 1 calc R . . C18 C 1.1248(3) 0.3931(4) 1.1482(4) 0.077(2) Uani 1 1 d . . . H18A H 1.1095 0.4250 1.1071 0.092 Uiso 1 1 calc R . . C19 C 1.2064(2) 0.3851(4) 1.3829(4) 0.0610(17) Uani 1 1 d . . . C20 C 1.1480(2) 0.3210(3) 0.8214(4) 0.0572(16) Uani 1 1 d . . . C21 C 1.1504(2) 0.2643(3) 0.7773(4) 0.0618(17) Uani 1 1 d . . . H21A H 1.1350 0.2258 0.7842 0.074 Uiso 1 1 calc R . . C22 C 1.1772(2) 0.2663(3) 0.7208(4) 0.0573(16) Uani 1 1 d . . . H22A H 1.1787 0.2287 0.6889 0.069 Uiso 1 1 calc R . . C23 C 1.2005(2) 0.3219(3) 0.7124(4) 0.0509(14) Uani 1 1 d . . . C24 C 1.2001(2) 0.3769(4) 0.7631(4) 0.0687(19) Uani 1 1 d . . . H24A H 1.2180 0.4142 0.7614 0.082 Uiso 1 1 calc R . . C25 C 1.1726(2) 0.3758(3) 0.8167(4) 0.0617(17) Uani 1 1 d . . . H25A H 1.1713 0.4129 0.8493 0.074 Uiso 1 1 calc R . . C26 C 1.2266(2) 0.3252(3) 0.6491(4) 0.0534(15) Uani 1 1 d . . . C27 C 0.7571(4) -0.0387(3) 1.1542(6) 0.094(3) Uani 1 1 d . . . H27A H 0.7549 -0.0118 1.2010 0.113 Uiso 1 1 d R . . C28 C 0.7520(4) -0.1038(4) 1.1478(5) 0.094(3) Uani 1 1 d . . . H28A H 0.7467 -0.1318 1.1886 0.113 Uiso 1 1 calc R . . C29 C 0.7614(2) -0.0681(3) 1.0301(4) 0.0561(17) Uani 1 1 d . . . H29A H 0.7637 -0.0669 0.9750 0.067 Uiso 1 1 calc R . . C30 C 0.7526(2) -0.1878(3) 1.0341(4) 0.0570(15) Uani 1 1 d . . . C31 C 0.7234(3) -0.2328(3) 1.0492(5) 0.073(2) Uani 1 1 d . . . H31A H 0.7055 -0.2216 1.0837 0.087 Uiso 1 1 calc R . . C32 C 0.7196(3) -0.2954(3) 1.0141(5) 0.074(2) Uani 1 1 d . . . H32A H 0.6972 -0.3216 1.0301 0.111 Uiso 1 1 d 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 0.0340(6) 0.0244(5) 0.0318(6) 0.0007(4) 0.0175(4) -0.0021(4) Mn2 0.0654(7) 0.0399(5) 0.0598(7) 0.0016(4) 0.0346(5) 0.0002(4) N1 0.090(4) 0.053(3) 0.066(4) 0.008(3) 0.041(3) 0.006(3) N2 0.089(4) 0.041(3) 0.069(4) -0.002(3) 0.041(3) -0.002(3) O1 0.071(4) 0.079(5) 0.051(4) 0.000 0.003(3) 0.000 O2 0.062(3) 0.082(4) 0.125(4) -0.001(3) 0.062(3) -0.004(3) O3 0.086(3) 0.058(3) 0.045(2) 0.003(2) 0.009(2) -0.001(2) O4 0.073(3) 0.089(4) 0.074(3) -0.019(3) 0.055(2) -0.020(3) O5 0.086(4) 0.061(3) 0.144(5) -0.001(3) 0.062(4) -0.005(3) O6 0.046(2) 0.080(3) 0.062(3) 0.014(2) 0.026(2) 0.006(2) O7 0.094(3) 0.053(3) 0.050(3) 0.007(2) 0.020(2) 0.015(2) O8 0.111(4) 0.062(3) 0.054(3) 0.004(2) 0.005(3) -0.003(3) O9 0.071(3) 0.046(2) 0.064(3) -0.004(2) 0.042(2) 0.000(2) O10 0.090(3) 0.051(3) 0.081(3) -0.006(2) 0.055(3) -0.011(2) C1 0.044(3) 0.065(4) 0.047(3) 0.004(3) 0.024(3) -0.001(3) C2 0.054(3) 0.064(4) 0.074(4) 0.000(3) 0.036(3) 0.000(3) C3 0.053(4) 0.082(5) 0.040(3) -0.003(3) 0.020(3) -0.005(3) C4 0.054(4) 0.092(5) 0.052(4) 0.000(3) 0.025(3) -0.018(3) C5 0.060(4) 0.067(4) 0.056(4) 0.003(3) 0.018(3) -0.007(3) C6 0.067(4) 0.062(4) 0.090(5) -0.002(4) 0.045(4) 0.000(4) C7 0.076(5) 0.066(5) 0.129(7) 0.002(4) 0.071(5) 0.003(4) C8 0.068(4) 0.062(5) 0.132(7) 0.004(4) 0.061(5) 0.005(4) C9 0.048(4) 0.074(5) 0.078(5) 0.002(4) 0.033(3) 0.006(3) C10 0.068(4) 0.056(4) 0.106(6) -0.012(4) 0.053(4) 0.000(3) C11 0.075(5) 0.070(5) 0.131(7) -0.021(5) 0.068(5) -0.016(4) C12 0.054(4) 0.061(4) 0.078(5) 0.010(4) 0.035(3) 0.012(3) C13 0.067(4) 0.070(5) 0.040(3) 0.003(3) 0.017(3) 0.006(3) C14 0.093(5) 0.053(4) 0.057(4) 0.005(3) 0.018(4) 0.007(4) C15 0.071(4) 0.067(5) 0.057(4) 0.016(3) 0.008(3) 0.019(4) C16 0.068(4) 0.044(4) 0.052(4) 0.006(3) 0.023(3) 0.004(3) C17 0.114(6) 0.058(5) 0.051(4) 0.008(3) 0.009(4) -0.002(4) C18 0.099(6) 0.060(5) 0.053(4) 0.015(3) 0.004(4) 0.002(4) C19 0.060(4) 0.074(5) 0.046(4) 0.008(4) 0.014(3) 0.007(4) C20 0.048(3) 0.077(5) 0.056(4) -0.005(3) 0.030(3) -0.003(3) C21 0.061(4) 0.059(4) 0.077(5) 0.000(3) 0.038(3) -0.006(3) C22 0.068(4) 0.054(4) 0.054(4) -0.004(3) 0.027(3) -0.011(3) C23 0.049(3) 0.051(4) 0.060(4) 0.001(3) 0.027(3) -0.004(3) C24 0.080(5) 0.075(5) 0.067(4) -0.018(4) 0.045(4) -0.016(4) C25 0.073(4) 0.067(4) 0.061(4) -0.023(3) 0.043(3) -0.024(3) C26 0.047(3) 0.058(4) 0.060(4) 0.002(3) 0.023(3) 0.000(3) C27 0.171(9) 0.040(4) 0.101(6) -0.003(4) 0.086(6) 0.007(5) C28 0.177(9) 0.052(4) 0.084(6) 0.008(4) 0.083(6) 0.008(5) C29 0.084(5) 0.022(3) 0.080(4) 0.012(3) 0.051(4) 0.010(3) C30 0.073(4) 0.039(3) 0.067(4) 0.009(3) 0.035(3) 0.008(3) C31 0.105(6) 0.038(4) 0.099(6) 0.008(3) 0.066(5) 0.007(3) C32 0.095(5) 0.047(4) 0.102(6) -0.004(4) 0.062(5) -0.011(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 Mn1 O9 2.127(4) 2_756 ? Mn1 O9 2.127(4) 8_456 ? Mn1 O7 2.188(4) 2_757 ? Mn1 O7 2.188(4) 8_455 ? Mn1 O6 2.201(4) 7_657 ? Mn1 O6 2.201(4) . ? Mn2 O10 2.075(4) 8_456 ? Mn2 N1 2.156(5) . ? Mn2 O5 2.177(5) . ? Mn2 O7 2.237(5) 8_455 ? Mn2 O8 2.334(5) 8_455 ? Mn2 O6 2.390(5) . ? Mn2 C12 2.638(7) . ? N1 C29 1.351(8) . ? N1 C27 1.387(9) . ? N2 C29 1.320(7) . ? N2 C28 1.377(8) . ? N2 C30 1.427(8) . ? O1 C5 1.400(7) 2_756 ? O1 C5 1.400(7) . ? O2 C6 1.367(8) . ? O2 C2 1.415(7) . ? O3 C13 1.350(7) . ? O3 C3 1.416(7) . ? O4 C20 1.386(7) . ? O4 C4 1.418(7) . ? O5 C12 1.242(8) . ? O6 C12 1.271(7) . ? O7 C19 1.231(7) . ? O7 Mn1 2.188(4) 2_757 ? O7 Mn2 2.237(5) 8_556 ? O8 C19 1.290(8) . ? O8 Mn2 2.334(5) 8_556 ? O9 C26 1.262(7) . ? O9 Mn1 2.127(4) 2_756 ? O10 C26 1.250(7) . ? O10 Mn2 2.075(4) 8 ? C1 C5 1.504(8) . ? C1 C3 1.524(8) . ? C1 C2 1.534(8) . ? C1 C4 1.567(8) . ? C6 C7 1.367(10) . ? C6 C11 1.400(9) . ? C7 C8 1.426(9) . ? C8 C9 1.387(9) . ? C9 C10 1.386(10) . ? C9 C12 1.470(9) . ? C10 C11 1.339(9) . ? C13 C18 1.353(9) . ? C13 C14 1.418(9) . ? C14 C15 1.367(9) . ? C15 C16 1.365(9) . ? C16 C17 1.357(9) . ? C16 C19 1.486(9) . ? C17 C18 1.419(10) . ? C20 C25 1.346(9) . ? C20 C21 1.369(9) . ? C21 C22 1.419(8) . ? C22 C23 1.355(8) . ? C23 C24 1.390(9) . ? C23 C26 1.500(8) . ? C24 C25 1.396(8) . ? C27 C28 1.325(10) . ? C30 C31 1.342(9) . ? C30 C32 1.373(9) 7_647 ? C31 C32 1.377(9) . ? C32 C30 1.373(9) 7_647 ? 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 O9 180.000(1) 2_756 8_456 ? O9 Mn1 O7 87.72(16) 2_756 2_757 ? O9 Mn1 O7 92.28(16) 8_456 2_757 ? O9 Mn1 O7 92.28(16) 2_756 8_455 ? O9 Mn1 O7 87.72(16) 8_456 8_455 ? O7 Mn1 O7 180.000(1) 2_757 8_455 ? O9 Mn1 O6 88.74(15) 2_756 7_657 ? O9 Mn1 O6 91.26(15) 8_456 7_657 ? O7 Mn1 O6 81.49(17) 2_757 7_657 ? O7 Mn1 O6 98.51(17) 8_455 7_657 ? O9 Mn1 O6 91.26(15) 2_756 . ? O9 Mn1 O6 88.74(15) 8_456 . ? O7 Mn1 O6 98.51(17) 2_757 . ? O7 Mn1 O6 81.49(17) 8_455 . ? O6 Mn1 O6 180.000(1) 7_657 . ? O10 Mn2 N1 90.19(19) 8_456 . ? O10 Mn2 O5 136.1(2) 8_456 . ? N1 Mn2 O5 104.5(2) . . ? O10 Mn2 O7 92.96(18) 8_456 8_455 ? N1 Mn2 O7 135.9(2) . 8_455 ? O5 Mn2 O7 103.2(2) . 8_455 ? O10 Mn2 O8 127.7(2) 8_456 8_455 ? N1 Mn2 O8 87.5(2) . 8_455 ? O5 Mn2 O8 94.6(2) . 8_455 ? O7 Mn2 O8 56.63(17) 8_455 8_455 ? O10 Mn2 O6 89.39(17) 8_456 . ? N1 Mn2 O6 147.66(19) . . ? O5 Mn2 O6 56.52(17) . . ? O7 Mn2 O6 76.44(15) 8_455 . ? O8 Mn2 O6 117.67(17) 8_455 . ? O10 Mn2 C12 115.1(2) 8_456 . ? N1 Mn2 C12 129.1(2) . . ? O5 Mn2 C12 27.85(18) . . ? O7 Mn2 C12 88.56(19) 8_455 . ? O8 Mn2 C12 106.3(2) 8_455 . ? O6 Mn2 C12 28.76(17) . . ? C29 N1 C27 104.4(5) . . ? C29 N1 Mn2 125.6(4) . . ? C27 N1 Mn2 129.6(5) . . ? C29 N2 C28 106.8(6) . . ? C29 N2 C30 124.9(5) . . ? C28 N2 C30 128.3(6) . . ? C5 O1 C5 115.9(8) 2_756 . ? C6 O2 C2 118.6(6) . . ? C13 O3 C3 118.7(5) . . ? C20 O4 C4 119.2(5) . . ? C12 O5 Mn2 97.2(4) . . ? C12 O6 Mn1 135.3(4) . . ? C12 O6 Mn2 86.5(4) . . ? Mn1 O6 Mn2 93.90(14) . . ? C19 O7 Mn1 153.1(4) . 2_757 ? C19 O7 Mn2 95.2(4) . 8_556 ? Mn1 O7 Mn2 98.68(18) 2_757 8_556 ? C19 O8 Mn2 89.1(4) . 8_556 ? C26 O9 Mn1 135.4(4) . 2_756 ? C26 O10 Mn2 130.1(4) . 8 ? C5 C1 C3 109.9(6) . . ? C5 C1 C2 111.1(5) . . ? C3 C1 C2 109.8(5) . . ? C5 C1 C4 108.9(5) . . ? C3 C1 C4 109.3(5) . . ? C2 C1 C4 107.8(5) . . ? O2 C2 C1 106.4(5) . . ? O3 C3 C1 108.2(6) . . ? O4 C4 C1 106.0(5) . . ? O1 C5 C1 108.9(6) . . ? C7 C6 O2 124.9(6) . . ? C7 C6 C11 119.7(6) . . ? O2 C6 C11 115.4(7) . . ? C6 C7 C8 117.9(6) . . ? C9 C8 C7 121.0(7) . . ? C10 C9 C8 119.0(6) . . ? C10 C9 C12 120.9(6) . . ? C8 C9 C12 120.1(7) . . ? C11 C10 C9 120.0(6) . . ? C10 C11 C6 122.2(7) . . ? O5 C12 O6 119.4(6) . . ? O5 C12 C9 120.7(6) . . ? O6 C12 C9 119.8(6) . . ? O5 C12 Mn2 55.0(3) . . ? O6 C12 Mn2 64.7(3) . . ? C9 C12 Mn2 171.7(5) . . ? O3 C13 C18 124.2(6) . . ? O3 C13 C14 114.9(6) . . ? C18 C13 C14 120.9(6) . . ? C15 C14 C13 117.5(7) . . ? C16 C15 C14 122.9(6) . . ? C17 C16 C15 119.0(6) . . ? C17 C16 C19 121.1(6) . . ? C15 C16 C19 120.0(6) . . ? C16 C17 C18 120.8(7) . . ? C13 C18 C17 118.8(6) . . ? O7 C19 O8 118.8(6) . . ? O7 C19 C16 120.7(7) . . ? O8 C19 C16 120.6(6) . . ? C25 C20 C21 121.9(6) . . ? C25 C20 O4 114.2(6) . . ? C21 C20 O4 123.9(6) . . ? C20 C21 C22 117.7(6) . . ? C23 C22 C21 121.1(6) . . ? C22 C23 C24 119.4(6) . . ? C22 C23 C26 121.2(6) . . ? C24 C23 C26 119.5(5) . . ? C23 C24 C25 119.5(6) . . ? C20 C25 C24 120.2(6) . . ? O10 C26 O9 124.9(6) . . ? O10 C26 C23 117.2(6) . . ? O9 C26 C23 117.8(5) . . ? C28 C27 N1 109.4(7) . . ? C27 C28 N2 107.8(6) . . ? N2 C29 N1 111.5(5) . . ? C31 C30 C32 120.2(6) . 7_647 ? C31 C30 N2 120.3(6) . . ? C32 C30 N2 119.5(6) 7_647 . ? C30 C31 C32 120.6(6) . . ? C30 C32 C31 119.2(6) 7_647 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.327 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.134 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 _platon_squeeze_void_content 1 0.000 -0.008 -0.010 2101 902 ' ' 2 0.500 -0.159 0.118 2101 902 ' ' _platon_squeeze_details ; the contribution of 3 DMF moleculs were removed by the SQUEEZE process. ; _database_code_depnum_ccdc_archive 'CCDC 950526' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H54 Mn3 N4 O21' _chemical_formula_weight 1379.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 47.138(12) _cell_length_b 75.02(2) _cell_length_c 10.521(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 37203(17) _cell_formula_units_Z 16 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 26.29 _exptl_crystal_description brick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11344 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5599 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details 'Sheldrick, G. M. (2008). SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51652 _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_av_sigmaI/netI 0.1496 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -91 _diffrn_reflns_limit_k_max 92 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 26.29 _reflns_number_total 17282 _reflns_number_gt 8708 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^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 -0.054(19) _refine_ls_number_reflns 17282 _refine_ls_number_parameters 804 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1240 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.054 _refine_ls_shift/su_mean 0.003 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 0.131728(18) 0.206622(12) -0.05233(9) 0.0468(2) Uani 1 1 d . . . Mn2 Mn 0.133990(17) 0.191262(11) 0.26682(8) 0.0410(2) Uani 1 1 d . . . Mn3 Mn 0.165192(17) 0.181714(11) 0.54772(8) 0.0423(2) Uani 1 1 d . . . N1 N 0.21093(10) 0.18549(7) 0.5664(5) 0.0566(14) Uani 1 1 d . . . N2 N 0.25244(11) 0.19494(7) 0.6391(6) 0.0719(18) Uani 1 1 d . . . N3 N 0.14454(12) 0.23590(7) -0.0799(6) 0.0677(16) Uani 1 1 d . . . N4 N 0.16711(11) 0.25950(7) -0.1444(5) 0.0623(15) Uani 1 1 d . . . O1 O 0.14227(8) 0.06584(6) -0.0440(4) 0.0668(13) Uani 1 1 d . . . O1W O 0.11951(10) 0.20902(6) -0.2465(4) 0.0762(14) Uani 1 1 d . . . H1WB H 0.1358 0.2122 -0.2964 0.114 Uiso 1 1 d R . . H1WA H 0.1053 0.2181 -0.2543 0.114 Uiso 1 1 d R . . O2 O 0.09292(11) 0.09676(6) -0.0703(5) 0.0807(15) Uani 1 1 d . . . O2W O 0.16718(9) 0.17417(6) 0.7477(4) 0.0617(12) Uani 1 1 d . . . H2WA H 0.1663 0.1847 0.7994 0.093 Uiso 1 1 d R . . H2WB H 0.1847 0.1681 0.7635 0.093 Uiso 1 1 d R . . O3 O 0.04170(8) 0.06496(7) -0.0384(4) 0.0696(13) Uani 1 1 d . . . O4 O 0.08986(10) 0.03493(5) -0.0049(5) 0.0771(14) Uani 1 1 d . . . O5 O 0.18512(9) 0.09966(6) 0.0316(5) 0.0681(12) Uani 1 1 d . . . O6 O 0.24238(8) 0.07455(7) -0.0293(4) 0.0682(14) Uani 1 1 d . . . O7 O 0.20227(10) 0.03890(6) -0.0635(5) 0.0874(17) Uani 1 1 d . . . O8 O 0.11577(9) 0.17423(6) 0.1286(4) 0.0586(12) Uani 1 1 d . . . O9 O 0.12189(8) 0.17889(5) -0.0774(4) 0.0517(11) Uani 1 1 d . . . O10 O -0.08774(8) 0.04879(6) -0.1378(4) 0.0498(10) Uani 1 1 d . . . O11 O -0.07161(8) 0.04954(6) -0.3295(4) 0.0545(11) Uani 1 1 d . . . O12 O 0.08536(10) -0.03325(6) 0.3510(5) 0.0684(13) Uani 1 1 d . . . O13 O 0.09047(8) -0.04549(5) 0.1666(4) 0.0520(11) Uani 1 1 d . . . O14 O 0.17040(10) 0.15461(6) 0.4822(5) 0.0710(14) Uani 1 1 d . . . O15 O 0.16475(9) 0.17164(6) 0.3214(5) 0.0679(14) Uani 1 1 d . . . O16 O 0.37164(9) 0.06957(6) -0.1619(4) 0.0625(13) Uani 1 1 d . . . O17 O 0.35365(9) 0.07006(6) -0.3558(5) 0.0602(12) Uani 1 1 d . . . O18 O 0.14173(9) -0.03556(6) 0.0019(5) 0.0662(13) Uani 1 1 d . . . O19 O 0.15280(8) -0.03503(6) -0.2032(5) 0.0584(11) Uani 1 1 d . . . C1 C 0.09259(12) 0.06585(8) -0.0402(6) 0.0515(16) Uani 1 1 d . . . C2 C 0.09249(13) 0.08393(7) 0.0305(7) 0.0569(17) Uani 1 1 d . . . H2A H 0.0756 0.0852 0.0821 0.068 Uiso 1 1 calc R . . H2B H 0.1091 0.0851 0.0844 0.068 Uiso 1 1 calc R . . C3 C 0.06609(12) 0.06421(8) -0.1231(7) 0.0557(17) Uani 1 1 d . . . H3A H 0.0653 0.0739 -0.1841 0.067 Uiso 1 1 calc R . . H3B H 0.0663 0.0530 -0.1692 0.067 Uiso 1 1 calc R . . C4 C 0.09285(13) 0.05134(7) 0.0630(6) 0.0543(17) Uani 1 1 d . . . H4A H 0.1105 0.0516 0.1101 0.065 Uiso 1 1 calc R . . H4B H 0.0773 0.0530 0.1220 0.065 Uiso 1 1 calc R . . C5 C 0.11784(12) 0.06418(9) -0.1170(7) 0.0571(17) Uani 1 1 d . . . H5A H 0.1178 0.0527 -0.1588 0.068 Uiso 1 1 calc R . . H5B H 0.1177 0.0733 -0.1823 0.068 Uiso 1 1 calc R . . C6 C 0.19231(12) 0.06946(8) -0.0272(6) 0.0458(15) Uani 1 1 d . . . C7 C 0.18816(13) 0.08288(8) 0.0781(6) 0.0546(17) Uani 1 1 d . . . H7A H 0.1714 0.0797 0.1269 0.065 Uiso 1 1 calc R . . H7B H 0.2044 0.0825 0.1348 0.065 Uiso 1 1 calc R . . C8 C 0.21834(12) 0.07411(10) -0.1090(7) 0.066(2) Uani 1 1 d . . . H8A H 0.2209 0.0652 -0.1750 0.080 Uiso 1 1 calc R . . H8B H 0.2157 0.0856 -0.1492 0.080 Uiso 1 1 calc R . . C9 C 0.19626(14) 0.05145(9) 0.0306(8) 0.077(2) Uani 1 1 d . . . H9A H 0.2117 0.0518 0.0914 0.092 Uiso 1 1 calc R . . H9B H 0.1792 0.0480 0.0755 0.092 Uiso 1 1 calc R . . C10 C 0.16749(12) 0.06987(10) -0.1187(8) 0.074(2) Uani 1 1 d . . . H10A H 0.1658 0.0815 -0.1577 0.089 Uiso 1 1 calc R . . H10B H 0.1700 0.0611 -0.1853 0.089 Uiso 1 1 calc R . . C11 C 0.09798(13) 0.11413(9) -0.0405(7) 0.0575(17) Uani 1 1 d . . . C12 C 0.09780(15) 0.12104(9) 0.0763(7) 0.067(2) Uani 1 1 d . . . H12A H 0.0937 0.1138 0.1456 0.081 Uiso 1 1 calc R . . C13 C 0.10367(14) 0.13906(9) 0.0954(6) 0.0609(18) Uani 1 1 d . . . H13A H 0.1043 0.1437 0.1773 0.073 Uiso 1 1 calc R . . C14 C 0.10836(12) 0.14972(8) -0.0055(6) 0.0514(16) Uani 1 1 d . . . C15 C 0.10912(15) 0.14302(9) -0.1263(7) 0.0641(19) Uani 1 1 d . . . H15A H 0.1131 0.1503 -0.1957 0.077 Uiso 1 1 calc R . . C16 C 0.10384(16) 0.12511(9) -0.1415(7) 0.076(2) Uani 1 1 d . . . H16A H 0.1043 0.1203 -0.2229 0.091 Uiso 1 1 calc R . . C17 C 0.11623(12) 0.16932(8) 0.0186(7) 0.0490(15) Uani 1 1 d . . . C18 C 0.01593(13) 0.06180(9) -0.0897(7) 0.0551(17) Uani 1 1 d . . . C19 C -0.00601(14) 0.05995(10) -0.0059(7) 0.070(2) Uani 1 1 d . . . H19A H -0.0023 0.0613 0.0804 0.084 Uiso 1 1 calc R . . C20 C -0.03245(13) 0.05629(8) -0.0424(6) 0.0546(17) Uani 1 1 d . . . H20A H -0.0467 0.0545 0.0174 0.065 Uiso 1 1 calc R . . C21 C -0.03819(13) 0.05523(8) -0.1688(6) 0.0495(16) Uani 1 1 d . . . C22 C -0.01659(14) 0.05751(10) -0.2555(7) 0.071(2) Uani 1 1 d . . . H22A H -0.0202 0.0568 -0.3423 0.085 Uiso 1 1 calc R . . C23 C 0.01052(13) 0.06089(9) -0.2117(8) 0.068(2) Uani 1 1 d . . . H23A H 0.0252 0.0626 -0.2697 0.082 Uiso 1 1 calc R . . C24 C -0.06788(13) 0.05098(7) -0.2160(6) 0.0470(15) Uani 1 1 d . . . C25 C 0.08908(13) 0.01935(8) 0.0623(8) 0.0622(19) Uani 1 1 d . . . C26 C 0.08437(15) 0.00448(8) -0.0089(7) 0.072(2) Uani 1 1 d . . . H26A H 0.0813 0.0054 -0.0960 0.087 Uiso 1 1 calc R . . C27 C 0.08417(14) -0.01223(8) 0.0500(7) 0.0600(18) Uani 1 1 d . . . H27A H 0.0815 -0.0225 0.0016 0.072 Uiso 1 1 calc R . . C28 C 0.08783(13) -0.01353(8) 0.1749(6) 0.0525(16) Uani 1 1 d . . . C29 C 0.09272(14) 0.00132(9) 0.2461(7) 0.069(2) Uani 1 1 d . . . H29A H 0.0957 0.0001 0.3331 0.083 Uiso 1 1 calc R . . C30 C 0.09337(15) 0.01814(8) 0.1919(7) 0.070(2) Uani 1 1 d . . . H30A H 0.0966 0.0282 0.2410 0.084 Uiso 1 1 calc R . . C31 C 0.08852(12) -0.03136(8) 0.2363(6) 0.0454(15) Uani 1 1 d . . . C32 C 0.18170(13) 0.11289(8) 0.1198(7) 0.0532(16) Uani 1 1 d . . . C33 C 0.18004(15) 0.11071(9) 0.2448(7) 0.0675(19) Uani 1 1 d . . . H33A H 0.1808 0.0992 0.2774 0.081 Uiso 1 1 calc R . . C34 C 0.17733(15) 0.12445(10) 0.3267(7) 0.072(2) Uani 1 1 d . . . H34A H 0.1778 0.1225 0.4139 0.087 Uiso 1 1 calc R . . C35 C 0.17380(11) 0.14147(8) 0.2798(7) 0.0488(15) Uani 1 1 d . . . C36 C 0.17549(15) 0.14370(9) 0.1514(6) 0.0656(19) Uani 1 1 d . . . H36A H 0.1738 0.1551 0.1169 0.079 Uiso 1 1 calc R . . C37 C 0.17965(16) 0.12945(10) 0.0729(7) 0.074(2) Uani 1 1 d . . . H37A H 0.1811 0.1313 -0.0143 0.089 Uiso 1 1 calc R . . C38 C 0.16939(12) 0.15631(8) 0.3675(8) 0.0510(16) Uani 1 1 d . . . C39 C 0.26817(13) 0.07450(9) -0.0915(7) 0.0573(17) Uani 1 1 d . . . C40 C 0.29119(13) 0.07382(10) -0.0101(7) 0.070(2) Uani 1 1 d . . . H40A H 0.2885 0.0739 0.0774 0.084 Uiso 1 1 calc R . . C41 C 0.31743(13) 0.07311(9) -0.0585(7) 0.0595(18) Uani 1 1 d . . . H41A H 0.3328 0.0727 -0.0031 0.071 Uiso 1 1 calc R . . C42 C 0.32235(12) 0.07296(8) -0.1850(7) 0.0517(17) Uani 1 1 d . . . C43 C 0.30003(15) 0.07446(10) -0.2649(7) 0.073(2) Uani 1 1 d . . . H43A H 0.3031 0.0749 -0.3522 0.088 Uiso 1 1 calc R . . C44 C 0.27152(13) 0.07544(9) -0.2161(7) 0.068(2) Uani 1 1 d . . . H44A H 0.2560 0.0767 -0.2703 0.082 Uiso 1 1 calc R . . C45 C 0.35119(12) 0.07057(8) -0.2426(7) 0.0471(15) Uani 1 1 d . . . C46 C 0.19091(13) 0.02217(9) -0.0543(8) 0.069(2) Uani 1 1 d . . . C47 C 0.19809(16) 0.01166(10) -0.1578(9) 0.090(3) Uani 1 1 d . . . H47A H 0.2102 0.0158 -0.2208 0.108 Uiso 1 1 calc R . . C48 C 0.18634(15) -0.00564(9) -0.1638(8) 0.083(3) Uani 1 1 d . . . H48A H 0.1916 -0.0132 -0.2297 0.100 Uiso 1 1 calc R . . C49 C 0.16755(14) -0.01140(9) -0.0754(7) 0.0611(18) Uani 1 1 d . . . C50 C 0.16237(15) -0.00091(9) 0.0251(8) 0.080(2) Uani 1 1 d . . . H50A H 0.1509 -0.0051 0.0905 0.095 Uiso 1 1 calc R . . C51 C 0.17401(17) 0.01639(9) 0.0333(8) 0.086(2) Uani 1 1 d . . . H51A H 0.1695 0.0237 0.1020 0.103 Uiso 1 1 calc R . . C52 C 0.15274(13) -0.02943(9) -0.0956(8) 0.0530(17) Uani 1 1 d . . . C53 C 0.22535(16) 0.19922(10) 0.6112(9) 0.082(2) Uani 1 1 d . . . H53A H 0.2177 0.2105 0.6223 0.098 Uiso 1 1 calc R . . C54 C 0.23168(17) 0.17200(10) 0.5632(8) 0.088(3) Uani 1 1 d . . . H54A H 0.2279 0.1604 0.5381 0.105 Uiso 1 1 calc R . . C55 C 0.25655(17) 0.17739(10) 0.5987(9) 0.097(3) Uani 1 1 d . . . H55A H 0.2734 0.1710 0.5975 0.116 Uiso 1 1 calc R . . C56 C 0.27306(14) 0.20652(9) 0.6955(7) 0.0608(18) Uani 1 1 d . . . C57 C 0.30009(17) 0.20143(10) 0.6957(9) 0.103(3) Uani 1 1 d . . . H57A H 0.3054 0.1906 0.6594 0.123 Uiso 1 1 calc R . . C58 C 0.3208(2) 0.21284(13) 0.7530(8) 0.106(3) Uiso 1 1 d . . . H58A H 0.3398 0.2095 0.7541 0.127 Uiso 1 1 calc R . . C59 C 0.31274(16) 0.22853(10) 0.8057(7) 0.072(2) Uiso 1 1 d . . . C60 C 0.2857(2) 0.23330(15) 0.8059(10) 0.124(3) Uiso 1 1 d . . . H60A H 0.2798 0.2440 0.8416 0.149 Uiso 1 1 calc R . . C61 C 0.2656(2) 0.22106(15) 0.7481(9) 0.120(3) Uiso 1 1 d . . . H61A H 0.2464 0.2240 0.7495 0.144 Uiso 1 1 calc R . . C62 C 0.16761(16) 0.24231(10) -0.1288(7) 0.072(2) Uani 1 1 d . . . H62A H 0.1831 0.2353 -0.1507 0.087 Uiso 1 1 calc R . . C63 C 0.1400(2) 0.26443(14) -0.1129(9) 0.109(3) Uiso 1 1 d . . . H63A H 0.1325 0.2759 -0.1148 0.131 Uiso 1 1 calc R . . C64 C 0.12637(18) 0.24928(10) -0.0783(12) 0.133(5) Uani 1 1 d . . . H64A H 0.1073 0.2484 -0.0570 0.160 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 0.0432(5) 0.0362(5) 0.0611(6) -0.0006(5) 0.0014(5) -0.0056(4) Mn2 0.0404(5) 0.0297(5) 0.0529(5) -0.0012(4) 0.0018(4) -0.0020(4) Mn3 0.0359(5) 0.0352(5) 0.0557(5) -0.0034(4) 0.0010(4) -0.0026(4) N1 0.037(3) 0.046(3) 0.087(4) -0.014(3) -0.003(3) -0.001(3) N2 0.037(3) 0.045(4) 0.133(6) 0.004(4) -0.009(3) -0.002(3) N3 0.049(4) 0.046(4) 0.108(5) 0.007(3) 0.015(3) -0.015(3) N4 0.056(4) 0.036(3) 0.094(4) 0.002(3) 0.012(3) -0.007(3) O1 0.040(3) 0.078(3) 0.081(3) 0.003(3) 0.006(2) -0.013(2) O1W 0.081(3) 0.071(3) 0.077(3) 0.015(3) 0.000(3) 0.002(3) O2 0.129(4) 0.036(3) 0.077(3) 0.002(3) -0.012(3) -0.017(3) O2W 0.067(3) 0.059(3) 0.059(3) -0.009(2) 0.000(2) 0.005(2) O3 0.029(2) 0.090(4) 0.090(3) -0.009(3) 0.002(2) -0.006(2) O4 0.112(4) 0.021(2) 0.098(4) -0.002(2) -0.002(3) -0.003(2) O5 0.083(3) 0.041(3) 0.081(3) -0.009(3) 0.006(3) 0.011(2) O6 0.025(2) 0.101(4) 0.078(3) -0.021(3) 0.009(2) -0.006(2) O7 0.086(4) 0.038(3) 0.138(5) -0.029(3) 0.057(3) -0.025(2) O8 0.086(3) 0.044(3) 0.046(3) -0.004(2) -0.002(2) -0.017(2) O9 0.055(3) 0.039(3) 0.061(3) 0.003(2) 0.007(2) -0.006(2) O10 0.033(2) 0.057(3) 0.059(2) 0.002(2) 0.008(2) 0.002(2) O11 0.037(2) 0.059(3) 0.068(3) 0.007(2) -0.001(2) 0.002(2) O12 0.089(4) 0.052(3) 0.063(3) 0.001(2) 0.002(3) 0.008(3) O13 0.054(3) 0.026(2) 0.076(3) -0.001(2) 0.005(2) 0.0102(19) O14 0.082(4) 0.053(3) 0.079(4) -0.019(3) -0.008(3) 0.005(2) O15 0.054(3) 0.030(3) 0.120(4) -0.009(3) 0.020(3) -0.005(2) O16 0.040(3) 0.071(3) 0.077(3) 0.005(3) 0.010(2) 0.004(2) O17 0.052(3) 0.066(3) 0.063(3) -0.003(2) 0.019(2) 0.011(2) O18 0.065(3) 0.038(3) 0.096(4) -0.010(3) 0.001(3) -0.011(2) O19 0.053(3) 0.052(3) 0.070(3) -0.017(3) -0.008(2) -0.006(2) C1 0.042(4) 0.035(4) 0.077(4) -0.001(3) 0.016(3) -0.004(3) C2 0.054(4) 0.031(3) 0.086(5) -0.001(4) -0.008(4) -0.006(3) C3 0.034(4) 0.044(4) 0.089(5) -0.015(4) 0.012(3) -0.015(3) C4 0.051(4) 0.029(3) 0.083(5) 0.001(3) -0.008(3) -0.004(3) C5 0.032(4) 0.049(4) 0.090(5) -0.001(4) -0.003(3) -0.013(3) C6 0.039(4) 0.033(4) 0.065(4) -0.009(3) 0.016(3) -0.003(3) C7 0.054(4) 0.038(4) 0.072(5) -0.021(3) 0.005(3) 0.002(3) C8 0.034(4) 0.067(5) 0.097(5) -0.028(4) 0.017(4) 0.009(3) C9 0.057(4) 0.061(5) 0.113(6) -0.029(5) 0.021(4) -0.019(4) C10 0.034(4) 0.079(6) 0.111(6) -0.033(5) 0.004(4) -0.009(4) C11 0.063(4) 0.045(4) 0.065(5) 0.005(4) -0.011(3) -0.015(3) C12 0.097(6) 0.043(4) 0.062(5) 0.008(4) 0.001(4) -0.021(4) C13 0.086(5) 0.049(4) 0.048(4) 0.003(3) -0.004(3) -0.016(4) C14 0.049(4) 0.043(4) 0.062(4) -0.004(3) -0.003(3) -0.008(3) C15 0.097(6) 0.037(4) 0.057(4) 0.005(3) -0.001(4) -0.012(4) C16 0.121(7) 0.045(5) 0.061(5) -0.008(4) -0.008(4) -0.009(4) C17 0.037(3) 0.042(4) 0.068(4) 0.002(4) -0.005(3) -0.009(3) C18 0.040(4) 0.056(4) 0.069(5) 0.006(4) 0.003(4) 0.001(3) C19 0.054(5) 0.076(5) 0.080(5) -0.015(4) 0.001(4) 0.008(4) C20 0.035(4) 0.062(5) 0.066(4) -0.004(4) 0.001(3) 0.006(3) C21 0.050(4) 0.042(4) 0.057(4) 0.009(3) 0.012(3) -0.002(3) C22 0.051(5) 0.095(6) 0.067(5) -0.007(4) 0.009(4) 0.004(4) C23 0.035(4) 0.087(6) 0.083(6) 0.004(5) 0.018(4) -0.006(3) C24 0.062(5) 0.034(3) 0.045(4) 0.011(3) 0.002(3) 0.010(3) C25 0.053(4) 0.034(4) 0.099(6) -0.007(4) -0.004(4) -0.001(3) C26 0.114(6) 0.028(4) 0.075(5) -0.005(3) -0.015(4) -0.009(4) C27 0.093(5) 0.023(3) 0.064(5) -0.005(3) -0.013(4) 0.009(3) C28 0.067(4) 0.031(4) 0.060(4) -0.009(3) 0.009(3) -0.008(3) C29 0.087(5) 0.048(4) 0.073(5) 0.004(4) -0.011(4) -0.014(4) C30 0.110(6) 0.027(4) 0.073(5) -0.003(4) -0.013(4) -0.011(4) C31 0.051(4) 0.036(4) 0.049(4) -0.002(3) -0.010(3) 0.003(3) C32 0.056(4) 0.038(4) 0.066(5) -0.012(4) -0.004(3) 0.011(3) C33 0.104(6) 0.031(4) 0.068(5) -0.001(3) 0.008(4) 0.002(4) C34 0.107(6) 0.056(5) 0.054(4) -0.006(4) 0.006(4) 0.017(4) C35 0.039(3) 0.034(4) 0.073(5) -0.010(3) -0.003(3) 0.006(3) C36 0.097(6) 0.042(4) 0.057(5) -0.005(3) 0.001(4) 0.014(4) C37 0.108(6) 0.053(5) 0.061(5) 0.001(4) 0.009(4) 0.002(4) C38 0.039(4) 0.032(4) 0.082(5) -0.012(4) -0.002(3) -0.007(3) C39 0.050(4) 0.062(5) 0.060(5) -0.005(3) 0.017(3) -0.007(3) C40 0.034(4) 0.095(6) 0.081(5) -0.017(4) 0.005(4) -0.007(4) C41 0.039(4) 0.071(5) 0.069(5) -0.005(4) -0.003(3) 0.000(3) C42 0.030(3) 0.052(4) 0.073(5) 0.000(4) -0.004(3) 0.004(3) C43 0.054(5) 0.096(6) 0.069(5) 0.010(4) 0.012(4) 0.002(4) C44 0.039(4) 0.083(5) 0.082(5) -0.002(4) -0.009(4) 0.007(3) C45 0.032(4) 0.039(4) 0.070(5) -0.003(4) 0.007(3) 0.007(3) C46 0.049(4) 0.041(4) 0.116(6) -0.011(4) 0.032(4) -0.008(3) C47 0.088(6) 0.048(5) 0.135(8) -0.027(5) 0.029(5) -0.018(4) C48 0.065(5) 0.049(5) 0.135(7) -0.036(5) 0.011(5) -0.008(4) C49 0.053(4) 0.040(4) 0.091(5) -0.004(4) 0.011(4) -0.014(3) C50 0.090(6) 0.060(5) 0.089(6) -0.026(5) 0.015(5) -0.031(4) C51 0.113(6) 0.059(5) 0.085(5) -0.034(4) 0.037(5) -0.036(4) C52 0.037(4) 0.046(4) 0.076(5) 0.008(4) -0.008(4) -0.001(3) C53 0.065(5) 0.044(4) 0.136(7) 0.003(4) -0.018(5) -0.004(4) C54 0.073(6) 0.053(5) 0.137(8) -0.021(5) -0.001(5) 0.002(4) C55 0.054(5) 0.053(5) 0.184(9) -0.016(5) -0.024(5) 0.000(4) C56 0.049(4) 0.055(4) 0.078(5) -0.022(4) -0.001(4) -0.010(3) C57 0.061(5) 0.073(6) 0.175(9) -0.060(6) -0.035(5) -0.003(4) C62 0.063(5) 0.046(5) 0.107(6) 0.010(4) 0.008(4) 0.017(4) C64 0.065(6) 0.040(5) 0.294(15) 0.033(7) 0.055(7) -0.002(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 Mn1 O19 2.032(4) 4 ? Mn1 O1W 2.130(5) . ? Mn1 O9 2.148(4) . ? Mn1 O11 2.266(4) 3 ? Mn1 O10 2.288(4) 3 ? Mn1 N3 2.297(5) . ? Mn1 C24 2.606(7) 3 ? Mn2 O8 2.118(4) . ? Mn2 O18 2.126(4) 4 ? Mn2 O17 2.136(4) 11_455 ? Mn2 O15 2.145(5) . ? Mn2 O13 2.218(4) 4 ? Mn2 O10 2.231(4) 3 ? Mn3 O16 2.099(4) 11_455 ? Mn3 O14 2.161(4) . ? Mn3 O2W 2.180(4) . ? Mn3 N1 2.184(5) . ? Mn3 O13 2.213(4) 4 ? Mn3 O15 2.498(5) . ? N1 C53 1.321(8) . ? N1 C54 1.407(8) . ? N2 C53 1.349(8) . ? N2 C55 1.397(9) . ? N2 C56 1.432(8) . ? N3 C62 1.296(8) . ? N3 C64 1.320(9) . ? N4 C62 1.300(8) . ? N4 C63 1.371(10) . ? N4 C59 1.409(8) 14_554 ? O1 C5 1.390(7) . ? O1 C10 1.457(7) . ? O1W H1WB 0.9600 . ? O1W H1WA 0.9598 . ? O2 C11 1.361(7) . ? O2 C2 1.432(7) . ? O2W H2WA 0.9595 . ? O2W H2WB 0.9600 . ? O3 C18 1.350(7) . ? O3 C3 1.456(7) . ? O4 C25 1.366(7) . ? O4 C4 1.430(7) . ? O5 C7 1.359(7) . ? O5 C32 1.368(7) . ? O6 C39 1.380(7) . ? O6 C8 1.410(7) . ? O7 C46 1.368(7) . ? O7 C9 1.395(8) . ? O8 C17 1.215(8) . ? O9 C17 1.267(7) . ? O10 C24 1.257(7) . ? O10 Mn2 2.231(4) 11_454 ? O10 Mn1 2.288(4) 11_454 ? O11 C24 1.212(7) . ? O11 Mn1 2.266(4) 11_454 ? O12 C31 1.225(7) . ? O13 C31 1.292(7) . ? O13 Mn3 2.213(4) 8_544 ? O13 Mn2 2.218(4) 8_544 ? O14 C38 1.215(7) . ? O15 C38 1.267(7) . ? O16 C45 1.286(7) . ? O16 Mn3 2.098(4) 3_554 ? O17 C45 1.198(7) . ? O17 Mn2 2.136(4) 3_554 ? O18 C52 1.238(8) . ? O18 Mn2 2.126(4) 8_544 ? O19 C52 1.208(8) . ? O19 Mn1 2.032(4) 8_544 ? C1 C5 1.444(8) . ? C1 C4 1.538(8) . ? C1 C3 1.528(8) . ? C1 C2 1.547(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C9 1.493(9) . ? C6 C10 1.515(9) . ? C6 C7 1.510(8) . ? C6 C8 1.538(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.334(9) . ? C11 C16 1.373(9) . ? C12 C13 1.394(9) . ? C12 H12A 0.9300 . ? C13 C14 1.347(8) . ? C13 H13A 0.9300 . ? C14 C15 1.367(8) . ? C14 C17 1.538(8) . ? C15 C16 1.376(9) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C18 C23 1.310(9) . ? C18 C19 1.366(9) . ? C19 C20 1.333(8) . ? C19 H19A 0.9300 . ? C20 C21 1.360(8) . ? C20 H20A 0.9300 . ? C21 C22 1.377(8) . ? C21 C24 1.519(8) . ? C22 C23 1.382(9) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 Mn1 2.606(7) 11_454 ? C25 C26 1.361(8) . ? C25 C30 1.382(9) . ? C26 C27 1.399(8) . ? C26 H26A 0.9300 . ? C27 C28 1.329(8) . ? C27 H27A 0.9300 . ? C28 C29 1.362(8) . ? C28 C31 1.486(8) . ? C29 C30 1.385(8) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C32 C33 1.328(9) . ? C32 C37 1.339(9) . ? C33 C34 1.349(9) . ? C33 H33A 0.9300 . ? C34 C35 1.379(8) . ? C34 H34A 0.9300 . ? C35 C36 1.364(9) . ? C35 C38 1.460(8) . ? C36 C37 1.365(9) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C39 C44 1.323(9) . ? C39 C40 1.383(9) . ? C40 C41 1.338(8) . ? C40 H40A 0.9300 . ? C41 C42 1.352(8) . ? C41 H41A 0.9300 . ? C42 C43 1.351(9) . ? C42 C45 1.499(8) . ? C43 C44 1.440(8) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C46 C51 1.293(9) . ? C46 C47 1.386(9) . ? C47 C48 1.413(9) . ? C47 H47A 0.9300 . ? C48 C49 1.355(9) . ? C48 H48A 0.9300 . ? C49 C50 1.341(9) . ? C49 C52 1.537(9) . ? C50 C51 1.411(9) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C53 H53A 0.9300 . ? C54 C55 1.295(9) . ? C54 H54A 0.9300 . ? C55 H55A 0.9300 . ? C56 C61 1.273(11) . ? C56 C57 1.330(9) . ? C57 C58 1.432(11) . ? C57 H57A 0.9300 . ? C58 C59 1.355(10) . ? C58 H58A 0.9300 . ? C59 C60 1.324(10) . ? C59 N4 1.409(8) 14_556 ? C60 C61 1.454(12) . ? C60 H60A 0.9300 . ? C61 H61A 0.9300 . ? C62 H62A 0.9300 . ? C63 C64 1.355(11) . ? C63 H63A 0.9300 . ? C64 H64A 0.9300 . ? 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 O19 Mn1 O1W 104.44(19) 4 . ? O19 Mn1 O9 100.87(16) 4 . ? O1W Mn1 O9 84.59(17) . . ? O19 Mn1 O11 154.86(18) 4 3 ? O1W Mn1 O11 99.15(17) . 3 ? O9 Mn1 O11 89.79(15) . 3 ? O19 Mn1 O10 99.81(17) 4 3 ? O1W Mn1 O10 155.63(17) . 3 ? O9 Mn1 O10 93.26(16) . 3 ? O11 Mn1 O10 56.52(15) 3 3 ? O19 Mn1 N3 88.89(19) 4 . ? O1W Mn1 N3 82.5(2) . . ? O9 Mn1 N3 165.4(2) . . ? O11 Mn1 N3 85.64(18) 3 . ? O10 Mn1 N3 95.73(19) 3 . ? O19 Mn1 C24 128.2(2) 4 3 ? O1W Mn1 C24 126.8(2) . 3 ? O9 Mn1 C24 91.58(16) . 3 ? O11 Mn1 C24 27.68(16) 3 3 ? O10 Mn1 C24 28.83(16) 3 3 ? N3 Mn1 C24 90.78(19) . 3 ? O8 Mn2 O18 102.20(18) . 4 ? O8 Mn2 O17 85.38(17) . 11_455 ? O18 Mn2 O17 89.41(18) 4 11_455 ? O8 Mn2 O15 92.53(17) . . ? O18 Mn2 O15 165.23(19) 4 . ? O17 Mn2 O15 90.68(18) 11_455 . ? O8 Mn2 O13 168.03(16) . 4 ? O18 Mn2 O13 89.75(17) 4 4 ? O17 Mn2 O13 95.50(17) 11_455 4 ? O15 Mn2 O13 75.54(16) . 4 ? O8 Mn2 O10 86.76(16) . 3 ? O18 Mn2 O10 90.76(17) 4 3 ? O17 Mn2 O10 171.99(17) 11_455 3 ? O15 Mn2 O10 91.20(16) . 3 ? O13 Mn2 O10 92.51(15) 4 3 ? O16 Mn3 O14 97.61(18) 11_455 . ? O16 Mn3 O2W 80.51(17) 11_455 . ? O14 Mn3 O2W 93.35(19) . . ? O16 Mn3 N1 162.52(19) 11_455 . ? O14 Mn3 N1 92.20(18) . . ? O2W Mn3 N1 84.52(18) . . ? O16 Mn3 O13 92.49(16) 11_455 4 ? O14 Mn3 O13 122.83(18) . 4 ? O2W Mn3 O13 143.81(16) . 4 ? N1 Mn3 O13 94.30(18) . 4 ? O16 Mn3 O15 99.84(16) 11_455 . ? O14 Mn3 O15 54.01(17) . . ? O2W Mn3 O15 147.28(15) . . ? N1 Mn3 O15 97.64(17) . . ? O13 Mn3 O15 68.82(15) 4 . ? C53 N1 C54 102.2(6) . . ? C53 N1 Mn3 129.9(5) . . ? C54 N1 Mn3 126.2(5) . . ? C53 N2 C55 106.8(6) . . ? C53 N2 C56 126.0(6) . . ? C55 N2 C56 127.1(6) . . ? C62 N3 C64 105.5(6) . . ? C62 N3 Mn1 128.7(5) . . ? C64 N3 Mn1 123.7(5) . . ? C62 N4 C63 104.7(7) . . ? C62 N4 C59 131.8(6) . 14_554 ? C63 N4 C59 123.1(7) . 14_554 ? C5 O1 C10 113.4(5) . . ? Mn1 O1W H1WB 109.2 . . ? Mn1 O1W H1WA 109.3 . . ? H1WB O1W H1WA 109.5 . . ? C11 O2 C2 118.4(5) . . ? Mn3 O2W H2WA 109.4 . . ? Mn3 O2W H2WB 109.2 . . ? H2WA O2W H2WB 109.5 . . ? C18 O3 C3 117.3(5) . . ? C25 O4 C4 118.8(5) . . ? C7 O5 C32 116.1(5) . . ? C39 O6 C8 115.2(5) . . ? C46 O7 C9 119.3(5) . . ? C17 O8 Mn2 146.1(4) . . ? C17 O9 Mn1 119.8(4) . . ? C24 O10 Mn2 151.4(4) . 11_454 ? C24 O10 Mn1 89.8(4) . 11_454 ? Mn2 O10 Mn1 103.60(15) 11_454 11_454 ? C24 O11 Mn1 92.0(4) . 11_454 ? C31 O13 Mn3 105.8(4) . 8_544 ? C31 O13 Mn2 144.0(4) . 8_544 ? Mn3 O13 Mn2 99.33(15) 8_544 8_544 ? C38 O14 Mn3 102.3(4) . . ? C38 O15 Mn2 147.4(4) . . ? C38 O15 Mn3 84.8(4) . . ? Mn2 O15 Mn3 93.05(16) . . ? C45 O16 Mn3 127.1(4) . 3_554 ? C45 O17 Mn2 134.6(4) . 3_554 ? C52 O18 Mn2 127.2(4) . 8_544 ? C52 O19 Mn1 125.9(4) . 8_544 ? C5 C1 C4 109.1(5) . . ? C5 C1 C3 110.3(6) . . ? C4 C1 C3 110.6(5) . . ? C5 C1 C2 110.4(5) . . ? C4 C1 C2 106.3(5) . . ? C3 C1 C2 110.0(5) . . ? O2 C2 C1 103.5(5) . . ? O2 C2 H2A 111.1 . . ? C1 C2 H2A 111.1 . . ? O2 C2 H2B 111.1 . . ? C1 C2 H2B 111.1 . . ? H2A C2 H2B 109.0 . . ? O3 C3 C1 107.1(5) . . ? O3 C3 H3A 110.3 . . ? C1 C3 H3A 110.3 . . ? O3 C3 H3B 110.3 . . ? C1 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? O4 C4 C1 104.8(5) . . ? O4 C4 H4A 110.8 . . ? C1 C4 H4A 110.8 . . ? O4 C4 H4B 110.8 . . ? C1 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? O1 C5 C1 111.5(6) . . ? O1 C5 H5A 109.3 . . ? C1 C5 H5A 109.3 . . ? O1 C5 H5B 109.3 . . ? C1 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C9 C6 C10 111.9(5) . . ? C9 C6 C7 108.7(5) . . ? C10 C6 C7 110.6(5) . . ? C9 C6 C8 109.5(5) . . ? C10 C6 C8 104.9(5) . . ? C7 C6 C8 111.2(5) . . ? O5 C7 C6 111.5(5) . . ? O5 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? O5 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? O6 C8 C6 108.3(6) . . ? O6 C8 H8A 110.0 . . ? C6 C8 H8A 110.0 . . ? O6 C8 H8B 110.0 . . ? C6 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? O7 C9 C6 110.3(6) . . ? O7 C9 H9A 109.6 . . ? C6 C9 H9A 109.6 . . ? O7 C9 H9B 109.6 . . ? C6 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? O1 C10 C6 106.5(6) . . ? O1 C10 H10A 110.4 . . ? C6 C10 H10A 110.4 . . ? O1 C10 H10B 110.4 . . ? C6 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? C12 C11 C16 118.8(6) . . ? C12 C11 O2 125.7(6) . . ? C16 C11 O2 115.6(6) . . ? C11 C12 C13 120.6(6) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 119.6(6) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 121.3(6) . . ? C13 C14 C17 118.5(6) . . ? C15 C14 C17 119.9(6) . . ? C14 C15 C16 117.5(6) . . ? C14 C15 H15A 121.2 . . ? C16 C15 H15A 121.2 . . ? C11 C16 C15 122.2(7) . . ? C11 C16 H16A 118.9 . . ? C15 C16 H16A 118.9 . . ? O8 C17 O9 126.2(6) . . ? O8 C17 C14 116.3(6) . . ? O9 C17 C14 117.5(6) . . ? C23 C18 O3 125.2(6) . . ? C23 C18 C19 118.7(6) . . ? O3 C18 C19 116.2(7) . . ? C20 C19 C18 122.9(7) . . ? C20 C19 H19A 118.6 . . ? C18 C19 H19A 118.6 . . ? C19 C20 C21 118.7(6) . . ? C19 C20 H20A 120.7 . . ? C21 C20 H20A 120.7 . . ? C20 C21 C22 119.6(6) . . ? C20 C21 C24 121.0(5) . . ? C22 C21 C24 119.4(6) . . ? C21 C22 C23 119.0(7) . . ? C21 C22 H22A 120.5 . . ? C23 C22 H22A 120.5 . . ? C18 C23 C22 121.1(6) . . ? C18 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? O11 C24 O10 121.7(6) . . ? O11 C24 C21 118.3(5) . . ? O10 C24 C21 120.0(6) . . ? O11 C24 Mn1 60.3(3) . 11_454 ? O10 C24 Mn1 61.4(3) . 11_454 ? C21 C24 Mn1 178.5(5) . 11_454 ? O4 C25 C26 114.9(7) . . ? O4 C25 C30 124.2(6) . . ? C26 C25 C30 120.9(7) . . ? C25 C26 C27 119.5(7) . . ? C25 C26 H26A 120.3 . . ? C27 C26 H26A 120.3 . . ? C28 C27 C26 120.2(6) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 120.4(6) . . ? C27 C28 C31 119.9(5) . . ? C29 C28 C31 119.5(6) . . ? C28 C29 C30 121.5(7) . . ? C28 C29 H29A 119.3 . . ? C30 C29 H29A 119.3 . . ? C25 C30 C29 117.6(6) . . ? C25 C30 H30A 121.2 . . ? C29 C30 H30A 121.2 . . ? O12 C31 O13 118.2(6) . . ? O12 C31 C28 122.0(6) . . ? O13 C31 C28 119.6(6) . . ? C33 C32 C37 118.3(6) . . ? C33 C32 O5 126.1(6) . . ? C37 C32 O5 115.6(6) . . ? C32 C33 C34 122.9(7) . . ? C32 C33 H33A 118.5 . . ? C34 C33 H33A 118.5 . . ? C33 C34 C35 119.4(7) . . ? C33 C34 H34A 120.3 . . ? C35 C34 H34A 120.3 . . ? C36 C35 C34 117.4(6) . . ? C36 C35 C38 122.7(6) . . ? C34 C35 C38 119.8(6) . . ? C35 C36 C37 120.8(7) . . ? C35 C36 H36A 119.6 . . ? C37 C36 H36A 119.6 . . ? C32 C37 C36 120.9(7) . . ? C32 C37 H37A 119.5 . . ? C36 C37 H37A 119.5 . . ? O14 C38 O15 118.8(6) . . ? O14 C38 C35 122.8(6) . . ? O15 C38 C35 118.4(7) . . ? C44 C39 O6 125.1(6) . . ? C44 C39 C40 121.4(6) . . ? O6 C39 C40 113.4(6) . . ? C41 C40 C39 119.4(7) . . ? C41 C40 H40A 120.3 . . ? C39 C40 H40A 120.3 . . ? C40 C41 C42 122.2(6) . . ? C40 C41 H41A 118.9 . . ? C42 C41 H41A 118.9 . . ? C41 C42 C43 118.6(6) . . ? C41 C42 C45 123.7(6) . . ? C43 C42 C45 117.7(6) . . ? C42 C43 C44 120.6(7) . . ? C42 C43 H43A 119.7 . . ? C44 C43 H43A 119.7 . . ? C39 C44 C43 117.5(6) . . ? C39 C44 H44A 121.2 . . ? C43 C44 H44A 121.2 . . ? O17 C45 O16 125.6(6) . . ? O17 C45 C42 119.6(6) . . ? O16 C45 C42 114.9(6) . . ? C51 C46 O7 126.8(7) . . ? C51 C46 C47 121.3(6) . . ? O7 C46 C47 111.8(6) . . ? C46 C47 C48 117.6(7) . . ? C46 C47 H47A 121.2 . . ? C48 C47 H47A 121.2 . . ? C49 C48 C47 121.2(7) . . ? C49 C48 H48A 119.4 . . ? C47 C48 H48A 119.4 . . ? C50 C49 C48 118.2(6) . . ? C50 C49 C52 122.9(7) . . ? C48 C49 C52 118.9(7) . . ? C49 C50 C51 121.1(7) . . ? C49 C50 H50A 119.4 . . ? C51 C50 H50A 119.4 . . ? C46 C51 C50 120.3(7) . . ? C46 C51 H51A 119.8 . . ? C50 C51 H51A 119.8 . . ? O19 C52 O18 130.5(7) . . ? O19 C52 C49 115.7(6) . . ? O18 C52 C49 113.8(7) . . ? N1 C53 N2 112.3(7) . . ? N1 C53 H53A 123.9 . . ? N2 C53 H53A 123.9 . . ? C55 C54 N1 113.4(7) . . ? C55 C54 H54A 123.3 . . ? N1 C54 H54A 123.3 . . ? C54 C55 N2 104.9(7) . . ? C54 C55 H55A 127.6 . . ? N2 C55 H55A 127.6 . . ? C61 C56 C57 120.7(8) . . ? C61 C56 N2 120.8(8) . . ? C57 C56 N2 118.5(6) . . ? C56 C57 C58 118.8(8) . . ? C56 C57 H57A 120.6 . . ? C58 C57 H57A 120.6 . . ? C59 C58 C57 120.0(8) . . ? C59 C58 H58A 120.0 . . ? C57 C58 H58A 120.0 . . ? C60 C59 C58 120.4(9) . . ? C60 C59 N4 118.4(8) . 14_556 ? C58 C59 N4 121.1(7) . 14_556 ? C59 C60 C61 117.2(10) . . ? C59 C60 H60A 121.4 . . ? C61 C60 H60A 121.4 . . ? C56 C61 C60 122.9(10) . . ? C56 C61 H61A 118.6 . . ? C60 C61 H61A 118.6 . . ? N3 C62 N4 113.8(6) . . ? N3 C62 H62A 123.1 . . ? N4 C62 H62A 123.1 . . ? C64 C63 N4 106.3(9) . . ? C64 C63 H63A 126.9 . . ? N4 C63 H63A 126.9 . . ? N3 C64 C63 109.1(8) . . ? N3 C64 H64A 125.5 . . ? C63 C64 H64A 125.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.29 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.577 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.078 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 _platon_squeeze_void_content 1 0.000 0.000 0.034 225 49 ' ' 2 0.092 0.131 0.620 15993 6021 ' ' 3 0.000 0.500 0.534 225 49 ' ' 4 0.250 0.250 0.284 225 49 ' ' 5 0.250 0.750 0.784 225 49 ' ' 6 0.500 0.500 1.034 225 49 ' ' 7 0.500 1.000 0.534 225 49 ' ' 8 0.750 0.250 0.784 225 49 ' ' 9 0.750 0.750 0.284 225 49 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 950527' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C131 H107 Mn6 N6 O43' _chemical_formula_weight 2782.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3269(12) _cell_length_b 25.4411(18) _cell_length_c 31.096(2) _cell_angle_alpha 73.244(2) _cell_angle_beta 80.178(2) _cell_angle_gamma 82.093(2) _cell_volume 11389.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 26.09 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2858 _exptl_absorpt_coefficient_mu 0.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6388 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details 'Sheldrick, G. M. (2008). SADABS' _exptl_special_details ; The ADP atoms containing carbon atoms [C(14), C(15), C(16), C(17), C(107) and C(117)] and oxygen atoms [O(8), O(29)] have been refined with isotropic thermal parameter. ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63483 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.2545 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 26.09 _reflns_number_total 44289 _reflns_number_gt 12274 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^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_number_reflns 44289 _refine_ls_number_parameters 1614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1870 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.1985 _refine_ls_wR_factor_gt 0.1836 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.002 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 0.79404(7) 0.26129(3) 0.47823(3) 0.0470(3) Uani 1 1 d . . . Mn2 Mn 0.81238(7) 0.11757(3) 0.47341(3) 0.0526(3) Uani 1 1 d . . . Mn3 Mn 0.78005(8) 0.40188(3) 0.48588(3) 0.0637(4) Uani 1 1 d . . . Mn4 Mn 0.25430(7) 0.77067(3) -0.02018(3) 0.0480(3) Uani 1 1 d . . . Mn5 Mn 0.04365(7) 0.83212(3) 0.02315(3) 0.0545(3) Uani 1 1 d . . . Mn6 Mn 0.44743(7) 0.70409(4) -0.07470(3) 0.0662(3) Uani 1 1 d . . . N1 N 0.8420(4) 0.02743(16) 0.49338(15) 0.0688(18) Uani 1 1 d . . . N2 N 0.8512(4) -0.06269(15) 0.50236(15) 0.0587(16) Uani 1 1 d . . . N5 N -0.0617(3) 0.89314(17) 0.03802(18) 0.0703(17) Uani 1 1 d . . . N6 N -0.1904(4) 0.94469(18) 0.03110(19) 0.0746(18) Uani 1 1 d . . . O1W O 0.7461(3) 0.10940(14) 0.41798(12) 0.0713(14) Uani 1 1 d . . . H1WA H 0.7240 0.1454 0.4014 0.107 Uiso 1 1 d R . . H1WB H 0.6974 0.0872 0.4308 0.107 Uiso 1 1 d R . . O1 O 0.3580(3) 0.12857(15) 0.74123(13) 0.0722(13) Uani 1 1 d . . . O2W O 0.8644(10) 0.4077(5) 0.5402(3) 0.427(10) Uani 1 1 d . . . H2WB H 0.8981 0.3732 0.5517 0.641 Uiso 1 1 d R . . H2WA H 0.8272 0.4186 0.5649 0.641 Uiso 1 1 d R . . O2 O 0.5458(4) 0.20139(15) 0.72132(14) 0.109(2) Uani 1 1 d . . . O3W O 0.5729(4) 0.7167(2) -0.0505(3) 0.181(3) Uani 1 1 d . . . H3WA H 0.5588 0.7420 -0.0321 0.271 Uiso 1 1 d R . . H3WB H 0.6155 0.7313 -0.0762 0.271 Uiso 1 1 d R . . O3 O 0.6049(3) 0.11956(15) 0.81837(13) 0.0690(13) Uani 1 1 d . . . O4W O 0.5384(4) 0.6501(2) -0.1089(2) 0.148(2) Uani 1 1 d . . . H4WA H 0.5051 0.6342 -0.1246 0.222 Uiso 1 1 d R . . H4WB H 0.5666 0.6214 -0.0867 0.222 Uiso 1 1 d R . . O4 O 0.4378(3) 0.04121(14) 0.82888(12) 0.0682(13) Uani 1 1 d . . . O5W O -0.0567(4) 0.7974(2) -0.0029(2) 0.148(3) Uani 1 1 d . . . H5WB H -0.0951 0.7765 0.0219 0.222 Uiso 1 1 d R . . H5WA H -0.0257 0.7737 -0.0208 0.222 Uiso 1 1 d R . . O5 O 0.3313(3) 0.16074(14) 0.64098(12) 0.0611(12) Uani 1 1 d . . . O6 O 0.1204(3) 0.09890(14) 0.67495(13) 0.0737(14) Uani 1 1 d . . . O7 O 0.1612(3) 0.05588(14) 0.77356(12) 0.0676(13) Uani 1 1 d . . . O8 O 0.6903(6) 0.3818(3) 0.5474(3) 0.214(3) Uiso 1 1 d . . . O9 O 0.7520(3) 0.31264(13) 0.52615(12) 0.0716(15) Uani 1 1 d . . . O10 O 0.8647(3) 0.13718(16) 0.94953(15) 0.0785(14) Uani 1 1 d . . . O11 O 0.7377(3) 0.17269(14) 0.98137(12) 0.0629(13) Uani 1 1 d . . . O12 O 0.3825(3) -0.20896(15) 0.93735(12) 0.0628(13) Uani 1 1 d . . . O13 O 0.4562(3) -0.21873(15) 0.87214(14) 0.0856(16) Uani 1 1 d . . . O14 O 0.6724(3) 0.22346(14) 0.49835(13) 0.0693(13) Uani 1 1 d . . . O15 O 0.6867(3) 0.13195(14) 0.50722(13) 0.0687(13) Uani 1 1 d . . . O16 O -0.1472(3) 0.20509(13) 0.53286(12) 0.0656(14) Uani 1 1 d . . . O17 O -0.1180(3) 0.11979(13) 0.52554(12) 0.0658(14) Uani 1 1 d . . . O18 O 0.1924(3) -0.16669(15) 0.92863(12) 0.0672(13) Uani 1 1 d . . . O19 O 0.0738(3) -0.1205(2) 0.95874(14) 0.116(2) Uani 1 1 d . . . O20 O 0.2210(3) 0.41610(15) 0.22104(13) 0.0695(13) Uani 1 1 d . . . O21 O 0.4050(3) 0.49456(15) 0.18675(14) 0.0846(15) Uani 1 1 d . . . O22 O 0.4636(3) 0.44553(14) 0.28472(14) 0.0824(16) Uani 1 1 d . . . O23 O 0.2623(3) 0.37902(14) 0.32091(13) 0.0729(14) Uani 1 1 d . . . O24 O 0.1245(3) 0.49846(13) 0.13601(12) 0.0654(13) Uani 1 1 d . . . O25 O -0.0298(3) 0.41139(16) 0.15192(15) 0.0793(14) Uani 1 1 d . . . O26 O 0.0599(3) 0.32882(14) 0.24554(12) 0.0669(13) Uani 1 1 d . . . O27 O 0.4261(4) 0.65667(17) -0.00917(14) 0.1009(18) Uani 1 1 d . . . O28 O 0.3252(3) 0.70953(14) 0.02772(13) 0.0669(13) Uani 1 1 d . . . O29 O 0.7085(3) 0.40076(18) 0.43573(15) 0.0987(16) Uiso 1 1 d . . . O30 O 0.7297(3) 0.31876(13) 0.42476(12) 0.0603(13) Uani 1 1 d . . . O31 O -0.0997(4) 0.38538(16) 0.45387(18) 0.114(2) Uani 1 1 d . . . O32 O -0.0825(3) 0.29667(13) 0.45300(12) 0.0607(13) Uani 1 1 d . . . O33 O 0.1255(3) 0.75049(13) 0.02270(11) 0.0553(12) Uani 1 1 d . . . O34 O 0.0322(3) 0.75771(15) 0.08250(13) 0.0862(16) Uani 1 1 d . . . O35 O -0.2289(3) 0.28815(15) 0.05324(13) 0.0729(14) Uani 1 1 d . . . O36 O -0.3428(3) 0.32069(19) 0.09839(14) 0.0904(16) Uani 1 1 d . . . O37 O -0.0689(3) 0.13945(13) 0.41917(12) 0.0616(13) Uani 1 1 d . . . O38 O -0.1684(3) 0.20656(13) 0.43173(11) 0.0487(11) Uani 1 1 d . . . C1 C 0.4844(5) 0.1238(3) 0.7772(2) 0.059(2) Uani 1 1 d . . . C2 C 0.5462(4) 0.1450(2) 0.7310(2) 0.063(2) Uani 1 1 d . . . H2A H 0.6063 0.1277 0.7333 0.076 Uiso 1 1 calc R . . H2B H 0.5246 0.1355 0.7069 0.076 Uiso 1 1 calc R . . C3 C 0.5159(4) 0.1420(2) 0.81345(19) 0.062(2) Uani 1 1 d . . . H3A H 0.5127 0.1819 0.8054 0.074 Uiso 1 1 calc R . . H3B H 0.4778 0.1296 0.8420 0.074 Uiso 1 1 calc R . . C4 C 0.4910(4) 0.0625(2) 0.78716(18) 0.058(2) Uani 1 1 d . . . H4A H 0.4706 0.0521 0.7631 0.070 Uiso 1 1 calc R . . H4B H 0.5524 0.0474 0.7889 0.070 Uiso 1 1 calc R . . C5 C 0.3909(5) 0.1490(2) 0.7729(2) 0.070(2) Uani 1 1 d . . . H5A H 0.3540 0.1392 0.8021 0.083 Uiso 1 1 calc R . . H5B H 0.3896 0.1888 0.7624 0.083 Uiso 1 1 calc R . . C6 C 0.2431(5) 0.1130(2) 0.7070(2) 0.0521(19) Uani 1 1 d . . . C7 C 0.3078(4) 0.1075(2) 0.6673(2) 0.061(2) Uani 1 1 d . . . H7A H 0.3605 0.0845 0.6773 0.073 Uiso 1 1 calc R . . H7B H 0.2821 0.0901 0.6491 0.073 Uiso 1 1 calc R . . C8 C 0.1529(5) 0.1395(2) 0.6922(2) 0.073(2) Uani 1 1 d . . . H8A H 0.1119 0.1469 0.7176 0.087 Uiso 1 1 calc R . . H8B H 0.1599 0.1738 0.6686 0.087 Uiso 1 1 calc R . . C9 C 0.2356(4) 0.0550(2) 0.73850(18) 0.063(2) Uani 1 1 d . . . H9A H 0.2273 0.0301 0.7214 0.075 Uiso 1 1 calc R . . H9B H 0.2899 0.0419 0.7520 0.075 Uiso 1 1 calc R . . C10 C 0.2693(4) 0.1494(2) 0.7319(2) 0.073(2) Uani 1 1 d . . . H10A H 0.2680 0.1873 0.7135 0.088 Uiso 1 1 calc R . . H10B H 0.2292 0.1478 0.7599 0.088 Uiso 1 1 calc R . . C11 C 0.5845(4) 0.2271(2) 0.67969(16) 0.136(4) Uani 1 1 d G . . C12 C 0.6416(4) 0.20343(14) 0.64913(18) 0.066(2) Uani 1 1 d G . . C13 C 0.6815(3) 0.2368(2) 0.60884(15) 0.067(2) Uani 1 1 d G . . C14 C 0.6643(4) 0.29374(19) 0.59909(17) 0.128(3) Uiso 1 1 d G . . C15 C 0.6072(5) 0.31741(15) 0.6297(2) 0.312(8) Uiso 1 1 d G . . C16 C 0.5673(5) 0.2841(3) 0.6700(2) 0.270(7) Uiso 1 1 d G . . C17 C 0.7209(6) 0.3259(3) 0.5553(3) 0.116(3) Uiso 1 1 d . . . C18 C 0.6452(6) 0.1292(3) 0.8512(2) 0.068(2) Uani 1 1 d . . . C19 C 0.6001(4) 0.1594(2) 0.8819(2) 0.0574(19) Uani 1 1 d . . . H19A H 0.5415 0.1744 0.8804 0.069 Uiso 1 1 calc R . . C20 C 0.6484(5) 0.1653(2) 0.9141(2) 0.060(2) Uani 1 1 d . . . H20A H 0.6212 0.1852 0.9344 0.072 Uiso 1 1 calc R . . C21 C 0.7322(5) 0.1433(3) 0.9170(2) 0.055(2) Uani 1 1 d . . . C22 C 0.7754(5) 0.1137(3) 0.8861(3) 0.072(2) Uani 1 1 d . . . H22A H 0.8339 0.0988 0.8881 0.086 Uiso 1 1 calc R . . C23 C 0.7332(6) 0.1064(3) 0.8535(2) 0.077(2) Uani 1 1 d . . . H23A H 0.7621 0.0869 0.8333 0.092 Uiso 1 1 calc R . . C24 C 0.7833(5) 0.1524(2) 0.9530(2) 0.069(2) Uani 1 1 d . . . C25 C 0.4359(4) -0.0147(2) 0.8432(2) 0.0512(18) Uani 1 1 d . . . C26 C 0.3924(5) -0.0366(3) 0.8868(2) 0.062(2) Uani 1 1 d . . . H26A H 0.3680 -0.0122 0.9040 0.075 Uiso 1 1 calc R . . C27 C 0.3836(5) -0.0911(3) 0.9057(2) 0.063(2) Uani 1 1 d . . . H27A H 0.3544 -0.1039 0.9350 0.076 Uiso 1 1 calc R . . C28 C 0.4195(5) -0.1270(3) 0.8799(2) 0.058(2) Uani 1 1 d . . . C29 C 0.4630(5) -0.1074(3) 0.8365(2) 0.066(2) Uani 1 1 d . . . H29A H 0.4863 -0.1319 0.8193 0.080 Uiso 1 1 calc R . . C30 C 0.4724(5) -0.0501(2) 0.8178(2) 0.066(2) Uani 1 1 d . . . H30A H 0.5029 -0.0370 0.7889 0.079 Uiso 1 1 calc R . . C31 C 0.4198(4) -0.1888(2) 0.89710(19) 0.0604(19) Uani 1 1 d . . . C32 C 0.4040(5) 0.1614(3) 0.6102(2) 0.057(2) Uani 1 1 d . . . C33 C 0.4473(6) 0.1193(3) 0.5951(2) 0.071(2) Uani 1 1 d . . . H33A H 0.4238 0.0854 0.6060 0.086 Uiso 1 1 calc R . . C34 C 0.5233(5) 0.1226(3) 0.5647(2) 0.064(2) Uani 1 1 d . . . H34A H 0.5509 0.0915 0.5563 0.076 Uiso 1 1 calc R . . C35 C 0.5587(5) 0.1724(3) 0.5468(2) 0.059(2) Uani 1 1 d . . . C36 C 0.5152(5) 0.2164(3) 0.5608(2) 0.060(2) Uani 1 1 d . . . H36A H 0.5389 0.2502 0.5492 0.072 Uiso 1 1 calc R . . C37 C 0.4394(5) 0.2134(2) 0.5909(2) 0.067(2) Uani 1 1 d . . . H37A H 0.4109 0.2447 0.5987 0.081 Uiso 1 1 calc R . . C38 C 0.6422(5) 0.1765(2) 0.5155(2) 0.071(2) Uani 1 1 d . . . C39 C 0.0599(4) 0.1160(3) 0.64483(18) 0.0539(19) Uani 1 1 d . . . C40 C 0.0472(4) 0.0762(2) 0.6251(2) 0.059(2) Uani 1 1 d . . . H40A H 0.0758 0.0408 0.6336 0.071 Uiso 1 1 calc R . . C41 C -0.0084(4) 0.0897(2) 0.59278(19) 0.0513(18) Uani 1 1 d . . . H41A H -0.0143 0.0638 0.5778 0.062 Uiso 1 1 calc R . . C42 C -0.0570(5) 0.1416(2) 0.58151(18) 0.0533(19) Uani 1 1 d . . . C43 C -0.0458(4) 0.1786(2) 0.60405(19) 0.0563(19) Uani 1 1 d . . . H43A H -0.0795 0.2126 0.5983 0.068 Uiso 1 1 calc R . . C44 C 0.0146(5) 0.1673(2) 0.63539(19) 0.057(2) Uani 1 1 d . . . H44A H 0.0235 0.1937 0.6492 0.068 Uiso 1 1 calc R . . C45 C -0.1103(4) 0.15598(19) 0.54385(18) 0.0474(18) Uani 1 1 d . . . C46 C 0.1577(5) 0.0094(3) 0.8079(2) 0.0563(19) Uani 1 1 d . . . C47 C 0.2133(5) -0.0379(3) 0.8098(2) 0.060(2) Uani 1 1 d . . . H47A H 0.2561 -0.0410 0.7854 0.072 Uiso 1 1 calc R . . C48 C 0.2045(5) -0.0809(3) 0.8487(3) 0.064(2) Uani 1 1 d . . . H48A H 0.2454 -0.1118 0.8510 0.077 Uiso 1 1 calc R . . C49 C 0.1389(6) -0.0802(3) 0.8840(2) 0.065(2) Uani 1 1 d . . . C50 C 0.0803(5) -0.0351(3) 0.8801(2) 0.074(2) Uani 1 1 d . . . H50A H 0.0333 -0.0340 0.9032 0.089 Uiso 1 1 calc R . . C51 C 0.0891(6) 0.0104(3) 0.8415(3) 0.080(2) Uani 1 1 d . . . H51A H 0.0478 0.0411 0.8391 0.097 Uiso 1 1 calc R . . C52 C 0.1334(5) -0.1271(3) 0.9279(2) 0.080(2) Uani 1 1 d . . . C53 C 0.3418(5) 0.4335(3) 0.2532(2) 0.061(2) Uani 1 1 d . . . C54 C 0.3390(5) 0.4932(2) 0.2255(2) 0.076(2) Uani 1 1 d . . . H54A H 0.2806 0.5060 0.2163 0.092 Uiso 1 1 calc R . . H54B H 0.3525 0.5164 0.2429 0.092 Uiso 1 1 calc R . . C55 C 0.4325(5) 0.4082(2) 0.2650(2) 0.074(2) Uani 1 1 d . . . H55A H 0.4286 0.3721 0.2864 0.089 Uiso 1 1 calc R . . H55B H 0.4724 0.4045 0.2380 0.089 Uiso 1 1 calc R . . C56 C 0.2770(5) 0.4343(2) 0.2938(2) 0.076(2) Uani 1 1 d . . . H56A H 0.2988 0.4539 0.3117 0.091 Uiso 1 1 calc R . . H56B H 0.2212 0.4536 0.2847 0.091 Uiso 1 1 calc R . . C57 C 0.3113(5) 0.3984(3) 0.2271(2) 0.081(2) Uani 1 1 d . . . H57A H 0.3480 0.4026 0.1978 0.098 Uiso 1 1 calc R . . H57B H 0.3169 0.3598 0.2439 0.098 Uiso 1 1 calc R . . C58 C 0.0952(5) 0.4125(2) 0.1885(2) 0.0514(19) Uani 1 1 d . . . C59 C 0.0780(5) 0.4744(2) 0.17934(18) 0.065(2) Uani 1 1 d . . . H59A H 0.0148 0.4855 0.1798 0.078 Uiso 1 1 calc R . . H59B H 0.0987 0.4865 0.2024 0.078 Uiso 1 1 calc R . . C60 C 0.0622(4) 0.3936(2) 0.1518(2) 0.066(2) Uani 1 1 d . . . H60A H 0.0949 0.4094 0.1223 0.080 Uiso 1 1 calc R . . H60B H 0.0713 0.3537 0.1582 0.080 Uiso 1 1 calc R . . C61 C 0.0394(4) 0.38874(19) 0.23460(19) 0.058(2) Uani 1 1 d . . . H61A H 0.0550 0.4030 0.2577 0.069 Uiso 1 1 calc R . . H61B H -0.0235 0.3985 0.2326 0.069 Uiso 1 1 calc R . . C62 C 0.1893(5) 0.3946(2) 0.18854(19) 0.065(2) Uani 1 1 d . . . H62A H 0.2216 0.4084 0.1585 0.077 Uiso 1 1 calc R . . H62B H 0.1984 0.3547 0.1971 0.077 Uiso 1 1 calc R . . C63 C 0.3964(5) 0.5393(3) 0.1491(3) 0.068(2) Uani 1 1 d . . . C64 C 0.3416(5) 0.5859(3) 0.1489(2) 0.082(2) Uani 1 1 d . . . H64A H 0.3075 0.5900 0.1757 0.099 Uiso 1 1 calc R . . C65 C 0.3357(5) 0.6277(3) 0.1090(2) 0.077(2) Uani 1 1 d . . . H65A H 0.2959 0.6587 0.1091 0.093 Uiso 1 1 calc R . . C66 C 0.3869(5) 0.6238(3) 0.0702(2) 0.065(2) Uani 1 1 d . . . C67 C 0.4482(6) 0.5755(3) 0.0701(3) 0.110(3) Uani 1 1 d . . . H67A H 0.4861 0.5724 0.0440 0.132 Uiso 1 1 calc R . . C68 C 0.4489(6) 0.5348(3) 0.1093(3) 0.099(3) Uani 1 1 d . . . H68A H 0.4859 0.5025 0.1095 0.119 Uiso 1 1 calc R . . C69 C 0.3740(5) 0.6688(3) 0.0263(2) 0.075(2) Uani 1 1 d . . . C70 C 0.5251(5) 0.4240(2) 0.3137(2) 0.073(2) Uani 1 1 d . . . C71 C 0.5391(6) 0.4581(2) 0.3385(3) 0.108(3) Uani 1 1 d . . . H71A H 0.5086 0.4930 0.3344 0.129 Uiso 1 1 calc R . . C72 C 0.5996(6) 0.4401(2) 0.3702(3) 0.100(3) Uani 1 1 d . . . H72A H 0.6112 0.4640 0.3858 0.120 Uiso 1 1 calc R . . C73 C 0.6423(5) 0.3872(2) 0.3786(2) 0.067(2) Uani 1 1 d . . . C74 C 0.6333(4) 0.3548(2) 0.3515(2) 0.062(2) Uani 1 1 d . . . H74A H 0.6668 0.3209 0.3550 0.075 Uiso 1 1 calc R . . C75 C 0.5739(5) 0.3715(2) 0.3181(2) 0.068(2) Uani 1 1 d . . . H75A H 0.5677 0.3491 0.3002 0.082 Uiso 1 1 calc R . . C76 C 0.1858(5) 0.3729(3) 0.3509(2) 0.069(2) Uani 1 1 d . . . C77 C 0.1370(6) 0.4129(3) 0.3696(3) 0.085(3) Uani 1 1 d . . . H77A H 0.1567 0.4480 0.3610 0.102 Uiso 1 1 calc R . . C78 C 0.0608(6) 0.4034(3) 0.4004(3) 0.080(3) Uani 1 1 d . . . H78A H 0.0326 0.4306 0.4138 0.096 Uiso 1 1 calc R . . C79 C 0.0269(5) 0.3527(3) 0.4109(2) 0.061(2) Uani 1 1 d . . . C80 C 0.0765(6) 0.3124(3) 0.3927(2) 0.063(2) Uani 1 1 d . . . H80A H 0.0573 0.2773 0.4014 0.076 Uiso 1 1 calc R . . C81 C 0.1513(5) 0.3219(2) 0.3630(2) 0.063(2) Uani 1 1 d . . . H81A H 0.1803 0.2941 0.3505 0.075 Uiso 1 1 calc R . . C82 C -0.0550(5) 0.3438(2) 0.4411(2) 0.067(2) Uani 1 1 d . . . C83 C 0.1135(5) 0.5555(3) 0.1214(2) 0.062(2) Uani 1 1 d . . . C84 C 0.1568(5) 0.5778(3) 0.0782(2) 0.063(2) Uani 1 1 d . . . H84A H 0.1920 0.5549 0.0623 0.076 Uiso 1 1 calc R . . C85 C 0.1473(5) 0.6345(2) 0.0589(2) 0.063(2) Uani 1 1 d . . . H85A H 0.1751 0.6493 0.0296 0.075 Uiso 1 1 calc R . . C86 C 0.0971(5) 0.6688(2) 0.0828(2) 0.0558(19) Uani 1 1 d . . . C87 C 0.0599(5) 0.6449(2) 0.1273(2) 0.071(2) Uani 1 1 d . . . H87A H 0.0299 0.6678 0.1446 0.086 Uiso 1 1 calc R . . C88 C 0.0660(5) 0.5900(3) 0.1460(2) 0.074(2) Uani 1 1 d . . . H88A H 0.0383 0.5753 0.1753 0.089 Uiso 1 1 calc R . . C89 C 0.0848(4) 0.7293(2) 0.06178(19) 0.061(2) Uani 1 1 d . . . C90 C -0.0793(6) 0.3872(3) 0.1324(3) 0.078(2) Uani 1 1 d . . . C91 C -0.0469(5) 0.3561(3) 0.1035(2) 0.083(2) Uani 1 1 d . . . H91A H 0.0139 0.3490 0.0951 0.099 Uiso 1 1 calc R . . C92 C -0.1119(7) 0.3347(3) 0.0867(2) 0.077(3) Uani 1 1 d . . . H92A H -0.0917 0.3143 0.0659 0.093 Uiso 1 1 calc R . . C93 C -0.2023(6) 0.3424(3) 0.0994(3) 0.072(2) Uani 1 1 d . . . C94 C -0.2335(6) 0.3739(4) 0.1270(3) 0.115(3) Uani 1 1 d . . . H94A H -0.2942 0.3808 0.1355 0.138 Uiso 1 1 calc R . . C95 C -0.1700(8) 0.3967(4) 0.1432(3) 0.120(3) Uani 1 1 d . . . H95A H -0.1910 0.4194 0.1621 0.144 Uiso 1 1 calc R . . C96 C -0.2605(5) 0.3148(2) 0.0806(2) 0.076(2) Uani 1 1 d . . . C97 C 0.0166(5) 0.2985(2) 0.2858(2) 0.057(2) Uani 1 1 d . . . C98 C 0.0530(5) 0.2442(2) 0.2986(2) 0.071(2) Uani 1 1 d . . . H98A H 0.1016 0.2310 0.2810 0.086 Uiso 1 1 calc R . . C99 C 0.0145(5) 0.2112(2) 0.3381(2) 0.071(2) Uani 1 1 d . . . H99A H 0.0400 0.1752 0.3479 0.086 Uiso 1 1 calc R . . C100 C -0.0616(5) 0.2282(2) 0.3651(2) 0.0530(19) Uani 1 1 d . . . C101 C -0.0981(4) 0.2823(2) 0.35023(19) 0.0474(18) Uani 1 1 d . . . H10C H -0.1489 0.2955 0.3664 0.057 Uiso 1 1 calc R . . C102 C -0.0567(5) 0.3160(2) 0.3107(2) 0.058(2) Uani 1 1 d . . . H10D H -0.0806 0.3524 0.3008 0.069 Uiso 1 1 calc R . . C103 C -0.1023(4) 0.19025(19) 0.40810(18) 0.0502(18) Uani 1 1 d . . . C104 C 0.8196(4) -0.01081(19) 0.47977(18) 0.0552(19) Uani 1 1 d . . . H10E H 0.7850 -0.0041 0.4566 0.066 Uiso 1 1 calc R . . C105 C 0.8981(6) -0.0549(3) 0.5317(3) 0.142(4) Uani 1 1 d . . . H10F H 0.9316 -0.0817 0.5511 0.170 Uiso 1 1 calc R . . C106 C 0.8874(7) -0.0003(3) 0.5278(3) 0.148(4) Uani 1 1 d . . . H10G H 0.9088 0.0162 0.5465 0.178 Uiso 1 1 calc R . . C107 C 0.8384(4) -0.1137(2) 0.49549(18) 0.0425(15) Uiso 1 1 d . . . C108 C 0.7728(5) -0.1188(2) 0.4729(2) 0.072(2) Uani 1 1 d . . . H10H H 0.7341 -0.0883 0.4616 0.086 Uiso 1 1 calc R . . C109 C 0.7639(5) -0.1684(2) 0.4669(2) 0.068(2) Uani 1 1 d . . . H10I H 0.7184 -0.1706 0.4513 0.081 Uiso 1 1 calc R . . C110 C 0.8162(5) -0.2142(2) 0.4818(2) 0.063(2) Uani 1 1 d . . . C111 C 0.8871(5) -0.2097(2) 0.5033(2) 0.062(2) Uani 1 1 d . . . H11B H 0.9276 -0.2400 0.5124 0.075 Uiso 1 1 calc R . . C112 C 0.8967(5) -0.1591(2) 0.5110(2) 0.066(2) Uani 1 1 d . . . H11C H 0.9421 -0.1562 0.5263 0.079 Uiso 1 1 calc R . . C113 C 0.8068(5) 0.7314(2) 0.4749(2) 0.066(2) Uani 1 1 d . . . C114 C 0.8206(6) 0.6844(2) 0.5048(2) 0.095(3) Uani 1 1 d . . . H11E H 0.8372 0.6844 0.5322 0.114 Uiso 1 1 calc R . . C115 C 0.8113(6) 0.6326(2) 0.4973(2) 0.103(3) Uani 1 1 d . . . H11F H 0.8286 0.5994 0.5174 0.124 Uiso 1 1 calc R . . C116 C 0.7782(5) 0.6337(2) 0.4617(2) 0.077(3) Uani 1 1 d . . . C117 C 0.7656(5) 0.6817(3) 0.4282(2) 0.077(2) Uiso 1 1 d . . . H11G H 0.7498 0.6813 0.4007 0.092 Uiso 1 1 calc R . . C118 C 0.7766(6) 0.7292(3) 0.4362(3) 0.109(3) Uani 1 1 d . . . H11H H 0.7633 0.7621 0.4147 0.131 Uiso 1 1 calc R . . C122 C -0.1474(5) 0.8968(2) 0.0320(2) 0.075(2) Uani 1 1 d . . . H12D H -0.1735 0.8675 0.0287 0.090 Uiso 1 1 calc R . . C123 C -0.1259(7) 0.9754(3) 0.0365(4) 0.157(5) Uani 1 1 d . . . H12E H -0.1348 1.0121 0.0371 0.189 Uiso 1 1 calc R . . C124 C -0.0490(7) 0.9431(3) 0.0406(4) 0.146(4) Uani 1 1 d . . . H12F H 0.0041 0.9536 0.0446 0.176 Uiso 1 1 calc R . . C125 C -0.2781(5) 0.9612(3) 0.0230(3) 0.067(2) Uani 1 1 d . . . C126 C -0.3444(6) 0.9265(3) 0.0431(3) 0.106(3) Uani 1 1 d . . . H12G H -0.3305 0.8928 0.0634 0.128 Uiso 1 1 calc R . . C127 C -0.4301(5) 0.9409(3) 0.0339(3) 0.088(3) Uani 1 1 d . . . H12H H -0.4723 0.9159 0.0471 0.106 Uiso 1 1 calc R . . C128 C -0.4556(4) 0.9913(3) 0.0058(2) 0.0505(18) Uani 1 1 d . . . C129 C -0.3891(6) 1.0277(3) -0.0102(2) 0.084(2) Uani 1 1 d . . . H12J H -0.4047 1.0632 -0.0275 0.101 Uiso 1 1 calc R . . C130 C -0.3027(6) 1.0142(3) -0.0021(3) 0.097(3) Uani 1 1 d . . . H13B H -0.2614 1.0402 -0.0131 0.116 Uiso 1 1 calc R . . C131 C 0.6980(5) 0.3669(2) 0.4157(2) 0.077(2) Uani 1 1 d . . . N3 N 0.7611(3) 0.49090(11) 0.46463(14) 0.109 Uani 1 1 d G . . N4 N 0.7901(3) 0.53003(16) 0.48241(12) 0.100 Uani 1 1 d G . . C119 C 0.7685(3) 0.58344(12) 0.45411(14) 0.050 Uani 1 1 d G . . C120 C 0.7262(3) 0.57732(14) 0.41884(12) 0.050 Uani 1 1 d G . . C121 C 0.7216(3) 0.52013(16) 0.42534(13) 0.050 Uani 1 1 d G . . 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 0.0677(8) 0.0222(4) 0.0514(6) 0.0001(4) -0.0274(5) -0.0027(5) Mn2 0.0868(9) 0.0232(5) 0.0492(6) 0.0011(4) -0.0264(6) -0.0125(5) Mn3 0.1085(11) 0.0279(5) 0.0559(7) -0.0021(5) -0.0345(7) -0.0018(6) Mn4 0.0562(8) 0.0415(5) 0.0457(6) 0.0009(5) -0.0222(5) -0.0112(5) Mn5 0.0497(8) 0.0481(6) 0.0585(7) 0.0032(5) -0.0180(6) -0.0058(5) Mn6 0.0679(9) 0.0572(6) 0.0693(7) -0.0024(6) -0.0197(6) -0.0112(6) N1 0.123(6) 0.026(3) 0.066(4) -0.005(2) -0.051(3) -0.008(3) N2 0.095(5) 0.025(2) 0.062(3) -0.004(2) -0.035(3) -0.013(3) N5 0.062(5) 0.041(3) 0.120(5) -0.030(3) -0.039(4) 0.008(3) N6 0.057(4) 0.047(3) 0.130(5) -0.033(3) -0.040(4) 0.013(3) O1W 0.108(4) 0.038(2) 0.076(3) 0.000(2) -0.044(3) -0.029(3) O1 0.073(4) 0.074(3) 0.074(3) -0.015(2) -0.033(3) -0.004(3) O2W 0.65(3) 0.443(15) 0.226(10) -0.220(11) -0.257(13) 0.332(16) O2 0.193(6) 0.048(3) 0.068(3) 0.008(2) 0.012(3) -0.042(3) O3W 0.091(6) 0.188(6) 0.312(9) -0.130(6) -0.022(5) -0.049(5) O3 0.071(4) 0.081(3) 0.067(3) -0.031(2) -0.022(3) -0.011(3) O4W 0.146(7) 0.113(4) 0.189(6) -0.060(4) -0.036(5) 0.031(4) O4 0.085(4) 0.056(3) 0.060(3) -0.004(2) -0.008(3) -0.019(3) O5W 0.076(5) 0.145(5) 0.277(8) -0.129(5) -0.096(5) 0.052(4) O5 0.063(4) 0.051(2) 0.061(3) 0.002(2) -0.012(2) -0.014(2) O6 0.086(4) 0.047(2) 0.087(3) 0.008(2) -0.050(3) -0.013(2) O7 0.072(4) 0.056(3) 0.061(3) 0.010(2) -0.017(2) -0.007(2) O9 0.119(5) 0.029(2) 0.053(3) 0.000(2) 0.005(3) -0.005(2) O10 0.058(4) 0.072(3) 0.127(4) -0.044(3) -0.054(3) 0.007(3) O11 0.076(4) 0.056(2) 0.067(3) -0.021(2) -0.020(3) -0.020(2) O12 0.059(4) 0.062(3) 0.064(3) -0.004(2) -0.013(2) -0.016(2) O13 0.115(5) 0.053(3) 0.073(3) 0.002(2) 0.005(3) -0.018(3) O14 0.075(4) 0.046(2) 0.081(3) 0.000(2) -0.019(3) -0.015(2) O15 0.079(4) 0.054(3) 0.072(3) -0.013(2) -0.011(3) -0.012(3) O16 0.112(4) 0.025(2) 0.060(3) 0.0018(19) -0.051(3) 0.012(2) O17 0.124(4) 0.026(2) 0.055(3) -0.0001(19) -0.045(3) -0.015(2) O18 0.069(4) 0.063(3) 0.056(3) 0.016(2) -0.028(2) -0.008(2) O19 0.076(5) 0.146(4) 0.058(3) 0.044(3) 0.022(3) 0.024(3) O20 0.068(4) 0.069(3) 0.075(3) -0.010(2) -0.033(3) -0.012(3) O21 0.090(4) 0.065(3) 0.076(3) 0.024(2) -0.036(3) 0.005(3) O22 0.101(4) 0.048(2) 0.100(3) 0.012(2) -0.075(3) -0.007(3) O23 0.098(4) 0.042(2) 0.072(3) 0.005(2) -0.020(3) -0.019(3) O24 0.094(4) 0.033(2) 0.060(3) 0.012(2) -0.018(3) -0.019(2) O25 0.068(4) 0.082(3) 0.112(4) -0.049(3) -0.052(3) 0.013(3) O26 0.088(4) 0.043(2) 0.057(3) 0.007(2) -0.011(3) -0.006(2) O27 0.136(5) 0.082(3) 0.063(3) 0.018(3) -0.043(3) 0.018(3) O28 0.080(4) 0.041(2) 0.078(3) -0.002(2) -0.041(3) 0.007(2) O30 0.083(4) 0.035(2) 0.060(3) 0.003(2) -0.037(2) 0.004(2) O31 0.114(5) 0.050(3) 0.161(5) -0.024(3) 0.024(4) -0.015(3) O32 0.070(4) 0.043(2) 0.069(3) 0.000(2) -0.023(2) -0.022(2) O33 0.066(3) 0.046(2) 0.050(3) 0.006(2) -0.024(2) -0.013(2) O34 0.142(5) 0.045(2) 0.063(3) -0.002(2) -0.008(3) -0.016(3) O35 0.087(4) 0.074(3) 0.071(3) -0.019(2) -0.030(3) -0.031(3) O36 0.078(4) 0.118(4) 0.081(3) -0.022(3) -0.020(3) -0.031(3) O37 0.104(4) 0.027(2) 0.054(3) 0.0017(19) -0.033(3) -0.004(2) O38 0.066(3) 0.032(2) 0.053(2) -0.0074(19) -0.021(2) -0.010(2) C1 0.073(6) 0.061(5) 0.049(4) -0.011(4) -0.026(4) -0.011(4) C2 0.074(6) 0.046(4) 0.070(5) -0.007(4) -0.018(4) -0.014(4) C3 0.078(6) 0.051(4) 0.058(4) -0.004(3) -0.027(4) -0.014(4) C4 0.082(6) 0.040(4) 0.052(4) 0.000(3) -0.018(4) -0.020(4) C5 0.105(7) 0.055(4) 0.056(4) -0.007(3) -0.038(4) -0.015(4) C6 0.065(6) 0.048(4) 0.041(4) 0.006(3) -0.025(4) -0.015(4) C7 0.075(6) 0.036(3) 0.057(5) 0.016(3) -0.024(4) 0.000(4) C8 0.059(6) 0.078(5) 0.073(5) 0.010(4) -0.030(4) -0.019(4) C9 0.071(6) 0.056(4) 0.053(4) 0.009(3) -0.023(4) -0.011(4) C10 0.071(6) 0.069(5) 0.073(5) 0.010(4) -0.039(4) -0.009(4) C11 0.265(13) 0.033(4) 0.099(7) -0.006(4) -0.003(8) -0.031(6) C12 0.085(7) 0.069(5) 0.046(4) -0.014(4) -0.015(4) -0.012(4) C13 0.120(7) 0.030(3) 0.045(4) 0.009(3) -0.037(4) 0.006(4) C18 0.100(8) 0.047(4) 0.076(5) -0.025(4) -0.035(5) -0.019(5) C19 0.046(5) 0.063(4) 0.070(5) -0.022(4) -0.016(4) -0.010(4) C20 0.071(6) 0.064(5) 0.058(5) -0.033(4) -0.019(4) -0.003(4) C21 0.057(6) 0.046(4) 0.068(5) -0.009(4) -0.028(4) -0.011(4) C22 0.060(6) 0.060(5) 0.108(6) -0.036(5) -0.038(5) 0.014(4) C23 0.076(7) 0.078(5) 0.086(6) -0.034(5) -0.029(5) 0.006(5) C24 0.093(6) 0.041(4) 0.090(5) -0.023(4) -0.037(5) -0.023(4) C25 0.058(5) 0.045(4) 0.055(4) -0.012(4) -0.015(4) -0.011(4) C26 0.085(6) 0.056(4) 0.050(5) -0.012(4) -0.009(4) -0.022(4) C27 0.069(6) 0.062(5) 0.058(5) -0.016(4) -0.015(4) 0.000(4) C28 0.060(6) 0.056(4) 0.052(5) 0.012(4) -0.015(4) -0.034(4) C29 0.078(6) 0.064(5) 0.060(5) -0.018(4) -0.013(4) -0.010(4) C30 0.094(7) 0.046(4) 0.057(5) -0.001(4) -0.020(4) -0.019(4) C31 0.042(5) 0.072(4) 0.060(4) 0.002(4) -0.015(4) -0.018(4) C32 0.080(6) 0.043(4) 0.054(4) -0.004(4) -0.043(4) -0.001(4) C33 0.084(7) 0.049(5) 0.082(6) -0.012(4) -0.009(5) -0.025(5) C34 0.081(7) 0.047(4) 0.067(5) -0.026(4) 0.001(5) -0.012(4) C35 0.077(7) 0.035(4) 0.060(5) 0.008(4) -0.021(4) -0.015(4) C36 0.068(6) 0.033(4) 0.078(5) -0.001(4) -0.024(5) -0.017(4) C37 0.072(7) 0.041(4) 0.086(6) -0.002(4) -0.014(5) -0.025(4) C38 0.101(7) 0.061(4) 0.051(4) 0.004(4) -0.034(5) -0.022(5) C39 0.063(5) 0.056(4) 0.041(4) 0.003(3) -0.027(4) -0.012(4) C40 0.059(6) 0.032(4) 0.082(5) -0.003(4) -0.025(4) 0.000(4) C41 0.071(6) 0.029(3) 0.057(4) -0.005(3) -0.031(4) -0.001(3) C42 0.096(6) 0.028(3) 0.038(4) -0.001(3) -0.034(4) 0.000(4) C43 0.066(6) 0.040(4) 0.063(4) -0.001(3) -0.037(4) 0.002(4) C44 0.088(6) 0.034(3) 0.054(4) -0.011(3) -0.037(4) 0.014(4) C45 0.070(5) 0.030(3) 0.047(4) -0.005(3) -0.025(4) -0.013(3) C46 0.052(6) 0.064(5) 0.046(4) -0.005(4) -0.013(4) 0.006(4) C47 0.056(6) 0.058(4) 0.056(5) 0.000(4) -0.007(4) -0.004(4) C48 0.060(6) 0.048(4) 0.084(6) -0.005(4) -0.037(5) -0.001(4) C49 0.071(7) 0.061(5) 0.054(5) -0.004(4) -0.008(5) -0.009(5) C50 0.053(6) 0.073(5) 0.077(5) 0.009(4) -0.023(4) 0.011(5) C51 0.086(7) 0.072(5) 0.067(6) -0.003(4) -0.023(5) 0.025(5) C52 0.083(6) 0.088(5) 0.049(4) 0.040(4) -0.041(4) -0.031(4) C53 0.072(6) 0.055(4) 0.051(5) 0.007(4) -0.033(4) -0.008(4) C54 0.086(7) 0.059(4) 0.069(5) 0.022(4) -0.033(4) -0.011(4) C55 0.096(7) 0.055(4) 0.074(5) 0.008(4) -0.056(5) -0.013(4) C56 0.093(7) 0.062(4) 0.078(5) -0.001(4) -0.043(5) -0.028(5) C57 0.080(6) 0.066(5) 0.096(6) 0.003(4) -0.053(5) -0.003(4) C58 0.065(6) 0.048(4) 0.045(4) -0.005(3) -0.029(4) -0.007(4) C59 0.108(7) 0.045(4) 0.049(4) -0.006(3) -0.027(4) -0.028(4) C60 0.092(6) 0.052(4) 0.058(4) -0.008(3) -0.027(4) -0.009(4) C61 0.082(6) 0.039(3) 0.052(4) 0.001(3) -0.018(4) -0.023(4) C62 0.083(7) 0.063(4) 0.051(4) 0.000(3) -0.026(4) -0.032(4) C63 0.056(6) 0.071(5) 0.073(6) -0.009(5) -0.028(5) 0.007(5) C64 0.092(7) 0.085(5) 0.053(5) 0.008(4) -0.025(5) 0.006(5) C65 0.113(8) 0.057(4) 0.054(5) 0.005(4) -0.032(5) -0.002(5) C66 0.080(7) 0.056(4) 0.050(5) 0.008(4) -0.027(4) 0.001(4) C67 0.126(9) 0.092(6) 0.070(6) 0.029(5) -0.016(6) 0.029(6) C68 0.109(8) 0.079(5) 0.080(6) 0.021(5) -0.032(6) 0.027(5) C69 0.081(6) 0.086(5) 0.055(4) 0.004(4) -0.023(4) -0.032(4) C70 0.080(6) 0.047(4) 0.087(5) 0.013(4) -0.055(4) -0.006(4) C71 0.142(9) 0.041(4) 0.162(8) -0.024(5) -0.115(7) 0.027(5) C72 0.158(9) 0.034(4) 0.135(7) -0.032(4) -0.095(7) 0.016(5) C73 0.088(6) 0.037(4) 0.079(5) 0.004(4) -0.054(5) -0.011(4) C74 0.068(6) 0.044(4) 0.057(4) 0.015(3) -0.020(4) 0.009(4) C75 0.080(6) 0.048(4) 0.079(5) -0.003(4) -0.046(4) -0.003(4) C76 0.075(6) 0.065(5) 0.064(5) 0.002(4) -0.029(4) -0.008(5) C77 0.097(8) 0.046(5) 0.115(7) -0.027(5) -0.009(6) -0.013(5) C78 0.104(8) 0.051(5) 0.088(6) -0.018(4) -0.008(5) -0.022(5) C79 0.061(6) 0.042(4) 0.078(5) -0.006(4) -0.022(5) -0.010(4) C80 0.078(7) 0.044(4) 0.065(5) 0.017(4) -0.038(5) -0.029(5) C81 0.090(7) 0.038(4) 0.065(5) -0.006(4) -0.030(5) -0.016(4) C82 0.071(6) 0.054(4) 0.077(5) -0.002(4) -0.029(5) -0.024(4) C83 0.070(6) 0.055(4) 0.059(5) -0.003(4) -0.013(4) -0.025(4) C84 0.071(6) 0.058(4) 0.056(5) -0.005(4) -0.005(4) -0.013(4) C85 0.088(7) 0.045(4) 0.047(4) 0.010(4) -0.011(4) -0.023(4) C86 0.059(6) 0.045(4) 0.060(5) -0.012(4) -0.003(4) -0.007(4) C87 0.105(7) 0.040(4) 0.057(5) -0.002(4) 0.005(5) -0.012(4) C88 0.107(7) 0.050(4) 0.049(5) 0.007(4) 0.009(4) -0.018(5) C89 0.093(6) 0.029(3) 0.060(4) 0.004(3) -0.025(4) -0.017(4) C90 0.067(7) 0.086(6) 0.110(7) -0.059(5) -0.031(6) -0.007(5) C91 0.075(7) 0.114(6) 0.075(5) -0.038(5) -0.015(5) -0.030(5) C92 0.134(9) 0.050(4) 0.061(5) -0.019(4) -0.036(6) -0.014(6) C93 0.059(7) 0.076(6) 0.094(6) -0.028(5) -0.044(5) 0.002(5) C94 0.083(8) 0.163(9) 0.149(8) -0.115(7) -0.053(6) 0.019(7) C95 0.107(10) 0.136(8) 0.158(9) -0.105(7) -0.040(8) 0.022(7) C96 0.109(7) 0.054(4) 0.064(5) -0.002(4) -0.027(5) -0.012(4) C97 0.078(7) 0.042(4) 0.055(5) -0.002(3) -0.027(4) -0.018(4) C98 0.100(7) 0.034(4) 0.057(5) 0.005(3) 0.012(4) 0.006(4) C99 0.114(8) 0.024(3) 0.070(5) -0.005(4) -0.020(5) 0.007(4) C100 0.088(6) 0.039(4) 0.039(4) -0.004(3) -0.026(4) -0.020(4) C101 0.059(5) 0.020(3) 0.062(4) -0.002(3) -0.027(4) 0.007(3) C102 0.079(7) 0.025(3) 0.060(5) 0.012(3) -0.024(4) -0.009(4) C103 0.088(6) 0.022(3) 0.044(4) 0.005(3) -0.028(4) -0.022(3) C104 0.079(6) 0.037(3) 0.047(4) 0.002(3) -0.021(4) -0.010(3) C105 0.246(12) 0.027(4) 0.190(9) -0.018(5) -0.160(9) -0.006(5) C106 0.284(13) 0.037(4) 0.161(8) -0.016(5) -0.164(9) -0.002(6) C108 0.091(6) 0.019(3) 0.118(6) -0.013(4) -0.069(5) 0.009(4) C109 0.088(6) 0.026(3) 0.102(5) -0.023(4) -0.060(5) 0.016(4) C110 0.091(7) 0.036(4) 0.068(5) -0.011(4) -0.031(5) -0.005(4) C111 0.081(7) 0.023(3) 0.074(5) -0.004(3) -0.016(4) 0.015(4) C112 0.078(6) 0.041(4) 0.083(5) -0.010(4) -0.036(4) -0.009(4) C113 0.134(7) 0.016(3) 0.052(4) 0.001(3) -0.040(5) -0.011(4) C114 0.193(10) 0.035(4) 0.068(5) -0.017(4) -0.043(5) -0.013(5) C115 0.193(10) 0.030(4) 0.097(6) 0.012(4) -0.083(6) -0.036(5) C116 0.142(8) 0.027(3) 0.069(5) 0.003(3) -0.053(5) -0.021(4) C118 0.189(10) 0.030(4) 0.124(7) -0.014(4) -0.072(7) -0.018(5) C122 0.099(7) 0.037(4) 0.091(5) -0.023(4) -0.012(5) -0.001(4) C123 0.123(10) 0.075(6) 0.314(14) -0.073(8) -0.103(10) -0.010(6) C124 0.100(9) 0.093(6) 0.296(13) -0.094(8) -0.134(9) 0.044(6) C125 0.043(5) 0.057(5) 0.103(6) -0.022(4) -0.020(5) -0.001(4) C126 0.079(8) 0.061(5) 0.164(9) 0.003(5) -0.036(7) -0.003(5) C127 0.054(6) 0.046(4) 0.157(8) 0.006(5) -0.049(6) -0.004(4) C128 0.040(5) 0.050(4) 0.057(4) -0.013(4) -0.003(4) 0.001(4) C129 0.068(7) 0.066(5) 0.097(6) 0.007(4) -0.025(5) 0.021(5) C130 0.072(8) 0.083(6) 0.120(7) 0.005(5) -0.022(6) -0.015(6) C131 0.130(8) 0.045(4) 0.060(4) -0.006(3) -0.055(5) 0.020(4) N3 0.111 0.078 0.110 -0.011 0.019 0.008 N4 0.141 0.033 0.148 -0.048 -0.036 -0.017 C119 0.050 0.050 0.050 -0.014 -0.007 -0.005 C120 0.050 0.050 0.050 -0.014 -0.007 -0.005 C121 0.050 0.050 0.050 -0.014 -0.007 -0.005 _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 O16 2.123(3) 1_655 ? Mn1 O14 2.131(4) . ? Mn1 O32 2.136(4) 1_655 ? Mn1 O30 2.153(4) . ? Mn1 O9 2.215(4) . ? Mn1 O38 2.240(4) 1_655 ? Mn2 O15 2.070(5) . ? Mn2 O17 2.105(4) 1_655 ? Mn2 N1 2.200(4) . ? Mn2 O1W 2.216(4) . ? Mn2 O37 2.271(4) 1_655 ? Mn2 O38 2.292(3) 1_655 ? Mn2 C103 2.617(5) 1_655 ? Mn3 O31 1.992(5) 1_655 ? Mn3 O29 2.062(5) . ? Mn3 O8 2.132(8) . ? Mn3 N3 2.162(3) . ? Mn3 O9 2.314(3) . ? Mn3 O2W 2.343(10) . ? Mn3 C17 2.575(9) . ? Mn4 O28 2.137(4) . ? Mn4 O18 2.147(4) 1_564 ? Mn4 O35 2.152(4) 2_565 ? Mn4 O11 2.156(4) 2_666 ? Mn4 O12 2.207(4) 1_564 ? Mn4 O33 2.219(4) . ? Mn5 O19 2.030(4) 1_564 ? Mn5 O10 2.096(4) 2_666 ? Mn5 N5 2.168(5) . ? Mn5 O34 2.233(4) . ? Mn5 O5W 2.239(5) . ? Mn5 O33 2.276(4) . ? Mn5 C89 2.584(6) . ? Mn6 O27 2.044(4) . ? Mn6 O36 2.112(5) 2_565 ? Mn6 O13 2.175(4) 1_564 ? Mn6 O4W 2.184(5) . ? Mn6 O3W 2.274(6) . ? Mn6 O12 2.402(4) 1_564 ? Mn6 C31 2.609(6) 1_564 ? N1 C104 1.273(6) . ? N1 C106 1.345(7) . ? N2 C105 1.324(7) . ? N2 C104 1.370(6) . ? N2 C107 1.419(6) . ? N5 C124 1.338(7) . ? N5 C122 1.345(8) . ? N6 C122 1.299(7) . ? N6 C125 1.395(7) . ? N6 C123 1.400(8) . ? O1 C5 1.424(6) . ? O1 C10 1.435(7) . ? O2 C11 1.346(5) . ? O2 C2 1.378(6) . ? O3 C18 1.374(6) . ? O3 C3 1.420(7) . ? O4 C25 1.365(6) . ? O4 C4 1.413(6) . ? O5 C32 1.338(7) . ? O5 C7 1.424(5) . ? O6 C39 1.370(6) . ? O6 C8 1.467(6) . ? O7 C46 1.346(6) . ? O7 C9 1.439(6) . ? O8 C17 1.401(9) . ? O9 C17 1.070(8) . ? O10 C24 1.251(8) . ? O10 Mn5 2.096(4) 2_666 ? O11 C24 1.220(7) . ? O11 Mn4 2.156(4) 2_666 ? O12 C31 1.274(6) . ? O12 Mn4 2.207(4) 1_546 ? O12 Mn6 2.402(4) 1_546 ? O13 C31 1.253(7) . ? O13 Mn6 2.175(4) 1_546 ? O14 C38 1.276(6) . ? O15 C38 1.308(7) . ? O16 C45 1.274(6) . ? O16 Mn1 2.123(3) 1_455 ? O17 C45 1.241(5) . ? O17 Mn2 2.105(4) 1_455 ? O18 C52 1.256(8) . ? O18 Mn4 2.147(4) 1_546 ? O19 C52 1.238(8) . ? O19 Mn5 2.030(4) 1_546 ? O20 C57 1.423(7) . ? O20 C62 1.455(6) . ? O21 C63 1.388(7) . ? O21 C54 1.431(7) . ? O22 C70 1.365(6) . ? O22 C55 1.437(6) . ? O23 C76 1.363(7) . ? O23 C56 1.441(6) . ? O24 C83 1.384(6) . ? O24 C59 1.419(6) . ? O25 C90 1.351(7) . ? O25 C60 1.420(7) . ? O26 C97 1.381(6) . ? O26 C61 1.464(6) . ? O27 C69 1.333(8) . ? O28 C69 1.199(8) . ? O29 C131 1.239(6) . ? O30 C131 1.225(6) . ? O31 C82 1.301(7) . ? O31 Mn3 1.992(5) 1_455 ? O32 C82 1.258(6) . ? O32 Mn1 2.136(4) 1_455 ? O33 C89 1.270(6) . ? O34 C89 1.233(7) . ? O35 C96 1.232(7) . ? O35 Mn4 2.152(4) 2_565 ? O36 C96 1.295(8) . ? O36 Mn6 2.112(5) 2_565 ? O37 C103 1.293(6) . ? O37 Mn2 2.271(4) 1_455 ? O38 C103 1.243(7) . ? O38 Mn1 2.240(4) 1_455 ? O38 Mn2 2.292(3) 1_455 ? C1 C4 1.494(7) . ? C1 C5 1.499(8) . ? C1 C3 1.505(7) . ? C1 C2 1.575(8) . ? C6 C7 1.474(8) . ? C6 C10 1.497(7) . ? C6 C9 1.524(7) . ? C6 C8 1.537(8) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C14 C17 1.558(9) . ? C15 C16 1.3900 . ? C18 C23 1.398(9) . ? C18 C19 1.424(8) . ? C19 C20 1.395(8) . ? C20 C21 1.336(8) . ? C21 C22 1.412(8) . ? C21 C24 1.554(8) . ? C22 C23 1.357(8) . ? C25 C30 1.366(7) . ? C25 C26 1.398(7) . ? C26 C27 1.357(7) . ? C27 C28 1.385(8) . ? C28 C29 1.383(8) . ? C28 C31 1.507(7) . ? C29 C30 1.423(7) . ? C31 Mn6 2.609(6) 1_546 ? C32 C33 1.339(8) . ? C32 C37 1.426(7) . ? C33 C34 1.364(8) . ? C34 C35 1.375(8) . ? C35 C36 1.365(8) . ? C35 C38 1.466(9) . ? C36 C37 1.357(8) . ? C39 C44 1.369(7) . ? C39 C40 1.377(7) . ? C40 C41 1.366(7) . ? C41 C42 1.405(7) . ? C42 C43 1.369(7) . ? C42 C45 1.473(7) . ? C43 C44 1.400(7) . ? C46 C51 1.353(8) . ? C46 C47 1.368(8) . ? C47 C48 1.378(7) . ? C48 C49 1.357(8) . ? C49 C50 1.346(8) . ? C49 C52 1.530(8) . ? C50 C51 1.410(8) . ? C53 C56 1.468(8) . ? C53 C55 1.507(8) . ? C53 C54 1.514(7) . ? C53 C57 1.531(8) . ? C58 C62 1.451(8) . ? C58 C59 1.513(7) . ? C58 C60 1.539(7) . ? C58 C61 1.542(7) . ? C63 C64 1.355(8) . ? C63 C68 1.382(9) . ? C64 C65 1.388(8) . ? C65 C66 1.343(8) . ? C66 C67 1.442(9) . ? C66 C69 1.531(8) . ? C67 C68 1.354(8) . ? C70 C71 1.375(8) . ? C70 C75 1.420(8) . ? C71 C72 1.406(8) . ? C72 C73 1.386(8) . ? C73 C74 1.368(7) . ? C73 C131 1.485(8) . ? C74 C75 1.432(8) . ? C76 C77 1.386(9) . ? C76 C81 1.394(8) . ? C77 C78 1.378(9) . ? C78 C79 1.386(8) . ? C79 C80 1.387(8) . ? C79 C82 1.437(9) . ? C80 C81 1.345(8) . ? C83 C88 1.381(8) . ? C83 C84 1.388(8) . ? C84 C85 1.390(7) . ? C85 C86 1.380(8) . ? C86 C87 1.395(7) . ? C86 C89 1.488(7) . ? C87 C88 1.347(7) . ? C90 C91 1.352(9) . ? C90 C95 1.379(10) . ? C91 C92 1.433(9) . ? C92 C93 1.378(9) . ? C93 C94 1.328(9) . ? C93 C96 1.489(9) . ? C94 C95 1.422(10) . ? C97 C102 1.350(8) . ? C97 C98 1.387(8) . ? C98 C99 1.363(8) . ? C99 C100 1.410(8) . ? C100 C101 1.388(7) . ? C100 C103 1.500(7) . ? C101 C102 1.388(7) . ? C103 Mn2 2.617(5) 1_455 ? C105 C106 1.349(8) . ? C107 C108 1.359(7) . ? C107 C112 1.382(7) . ? C108 C109 1.357(6) . ? C109 C110 1.332(8) . ? C110 C111 1.402(8) . ? C110 C113 1.488(7) 1_545 ? C111 C112 1.405(7) . ? C113 C114 1.303(7) . ? C113 C118 1.381(8) . ? C113 C110 1.488(7) 1_565 ? C114 C115 1.434(7) . ? C115 C116 1.284(8) . ? C116 C117 1.374(8) . ? C116 C119 1.398(6) . ? C117 C118 1.339(7) . ? C123 C124 1.344(10) . ? C125 C126 1.384(9) . ? C125 C130 1.387(8) . ? C126 C127 1.369(9) . ? C127 C128 1.377(8) . ? C128 C129 1.400(9) . ? C128 C128 1.446(11) 2_475 ? C129 C130 1.369(9) . ? N3 N4 1.4200 . ? N3 C121 1.4200 . ? N4 C119 1.4200 . ? C119 C120 1.4200 . ? C120 C121 1.4200 . ? 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 O16 Mn1 O14 92.09(16) 1_655 . ? O16 Mn1 O32 89.82(16) 1_655 1_655 ? O14 Mn1 O32 175.08(16) . 1_655 ? O16 Mn1 O30 177.64(18) 1_655 . ? O14 Mn1 O30 86.31(15) . . ? O32 Mn1 O30 91.91(15) 1_655 . ? O16 Mn1 O9 84.64(15) 1_655 . ? O14 Mn1 O9 91.14(16) . . ? O32 Mn1 O9 93.56(16) 1_655 . ? O30 Mn1 O9 93.66(15) . . ? O16 Mn1 O38 94.52(14) 1_655 1_655 ? O14 Mn1 O38 86.21(15) . 1_655 ? O32 Mn1 O38 89.12(15) 1_655 1_655 ? O30 Mn1 O38 87.10(14) . 1_655 ? O9 Mn1 O38 177.19(15) . 1_655 ? O15 Mn2 O17 95.87(17) . 1_655 ? O15 Mn2 N1 105.03(19) . . ? O17 Mn2 N1 87.47(16) 1_655 . ? O15 Mn2 O1W 87.35(17) . . ? O17 Mn2 O1W 175.49(16) 1_655 . ? N1 Mn2 O1W 88.65(16) . . ? O15 Mn2 O37 154.96(14) . 1_655 ? O17 Mn2 O37 92.82(16) 1_655 1_655 ? N1 Mn2 O37 98.76(17) . 1_655 ? O1W Mn2 O37 85.50(15) . 1_655 ? O15 Mn2 O38 97.97(15) . 1_655 ? O17 Mn2 O38 95.26(13) 1_655 1_655 ? N1 Mn2 O38 156.45(19) . 1_655 ? O1W Mn2 O38 87.39(12) . 1_655 ? O37 Mn2 O38 57.79(14) 1_655 1_655 ? O15 Mn2 C103 125.60(18) . 1_655 ? O17 Mn2 C103 97.17(16) 1_655 1_655 ? N1 Mn2 C103 128.1(2) . 1_655 ? O1W Mn2 C103 83.44(15) . 1_655 ? O37 Mn2 C103 29.62(16) 1_655 1_655 ? O38 Mn2 C103 28.37(14) 1_655 1_655 ? O31 Mn3 O29 97.1(2) 1_655 . ? O31 Mn3 O8 146.1(3) 1_655 . ? O29 Mn3 O8 105.3(3) . . ? O31 Mn3 N3 102.96(17) 1_655 . ? O29 Mn3 N3 88.32(18) . . ? O8 Mn3 N3 102.8(3) . . ? O31 Mn3 O9 98.36(17) 1_655 . ? O29 Mn3 O9 92.18(17) . . ? O8 Mn3 O9 56.3(2) . . ? N3 Mn3 O9 158.45(18) . . ? O31 Mn3 O2W 81.8(4) 1_655 . ? O29 Mn3 O2W 176.8(4) . . ? O8 Mn3 O2W 77.1(4) . . ? N3 Mn3 O2W 89.0(3) . . ? O9 Mn3 O2W 91.0(3) . . ? O31 Mn3 C17 116.9(3) 1_655 . ? O29 Mn3 C17 104.5(2) . . ? O8 Mn3 C17 33.0(3) . . ? N3 Mn3 C17 135.6(3) . . ? O9 Mn3 C17 24.55(19) . . ? O2W Mn3 C17 78.6(4) . . ? O28 Mn4 O18 175.75(18) . 1_564 ? O28 Mn4 O35 92.96(15) . 2_565 ? O18 Mn4 O35 87.31(15) 1_564 2_565 ? O28 Mn4 O11 87.38(15) . 2_666 ? O18 Mn4 O11 92.94(15) 1_564 2_666 ? O35 Mn4 O11 172.11(18) 2_565 2_666 ? O28 Mn4 O12 88.94(16) . 1_564 ? O18 Mn4 O12 86.81(16) 1_564 1_564 ? O35 Mn4 O12 95.49(16) 2_565 1_564 ? O11 Mn4 O12 92.40(15) 2_666 1_564 ? O28 Mn4 O33 91.06(16) . . ? O18 Mn4 O33 93.19(15) 1_564 . ? O35 Mn4 O33 84.79(15) 2_565 . ? O11 Mn4 O33 87.32(15) 2_666 . ? O12 Mn4 O33 179.72(15) 1_564 . ? O19 Mn5 O10 95.4(2) 1_564 2_666 ? O19 Mn5 N5 91.6(2) 1_564 . ? O10 Mn5 N5 92.18(19) 2_666 . ? O19 Mn5 O34 160.3(2) 1_564 . ? O10 Mn5 O34 92.12(17) 2_666 . ? N5 Mn5 O34 106.4(2) . . ? O19 Mn5 O5W 87.1(2) 1_564 . ? O10 Mn5 O5W 177.5(2) 2_666 . ? N5 Mn5 O5W 87.35(19) . . ? O34 Mn5 O5W 85.6(2) . . ? O19 Mn5 O33 103.16(18) 1_564 . ? O10 Mn5 O33 95.67(16) 2_666 . ? N5 Mn5 O33 162.54(17) . . ? O34 Mn5 O33 57.82(15) . . ? O5W Mn5 O33 84.12(16) . . ? O19 Mn5 C89 132.1(2) 1_564 . ? O10 Mn5 C89 95.99(18) 2_666 . ? N5 Mn5 C89 134.1(2) . . ? O34 Mn5 C89 28.47(16) . . ? O5W Mn5 C89 82.6(2) . . ? O33 Mn5 C89 29.43(16) . . ? O27 Mn6 O36 97.36(19) . 2_565 ? O27 Mn6 O13 154.83(19) . 1_564 ? O36 Mn6 O13 94.52(18) 2_565 1_564 ? O27 Mn6 O4W 103.3(2) . . ? O36 Mn6 O4W 87.6(2) 2_565 . ? O13 Mn6 O4W 99.2(2) 1_564 . ? O27 Mn6 O3W 80.8(2) . . ? O36 Mn6 O3W 170.1(2) 2_565 . ? O13 Mn6 O3W 91.0(2) 1_564 . ? O4W Mn6 O3W 83.4(2) . . ? O27 Mn6 O12 98.34(17) . 1_564 ? O36 Mn6 O12 101.26(18) 2_565 1_564 ? O13 Mn6 O12 57.46(15) 1_564 1_564 ? O4W Mn6 O12 155.34(18) . 1_564 ? O3W Mn6 O12 88.65(18) . 1_564 ? O27 Mn6 C31 126.6(2) . 1_564 ? O36 Mn6 C31 101.35(19) 2_565 1_564 ? O13 Mn6 C31 28.57(16) 1_564 1_564 ? O4W Mn6 C31 126.8(2) . 1_564 ? O3W Mn6 C31 87.4(2) . 1_564 ? O12 Mn6 C31 29.08(15) 1_564 1_564 ? C104 N1 C106 103.2(5) . . ? C104 N1 Mn2 132.6(4) . . ? C106 N1 Mn2 124.0(4) . . ? C105 N2 C104 104.8(5) . . ? C105 N2 C107 127.2(5) . . ? C104 N2 C107 127.9(5) . . ? C124 N5 C122 105.2(6) . . ? C124 N5 Mn5 124.8(5) . . ? C122 N5 Mn5 126.9(4) . . ? C122 N6 C125 126.7(6) . . ? C122 N6 C123 103.4(7) . . ? C125 N6 C123 129.7(6) . . ? C5 O1 C10 116.2(5) . . ? C11 O2 C2 116.2(5) . . ? C18 O3 C3 119.3(5) . . ? C25 O4 C4 116.5(5) . . ? C32 O5 C7 115.6(5) . . ? C39 O6 C8 119.5(4) . . ? C46 O7 C9 114.5(5) . . ? C17 O8 Mn3 91.2(6) . . ? C17 O9 Mn1 161.4(6) . . ? C17 O9 Mn3 91.5(5) . . ? Mn1 O9 Mn3 106.43(16) . . ? C24 O10 Mn5 123.7(4) . 2_666 ? C24 O11 Mn4 140.0(4) . 2_666 ? C31 O12 Mn4 144.6(4) . 1_546 ? C31 O12 Mn6 84.5(4) . 1_546 ? Mn4 O12 Mn6 103.23(14) 1_546 1_546 ? C31 O13 Mn6 95.3(4) . 1_546 ? C38 O14 Mn1 141.6(5) . . ? C38 O15 Mn2 132.5(4) . . ? C45 O16 Mn1 140.1(4) . 1_455 ? C45 O17 Mn2 133.9(3) . 1_455 ? C52 O18 Mn4 136.2(4) . 1_546 ? C52 O19 Mn5 131.3(5) . 1_546 ? C57 O20 C62 114.1(5) . . ? C63 O21 C54 116.7(5) . . ? C70 O22 C55 117.0(4) . . ? C76 O23 C56 116.7(5) . . ? C83 O24 C59 115.5(5) . . ? C90 O25 C60 118.8(5) . . ? C97 O26 C61 116.5(5) . . ? C69 O27 Mn6 129.0(4) . . ? C69 O28 Mn4 134.6(5) . . ? C131 O29 Mn3 136.5(5) . . ? C131 O30 Mn1 137.8(4) . . ? C82 O31 Mn3 137.2(4) . 1_455 ? C82 O32 Mn1 137.7(5) . 1_455 ? C89 O33 Mn4 147.6(4) . . ? C89 O33 Mn5 88.9(4) . . ? Mn4 O33 Mn5 106.81(14) . . ? C89 O34 Mn5 91.8(4) . . ? C96 O35 Mn4 145.2(5) . 2_565 ? C96 O36 Mn6 122.5(5) . 2_565 ? C103 O37 Mn2 90.2(4) . 1_455 ? C103 O38 Mn1 140.3(4) . 1_455 ? C103 O38 Mn2 90.5(3) . 1_455 ? Mn1 O38 Mn2 108.27(15) 1_455 1_455 ? C4 C1 C5 111.7(6) . . ? C4 C1 C3 111.9(5) . . ? C5 C1 C3 107.9(6) . . ? C4 C1 C2 106.5(5) . . ? C5 C1 C2 109.8(5) . . ? C3 C1 C2 109.0(5) . . ? O2 C2 C1 108.7(5) . . ? O3 C3 C1 109.9(5) . . ? O4 C4 C1 108.8(5) . . ? O1 C5 C1 108.3(5) . . ? C7 C6 C10 113.6(6) . . ? C7 C6 C9 106.5(5) . . ? C10 C6 C9 109.6(5) . . ? C7 C6 C8 110.3(5) . . ? C10 C6 C8 105.5(5) . . ? C9 C6 C8 111.4(5) . . ? O5 C7 C6 109.3(5) . . ? O6 C8 C6 105.1(5) . . ? O7 C9 C6 109.3(5) . . ? O1 C10 C6 105.7(5) . . ? O2 C11 C12 127.6(5) . . ? O2 C11 C16 112.2(5) . . ? C12 C11 C16 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 C17 114.2(5) . . ? C15 C14 C17 125.5(5) . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? O9 C17 O8 116.1(9) . . ? O9 C17 C14 129.5(8) . . ? O8 C17 C14 107.7(8) . . ? O9 C17 Mn3 63.9(5) . . ? O8 C17 Mn3 55.9(5) . . ? C14 C17 Mn3 163.3(6) . . ? O3 C18 C23 115.9(7) . . ? O3 C18 C19 122.4(7) . . ? C23 C18 C19 121.7(6) . . ? C20 C19 C18 116.5(7) . . ? C21 C20 C19 122.5(7) . . ? C20 C21 C22 119.7(6) . . ? C20 C21 C24 120.1(7) . . ? C22 C21 C24 120.1(7) . . ? C23 C22 C21 121.4(7) . . ? C22 C23 C18 118.1(7) . . ? O11 C24 O10 128.8(6) . . ? O11 C24 C21 115.0(7) . . ? O10 C24 C21 116.2(7) . . ? O4 C25 C30 124.7(6) . . ? O4 C25 C26 116.8(6) . . ? C30 C25 C26 118.5(6) . . ? C27 C26 C25 124.0(6) . . ? C26 C27 C28 117.7(6) . . ? C29 C28 C27 120.5(6) . . ? C29 C28 C31 115.5(7) . . ? C27 C28 C31 123.9(6) . . ? C28 C29 C30 120.6(6) . . ? C25 C30 C29 118.7(6) . . ? O13 C31 O12 121.9(6) . . ? O13 C31 C28 120.2(6) . . ? O12 C31 C28 117.9(6) . . ? O13 C31 Mn6 56.1(3) . 1_546 ? O12 C31 Mn6 66.4(3) . 1_546 ? C28 C31 Mn6 171.0(5) . 1_546 ? O5 C32 C33 128.1(6) . . ? O5 C32 C37 115.9(6) . . ? C33 C32 C37 116.0(7) . . ? C32 C33 C34 124.8(7) . . ? C33 C34 C35 119.3(7) . . ? C36 C35 C34 117.4(7) . . ? C36 C35 C38 122.3(6) . . ? C34 C35 C38 120.3(7) . . ? C37 C36 C35 123.6(7) . . ? C36 C37 C32 118.9(7) . . ? O14 C38 O15 120.9(7) . . ? O14 C38 C35 119.1(6) . . ? O15 C38 C35 119.9(6) . . ? C44 C39 O6 124.0(6) . . ? C44 C39 C40 122.4(6) . . ? O6 C39 C40 113.7(5) . . ? C41 C40 C39 118.5(5) . . ? C40 C41 C42 121.8(6) . . ? C43 C42 C41 117.1(5) . . ? C43 C42 C45 122.8(5) . . ? C41 C42 C45 119.8(5) . . ? C42 C43 C44 122.5(6) . . ? C39 C44 C43 117.4(6) . . ? O17 C45 O16 124.2(5) . . ? O17 C45 C42 118.7(5) . . ? O16 C45 C42 117.0(5) . . ? O7 C46 C51 114.8(6) . . ? O7 C46 C47 125.7(7) . . ? C51 C46 C47 119.3(6) . . ? C46 C47 C48 118.6(7) . . ? C49 C48 C47 123.1(7) . . ? C50 C49 C48 117.5(7) . . ? C50 C49 C52 120.2(7) . . ? C48 C49 C52 122.1(7) . . ? C49 C50 C51 120.8(7) . . ? C46 C51 C50 120.1(7) . . ? O19 C52 O18 128.0(6) . . ? O19 C52 C49 116.5(7) . . ? O18 C52 C49 115.5(7) . . ? C56 C53 C55 112.2(6) . . ? C56 C53 C54 104.0(6) . . ? C55 C53 C54 114.5(6) . . ? C56 C53 C57 109.5(6) . . ? C55 C53 C57 106.8(6) . . ? C54 C53 C57 109.9(5) . . ? O21 C54 C53 105.6(5) . . ? O22 C55 C53 105.4(5) . . ? O23 C56 C53 110.9(5) . . ? O20 C57 C53 108.4(5) . . ? C62 C58 C59 111.4(5) . . ? C62 C58 C60 108.5(5) . . ? C59 C58 C60 110.0(5) . . ? C62 C58 C61 112.5(5) . . ? C59 C58 C61 105.4(5) . . ? C60 C58 C61 109.0(5) . . ? O24 C59 C58 107.7(5) . . ? O25 C60 C58 108.0(5) . . ? O26 C61 C58 106.2(5) . . ? C58 C62 O20 107.9(5) . . ? C64 C63 C68 118.9(7) . . ? C64 C63 O21 125.1(7) . . ? C68 C63 O21 115.9(7) . . ? C63 C64 C65 120.6(7) . . ? C66 C65 C64 120.8(7) . . ? C65 C66 C67 119.4(6) . . ? C65 C66 C69 119.2(7) . . ? C67 C66 C69 121.2(7) . . ? C68 C67 C66 117.7(8) . . ? C67 C68 C63 122.4(8) . . ? O28 C69 O27 129.1(6) . . ? O28 C69 C66 119.6(7) . . ? O27 C69 C66 111.2(6) . . ? O22 C70 C71 114.6(6) . . ? O22 C70 C75 124.6(6) . . ? C71 C70 C75 120.8(6) . . ? C70 C71 C72 119.9(6) . . ? C73 C72 C71 120.9(6) . . ? C74 C73 C72 118.9(6) . . ? C74 C73 C131 121.2(6) . . ? C72 C73 C131 119.9(6) . . ? C73 C74 C75 122.1(6) . . ? C70 C75 C74 116.9(6) . . ? O23 C76 C77 126.5(7) . . ? O23 C76 C81 117.3(7) . . ? C77 C76 C81 116.2(7) . . ? C78 C77 C76 123.2(7) . . ? C77 C78 C79 119.1(8) . . ? C78 C79 C80 117.4(7) . . ? C78 C79 C82 119.1(8) . . ? C80 C79 C82 123.5(7) . . ? C81 C80 C79 122.9(7) . . ? C80 C81 C76 120.9(7) . . ? O32 C82 O31 122.5(7) . . ? O32 C82 C79 118.8(7) . . ? O31 C82 C79 118.7(6) . . ? C88 C83 O24 125.9(6) . . ? C88 C83 C84 119.7(6) . . ? O24 C83 C84 114.4(6) . . ? C83 C84 C85 119.8(7) . . ? C86 C85 C84 120.4(6) . . ? C85 C86 C87 117.8(6) . . ? C85 C86 C89 120.5(6) . . ? C87 C86 C89 121.6(6) . . ? C88 C87 C86 122.4(7) . . ? C87 C88 C83 119.7(6) . . ? O34 C89 O33 121.2(5) . . ? O34 C89 C86 118.4(6) . . ? O33 C89 C86 120.4(6) . . ? O34 C89 Mn5 59.7(3) . . ? O33 C89 Mn5 61.7(3) . . ? C86 C89 Mn5 172.5(5) . . ? O25 C90 C91 125.5(8) . . ? O25 C90 C95 115.2(8) . . ? C91 C90 C95 119.3(7) . . ? C90 C91 C92 115.9(8) . . ? C93 C92 C91 124.2(7) . . ? C94 C93 C92 119.3(8) . . ? C94 C93 C96 123.3(9) . . ? C92 C93 C96 117.4(8) . . ? C93 C94 C95 117.2(9) . . ? C90 C95 C94 124.0(8) . . ? O35 C96 O36 127.5(7) . . ? O35 C96 C93 121.0(8) . . ? O36 C96 C93 111.4(7) . . ? C102 C97 O26 126.6(6) . . ? C102 C97 C98 120.4(6) . . ? O26 C97 C98 112.9(7) . . ? C99 C98 C97 117.0(7) . . ? C98 C99 C100 124.0(6) . . ? C101 C100 C99 117.2(6) . . ? C101 C100 C103 120.7(7) . . ? C99 C100 C103 122.1(6) . . ? C100 C101 C102 118.3(6) . . ? C97 C102 C101 123.0(6) . . ? O38 C103 O37 120.7(5) . . ? O38 C103 C100 121.0(5) . . ? O37 C103 C100 118.3(6) . . ? O38 C103 Mn2 61.1(3) . 1_455 ? O37 C103 Mn2 60.2(3) . 1_455 ? C100 C103 Mn2 169.5(4) . 1_455 ? N1 C104 N2 113.9(5) . . ? N2 C105 C106 106.2(7) . . ? N1 C106 C105 111.6(6) . . ? C108 C107 C112 119.3(5) . . ? C108 C107 N2 122.3(5) . . ? C112 C107 N2 118.4(5) . . ? C109 C108 C107 119.9(6) . . ? C110 C109 C108 124.2(6) . . ? C109 C110 C111 117.2(6) . . ? C109 C110 C113 124.1(6) . 1_545 ? C111 C110 C113 118.6(6) . 1_545 ? C110 C111 C112 119.8(6) . . ? C107 C112 C111 119.5(6) . . ? C114 C113 C118 116.2(6) . . ? C114 C113 C110 123.9(6) . 1_565 ? C118 C113 C110 119.8(5) . 1_565 ? C113 C114 C115 122.8(6) . . ? C116 C115 C114 117.5(6) . . ? C115 C116 C117 121.8(6) . . ? C115 C116 C119 118.0(6) . . ? C117 C116 C119 119.4(6) . . ? C118 C117 C116 118.1(7) . . ? C117 C118 C113 122.8(7) . . ? N6 C122 N5 114.2(6) . . ? C124 C123 N6 108.7(7) . . ? N5 C124 C123 108.6(7) . . ? C126 C125 C130 118.0(7) . . ? C126 C125 N6 120.6(7) . . ? C130 C125 N6 121.2(7) . . ? C127 C126 C125 121.5(7) . . ? C126 C127 C128 122.0(7) . . ? C127 C128 C129 115.1(6) . . ? C127 C128 C128 124.7(8) . 2_475 ? C129 C128 C128 120.2(8) . 2_475 ? C130 C129 C128 124.1(7) . . ? C129 C130 C125 118.7(7) . . ? O30 C131 O29 124.6(6) . . ? O30 C131 C73 118.9(6) . . ? O29 C131 C73 116.5(6) . . ? N4 N3 C121 108.0 . . ? N4 N3 Mn3 129.5(2) . . ? C121 N3 Mn3 122.2(2) . . ? C119 N4 N3 108.0 . . ? C116 C119 C120 125.1(4) . . ? C116 C119 N4 126.6(4) . . ? C120 C119 N4 108.0 . . ? C119 C120 C121 108.0 . . ? N3 C121 C120 108.0 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.926 _refine_diff_density_min -2.217 _refine_diff_density_rms 0.077 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 _platon_squeeze_void_content 1 0.023 0.419 -0.010 6624 2243 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 950528'