# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_jopm90a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H38 Mn3 N6 O14, 2(C4 H12 N), 2(C H2 Cl2)' _chemical_formula_sum 'C66 H66 Cl4 Mn3 N8 O14' _chemical_formula_weight 1501.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.708(3) _cell_length_b 24.299(5) _cell_length_c 11.426(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.26(2) _cell_angle_gamma 90.00 _cell_volume 3471.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 577 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1546 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(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 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26986 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 32.20 _reflns_number_total 9399 _reflns_number_gt 8249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MARXDS (Claudio Klein, 2005)' _computing_cell_refinement 'AUTOMAR (Claudio Klein, 2007)' _computing_data_reduction 'MARSCALE (Claudio Klein, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. Regarding the crystal refinement parameter, for the structural resolution, it has been considered only reflections that have a value max of theta = 25\% (ACTA 50). Reflections between 25\% and 32\% have not been taken into account due to the poor quality of the reflections over this value. The poor quality of reflections could be due to the fact that the crystal does not diffract very well and to the kind of detector (image plate with spindle axis only) that was used. Other attempts of crystallization were done, but no single crystals of better quality were obtained. The displacement parameters of some lengths in the direction of the bond are restrained to be equal within an effective standard deviation (DELU sentences) ; _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^)+(0.0681P)^2^+0.4418P] 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 SHELXL _refine_ls_extinction_coef 0.0056(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9399 _refine_ls_number_parameters 431 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.757787(18) 0.014820(9) 0.91901(2) 0.02809(8) Uani 1 1 d U . . Mn2 Mn 0.5000 0.0000 1.0000 0.02742(9) Uani 1 2 d SU . . O1 O 0.66256(9) 0.02634(5) 1.07259(10) 0.0303(2) Uani 1 1 d U . . O2 O 0.82061(9) -0.01405(5) 1.10864(10) 0.0333(2) Uani 1 1 d U . . O3 O 0.80485(10) 0.12887(6) 1.01407(12) 0.0414(3) Uani 1 1 d U . . O4 O 0.88613(9) 0.06824(5) 0.91393(10) 0.0346(2) Uani 1 1 d U . . O5 O 0.50821(9) 0.05731(5) 0.86202(10) 0.0344(2) Uani 1 1 d U . . O6 O 0.65417(9) 0.05540(5) 0.77754(10) 0.0352(2) Uani 1 1 d U . . O7 O 0.55478(9) -0.07023(4) 0.90582(10) 0.0312(2) Uani 1 1 d . . . N1 N 0.84727(10) -0.04892(5) 0.82875(11) 0.0296(2) Uani 1 1 d U . . N2 N 0.58886(12) -0.19645(6) 0.79021(14) 0.0390(3) Uani 1 1 d . . . N3 N 0.65166(10) -0.06398(5) 0.88084(11) 0.0298(2) Uani 1 1 d . . . C1 C 0.73925(12) 0.00335(6) 1.14585(13) 0.0287(3) Uani 1 1 d . . . C2 C 0.73218(13) -0.00066(6) 1.27416(14) 0.0319(3) Uani 1 1 d . . . C3 C 0.64243(14) 0.01993(7) 1.31609(15) 0.0349(3) Uani 1 1 d . . . H3 H 0.5881 0.0374 1.2641 0.042 Uiso 1 1 calc R . . C4 C 0.63503(16) 0.01416(7) 1.43490(17) 0.0406(4) Uani 1 1 d . . . H4 H 0.5752 0.0274 1.4624 0.049 Uiso 1 1 calc R . . C5 C 0.71676(19) -0.01128(9) 1.51326(18) 0.0486(4) Uani 1 1 d . . . H5 H 0.7114 -0.0152 1.5930 0.058 Uiso 1 1 calc R . . C6 C 0.80654(17) -0.03094(9) 1.47275(17) 0.0463(4) Uani 1 1 d . . . H6 H 0.8618 -0.0473 1.5256 0.056 Uiso 1 1 calc R . . C7 C 0.81358(15) -0.02606(8) 1.35302(17) 0.0408(4) Uani 1 1 d . . . H7 H 0.8730 -0.0399 1.3257 0.049 Uiso 1 1 calc R . . C8 C 0.88053(13) 0.11500(6) 0.96469(14) 0.0322(3) Uani 1 1 d U . . C9 C 0.97285(13) 0.15340(6) 0.96493(14) 0.0316(3) Uani 1 1 d U . . C10 C 0.96780(16) 0.20776(8) 1.00346(17) 0.0427(4) Uani 1 1 d U . . H10 H 0.9069 0.2199 1.0303 0.051 Uiso 1 1 calc R . . C11 C 1.05203(19) 0.24390(9) 1.0023(2) 0.0526(5) Uani 1 1 d . . . H11 H 1.0474 0.2801 1.0272 0.063 Uiso 1 1 calc R . . C12 C 1.14367(18) 0.22544(9) 0.9635(2) 0.0511(5) Uani 1 1 d . . . H12 H 1.2007 0.2494 0.9630 0.061 Uiso 1 1 calc R . . C13 C 1.15030(16) 0.17171(8) 0.92556(18) 0.0453(4) Uani 1 1 d . . . H13 H 1.2118 0.1595 0.9000 0.054 Uiso 1 1 calc R . . C14 C 1.06514(13) 0.13594(7) 0.92566(15) 0.0362(3) Uani 1 1 d . . . H14 H 1.0697 0.1000 0.8993 0.043 Uiso 1 1 calc R . . C15 C 0.55971(12) 0.07023(6) 0.78121(13) 0.0307(3) Uani 1 1 d . . . C16 C 0.50281(13) 0.10738(6) 0.68496(14) 0.0321(3) Uani 1 1 d . . . C17 C 0.39887(13) 0.12464(7) 0.68736(15) 0.0359(3) Uani 1 1 d . . . H17 H 0.3644 0.1130 0.7483 0.043 Uiso 1 1 calc R . . C18 C 0.34622(15) 0.15929(7) 0.59855(17) 0.0404(4) Uani 1 1 d . . . H18 H 0.2767 0.1708 0.6000 0.049 Uiso 1 1 calc R . . C19 C 0.39808(15) 0.17651(7) 0.50800(16) 0.0400(4) Uani 1 1 d . . . H19 H 0.3631 0.1996 0.4487 0.048 Uiso 1 1 calc R . . C20 C 0.50223(15) 0.15939(7) 0.50546(16) 0.0402(4) Uani 1 1 d . . . H20 H 0.5365 0.1710 0.4443 0.048 Uiso 1 1 calc R . . C21 C 0.55485(14) 0.12514(7) 0.59386(15) 0.0360(3) Uani 1 1 d . . . H21 H 0.6246 0.1140 0.5926 0.043 Uiso 1 1 calc R . . C22 C 0.94702(12) -0.04101(6) 0.80753(14) 0.0310(3) Uani 1 1 d . . . H22 H 0.9806 -0.0074 0.8273 0.037 Uiso 1 1 calc R . . C23 C 1.00163(13) -0.08218(7) 0.75632(14) 0.0348(3) Uani 1 1 d . . . H23 H 1.0701 -0.0755 0.7415 0.042 Uiso 1 1 calc R . . C24 C 0.95381(13) -0.13233(7) 0.72803(15) 0.0366(3) Uani 1 1 d . . . H24 H 0.9892 -0.1598 0.6937 0.044 Uiso 1 1 calc R . . C25 C 0.85150(13) -0.14122(7) 0.75176(14) 0.0341(3) Uani 1 1 d . . . H25 H 0.8176 -0.1749 0.7345 0.041 Uiso 1 1 calc R . . C26 C 0.80063(12) -0.09858(6) 0.80203(13) 0.0307(3) Uani 1 1 d . . . C27 C 0.69348(12) -0.10521(6) 0.83142(13) 0.0297(3) Uani 1 1 d . . . C28 C 0.63530(13) -0.15599(6) 0.80777(14) 0.0322(3) Uani 1 1 d . . . Cl1 Cl 0.82750(5) 0.18147(2) 0.66700(5) 0.05612(14) Uani 1 1 d . . . Cl2 Cl 0.93238(6) 0.10524(3) 0.52683(6) 0.06598(16) Uani 1 1 d . . . C29 C 0.86887(17) 0.11276(8) 0.64947(18) 0.0457(4) Uani 1 1 d . . . H29A H 0.9175 0.1015 0.7208 0.055 Uiso 1 1 calc R . . H29B H 0.8069 0.0888 0.6399 0.055 Uiso 1 1 calc R . . C30 C 0.72533(17) 0.16080(9) 0.26979(18) 0.0481(4) Uani 1 1 d . . . H30A H 0.7617 0.1865 0.3268 0.072 Uiso 1 1 calc R . . H30B H 0.7766 0.1366 0.2444 0.072 Uiso 1 1 calc R . . H30C H 0.6756 0.1397 0.3055 0.072 Uiso 1 1 calc R . . C31 C 0.66598(14) 0.19157(7) 0.16419(16) 0.0388(3) Uani 1 1 d . . . H31 H 0.7161 0.2137 0.1296 0.047 Uiso 1 1 calc R . . H31A H 0.6145 0.2162 0.1900 0.047 Uiso 1 1 calc R . . N4 N 0.60867(11) 0.15284(5) 0.07164(12) 0.0326(3) Uani 1 1 d . . . H4NA H 0.6573 0.1323 0.0430 0.039 Uiso 1 1 calc R . . H4NB H 0.5677 0.1299 0.1061 0.039 Uiso 1 1 calc R . . C33 C 0.53954(14) 0.18192(7) -0.02987(15) 0.0354(3) Uani 1 1 d . . . H33 H 0.4968 0.2094 0.0016 0.042 Uiso 1 1 calc R . . H33A H 0.4911 0.1556 -0.0749 0.042 Uiso 1 1 calc R . . C34 C 0.60433(16) 0.20948(8) -0.11205(17) 0.0437(4) Uani 1 1 d . . . H34A H 0.5570 0.2276 -0.1752 0.066 Uiso 1 1 calc R . . H34B H 0.6455 0.1823 -0.1450 0.066 Uiso 1 1 calc R . . H34C H 0.6516 0.2360 -0.0682 0.066 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 0.02601(13) 0.02936(12) 0.02970(12) 0.00019(8) 0.00713(9) -0.00008(8) Mn2 0.02527(16) 0.02870(15) 0.02903(15) 0.00066(11) 0.00687(11) 0.00058(11) O1 0.0270(5) 0.0328(5) 0.0315(5) 0.0000(4) 0.0060(4) -0.0013(4) O2 0.0304(5) 0.0360(5) 0.0345(5) -0.0001(4) 0.0084(4) 0.0008(4) O3 0.0347(6) 0.0462(6) 0.0452(6) -0.0004(5) 0.0124(5) 0.0007(5) O4 0.0329(6) 0.0342(5) 0.0376(6) -0.0006(4) 0.0090(4) -0.0026(4) O5 0.0340(6) 0.0351(5) 0.0346(5) 0.0034(4) 0.0077(4) 0.0003(4) O6 0.0321(6) 0.0372(5) 0.0368(6) 0.0026(5) 0.0074(4) 0.0020(4) O7 0.0274(5) 0.0312(5) 0.0366(5) -0.0001(4) 0.0100(4) 0.0001(4) N1 0.0276(6) 0.0310(6) 0.0307(6) 0.0013(5) 0.0066(5) -0.0002(5) N2 0.0378(7) 0.0393(7) 0.0412(7) -0.0024(6) 0.0109(6) -0.0018(6) N3 0.0275(6) 0.0319(6) 0.0311(6) 0.0008(5) 0.0079(5) 0.0004(5) C1 0.0264(7) 0.0306(6) 0.0294(6) 0.0001(5) 0.0061(5) -0.0021(5) C2 0.0321(7) 0.0325(7) 0.0316(7) -0.0003(6) 0.0071(6) -0.0020(6) C3 0.0348(8) 0.0343(7) 0.0363(7) -0.0010(6) 0.0083(6) -0.0018(6) C4 0.0437(9) 0.0418(8) 0.0385(8) -0.0035(7) 0.0129(7) -0.0049(7) C5 0.0553(12) 0.0529(10) 0.0390(9) 0.0001(8) 0.0118(8) -0.0049(9) C6 0.0485(10) 0.0492(10) 0.0402(9) 0.0033(8) 0.0054(8) -0.0003(8) C7 0.0386(9) 0.0449(8) 0.0395(8) 0.0025(7) 0.0080(7) 0.0011(7) C8 0.0298(7) 0.0336(7) 0.0340(7) 0.0012(6) 0.0083(5) -0.0013(5) C9 0.0298(7) 0.0317(7) 0.0333(7) 0.0013(6) 0.0054(5) -0.0007(5) C10 0.0431(9) 0.0405(8) 0.0452(9) -0.0018(7) 0.0098(7) -0.0008(7) C11 0.0569(12) 0.0434(9) 0.0568(11) -0.0017(9) 0.0085(9) -0.0067(9) C12 0.0483(11) 0.0491(10) 0.0566(11) 0.0011(9) 0.0109(9) -0.0102(8) C13 0.0387(9) 0.0494(10) 0.0491(10) 0.0002(8) 0.0111(8) -0.0059(7) C14 0.0326(8) 0.0382(8) 0.0386(8) 0.0012(6) 0.0082(6) -0.0003(6) C15 0.0303(7) 0.0309(6) 0.0311(6) -0.0009(5) 0.0057(5) -0.0004(5) C16 0.0318(7) 0.0317(7) 0.0332(7) 0.0001(6) 0.0071(6) -0.0016(5) C17 0.0342(8) 0.0353(7) 0.0387(8) 0.0031(6) 0.0077(6) 0.0013(6) C18 0.0379(9) 0.0414(8) 0.0422(8) 0.0026(7) 0.0076(7) 0.0031(7) C19 0.0401(9) 0.0393(8) 0.0400(8) 0.0040(7) 0.0057(7) 0.0033(7) C20 0.0419(9) 0.0421(8) 0.0375(8) 0.0035(7) 0.0097(7) 0.0006(7) C21 0.0338(8) 0.0371(7) 0.0377(8) 0.0016(6) 0.0082(6) 0.0023(6) C22 0.0273(7) 0.0340(7) 0.0325(7) 0.0002(6) 0.0072(5) -0.0002(5) C23 0.0308(7) 0.0387(8) 0.0358(7) 0.0008(6) 0.0087(6) 0.0016(6) C24 0.0327(8) 0.0399(8) 0.0384(8) -0.0022(6) 0.0096(6) 0.0026(6) C25 0.0319(7) 0.0352(7) 0.0357(7) -0.0020(6) 0.0071(6) 0.0004(6) C26 0.0280(7) 0.0337(7) 0.0312(6) -0.0007(6) 0.0072(5) 0.0006(5) C27 0.0284(7) 0.0302(6) 0.0308(6) -0.0006(5) 0.0064(5) 0.0011(5) C28 0.0306(7) 0.0340(7) 0.0331(7) -0.0015(6) 0.0086(6) 0.0013(6) Cl1 0.0550(3) 0.0514(3) 0.0637(3) 0.0007(2) 0.0153(2) 0.0024(2) Cl2 0.0776(4) 0.0663(3) 0.0586(3) 0.0009(3) 0.0245(3) 0.0037(3) C29 0.0454(10) 0.0460(9) 0.0475(9) 0.0029(8) 0.0132(8) 0.0013(8) C30 0.0466(10) 0.0508(10) 0.0468(10) -0.0038(8) 0.0075(8) 0.0045(8) C31 0.0357(8) 0.0382(8) 0.0430(8) -0.0048(7) 0.0087(7) -0.0011(6) N4 0.0315(6) 0.0321(6) 0.0363(6) 0.0002(5) 0.0114(5) -0.0007(5) C33 0.0351(8) 0.0343(7) 0.0377(7) 0.0017(6) 0.0088(6) 0.0017(6) C34 0.0468(10) 0.0421(9) 0.0436(9) 0.0032(7) 0.0116(7) 0.0002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 2.0933(12) . ? Mn1 O6 2.1355(12) . ? Mn1 N1 2.2745(14) . ? Mn1 O2 2.2821(13) . ? Mn1 O1 2.3192(13) . ? Mn1 N3 2.3379(14) . ? Mn2 O5 2.1200(12) 3_657 ? Mn2 O5 2.1200(12) . ? Mn2 O1 2.1806(12) 3_657 ? Mn2 O1 2.1806(12) . ? Mn2 O7 2.1958(11) . ? Mn2 O7 2.1958(11) 3_657 ? O1 C1 1.2929(18) . ? O2 C1 1.2590(19) . ? O3 C8 1.245(2) . ? O4 C8 1.2836(19) . ? O5 C15 1.2628(19) . ? O6 C15 1.2613(19) . ? O7 N3 1.3211(16) . ? N1 C22 1.346(2) . ? N1 C26 1.3552(19) . ? N2 C28 1.146(2) . ? N3 C27 1.3084(19) . ? C1 C2 1.488(2) . ? C2 C7 1.390(2) . ? C2 C3 1.405(2) . ? C3 C4 1.385(3) . ? C3 H3 0.9300 . ? C4 C5 1.390(3) . ? C4 H4 0.9300 . ? C5 C6 1.390(3) . ? C5 H5 0.9300 . ? C6 C7 1.392(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.499(2) . ? C9 C14 1.394(2) . ? C9 C10 1.397(2) . ? C10 C11 1.386(3) . ? C10 H10 0.9300 . ? C11 C12 1.392(3) . ? C11 H11 0.9300 . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 C14 1.388(2) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.505(2) . ? C16 C17 1.391(2) . ? C16 C21 1.397(2) . ? C17 C18 1.394(2) . ? C17 H17 0.9300 . ? C18 C19 1.387(3) . ? C18 H18 0.9300 . ? C19 C20 1.393(3) . ? C19 H19 0.9300 . ? C20 C21 1.385(2) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.403(2) . ? C22 H22 0.9300 . ? C23 C24 1.374(2) . ? C23 H23 0.9300 . ? C24 C25 1.391(2) . ? C24 H24 0.9300 . ? C25 C26 1.398(2) . ? C25 H25 0.9300 . ? C26 C27 1.468(2) . ? C27 C28 1.439(2) . ? Cl1 C29 1.772(2) . ? Cl2 C29 1.747(2) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.503(3) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N4 1.503(2) . ? C31 H31 0.9700 . ? C31 H31A 0.9700 . ? N4 C33 1.501(2) . ? N4 H4NA 0.9000 . ? N4 H4NB 0.9000 . ? C33 C34 1.511(3) . ? C33 H33 0.9700 . ? C33 H33A 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O6 94.08(5) . . ? O4 Mn1 N1 87.40(5) . . ? O6 Mn1 N1 105.18(5) . . ? O4 Mn1 O2 94.27(5) . . ? O6 Mn1 O2 157.64(5) . . ? N1 Mn1 O2 95.89(5) . . ? O4 Mn1 O1 117.41(4) . . ? O6 Mn1 O1 100.52(5) . . ? N1 Mn1 O1 142.72(4) . . ? O2 Mn1 O1 57.32(4) . . ? O4 Mn1 N3 158.29(5) . . ? O6 Mn1 N3 88.82(5) . . ? N1 Mn1 N3 71.10(5) . . ? O2 Mn1 N3 91.03(5) . . ? O1 Mn1 N3 83.03(4) . . ? O5 Mn2 O5 180.0 3_657 . ? O5 Mn2 O1 85.48(5) 3_657 3_657 ? O5 Mn2 O1 94.52(5) . 3_657 ? O5 Mn2 O1 94.52(5) 3_657 . ? O5 Mn2 O1 85.48(5) . . ? O1 Mn2 O1 180.0 3_657 . ? O5 Mn2 O7 85.17(5) 3_657 . ? O5 Mn2 O7 94.83(5) . . ? O1 Mn2 O7 86.96(4) 3_657 . ? O1 Mn2 O7 93.04(4) . . ? O5 Mn2 O7 94.83(5) 3_657 3_657 ? O5 Mn2 O7 85.17(5) . 3_657 ? O1 Mn2 O7 93.04(4) 3_657 3_657 ? O1 Mn2 O7 86.96(4) . 3_657 ? O7 Mn2 O7 180.0 . 3_657 ? C1 O1 Mn2 132.32(10) . . ? C1 O1 Mn1 90.17(9) . . ? Mn2 O1 Mn1 105.27(5) . . ? C1 O2 Mn1 92.75(9) . . ? C8 O4 Mn1 115.48(10) . . ? C15 O5 Mn2 143.86(11) . . ? C15 O6 Mn1 124.68(11) . . ? N3 O7 Mn2 113.92(9) . . ? C22 N1 C26 118.34(13) . . ? C22 N1 Mn1 123.19(10) . . ? C26 N1 Mn1 118.33(10) . . ? C27 N3 O7 118.10(13) . . ? C27 N3 Mn1 116.26(10) . . ? O7 N3 Mn1 125.64(9) . . ? O2 C1 O1 119.74(14) . . ? O2 C1 C2 120.53(13) . . ? O1 C1 C2 119.69(14) . . ? C7 C2 C3 119.51(16) . . ? C7 C2 C1 119.96(15) . . ? C3 C2 C1 120.51(14) . . ? C4 C3 C2 119.95(16) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.21(19) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.13(19) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 119.89(18) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C2 C7 C6 120.30(18) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? O3 C8 O4 123.63(15) . . ? O3 C8 C9 119.89(14) . . ? O4 C8 C9 116.47(14) . . ? C14 C9 C10 118.53(15) . . ? C14 C9 C8 120.86(14) . . ? C10 C9 C8 120.61(15) . . ? C11 C10 C9 121.12(19) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 119.3(2) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 120.34(19) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.00(19) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C9 120.67(17) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O6 C15 O5 125.00(15) . . ? O6 C15 C16 118.91(14) . . ? O5 C15 C16 116.07(14) . . ? C17 C16 C21 119.92(15) . . ? C17 C16 C15 120.06(14) . . ? C21 C16 C15 120.02(15) . . ? C16 C17 C18 120.14(16) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 119.67(17) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.34(17) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 120.09(17) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C16 119.85(16) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? N1 C22 C23 121.66(15) . . ? N1 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 119.96(15) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 118.75(16) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C24 C25 C26 118.81(15) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? N1 C26 C25 122.47(14) . . ? N1 C26 C27 115.62(13) . . ? C25 C26 C27 121.90(14) . . ? N3 C27 C28 120.20(14) . . ? N3 C27 C26 118.64(14) . . ? C28 C27 C26 121.16(13) . . ? N2 C28 C27 179.25(18) . . ? Cl2 C29 Cl1 112.20(11) . . ? Cl2 C29 H29A 109.2 . . ? Cl1 C29 H29A 109.2 . . ? Cl2 C29 H29B 109.2 . . ? Cl1 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C30 C31 N4 111.36(15) . . ? C30 C31 H31 109.4 . . ? N4 C31 H31 109.4 . . ? C30 C31 H31A 109.4 . . ? N4 C31 H31A 109.4 . . ? H31 C31 H31A 108.0 . . ? C33 N4 C31 113.10(13) . . ? C33 N4 H4NA 109.0 . . ? C31 N4 H4NA 109.0 . . ? C33 N4 H4NB 109.0 . . ? C31 N4 H4NB 109.0 . . ? H4NA N4 H4NB 107.8 . . ? N4 C33 C34 112.34(14) . . ? N4 C33 H33 109.1 . . ? C34 C33 H33 109.1 . . ? N4 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? H33 C33 H33A 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.768 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.120 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 916862' ####################################################################### # # 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_af29laz1na1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C56 H32 Mn4 N24 O8), C4 H10 O, 10(C H4 O), 2(H2 O)' _chemical_formula_sum 'C126 H74 Mn8 N48 O29' _chemical_formula_weight 3163.85 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1707(6) _cell_length_b 24.1765(9) _cell_length_c 25.4451(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.261(2) _cell_angle_gamma 90.00 _cell_volume 7816.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1869 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 16.98 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3196 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9261 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 21.73 _reflns_number_total 9261 _reflns_number_gt 6042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. The displacement parameters of some lengths in the direction of the bond are restrained to be equal within an effective standard deviation (DELU sentences) The distance of diethyleter are restrained (DFIX sentences) The quality of the crystal was poor, but unfortunately attempts to obtain better ones using different solvents were unsuccesful. ; _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^)+(0.0651P)^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 9261 _refine_ls_number_parameters 966 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.029 _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 0.56818(7) 0.13886(3) 0.11228(3) 0.0232(2) Uani 1 1 d . . . Mn2 Mn 0.43679(7) 0.34508(3) 0.09138(3) 0.0235(2) Uani 1 1 d . . . Mn3 Mn 0.30402(7) 0.20622(3) 0.03284(3) 0.0219(2) Uani 1 1 d . . . Mn4 Mn 0.70263(7) 0.27693(3) 0.09439(3) 0.0231(2) Uani 1 1 d . . . O1 O 0.3214(3) 0.11993(13) 0.04176(15) 0.0269(10) Uani 1 1 d . . . O2 O 0.2733(3) 0.33695(14) 0.05529(14) 0.0268(9) Uani 1 1 d . . . O3 O 0.7350(3) 0.14815(14) 0.12797(15) 0.0295(10) Uani 1 1 d . . . O4 O 0.3755(3) 0.22041(14) 0.11537(14) 0.0282(10) Uani 1 1 d . . . O5 O 0.6902(3) 0.36238(14) 0.11018(15) 0.0311(10) Uani 1 1 d . . . O6 O 0.5463(3) 0.17745(14) 0.03552(14) 0.0264(10) Uani 1 1 d . . . O7 O 0.4715(3) 0.30342(14) 0.02607(14) 0.0268(10) Uani 1 1 d . . . O8 O 0.6158(3) 0.25720(14) 0.15021(14) 0.0284(10) Uani 1 1 d . . . N1 N 0.1324(4) 0.18948(17) 0.03247(17) 0.0245(12) Uani 1 1 d . . . N2 N 0.2263(4) 0.28854(17) 0.04563(17) 0.0235(11) Uani 1 1 d . . . N3 N 0.0290(4) 0.3804(2) 0.0376(2) 0.0376(14) Uani 1 1 d . . . N4 N 0.6036(4) 0.04859(17) 0.09693(18) 0.0248(11) Uani 1 1 d . . . N5 N 0.4128(4) 0.09656(17) 0.06108(17) 0.0236(12) Uani 1 1 d . . . N6 N 0.2458(4) -0.0161(2) 0.0236(2) 0.0421(14) Uani 1 1 d . . . N7 N 0.8792(4) 0.29349(18) 0.13766(18) 0.0265(12) Uani 1 1 d . . . N8 N 0.7824(4) 0.19601(17) 0.12850(17) 0.0244(12) Uani 1 1 d . . . N9 N 0.9819(5) 0.1045(2) 0.1766(3) 0.082(2) Uani 1 1 d . . . N10 N 0.5899(4) 0.11665(18) 0.20196(18) 0.0287(12) Uani 1 1 d . . . N11 N 0.4444(4) 0.18410(17) 0.14260(18) 0.0248(12) Uani 1 1 d . . . N12 N 0.3051(4) 0.2246(2) 0.2345(2) 0.0392(14) Uani 1 1 d . . . N13 N 0.4092(4) 0.43590(17) 0.06457(18) 0.0258(12) Uani 1 1 d . . . N14 N 0.5973(4) 0.38686(18) 0.09638(18) 0.0262(12) Uani 1 1 d . . . N15 N 0.7726(5) 0.4942(2) 0.1105(2) 0.0478(15) Uani 1 1 d . . . N16 N 0.7292(3) 0.30173(17) 0.01236(18) 0.0223(11) Uani 1 1 d . . . N17 N 0.6115(4) 0.21644(16) 0.02929(18) 0.0242(12) Uani 1 1 d . . . N18 N 0.5218(4) 0.1634(2) -0.1010(2) 0.0355(13) Uani 1 1 d . . . N19 N 0.2514(4) 0.20108(17) -0.06001(17) 0.0228(11) Uani 1 1 d . . . N20 N 0.4010(3) 0.26852(16) -0.00165(18) 0.0203(11) Uani 1 1 d . . . N21 N 0.4656(4) 0.34539(19) -0.10300(19) 0.0356(14) Uani 1 1 d . . . N22 N 0.4015(4) 0.36601(18) 0.17193(18) 0.0263(12) Uani 1 1 d . . . N23 N 0.5463(4) 0.29371(18) 0.15687(18) 0.0274(12) Uani 1 1 d . . . N24 N 0.6582(4) 0.2485(2) 0.2878(2) 0.0400(14) Uani 1 1 d . . . C1 C 0.0869(5) 0.1389(2) 0.0287(2) 0.0337(16) Uani 1 1 d . . . H1 H 0.1288 0.1078 0.0296 0.040 Uiso 1 1 calc R . . C2 C -0.0189(5) 0.1316(2) 0.0236(2) 0.0364(16) Uani 1 1 d . . . H2 H -0.0472 0.0962 0.0227 0.044 Uiso 1 1 calc R . . C3 C -0.0827(5) 0.1778(2) 0.0200(2) 0.0350(16) Uani 1 1 d . . . H3 H -0.1548 0.1742 0.0154 0.042 Uiso 1 1 calc R . . C4 C -0.0368(5) 0.2291(2) 0.0232(2) 0.0289(15) Uani 1 1 d . . . H4 H -0.0780 0.2608 0.0207 0.035 Uiso 1 1 calc R . . C5 C 0.0702(4) 0.2337(2) 0.0301(2) 0.0211(14) Uani 1 1 d . . . C6 C 0.1249(5) 0.2877(2) 0.0372(2) 0.0229(14) Uani 1 1 d . . . C7 C 0.0685(5) 0.3395(2) 0.0370(2) 0.0258(15) Uani 1 1 d . . . C8 C 0.6977(5) 0.0255(2) 0.1094(2) 0.0255(14) Uani 1 1 d . . . H8 H 0.7552 0.0482 0.1241 0.031 Uiso 1 1 calc R . . C9 C 0.7175(5) -0.0300(2) 0.1022(2) 0.0299(15) Uani 1 1 d . . . H9 H 0.7855 -0.0442 0.1116 0.036 Uiso 1 1 calc R . . C10 C 0.6304(5) -0.0636(2) 0.0801(2) 0.0304(15) Uani 1 1 d . . . H10 H 0.6399 -0.1010 0.0746 0.036 Uiso 1 1 calc R . . C11 C 0.5315(5) -0.0417(2) 0.0666(2) 0.0284(15) Uani 1 1 d . . . H11 H 0.4730 -0.0638 0.0520 0.034 Uiso 1 1 calc R . . C12 C 0.5206(4) 0.0148(2) 0.0753(2) 0.0224(14) Uani 1 1 d . . . C13 C 0.4167(5) 0.0423(2) 0.0592(2) 0.0248(14) Uani 1 1 d U . . C14 C 0.3214(5) 0.0097(2) 0.0385(2) 0.0286(14) Uani 1 1 d U . . C15 C 0.9257(5) 0.3429(2) 0.1446(2) 0.0327(16) Uani 1 1 d . . . H15 H 0.8835 0.3742 0.1360 0.039 Uiso 1 1 calc R . . C16 C 1.0352(5) 0.3503(2) 0.1643(2) 0.0362(16) Uani 1 1 d . . . H16 H 1.0645 0.3855 0.1691 0.043 Uiso 1 1 calc R . . C17 C 1.0980(5) 0.3036(2) 0.1763(2) 0.0325(16) Uani 1 1 d . . . H17 H 1.1709 0.3066 0.1882 0.039 Uiso 1 1 calc R . . C18 C 1.0492(5) 0.2521(2) 0.1701(2) 0.0290(15) Uani 1 1 d . . . H18 H 1.0893 0.2200 0.1783 0.035 Uiso 1 1 calc R . . C19 C 0.9420(5) 0.2487(2) 0.1518(2) 0.0264(15) Uani 1 1 d . . . C20 C 0.8853(5) 0.1963(2) 0.1468(2) 0.0261(15) Uani 1 1 d . . . C21 C 0.9395(5) 0.1450(3) 0.1645(3) 0.0468(19) Uani 1 1 d . . . C22 C 0.6657(5) 0.0839(2) 0.2325(2) 0.0358(16) Uani 1 1 d . . . H22 H 0.7156 0.0690 0.2166 0.043 Uiso 1 1 calc R . . C23 C 0.6728(5) 0.0714(2) 0.2871(2) 0.0402(18) Uani 1 1 d . . . H23 H 0.7269 0.0490 0.3069 0.048 Uiso 1 1 calc R . . C24 C 0.6004(5) 0.0923(2) 0.3112(2) 0.0394(17) Uani 1 1 d . . . H24 H 0.6033 0.0836 0.3472 0.047 Uiso 1 1 calc R . . C25 C 0.5229(5) 0.1262(2) 0.2816(2) 0.0298(15) Uani 1 1 d . . . H25 H 0.4735 0.1417 0.2974 0.036 Uiso 1 1 calc R . . C26 C 0.5190(5) 0.1371(2) 0.2269(2) 0.0242(14) Uani 1 1 d . . . C27 C 0.4423(4) 0.1753(2) 0.1929(2) 0.0246(14) Uani 1 1 d . . . C28 C 0.3659(5) 0.2033(2) 0.2162(2) 0.0291(15) Uani 1 1 d . . . C29 C 0.3160(5) 0.4592(2) 0.0437(2) 0.0314(15) Uani 1 1 d . . . H29 H 0.2563 0.4370 0.0366 0.038 Uiso 1 1 calc R . . C30 C 0.3037(5) 0.5149(2) 0.0320(2) 0.0309(15) Uani 1 1 d . . . H30 H 0.2371 0.5298 0.0177 0.037 Uiso 1 1 calc R . . C31 C 0.3907(5) 0.5478(2) 0.0418(2) 0.0326(16) Uani 1 1 d . . . H31 H 0.3839 0.5855 0.0341 0.039 Uiso 1 1 calc R . . C32 C 0.4885(5) 0.5250(2) 0.0629(2) 0.0293(15) Uani 1 1 d . . . H32 H 0.5486 0.5470 0.0703 0.035 Uiso 1 1 calc R . . C33 C 0.4955(4) 0.4687(2) 0.0729(2) 0.0223(14) Uani 1 1 d . . . C34 C 0.5966(5) 0.4412(2) 0.0919(2) 0.0244(13) Uani 1 1 d U . . C35 C 0.6945(5) 0.4707(2) 0.1020(2) 0.0296(15) Uani 1 1 d U . . C36 C 0.7880(4) 0.3442(2) 0.0037(2) 0.0253(14) Uani 1 1 d . . . H36 H 0.8175 0.3674 0.0329 0.030 Uiso 1 1 calc R . . C37 C 0.8073(4) 0.3556(2) -0.0455(2) 0.0277(15) Uani 1 1 d . . . H37 H 0.8482 0.3859 -0.0494 0.033 Uiso 1 1 calc R . . C38 C 0.7649(4) 0.3212(2) -0.0895(2) 0.0289(15) Uani 1 1 d . . . H38 H 0.7781 0.3272 -0.1232 0.035 Uiso 1 1 calc R . . C39 C 0.7019(5) 0.2774(2) -0.0815(2) 0.0276(15) Uani 1 1 d . . . H39 H 0.6710 0.2539 -0.1102 0.033 Uiso 1 1 calc R . . C40 C 0.6858(4) 0.2691(2) -0.0307(2) 0.0226(14) Uani 1 1 d . . . C41 C 0.6208(4) 0.2233(2) -0.0203(2) 0.0206(13) Uani 1 1 d . . . C42 C 0.5645(5) 0.1891(2) -0.0642(3) 0.0252(15) Uani 1 1 d . . . C43 C 0.1771(5) 0.1665(2) -0.0888(2) 0.0289(15) Uani 1 1 d . . . H43 H 0.1423 0.1433 -0.0701 0.035 Uiso 1 1 calc R . . C44 C 0.1506(5) 0.1645(2) -0.1454(2) 0.0348(16) Uani 1 1 d . . . H44 H 0.0989 0.1402 -0.1641 0.042 Uiso 1 1 calc R . . C45 C 0.2017(5) 0.1990(2) -0.1737(2) 0.0362(16) Uani 1 1 d . . . H45 H 0.1849 0.1985 -0.2116 0.043 Uiso 1 1 calc R . . C46 C 0.2788(5) 0.2343(2) -0.1439(2) 0.0300(15) Uani 1 1 d . . . H46 H 0.3148 0.2578 -0.1616 0.036 Uiso 1 1 calc R . . C47 C 0.3015(4) 0.2340(2) -0.0876(2) 0.0213(14) Uani 1 1 d . . . C48 C 0.3802(4) 0.2713(2) -0.0540(2) 0.0232(14) Uani 1 1 d . . . C49 C 0.4301(5) 0.3127(2) -0.0806(2) 0.0254(15) Uani 1 1 d . . . C50 C 0.3274(5) 0.4012(2) 0.1786(2) 0.0342(16) Uani 1 1 d . . . H50 H 0.2857 0.4189 0.1480 0.041 Uiso 1 1 calc R . . C51 C 0.3097(5) 0.4126(2) 0.2285(3) 0.0375(17) Uani 1 1 d . . . H51 H 0.2581 0.4378 0.2314 0.045 Uiso 1 1 calc R . . C52 C 0.3696(5) 0.3860(2) 0.2740(3) 0.0403(17) Uani 1 1 d . . . H52 H 0.3596 0.3931 0.3082 0.048 Uiso 1 1 calc R . . C53 C 0.4454(5) 0.3485(2) 0.2678(2) 0.0389(17) Uani 1 1 d . . . H53 H 0.4862 0.3294 0.2977 0.047 Uiso 1 1 calc R . . C54 C 0.4596(5) 0.3397(2) 0.2160(2) 0.0299(15) Uani 1 1 d . . . C55 C 0.5385(5) 0.2997(2) 0.2071(2) 0.0298(15) Uani 1 1 d . . . C56 C 0.6056(5) 0.2705(2) 0.2516(3) 0.0320(16) Uani 1 1 d . . . O9 O 0.3066(7) 0.0341(4) 0.2326(4) 0.075(3) Uani 0.50 1 d PD . . C57 C 0.4195(9) -0.0218(5) 0.1968(5) 0.0516(19) Uani 0.50 1 d PD . . H57A H 0.4357 -0.0306 0.1631 0.077 Uiso 0.50 1 calc PR . . H57B H 0.4026 -0.0551 0.2132 0.077 Uiso 0.50 1 calc PR . . H57C H 0.4793 -0.0044 0.2210 0.077 Uiso 0.50 1 calc PR . . C58 C 0.3274(9) 0.0167(5) 0.1859(4) 0.0516(19) Uani 0.50 1 d PD . . H58A H 0.3418 0.0486 0.1658 0.062 Uiso 0.50 1 calc PR . . H58B H 0.2659 -0.0019 0.1635 0.062 Uiso 0.50 1 calc PR . . C59 C 0.2298(9) 0.0748(5) 0.2249(4) 0.0516(19) Uani 0.50 1 d PD . . H59A H 0.1635 0.0601 0.2032 0.062 Uiso 0.50 1 calc PR . . H59B H 0.2494 0.1056 0.2051 0.062 Uiso 0.50 1 calc PR . . C60 C 0.2162(10) 0.0954(5) 0.2790(4) 0.0516(19) Uani 0.50 1 d PD . . H60A H 0.1737 0.1282 0.2732 0.077 Uiso 0.50 1 calc PR . . H60B H 0.2839 0.1036 0.3031 0.077 Uiso 0.50 1 calc PR . . H60C H 0.1823 0.0673 0.2951 0.077 Uiso 0.50 1 calc PR . . O1W O 0.0075(4) 0.43801(19) 0.3831(2) 0.0772(16) Uani 1 1 d . . . C1W C 0.0009(6) 0.4843(3) 0.4172(3) 0.062(2) Uani 1 1 d . . . O2W O 0.8947(5) 0.3436(2) 0.3820(2) 0.0882(18) Uani 1 1 d . . . C2W C 0.7885(7) 0.3618(3) 0.3788(4) 0.087(3) Uani 1 1 d . . . O3W O 0.0248(5) 0.1467(2) 0.3988(2) 0.0811(17) Uani 1 1 d . . . C3W C 0.1391(7) 0.1413(3) 0.4060(3) 0.073(2) Uani 1 1 d . . . O4W O 0.0801(4) 0.55029(18) 0.1250(2) 0.0644(14) Uani 1 1 d . . . C4W C 0.0316(6) 0.5134(3) 0.0809(3) 0.071(2) Uani 1 1 d . . . O5W O 0.9494(4) 0.2419(2) 0.3506(2) 0.0841(17) Uani 1 1 d . . . C5W C 0.9273(7) 0.2392(4) 0.2912(4) 0.088(3) Uani 1 1 d . . . O6W O 0.7715(10) 0.3999(5) 0.2395(4) 0.098(4) Uani 0.50 1 d P . . O7W O 0.1008(6) 0.4919(3) 0.2179(3) 0.051(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0296(6) 0.0190(5) 0.0208(5) 0.0020(4) 0.0063(4) 0.0024(4) Mn2 0.0278(6) 0.0213(5) 0.0209(5) -0.0014(4) 0.0057(4) 0.0002(4) Mn3 0.0288(6) 0.0175(5) 0.0192(5) 0.0014(4) 0.0056(4) 0.0020(4) Mn4 0.0287(6) 0.0188(5) 0.0206(5) -0.0001(4) 0.0044(4) 0.0016(4) O1 0.030(3) 0.018(2) 0.032(2) 0.0008(18) 0.008(2) 0.0057(19) O2 0.029(3) 0.020(2) 0.030(2) -0.0016(18) 0.0045(19) -0.0038(19) O3 0.034(3) 0.021(2) 0.032(2) 0.0020(19) 0.006(2) 0.0000(19) O4 0.037(3) 0.026(2) 0.017(2) 0.0033(19) 0.0005(19) 0.013(2) O5 0.027(3) 0.025(2) 0.042(3) -0.004(2) 0.010(2) 0.002(2) O6 0.036(3) 0.025(2) 0.016(2) 0.0024(18) 0.0036(19) -0.0036(19) O7 0.032(3) 0.029(2) 0.018(2) -0.0052(19) 0.0050(19) -0.001(2) O8 0.033(3) 0.029(2) 0.024(2) 0.0073(18) 0.009(2) 0.008(2) N1 0.031(3) 0.018(3) 0.024(3) 0.004(2) 0.006(2) 0.004(2) N2 0.027(3) 0.021(3) 0.021(3) 0.003(2) 0.004(2) -0.003(2) N3 0.033(4) 0.022(3) 0.058(4) -0.004(3) 0.012(3) -0.003(3) N4 0.025(3) 0.024(3) 0.026(3) 0.003(2) 0.008(2) 0.000(3) N5 0.032(3) 0.017(3) 0.021(3) 0.003(2) 0.006(2) 0.009(2) N6 0.036(4) 0.030(3) 0.054(4) 0.000(3) 0.003(3) -0.005(3) N7 0.035(3) 0.019(3) 0.024(3) 0.003(2) 0.004(2) -0.001(3) N8 0.045(4) 0.014(3) 0.015(3) -0.001(2) 0.009(3) -0.003(2) N9 0.057(5) 0.043(4) 0.122(6) 0.012(4) -0.018(4) 0.020(3) N10 0.029(3) 0.030(3) 0.027(3) -0.001(2) 0.008(3) 0.012(2) N11 0.036(3) 0.018(3) 0.020(3) -0.001(2) 0.005(2) 0.001(2) N12 0.046(4) 0.046(3) 0.026(3) 0.000(3) 0.008(3) 0.014(3) N13 0.030(3) 0.025(3) 0.022(3) 0.000(2) 0.006(2) 0.001(3) N14 0.022(3) 0.031(3) 0.027(3) -0.002(2) 0.006(2) 0.002(2) N15 0.048(4) 0.037(3) 0.059(4) -0.003(3) 0.014(3) -0.009(3) N16 0.022(3) 0.016(2) 0.028(3) 0.004(2) 0.005(2) 0.002(2) N17 0.028(3) 0.016(3) 0.029(3) 0.007(2) 0.007(2) -0.006(2) N18 0.046(4) 0.032(3) 0.029(3) 0.000(3) 0.011(3) -0.007(3) N19 0.027(3) 0.016(2) 0.024(3) -0.001(2) 0.004(2) 0.004(2) N20 0.024(3) 0.018(3) 0.020(3) -0.007(2) 0.008(2) 0.001(2) N21 0.053(4) 0.029(3) 0.025(3) 0.004(3) 0.012(3) 0.000(3) N22 0.027(3) 0.027(3) 0.025(3) -0.003(2) 0.005(3) -0.004(2) N23 0.028(3) 0.032(3) 0.023(3) 0.000(2) 0.007(2) -0.004(2) N24 0.050(4) 0.044(3) 0.027(3) 0.008(3) 0.011(3) -0.008(3) C1 0.045(5) 0.029(4) 0.029(4) 0.007(3) 0.013(3) 0.006(3) C2 0.039(5) 0.032(4) 0.040(4) 0.004(3) 0.013(3) -0.004(3) C3 0.026(4) 0.031(4) 0.045(4) 0.002(3) 0.003(3) 0.004(3) C4 0.029(4) 0.018(3) 0.040(4) 0.002(3) 0.010(3) 0.008(3) C5 0.022(4) 0.020(3) 0.020(3) 0.003(3) 0.004(3) 0.000(3) C6 0.025(4) 0.026(3) 0.018(3) 0.002(3) 0.006(3) 0.005(3) C7 0.035(4) 0.016(3) 0.026(4) -0.006(3) 0.008(3) 0.001(3) C8 0.026(4) 0.024(3) 0.025(4) 0.002(3) 0.005(3) -0.001(3) C9 0.029(4) 0.026(4) 0.034(4) 0.005(3) 0.007(3) 0.009(3) C10 0.036(4) 0.018(3) 0.042(4) 0.004(3) 0.018(3) 0.001(3) C11 0.034(4) 0.023(3) 0.031(4) -0.004(3) 0.013(3) 0.000(3) C12 0.027(4) 0.025(3) 0.018(3) 0.002(3) 0.010(3) 0.006(3) C13 0.036(4) 0.017(3) 0.026(4) 0.004(3) 0.016(3) 0.001(2) C14 0.030(4) 0.018(3) 0.038(4) 0.004(3) 0.009(3) 0.007(2) C15 0.037(5) 0.031(4) 0.026(4) 0.003(3) 0.002(3) 0.001(3) C16 0.045(5) 0.029(4) 0.032(4) -0.005(3) 0.007(3) -0.012(3) C17 0.030(4) 0.031(4) 0.030(4) 0.011(3) -0.005(3) 0.004(3) C18 0.027(4) 0.026(4) 0.030(4) 0.001(3) 0.001(3) 0.003(3) C19 0.037(5) 0.018(3) 0.024(4) 0.002(3) 0.008(3) 0.001(3) C20 0.030(4) 0.027(4) 0.020(3) 0.002(3) 0.003(3) 0.006(3) C21 0.032(4) 0.034(4) 0.061(5) -0.002(4) -0.012(4) 0.002(4) C22 0.031(4) 0.032(4) 0.044(4) 0.000(3) 0.009(3) 0.013(3) C23 0.053(5) 0.036(4) 0.019(4) 0.013(3) -0.012(3) 0.005(3) C24 0.055(5) 0.040(4) 0.021(4) 0.001(3) 0.007(4) 0.004(4) C25 0.035(4) 0.039(4) 0.017(4) 0.000(3) 0.010(3) 0.008(3) C26 0.034(4) 0.018(3) 0.020(4) -0.007(3) 0.006(3) -0.003(3) C27 0.020(4) 0.026(3) 0.026(4) 0.001(3) 0.004(3) 0.006(3) C28 0.038(5) 0.032(4) 0.012(3) 0.005(3) -0.003(3) -0.003(3) C29 0.038(5) 0.029(4) 0.028(4) -0.005(3) 0.010(3) -0.002(3) C30 0.032(4) 0.025(4) 0.033(4) 0.000(3) 0.003(3) 0.010(3) C31 0.036(4) 0.023(3) 0.037(4) 0.005(3) 0.007(3) 0.001(3) C32 0.025(4) 0.028(4) 0.037(4) 0.004(3) 0.012(3) -0.002(3) C33 0.023(4) 0.023(3) 0.019(3) 0.001(3) 0.002(3) 0.005(3) C34 0.033(4) 0.016(3) 0.024(3) 0.003(3) 0.007(3) 0.001(2) C35 0.036(4) 0.021(3) 0.032(4) 0.011(3) 0.011(3) -0.001(3) C36 0.022(4) 0.025(3) 0.027(4) 0.005(3) 0.003(3) 0.002(3) C37 0.029(4) 0.018(3) 0.038(4) 0.004(3) 0.012(3) 0.003(3) C38 0.024(4) 0.038(4) 0.026(4) 0.003(3) 0.010(3) 0.001(3) C39 0.038(4) 0.024(3) 0.022(4) -0.001(3) 0.011(3) 0.000(3) C40 0.020(4) 0.028(3) 0.020(3) -0.002(3) 0.005(3) 0.002(3) C41 0.020(4) 0.027(3) 0.015(3) 0.008(3) 0.005(3) 0.003(3) C42 0.026(4) 0.027(4) 0.027(4) 0.004(3) 0.014(3) -0.005(3) C43 0.036(4) 0.013(3) 0.035(4) 0.002(3) 0.005(3) 0.005(3) C44 0.035(4) 0.037(4) 0.026(4) -0.003(3) -0.004(3) 0.008(3) C45 0.041(5) 0.045(4) 0.018(4) -0.003(3) 0.000(3) 0.004(3) C46 0.032(4) 0.035(4) 0.025(4) 0.007(3) 0.010(3) 0.003(3) C47 0.023(4) 0.019(3) 0.023(4) 0.003(3) 0.008(3) 0.012(3) C48 0.027(4) 0.023(3) 0.021(4) -0.001(3) 0.008(3) -0.002(3) C49 0.032(4) 0.028(4) 0.013(3) 0.000(3) 0.000(3) 0.003(3) C50 0.036(4) 0.030(4) 0.039(4) 0.000(3) 0.014(3) -0.001(3) C51 0.049(5) 0.025(3) 0.045(5) -0.017(3) 0.024(4) -0.003(3) C52 0.049(5) 0.041(4) 0.036(4) -0.012(4) 0.020(4) -0.005(4) C53 0.054(5) 0.036(4) 0.026(4) 0.000(3) 0.009(3) -0.008(4) C54 0.038(4) 0.027(3) 0.027(4) -0.007(3) 0.011(3) -0.012(3) C55 0.041(4) 0.030(4) 0.017(4) 0.000(3) 0.005(3) -0.012(3) C56 0.049(5) 0.031(4) 0.015(4) 0.001(3) 0.007(3) -0.007(3) O9 0.040(7) 0.106(8) 0.077(8) 0.012(7) 0.012(6) 0.015(6) C57 0.046(5) 0.061(5) 0.044(4) -0.003(4) 0.004(4) -0.013(4) C58 0.046(5) 0.061(5) 0.044(4) -0.003(4) 0.004(4) -0.013(4) C59 0.046(5) 0.061(5) 0.044(4) -0.003(4) 0.004(4) -0.013(4) C60 0.046(5) 0.061(5) 0.044(4) -0.003(4) 0.004(4) -0.013(4) O1W 0.090(5) 0.055(3) 0.099(4) -0.005(3) 0.046(4) -0.006(3) C1W 0.073(6) 0.044(4) 0.074(6) -0.012(4) 0.027(5) 0.002(4) O2W 0.100(5) 0.077(4) 0.089(4) -0.007(3) 0.029(4) 0.001(4) C2W 0.068(7) 0.088(6) 0.104(7) 0.006(6) 0.022(6) 0.012(5) O3W 0.080(5) 0.074(4) 0.091(4) -0.004(3) 0.024(4) -0.003(3) C3W 0.060(6) 0.077(6) 0.088(6) -0.011(5) 0.030(5) -0.018(5) O4W 0.062(4) 0.059(3) 0.072(4) -0.004(3) 0.016(3) -0.001(3) C4W 0.080(7) 0.058(5) 0.079(6) -0.023(5) 0.027(5) -0.020(4) O5W 0.086(5) 0.078(4) 0.093(5) 0.005(3) 0.033(4) -0.001(3) C5W 0.091(8) 0.115(7) 0.058(6) -0.006(5) 0.021(5) 0.000(6) O6W 0.118(11) 0.125(10) 0.052(7) -0.001(7) 0.024(7) -0.017(8) O7W 0.036(6) 0.037(5) 0.063(6) 0.031(5) -0.016(5) -0.005(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 O6 2.115(3) . ? Mn1 O3 2.139(4) . ? Mn1 N11 2.261(5) . ? Mn1 N4 2.287(4) . ? Mn1 N10 2.288(4) . ? Mn1 N5 2.351(5) . ? Mn2 O7 2.094(3) . ? Mn2 O2 2.116(4) . ? Mn2 N23 2.266(5) . ? Mn2 N22 2.275(5) . ? Mn2 N13 2.300(4) . ? Mn2 N14 2.316(5) . ? Mn3 O4 2.091(4) . ? Mn3 O1 2.105(3) . ? Mn3 N19 2.284(4) . ? Mn3 N20 2.294(4) . ? Mn3 N1 2.294(5) . ? Mn3 N2 2.300(4) . ? Mn4 O8 2.099(4) . ? Mn4 O5 2.119(3) . ? Mn4 N8 2.281(4) . ? Mn4 N16 2.285(4) . ? Mn4 N17 2.297(4) . ? Mn4 N7 2.330(5) . ? O1 N5 1.303(5) . ? O2 N2 1.317(5) . ? O3 N8 1.313(5) . ? O4 N11 1.320(5) . ? O5 N14 1.322(5) . ? O6 N17 1.313(5) . ? O7 N20 1.314(5) . ? O8 N23 1.315(5) . ? N1 C5 1.339(6) . ? N1 C1 1.354(7) . ? N2 C6 1.296(6) . ? N3 C7 1.118(6) . ? N4 C8 1.319(7) . ? N4 C12 1.360(7) . ? N5 C13 1.313(6) . ? N6 C14 1.153(7) . ? N7 C15 1.332(7) . ? N7 C19 1.353(7) . ? N8 C20 1.312(7) . ? N9 C21 1.131(7) . ? N10 C22 1.349(7) . ? N10 C26 1.354(7) . ? N11 C27 1.305(7) . ? N12 C28 1.148(7) . ? N13 C29 1.328(7) . ? N13 C33 1.356(7) . ? N14 C34 1.318(6) . ? N15 C35 1.144(7) . ? N16 C36 1.338(6) . ? N16 C40 1.349(6) . ? N17 C41 1.311(6) . ? N18 C42 1.142(7) . ? N19 C47 1.343(6) . ? N19 C43 1.347(7) . ? N20 C48 1.289(6) . ? N21 C49 1.143(6) . ? N22 C50 1.340(7) . ? N22 C54 1.340(7) . ? N23 C55 1.317(7) . ? N24 C56 1.128(7) . ? C1 C2 1.377(8) . ? C1 H1 0.9300 . ? C2 C3 1.386(8) . ? C2 H2 0.9300 . ? C3 C4 1.373(7) . ? C3 H3 0.9300 . ? C4 C5 1.379(7) . ? C4 H4 0.9300 . ? C5 C6 1.478(7) . ? C6 C7 1.456(8) . ? C8 C9 1.390(7) . ? C8 H8 0.9300 . ? C9 C10 1.396(8) . ? C9 H9 0.9300 . ? C10 C11 1.363(8) . ? C10 H10 0.9300 . ? C11 C12 1.398(7) . ? C11 H11 0.9300 . ? C12 C13 1.479(8) . ? C13 C14 1.458(8) . ? C15 C16 1.409(8) . ? C15 H15 0.9300 . ? C16 C17 1.386(8) . ? C16 H16 0.9300 . ? C17 C18 1.391(7) . ? C17 H17 0.9300 . ? C18 C19 1.368(8) . ? C18 H18 0.9300 . ? C19 C20 1.458(8) . ? C20 C21 1.443(8) . ? C22 C23 1.402(8) . ? C22 H22 0.9300 . ? C23 C24 1.358(8) . ? C23 H23 0.9300 . ? C24 C25 1.370(8) . ? C24 H24 0.9300 . ? C25 C26 1.403(7) . ? C25 H25 0.9300 . ? C26 C27 1.470(7) . ? C27 C28 1.462(8) . ? C29 C30 1.379(7) . ? C29 H29 0.9300 . ? C30 C31 1.362(8) . ? C30 H30 0.9300 . ? C31 C32 1.373(8) . ? C31 H31 0.9300 . ? C32 C33 1.384(7) . ? C32 H32 0.9300 . ? C33 C34 1.454(7) . ? C34 C35 1.436(8) . ? C36 C37 1.372(7) . ? C36 H36 0.9300 . ? C37 C38 1.387(7) . ? C37 H37 0.9300 . ? C38 C39 1.394(7) . ? C38 H38 0.9300 . ? C39 C40 1.379(7) . ? C39 H39 0.9300 . ? C40 C41 1.464(7) . ? C41 C42 1.429(8) . ? C43 C44 1.392(8) . ? C43 H43 0.9300 . ? C44 C45 1.387(8) . ? C44 H44 0.9300 . ? C45 C46 1.389(8) . ? C45 H45 0.9300 . ? C46 C47 1.386(7) . ? C46 H46 0.9300 . ? C47 C48 1.467(7) . ? C48 C49 1.458(8) . ? C50 C51 1.377(8) . ? C50 H50 0.9300 . ? C51 C52 1.377(8) . ? C51 H51 0.9300 . ? C52 C53 1.390(8) . ? C52 H52 0.9300 . ? C53 C54 1.394(8) . ? C53 H53 0.9300 . ? C54 C55 1.480(8) . ? C55 C56 1.426(9) . ? O9 C58 1.353(8) . ? O9 C59 1.389(8) . ? C57 C58 1.497(8) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.520(8) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? O1W C1W 1.433(8) . ? O2W C2W 1.447(10) . ? O3W C3W 1.473(9) . ? O4W C4W 1.444(8) . ? O5W C5W 1.462(9) . ? 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 O6 Mn1 O3 90.54(14) . . ? O6 Mn1 N11 99.60(16) . . ? O3 Mn1 N11 133.09(15) . . ? O6 Mn1 N4 104.33(15) . . ? O3 Mn1 N4 83.46(15) . . ? N11 Mn1 N4 135.89(16) . . ? O6 Mn1 N10 167.35(15) . . ? O3 Mn1 N10 89.18(16) . . ? N11 Mn1 N10 71.67(16) . . ? N4 Mn1 N10 88.21(15) . . ? O6 Mn1 N5 78.06(14) . . ? O3 Mn1 N5 148.26(15) . . ? N11 Mn1 N5 78.40(16) . . ? N4 Mn1 N5 71.17(16) . . ? N10 Mn1 N5 108.23(16) . . ? O7 Mn2 O2 91.19(15) . . ? O7 Mn2 N23 95.18(16) . . ? O2 Mn2 N23 130.26(15) . . ? O7 Mn2 N22 163.97(15) . . ? O2 Mn2 N22 89.19(16) . . ? N23 Mn2 N22 72.58(17) . . ? O7 Mn2 N13 105.92(15) . . ? O2 Mn2 N13 84.07(16) . . ? N23 Mn2 N13 139.63(17) . . ? N22 Mn2 N13 90.06(16) . . ? O7 Mn2 N14 82.32(15) . . ? O2 Mn2 N14 150.94(15) . . ? N23 Mn2 N14 78.69(16) . . ? N22 Mn2 N14 104.68(16) . . ? N13 Mn2 N14 70.76(17) . . ? O4 Mn3 O1 92.69(14) . . ? O4 Mn3 N19 168.98(16) . . ? O1 Mn3 N19 92.99(14) . . ? O4 Mn3 N20 97.34(16) . . ? O1 Mn3 N20 129.52(15) . . ? N19 Mn3 N20 71.80(16) . . ? O4 Mn3 N1 102.46(15) . . ? O1 Mn3 N1 84.55(15) . . ? N19 Mn3 N1 87.47(16) . . ? N20 Mn3 N1 139.61(15) . . ? O4 Mn3 N2 79.36(14) . . ? O1 Mn3 N2 151.95(15) . . ? N19 Mn3 N2 99.70(15) . . ? N20 Mn3 N2 78.42(15) . . ? N1 Mn3 N2 71.25(16) . . ? O8 Mn4 O5 90.60(14) . . ? O8 Mn4 N8 79.98(15) . . ? O5 Mn4 N8 144.55(16) . . ? O8 Mn4 N16 156.80(15) . . ? O5 Mn4 N16 87.44(15) . . ? N8 Mn4 N16 113.99(15) . . ? O8 Mn4 N17 93.97(15) . . ? O5 Mn4 N17 134.89(15) . . ? N8 Mn4 N17 80.16(15) . . ? N16 Mn4 N17 71.63(16) . . ? O8 Mn4 N7 111.88(15) . . ? O5 Mn4 N7 81.95(15) . . ? N8 Mn4 N7 70.45(16) . . ? N16 Mn4 N7 90.73(16) . . ? N17 Mn4 N7 135.80(16) . . ? N5 O1 Mn3 122.3(3) . . ? N2 O2 Mn2 122.6(3) . . ? N8 O3 Mn1 123.8(3) . . ? N11 O4 Mn3 118.9(3) . . ? N14 O5 Mn4 119.9(3) . . ? N17 O6 Mn1 119.6(3) . . ? N20 O7 Mn2 117.6(3) . . ? N23 O8 Mn4 117.2(3) . . ? C5 N1 C1 117.7(5) . . ? C5 N1 Mn3 116.7(3) . . ? C1 N1 Mn3 125.2(4) . . ? C6 N2 O2 117.3(4) . . ? C6 N2 Mn3 116.2(3) . . ? O2 N2 Mn3 126.2(3) . . ? C8 N4 C12 116.6(4) . . ? C8 N4 Mn1 125.7(4) . . ? C12 N4 Mn1 117.6(4) . . ? O1 N5 C13 117.4(5) . . ? O1 N5 Mn1 127.1(3) . . ? C13 N5 Mn1 114.7(4) . . ? C15 N7 C19 117.0(5) . . ? C15 N7 Mn4 125.7(4) . . ? C19 N7 Mn4 116.9(4) . . ? C20 N8 O3 116.9(4) . . ? C20 N8 Mn4 117.3(3) . . ? O3 N8 Mn4 125.6(4) . . ? C22 N10 C26 116.2(5) . . ? C22 N10 Mn1 126.3(4) . . ? C26 N10 Mn1 117.5(4) . . ? C27 N11 O4 115.7(4) . . ? C27 N11 Mn1 117.3(4) . . ? O4 N11 Mn1 126.9(3) . . ? C29 N13 C33 117.5(5) . . ? C29 N13 Mn2 125.6(4) . . ? C33 N13 Mn2 116.9(4) . . ? C34 N14 O5 117.0(5) . . ? C34 N14 Mn2 116.4(4) . . ? O5 N14 Mn2 126.0(3) . . ? C36 N16 C40 117.1(5) . . ? C36 N16 Mn4 125.8(4) . . ? C40 N16 Mn4 117.0(3) . . ? C41 N17 O6 116.0(4) . . ? C41 N17 Mn4 116.8(3) . . ? O6 N17 Mn4 127.2(3) . . ? C47 N19 C43 118.1(5) . . ? C47 N19 Mn3 116.8(4) . . ? C43 N19 Mn3 125.1(4) . . ? C48 N20 O7 116.7(4) . . ? C48 N20 Mn3 116.2(4) . . ? O7 N20 Mn3 127.0(3) . . ? C50 N22 C54 118.0(5) . . ? C50 N22 Mn2 125.8(4) . . ? C54 N22 Mn2 116.2(4) . . ? O8 N23 C55 115.7(5) . . ? O8 N23 Mn2 127.1(3) . . ? C55 N23 Mn2 117.2(4) . . ? N1 C1 C2 122.7(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 118.9(6) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 118.4(6) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 122.2(5) . . ? N1 C5 C6 115.3(5) . . ? C4 C5 C6 122.4(5) . . ? N2 C6 C7 119.3(5) . . ? N2 C6 C5 118.8(5) . . ? C7 C6 C5 121.9(5) . . ? N3 C7 C6 177.2(6) . . ? N4 C8 C9 125.0(5) . . ? N4 C8 H8 117.5 . . ? C9 C8 H8 117.5 . . ? C8 C9 C10 116.9(5) . . ? C8 C9 H9 121.6 . . ? C10 C9 H9 121.6 . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 118.1(6) . . ? C10 C11 H11 121.0 . . ? C12 C11 H11 121.0 . . ? N4 C12 C11 123.1(5) . . ? N4 C12 C13 115.4(5) . . ? C11 C12 C13 121.5(5) . . ? N5 C13 C14 121.0(5) . . ? N5 C13 C12 118.7(5) . . ? C14 C13 C12 120.1(5) . . ? N6 C14 C13 178.0(7) . . ? N7 C15 C16 123.6(5) . . ? N7 C15 H15 118.2 . . ? C16 C15 H15 118.2 . . ? C17 C16 C15 118.1(5) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 C18 118.2(6) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C19 C18 C17 119.8(5) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? N7 C19 C18 123.2(5) . . ? N7 C19 C20 114.1(5) . . ? C18 C19 C20 122.7(5) . . ? N8 C20 C21 119.1(5) . . ? N8 C20 C19 119.6(5) . . ? C21 C20 C19 121.3(6) . . ? N9 C21 C20 177.7(8) . . ? N10 C22 C23 122.9(6) . . ? N10 C22 H22 118.5 . . ? C23 C22 H22 118.5 . . ? C24 C23 C22 119.7(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 119.0(6) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C24 C25 C26 119.1(5) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? N10 C26 C25 123.1(5) . . ? N10 C26 C27 113.9(5) . . ? C25 C26 C27 122.9(5) . . ? N11 C27 C28 121.1(5) . . ? N11 C27 C26 119.5(5) . . ? C28 C27 C26 119.5(5) . . ? N12 C28 C27 179.0(6) . . ? N13 C29 C30 123.0(6) . . ? N13 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? C31 C30 C29 119.0(6) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 119.6(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 118.5(5) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? N13 C33 C32 122.3(5) . . ? N13 C33 C34 116.2(5) . . ? C32 C33 C34 121.5(5) . . ? N14 C34 C35 119.7(5) . . ? N14 C34 C33 118.0(5) . . ? C35 C34 C33 122.2(5) . . ? N15 C35 C34 179.5(7) . . ? N16 C36 C37 124.0(5) . . ? N16 C36 H36 118.0 . . ? C37 C36 H36 118.0 . . ? C36 C37 C38 118.9(5) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C37 C38 C39 117.9(5) . . ? C37 C38 H38 121.1 . . ? C39 C38 H38 121.1 . . ? C40 C39 C38 119.5(5) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? N16 C40 C39 122.6(5) . . ? N16 C40 C41 116.0(5) . . ? C39 C40 C41 121.3(5) . . ? N17 C41 C42 121.2(5) . . ? N17 C41 C40 118.4(5) . . ? C42 C41 C40 120.3(5) . . ? N18 C42 C41 176.4(6) . . ? N19 C43 C44 122.2(6) . . ? N19 C43 H43 118.9 . . ? C44 C43 H43 118.9 . . ? C45 C44 C43 119.5(6) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 118.1(5) . . ? C44 C45 H45 120.9 . . ? C46 C45 H45 120.9 . . ? C47 C46 C45 119.3(5) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? N19 C47 C46 122.8(5) . . ? N19 C47 C48 115.5(5) . . ? C46 C47 C48 121.8(5) . . ? N20 C48 C49 121.1(5) . . ? N20 C48 C47 119.6(5) . . ? C49 C48 C47 119.2(5) . . ? N21 C49 C48 177.3(6) . . ? N22 C50 C51 123.4(6) . . ? N22 C50 H50 118.3 . . ? C51 C50 H50 118.3 . . ? C50 C51 C52 118.9(6) . . ? C50 C51 H51 120.6 . . ? C52 C51 H51 120.6 . . ? C51 C52 C53 118.6(6) . . ? C51 C52 H52 120.7 . . ? C53 C52 H52 120.7 . . ? C52 C53 C54 119.1(6) . . ? C52 C53 H53 120.4 . . ? C54 C53 H53 120.4 . . ? N22 C54 C53 122.0(6) . . ? N22 C54 C55 116.8(5) . . ? C53 C54 C55 121.2(6) . . ? N23 C55 C56 121.8(6) . . ? N23 C55 C54 117.2(5) . . ? C56 C55 C54 121.0(5) . . ? N24 C56 C55 178.1(7) . . ? C58 O9 C59 113.8(8) . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O9 C58 C57 111.8(8) . . ? O9 C58 H58A 109.3 . . ? C57 C58 H58A 109.3 . . ? O9 C58 H58B 109.3 . . ? C57 C58 H58B 109.3 . . ? H58A C58 H58B 107.9 . . ? O9 C59 C60 111.1(8) . . ? O9 C59 H59A 109.4 . . ? C60 C59 H59A 109.4 . . ? O9 C59 H59B 109.4 . . ? C60 C59 H59B 109.4 . . ? H59A C59 H59B 108.0 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.160 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.072 _database_code_depnum_ccdc_archive 'CCDC 916863' ####################################################################### # # 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_af19laz1na _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H32 Mn4 N24 O8, 4(C H2 Cl2)' _chemical_formula_sum 'C60 H40 Cl8 Mn4 N24 O8' _chemical_formula_weight 1728.52 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 23.9923(12) _cell_length_b 23.9923(12) _cell_length_c 25.2740(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14548.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1770 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 21.12 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6944 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 KappaAPEXII' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5246 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 23.25 _reflns_number_total 5246 _reflns_number_gt 3460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER APEX2' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. It has been mesurated only reflections that have a value max of theta = 23.25\%, due to the poor quality of reflections. But other attempts of crystallization were done, but no single crystals of better quality were obtained. Regarding the crystal refinement parameter, for the structural resolution, it has been considered only reflections that have a value max of theta = 25\% (ACTA 50). Reflections between 25\% and 32\% have not been taken into account due to the poor quality of the reflections over this value. The poor quality of reflections could be due to the fact that the crystal does not diffract very well and to the kind of detector (image plate with spindle axis only) that was used. Other attempts of crystallization were done, but no single crystals of better quality were obtained. ; _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^)+(0.0119P)^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 5246 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _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 0.95586(2) 0.35405(2) 0.10827(2) 0.01720(14) Uani 1 1 d . . . O11 O 0.97267(9) 0.31162(9) 0.17960(9) 0.0235(6) Uani 1 1 d . . . O12 O 0.86981(9) 0.33717(9) 0.11994(9) 0.0241(6) Uani 1 1 d . . . N11 N 0.93288(11) 0.44372(11) 0.13315(10) 0.0191(7) Uani 1 1 d . . . N12 N 1.12134(13) 0.50825(12) 0.16266(13) 0.0370(9) Uani 1 1 d . . . N13 N 1.03625(11) 0.40071(11) 0.13051(10) 0.0192(7) Uani 1 1 d . . . N14 N 0.93323(11) 0.37204(11) 0.02298(11) 0.0199(7) Uani 1 1 d . . . N15 N 1.08465(12) 0.27832(13) -0.06254(12) 0.0356(9) Uani 1 1 d . . . N16 N 1.01955(11) 0.30887(11) 0.05597(11) 0.0209(7) Uani 1 1 d . . . C11 C 0.88128(13) 0.46516(14) 0.13638(13) 0.0235(9) Uani 1 1 d . . . H11 H 0.8513 0.4416 0.1298 0.028 Uiso 1 1 calc R . . C12 C 0.86985(14) 0.51998(14) 0.14886(13) 0.0249(9) Uani 1 1 d . . . H12 H 0.8333 0.5326 0.1510 0.030 Uiso 1 1 calc R . . C13 C 0.91391(14) 0.55543(14) 0.15801(13) 0.0249(9) Uani 1 1 d . . . H13 H 0.9076 0.5927 0.1660 0.030 Uiso 1 1 calc R . . C14 C 0.96749(13) 0.53487(13) 0.15522(13) 0.0208(9) Uani 1 1 d . . . H14 H 0.9977 0.5583 0.1615 0.025 Uiso 1 1 calc R . . C15 C 0.97622(13) 0.47900(13) 0.14300(13) 0.0183(8) Uani 1 1 d . . . C16 C 1.03123(13) 0.45375(13) 0.14126(13) 0.0161(8) Uani 1 1 d . . . C17 C 1.08108(15) 0.48518(13) 0.15323(14) 0.0215(9) Uani 1 1 d . . . C18 C 0.88967(14) 0.40178(14) 0.00673(14) 0.0260(9) Uani 1 1 d . . . H18 H 0.8665 0.4173 0.0323 0.031 Uiso 1 1 calc R . . C19 C 0.87676(14) 0.41097(14) -0.04620(15) 0.0256(9) Uani 1 1 d . . . H19 H 0.8467 0.4333 -0.0558 0.031 Uiso 1 1 calc R . . C110 C 0.90989(15) 0.38604(14) -0.08398(15) 0.0289(10) Uani 1 1 d . . . H110 H 0.9017 0.3903 -0.1197 0.035 Uiso 1 1 calc R . . C111 C 0.95506(14) 0.35486(13) -0.06841(14) 0.0245(9) Uani 1 1 d . . . H111 H 0.9781 0.3381 -0.0933 0.029 Uiso 1 1 calc R . . C112 C 0.96551(13) 0.34901(13) -0.01465(14) 0.0206(9) Uani 1 1 d . . . C113 C 1.01311(13) 0.31597(13) 0.00493(14) 0.0193(9) Uani 1 1 d . . . C114 C 1.05312(15) 0.29383(15) -0.03231(14) 0.0254(9) Uani 1 1 d . . . Mn2 Mn 0.50544(2) 0.63586(2) 0.11038(2) 0.01730(14) Uani 1 1 d . . . O21 O 0.59355(8) 0.62510(8) 0.11154(9) 0.0201(6) Uani 1 1 d . . . O22 O 0.50703(9) 0.68496(8) 0.17898(8) 0.0194(6) Uani 1 1 d . . . N21 N 0.50381(11) 0.55226(11) 0.15388(10) 0.0191(7) Uani 1 1 d . . . N22 N 0.31637(13) 0.56195(13) 0.22106(13) 0.0428(10) Uani 1 1 d . . . N23 N 0.41671(11) 0.62150(11) 0.14251(11) 0.0196(7) Uani 1 1 d . . . N24 N 0.51435(11) 0.60431(11) 0.02633(11) 0.0188(7) Uani 1 1 d . . . N25 N 0.41406(12) 0.75187(12) -0.06035(12) 0.0281(8) Uani 1 1 d . . . N26 N 0.46197(10) 0.69758(11) 0.05722(11) 0.0178(7) Uani 1 1 d . . . C21 C 0.54860(14) 0.52006(14) 0.16153(13) 0.0238(9) Uani 1 1 d . . . H21 H 0.5815 0.5290 0.1440 0.029 Uiso 1 1 calc R . . C22 C 0.54800(15) 0.47421(14) 0.19433(14) 0.0299(10) Uani 1 1 d . . . H22 H 0.5799 0.4527 0.1988 0.036 Uiso 1 1 calc R . . C23 C 0.49933(16) 0.46077(14) 0.22038(14) 0.0297(10) Uani 1 1 d . . . H23 H 0.4980 0.4300 0.2427 0.036 Uiso 1 1 calc R . . C24 C 0.45278(14) 0.49345(13) 0.21291(13) 0.0219(9) Uani 1 1 d . . . H24 H 0.4196 0.4849 0.2301 0.026 Uiso 1 1 calc R . . C25 C 0.45599(14) 0.53927(13) 0.17942(13) 0.0201(9) Uani 1 1 d . . . C26 C 0.40944(13) 0.57732(14) 0.17151(13) 0.0188(9) Uani 1 1 d . . . C27 C 0.35706(16) 0.56917(14) 0.19906(15) 0.0270(10) Uani 1 1 d . . . C28 C 0.54357(13) 0.55945(14) 0.01150(14) 0.0245(9) Uani 1 1 d . . . H28 H 0.5569 0.5357 0.0376 0.029 Uiso 1 1 calc R . . C29 C 0.55503(14) 0.54660(14) -0.04109(14) 0.0284(10) Uani 1 1 d . . . H29 H 0.5755 0.5150 -0.0499 0.034 Uiso 1 1 calc R . . C210 C 0.53511(14) 0.58208(14) -0.07976(15) 0.0277(9) Uani 1 1 d . . . H210 H 0.5422 0.5747 -0.1152 0.033 Uiso 1 1 calc R . . C211 C 0.50474(13) 0.62852(14) -0.06556(13) 0.0224(9) Uani 1 1 d . . . H211 H 0.4909 0.6526 -0.0912 0.027 Uiso 1 1 calc R . . C212 C 0.49533(13) 0.63850(13) -0.01246(13) 0.0177(8) Uani 1 1 d . . . C213 C 0.46455(13) 0.68761(13) 0.00646(13) 0.0169(8) Uani 1 1 d . . . C214 C 0.43692(14) 0.72401(14) -0.03065(14) 0.0193(9) Uani 1 1 d . . . Cl1 Cl 0.28479(5) 0.54466(4) 0.08145(5) 0.0622(4) Uani 1 1 d . . . Cl2 Cl 0.36563(5) 0.58663(5) 0.00563(6) 0.0838(5) Uani 1 1 d . . . C1W C 0.29840(15) 0.56078(15) 0.01424(15) 0.0441(12) Uani 1 1 d . . . H1W1 H 0.2937 0.5275 -0.0071 0.053 Uiso 1 1 calc R . . H1W2 H 0.2717 0.5883 0.0021 0.053 Uiso 1 1 calc R . . Cl3 Cl 0.82050(4) 0.54956(4) 0.00672(4) 0.0487(3) Uani 1 1 d . . . Cl4 Cl 0.94212(4) 0.53960(4) 0.00793(4) 0.0438(3) Uani 1 1 d . . . C2W C 0.88321(15) 0.57898(19) -0.0058(2) 0.0826(19) Uani 1 1 d . . . H2W1 H 0.8856 0.6133 0.0144 0.099 Uiso 1 1 calc R . . H2W2 H 0.8843 0.5891 -0.0429 0.099 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 0.0158(3) 0.0155(3) 0.0203(3) -0.0003(3) 0.0008(3) -0.0001(2) O11 0.0259(15) 0.0206(14) 0.0240(16) 0.0063(12) -0.0027(12) -0.0059(12) O12 0.0187(14) 0.0149(14) 0.0385(18) 0.0005(12) 0.0042(12) -0.0019(11) N11 0.0155(17) 0.0218(17) 0.0199(18) 0.0022(14) 0.0024(14) -0.0001(14) N12 0.032(2) 0.026(2) 0.053(3) -0.0020(17) -0.0141(18) -0.0033(17) N13 0.0202(17) 0.0178(17) 0.0195(19) 0.0016(14) 0.0014(14) 0.0041(15) N14 0.0159(17) 0.0198(17) 0.024(2) 0.0013(14) -0.0016(15) 0.0004(14) N15 0.026(2) 0.054(2) 0.026(2) -0.0034(18) 0.0047(17) 0.0035(18) N16 0.0227(18) 0.0224(18) 0.0176(19) -0.0014(15) -0.0008(14) 0.0024(15) C11 0.018(2) 0.030(2) 0.023(2) -0.0047(19) 0.0018(17) 0.0034(18) C12 0.021(2) 0.022(2) 0.032(3) 0.0042(19) 0.0026(18) 0.0039(19) C13 0.030(2) 0.017(2) 0.028(2) 0.0018(17) 0.0035(19) 0.0056(19) C14 0.021(2) 0.019(2) 0.023(2) -0.0069(17) -0.0003(17) 0.0023(17) C15 0.021(2) 0.019(2) 0.016(2) 0.0018(17) 0.0015(17) -0.0044(18) C16 0.016(2) 0.016(2) 0.016(2) 0.0046(17) 0.0022(16) -0.0041(17) C17 0.025(2) 0.0089(19) 0.031(3) 0.0034(17) -0.0074(19) 0.0026(18) C18 0.024(2) 0.023(2) 0.031(3) -0.0015(19) 0.0068(19) -0.0014(19) C19 0.024(2) 0.018(2) 0.035(3) 0.0055(19) -0.006(2) 0.0003(18) C110 0.036(3) 0.026(2) 0.025(2) 0.0043(19) -0.009(2) -0.006(2) C111 0.033(2) 0.023(2) 0.018(2) 0.0043(18) 0.0018(19) -0.0052(19) C112 0.016(2) 0.021(2) 0.026(2) 0.0002(18) 0.0036(18) -0.0063(17) C113 0.017(2) 0.024(2) 0.017(2) -0.0009(18) 0.0018(17) 0.0024(17) C114 0.020(2) 0.036(3) 0.020(2) 0.0007(19) -0.0084(19) -0.0013(19) Mn2 0.0171(3) 0.0175(3) 0.0173(3) -0.0001(3) -0.0004(3) -0.0003(2) O21 0.0148(13) 0.0174(13) 0.0282(15) -0.0011(11) 0.0019(12) -0.0052(11) O22 0.0151(13) 0.0187(13) 0.0242(15) -0.0047(11) -0.0009(11) -0.0035(11) N21 0.0192(17) 0.0193(17) 0.0187(19) -0.0049(14) -0.0013(14) 0.0011(15) N22 0.033(2) 0.039(2) 0.056(3) 0.0186(18) 0.0229(19) 0.0038(18) N23 0.0217(17) 0.0157(17) 0.0216(19) -0.0014(15) 0.0009(14) -0.0012(15) N24 0.0186(17) 0.0165(17) 0.0214(19) 0.0001(14) -0.0011(14) -0.0006(14) N25 0.0264(19) 0.036(2) 0.022(2) -0.0030(16) -0.0041(16) 0.0032(16) N26 0.0113(16) 0.0199(17) 0.022(2) 0.0030(14) 0.0003(14) -0.0054(14) C21 0.023(2) 0.022(2) 0.026(2) -0.0014(18) -0.0035(18) 0.0008(19) C22 0.032(2) 0.024(2) 0.033(3) -0.003(2) -0.012(2) 0.003(2) C23 0.047(3) 0.022(2) 0.020(2) 0.0030(18) -0.009(2) -0.004(2) C24 0.029(2) 0.018(2) 0.018(2) -0.0066(17) 0.0006(18) -0.0056(18) C25 0.027(2) 0.015(2) 0.018(2) -0.0036(17) -0.0028(18) -0.0004(18) C26 0.019(2) 0.020(2) 0.017(2) 0.0009(17) 0.0026(17) -0.0002(18) C27 0.032(3) 0.017(2) 0.033(3) 0.0053(19) 0.004(2) 0.0048(19) C28 0.024(2) 0.022(2) 0.028(3) -0.0018(18) 0.0024(19) 0.0009(18) C29 0.029(2) 0.023(2) 0.033(3) -0.010(2) -0.001(2) 0.0017(18) C210 0.031(2) 0.030(2) 0.022(2) -0.0081(19) 0.0027(19) -0.001(2) C211 0.025(2) 0.025(2) 0.017(2) -0.0001(18) 0.0001(18) 0.0031(19) C212 0.011(2) 0.021(2) 0.022(2) -0.0033(18) 0.0015(17) -0.0045(17) C213 0.017(2) 0.017(2) 0.017(2) 0.0029(17) -0.0025(17) -0.0020(17) C214 0.015(2) 0.029(2) 0.014(2) -0.0039(19) 0.0024(17) -0.0057(18) Cl1 0.0952(10) 0.0361(7) 0.0555(9) 0.0021(6) -0.0222(7) -0.0058(7) Cl2 0.0451(8) 0.0744(9) 0.1319(14) 0.0393(9) -0.0309(8) -0.0251(7) C1W 0.044(3) 0.035(3) 0.053(3) -0.002(2) -0.008(2) -0.002(2) Cl3 0.0317(6) 0.0483(7) 0.0663(9) 0.0119(6) 0.0018(6) -0.0013(5) Cl4 0.0312(6) 0.0408(7) 0.0594(8) 0.0087(6) -0.0043(5) -0.0056(5) C2W 0.024(3) 0.098(4) 0.126(5) 0.065(4) 0.014(3) 0.007(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 O11 2.109(2) . ? Mn1 O12 2.125(2) . ? Mn1 N14 2.264(3) . ? Mn1 N16 2.293(3) . ? Mn1 N13 2.300(3) . ? Mn1 N11 2.308(3) . ? O11 N16 1.313(3) 12_756 ? O12 N13 1.317(3) 12_756 ? N11 C11 1.343(4) . ? N11 C15 1.364(4) . ? N12 C17 1.139(4) . ? N13 C16 1.307(4) . ? N13 O12 1.317(3) 15_665 ? N14 C18 1.331(4) . ? N14 C112 1.345(4) . ? N15 C114 1.138(4) . ? N16 C113 1.310(4) . ? N16 O11 1.313(3) 15_665 ? C11 C12 1.380(4) . ? C11 H11 0.9300 . ? C12 C13 1.376(4) . ? C12 H12 0.9300 . ? C13 C14 1.379(4) . ? C13 H13 0.9300 . ? C14 C15 1.391(4) . ? C14 H14 0.9300 . ? C15 C16 1.453(4) . ? C16 C17 1.446(4) . ? C18 C19 1.391(4) . ? C18 H18 0.9300 . ? C19 C110 1.379(5) . ? C19 H19 0.9300 . ? C110 C111 1.374(4) . ? C110 H110 0.9300 . ? C111 C112 1.389(4) . ? C111 H111 0.9300 . ? C112 C113 1.475(4) . ? C113 C114 1.446(5) . ? Mn2 O22 2.096(2) . ? Mn2 O21 2.130(2) . ? Mn2 N26 2.255(3) . ? Mn2 N24 2.265(3) . ? Mn2 N21 2.288(3) . ? Mn2 N23 2.304(3) . ? O21 N23 1.308(3) 12_766 ? O22 N26 1.314(3) 12_766 ? N21 C21 1.338(4) . ? N21 C25 1.353(4) . ? N22 C27 1.137(4) . ? N23 C26 1.300(4) . ? N23 O21 1.308(3) 15_565 ? N24 C28 1.338(4) . ? N24 C212 1.357(4) . ? N25 C214 1.145(4) . ? N26 C213 1.306(4) . ? N26 O22 1.314(3) 15_565 ? C21 C22 1.377(4) . ? C21 H21 0.9300 . ? C22 C23 1.379(5) . ? C22 H22 0.9300 . ? C23 C24 1.378(4) . ? C23 H23 0.9300 . ? C24 C25 1.390(4) . ? C24 H24 0.9300 . ? C25 C26 1.456(4) . ? C26 C27 1.450(5) . ? C28 C29 1.392(4) . ? C28 H28 0.9300 . ? C29 C210 1.381(4) . ? C29 H29 0.9300 . ? C210 C211 1.379(4) . ? C210 H210 0.9300 . ? C211 C212 1.382(4) . ? C211 H211 0.9300 . ? C212 C213 1.470(4) . ? C213 C214 1.443(5) . ? Cl1 C1W 1.773(4) . ? Cl2 C1W 1.742(4) . ? C1W H1W1 0.9700 . ? C1W H1W2 0.9700 . ? Cl3 C2W 1.691(4) . ? Cl4 C2W 1.735(4) . ? C2W H2W1 0.9700 . ? C2W H2W2 0.9700 . ? 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 O11 Mn1 O12 88.58(8) . . ? O11 Mn1 N14 162.07(9) . . ? O12 Mn1 N14 86.30(9) . . ? O11 Mn1 N16 97.88(9) . . ? O12 Mn1 N16 129.60(9) . . ? N14 Mn1 N16 72.61(10) . . ? O11 Mn1 N13 82.29(9) . . ? O12 Mn1 N13 150.92(9) . . ? N14 Mn1 N13 109.93(9) . . ? N16 Mn1 N13 79.17(9) . . ? O11 Mn1 N11 105.23(9) . . ? O12 Mn1 N11 84.71(9) . . ? N14 Mn1 N11 91.40(10) . . ? N16 Mn1 N11 139.19(9) . . ? N13 Mn1 N11 71.34(9) . . ? N16 O11 Mn1 119.88(18) 12_756 . ? N13 O12 Mn1 122.61(18) 12_756 . ? C11 N11 C15 117.0(3) . . ? C11 N11 Mn1 126.4(2) . . ? C15 N11 Mn1 116.5(2) . . ? C16 N13 O12 116.8(3) . 15_665 ? C16 N13 Mn1 116.6(2) . . ? O12 N13 Mn1 126.43(19) 15_665 . ? C18 N14 C112 117.0(3) . . ? C18 N14 Mn1 125.8(2) . . ? C112 N14 Mn1 117.2(2) . . ? C113 N16 O11 116.0(3) . 15_665 ? C113 N16 Mn1 115.3(2) . . ? O11 N16 Mn1 128.6(2) 15_665 . ? N11 C11 C12 124.2(3) . . ? N11 C11 H11 117.9 . . ? C12 C11 H11 117.9 . . ? C13 C12 C11 118.4(3) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C12 C13 C14 119.1(3) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 119.8(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N11 C15 C14 121.6(3) . . ? N11 C15 C16 115.4(3) . . ? C14 C15 C16 123.0(3) . . ? N13 C16 C17 118.4(3) . . ? N13 C16 C15 119.7(3) . . ? C17 C16 C15 121.9(3) . . ? N12 C17 C16 177.6(4) . . ? N14 C18 C19 123.8(3) . . ? N14 C18 H18 118.1 . . ? C19 C18 H18 118.1 . . ? C110 C19 C18 118.0(3) . . ? C110 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? C111 C110 C19 119.5(4) . . ? C111 C110 H110 120.3 . . ? C19 C110 H110 120.3 . . ? C110 C111 C112 118.5(3) . . ? C110 C111 H111 120.7 . . ? C112 C111 H111 120.7 . . ? N14 C112 C111 123.1(3) . . ? N14 C112 C113 115.4(3) . . ? C111 C112 C113 121.5(3) . . ? N16 C113 C114 121.0(3) . . ? N16 C113 C112 119.4(3) . . ? C114 C113 C112 119.5(3) . . ? N15 C114 C113 177.4(4) . . ? O22 Mn2 O21 92.22(8) . . ? O22 Mn2 N26 97.59(9) . . ? O21 Mn2 N26 123.14(9) . . ? O22 Mn2 N24 164.06(9) . . ? O21 Mn2 N24 83.04(9) . . ? N26 Mn2 N24 72.80(10) . . ? O22 Mn2 N21 95.48(9) . . ? O21 Mn2 N21 84.50(9) . . ? N26 Mn2 N21 148.66(9) . . ? N24 Mn2 N21 99.17(9) . . ? O22 Mn2 N23 79.01(9) . . ? O21 Mn2 N23 153.38(9) . . ? N26 Mn2 N23 83.16(10) . . ? N24 Mn2 N23 111.57(9) . . ? N21 Mn2 N23 71.56(10) . . ? N23 O21 Mn2 122.88(17) 12_766 . ? N26 O22 Mn2 120.77(18) 12_766 . ? C21 N21 C25 118.6(3) . . ? C21 N21 Mn2 124.2(2) . . ? C25 N21 Mn2 116.5(2) . . ? C26 N23 O21 117.7(3) . 15_565 ? C26 N23 Mn2 116.4(2) . . ? O21 N23 Mn2 125.58(19) 15_565 . ? C28 N24 C212 117.4(3) . . ? C28 N24 Mn2 125.5(2) . . ? C212 N24 Mn2 116.3(2) . . ? C213 N26 O22 115.8(3) . 15_565 ? C213 N26 Mn2 116.3(2) . . ? O22 N26 Mn2 127.9(2) 15_565 . ? N21 C21 C22 122.7(3) . . ? N21 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C21 C22 C23 118.9(3) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 119.2(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 119.3(3) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? N21 C25 C24 121.3(3) . . ? N21 C25 C26 116.1(3) . . ? C24 C25 C26 122.5(3) . . ? N23 C26 C27 119.8(3) . . ? N23 C26 C25 119.0(3) . . ? C27 C26 C25 120.9(3) . . ? N22 C27 C26 178.8(4) . . ? N24 C28 C29 123.3(3) . . ? N24 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C210 C29 C28 118.1(3) . . ? C210 C29 H29 121.0 . . ? C28 C29 H29 121.0 . . ? C211 C210 C29 119.8(3) . . ? C211 C210 H210 120.1 . . ? C29 C210 H210 120.1 . . ? C210 C211 C212 118.6(3) . . ? C210 C211 H211 120.7 . . ? C212 C211 H211 120.7 . . ? N24 C212 C211 122.8(3) . . ? N24 C212 C213 114.7(3) . . ? C211 C212 C213 122.5(3) . . ? N26 C213 C214 120.4(3) . . ? N26 C213 C212 119.3(3) . . ? C214 C213 C212 120.3(3) . . ? N25 C214 C213 178.3(4) . . ? Cl2 C1W Cl1 111.6(2) . . ? Cl2 C1W H1W1 109.3 . . ? Cl1 C1W H1W1 109.3 . . ? Cl2 C1W H1W2 109.3 . . ? Cl1 C1W H1W2 109.3 . . ? H1W1 C1W H1W2 108.0 . . ? Cl3 C2W Cl4 117.4(2) . . ? Cl3 C2W H2W1 108.0 . . ? Cl4 C2W H2W1 108.0 . . ? Cl3 C2W H2W2 108.0 . . ? Cl4 C2W H2W2 108.0 . . ? H2W1 C2W H2W2 107.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.348 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 916864' ####################################################################### # # 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_af13fua1na _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H40 Cl4 Mn8 N24 O16, 3(C H2 Cl2),2(H2 O)' _chemical_formula_sum 'C60 H52 Cl12 Mn8 N24 O16' _chemical_formula_weight 2230.18 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 25.055(2) _cell_length_b 15.5062(13) _cell_length_c 21.1912(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.701(5) _cell_angle_gamma 90.00 _cell_volume 8192.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1965 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 21.09 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 1.661 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.19 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8434 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.48 _reflns_number_total 8434 _reflns_number_gt 5320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. The displacement parameters of some lengths in the direction of the bond are restrained to be equal within an effective standard deviation (DELU sentences) The distance of dichloride methane are restrained (DFIX and EADP sentences) ; _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^)+(0.0639P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8434 _refine_ls_number_parameters 556 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1301 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.010 _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 0.45168(3) 0.28296(4) 0.20977(3) 0.01552(17) Uani 1 1 d . . . Mn2 Mn 0.46688(3) 0.12559(4) 0.30006(3) 0.01596(17) Uani 1 1 d D . . Mn3 Mn 0.39248(3) 0.08311(5) 0.15111(3) 0.01892(18) Uani 1 1 d . . . Mn4 Mn 0.42531(3) 0.32682(5) 0.36564(3) 0.01838(18) Uani 1 1 d . . . Cl1 Cl 0.40053(5) -0.06965(8) 0.17066(6) 0.0322(3) Uani 1 1 d . . . Cl2 Cl 0.43614(5) 0.47842(7) 0.33347(5) 0.0230(3) Uani 1 1 d D . . O1 O 0.39023(12) 0.1231(2) 0.30487(13) 0.0197(7) Uani 1 1 d . . . O2 O 0.37516(12) 0.29098(19) 0.22174(13) 0.0190(7) Uani 1 1 d . . . O3 O 0.47478(11) 0.13178(19) 0.39320(13) 0.0178(7) Uani 1 1 d . . . O4 O 0.45894(11) 0.13354(18) 0.21096(13) 0.0158(7) Uani 1 1 d . . . O5 O 0.43104(12) 0.28207(19) 0.11882(13) 0.0195(7) Uani 1 1 d . . . O6 O 0.44774(12) 0.4268(2) 0.19387(14) 0.0200(7) Uani 1 1 d D . . H6O H 0.4403(17) 0.447(3) 0.2303(12) 0.024 Uiso 1 1 d D . . H6AO H 0.4820(10) 0.435(3) 0.188(2) 0.024 Uiso 1 1 d D . . O7 O 0.47308(11) 0.27624(19) 0.29655(13) 0.0170(7) Uani 1 1 d . . . O8 O 0.47460(14) -0.0159(2) 0.31730(15) 0.0292(8) Uani 1 1 d D . . H8OA H 0.5094(7) -0.0204(9) 0.3099(17) 0.035 Uiso 1 1 d D . . H8OB H 0.4701(15) -0.022(3) 0.3586(7) 0.035 Uiso 1 1 d D . . N1 N 0.29979(15) 0.0882(2) 0.13945(17) 0.0206(9) Uani 1 1 d . . . N2 N 0.26910(17) 0.1390(3) 0.3579(2) 0.0299(10) Uani 1 1 d . . . N3 N 0.33830(15) 0.3300(3) 0.39967(18) 0.0232(9) Uani 1 1 d . . . N4 N 0.23608(19) 0.3211(3) 0.1982(2) 0.0432(12) Uani 1 1 d . . . N5 N 0.44966(15) 0.3628(2) 0.46801(17) 0.0202(9) Uani 1 1 d . . . N6 N 0.50699(16) 0.0896(3) 0.55267(19) 0.0280(10) Uani 1 1 d . . . N7 N 0.38766(14) 0.0554(3) 0.04168(17) 0.0213(9) Uani 1 1 d . . . N8 N 0.41018(16) 0.3451(3) -0.0315(2) 0.0298(10) Uani 1 1 d . . . N9 N 0.41009(14) 0.2079(2) 0.09515(17) 0.0186(9) Uani 1 1 d . . . N10 N 0.36043(15) 0.1075(2) 0.24977(17) 0.0190(9) Uani 1 1 d . . . N11 N 0.46006(14) 0.2057(2) 0.41809(16) 0.0162(8) Uani 1 1 d . . . N12 N 0.36260(15) 0.3081(2) 0.28089(17) 0.0206(9) Uani 1 1 d . . . C1 C 0.26800(18) 0.0756(3) 0.0857(2) 0.0246(11) Uani 1 1 d . . . H1 H 0.2842 0.0727 0.0481 0.029 Uiso 1 1 calc R . . C2 C 0.21351(19) 0.0667(3) 0.0818(2) 0.0258(11) Uani 1 1 d . . . H2 H 0.1937 0.0581 0.0428 0.031 Uiso 1 1 calc R . . C3 C 0.18859(19) 0.0707(3) 0.1364(2) 0.0276(12) Uani 1 1 d . . . H3 H 0.1515 0.0657 0.1351 0.033 Uiso 1 1 calc R . . C4 C 0.21982(19) 0.0824(3) 0.1937(2) 0.0270(12) Uani 1 1 d . . . H4 H 0.2042 0.0842 0.2317 0.032 Uiso 1 1 calc R . . C5 C 0.27426(18) 0.0913(3) 0.1931(2) 0.0200(10) Uani 1 1 d . . . C6 C 0.30916(18) 0.1079(3) 0.2523(2) 0.0188(10) Uani 1 1 d . . . C7 C 0.28638(18) 0.1240(3) 0.3110(2) 0.0201(10) Uani 1 1 d . . . C8 C 0.32437(19) 0.3360(3) 0.4598(2) 0.0247(11) Uani 1 1 d . . . H8 H 0.3515 0.3324 0.4930 0.030 Uiso 1 1 calc R . . C9 C 0.2728(2) 0.3469(3) 0.4746(2) 0.0274(12) Uani 1 1 d . . . H9 H 0.2652 0.3500 0.5167 0.033 Uiso 1 1 calc R . . C10 C 0.2321(2) 0.3531(3) 0.4256(2) 0.0306(12) Uani 1 1 d . . . H10 H 0.1967 0.3611 0.4342 0.037 Uiso 1 1 calc R . . C11 C 0.2448(2) 0.3474(3) 0.3639(2) 0.0271(12) Uani 1 1 d . . . H11 H 0.2183 0.3517 0.3301 0.033 Uiso 1 1 calc R . . C12 C 0.29790(18) 0.3352(3) 0.3531(2) 0.0198(10) Uani 1 1 d . . . C13 C 0.31230(18) 0.3225(3) 0.2881(2) 0.0188(10) Uani 1 1 d . . . C14 C 0.2710(2) 0.3208(3) 0.2361(2) 0.0255(12) Uani 1 1 d . . . C15 C 0.44290(18) 0.4406(3) 0.4921(2) 0.0227(11) Uani 1 1 d . . . H15 H 0.4371 0.4870 0.4644 0.027 Uiso 1 1 calc R . . C16 C 0.44418(19) 0.4555(3) 0.5564(2) 0.0286(12) Uani 1 1 d . . . H16 H 0.4392 0.5110 0.5715 0.034 Uiso 1 1 calc R . . C17 C 0.4529(2) 0.3875(3) 0.5983(2) 0.0288(12) Uani 1 1 d . . . H17 H 0.4541 0.3965 0.6418 0.035 Uiso 1 1 calc R . . C18 C 0.45967(18) 0.3065(3) 0.5744(2) 0.0236(11) Uani 1 1 d . . . H18 H 0.4647 0.2593 0.6014 0.028 Uiso 1 1 calc R . . C19 C 0.45900(17) 0.2960(3) 0.5094(2) 0.0182(10) Uani 1 1 d . . . C20 C 0.46844(17) 0.2121(3) 0.4799(2) 0.0182(10) Uani 1 1 d . . . C21 C 0.37800(18) -0.0214(3) 0.0149(2) 0.0253(11) Uani 1 1 d . . . H21 H 0.3818 -0.0702 0.0406 0.030 Uiso 1 1 calc R . . C22 C 0.3627(2) -0.0322(4) -0.0486(2) 0.0330(13) Uani 1 1 d . . . H22 H 0.3585 -0.0873 -0.0657 0.040 Uiso 1 1 calc R . . C23 C 0.3538(2) 0.0391(3) -0.0868(2) 0.0314(13) Uani 1 1 d . . . H23 H 0.3413 0.0335 -0.1295 0.038 Uiso 1 1 calc R . . C24 C 0.36376(19) 0.1190(3) -0.0600(2) 0.0287(12) Uani 1 1 d . . . H24 H 0.3584 0.1685 -0.0845 0.034 Uiso 1 1 calc R . . C25 C 0.38182(18) 0.1255(3) 0.0036(2) 0.0211(11) Uani 1 1 d . . . C26 C 0.39850(18) 0.2068(3) 0.0345(2) 0.0189(10) Uani 1 1 d . . . C27 C 0.40506(18) 0.2836(3) -0.0034(2) 0.0211(11) Uani 1 1 d . . . C28 C 0.48960(18) 0.1426(3) 0.5192(2) 0.0197(10) Uani 1 1 d . . . Cl3 Cl 0.71830(6) 0.31014(10) 0.44230(7) 0.0416(4) Uani 1 1 d . . . Cl4 Cl 0.70695(6) 0.48732(10) 0.39749(7) 0.0491(4) Uani 1 1 d . . . C1W C 0.6742(2) 0.3889(4) 0.4054(3) 0.0483(13) Uani 1 1 d . . . H1W1 H 0.6601 0.3684 0.3638 0.058 Uiso 1 1 calc R . . H1W2 H 0.6443 0.3972 0.4305 0.058 Uiso 1 1 calc R . . C2W C 0.3892(5) 0.2304(6) 0.7658(4) 0.0483(13) Uani 0.50 1 d PD A 1 H2W1 H 0.3595 0.1969 0.7789 0.058 Uiso 0.50 1 calc PR A 1 H2W2 H 0.4151 0.1901 0.7516 0.058 Uiso 0.50 1 calc PR A 1 Cl5 Cl 0.41879(13) 0.2835(2) 0.83085(14) 0.0510(7) Uani 0.50 1 d PD A 1 Cl6 Cl 0.3655(3) 0.2936(5) 0.7023(3) 0.0510(7) Uani 0.50 1 d PD A 1 Cl5' Cl 0.47220(14) 0.2728(3) 0.76225(17) 0.0705(10) Uani 0.50 1 d PD . 2 Cl6' Cl 0.3647(4) 0.3060(6) 0.7076(4) 0.0705(10) Uani 0.50 1 d PD B 2 C2W' C 0.4058(3) 0.2572(9) 0.7691(5) 0.0483(13) Uani 0.50 1 d PD B 2 H2W3 H 0.3971 0.2805 0.8093 0.058 Uiso 0.50 1 calc PR B 2 H2W4 H 0.3984 0.1958 0.7691 0.058 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0147(4) 0.0154(4) 0.0165(3) 0.0005(3) 0.0018(3) 0.0000(3) Mn2 0.0141(4) 0.0153(4) 0.0185(3) 0.0010(3) 0.0019(3) -0.0002(3) Mn3 0.0160(4) 0.0182(4) 0.0226(4) -0.0010(3) 0.0020(3) -0.0013(3) Mn4 0.0175(4) 0.0187(4) 0.0192(4) 0.0002(3) 0.0031(3) 0.0019(3) Cl1 0.0302(7) 0.0247(7) 0.0409(7) 0.0001(6) 0.0001(6) -0.0015(6) Cl2 0.0230(6) 0.0207(7) 0.0259(6) 0.0001(5) 0.0048(5) 0.0024(5) O1 0.0194(18) 0.0211(18) 0.0188(16) 0.0020(14) 0.0018(13) -0.0012(14) O2 0.0184(18) 0.0192(18) 0.0195(16) 0.0016(13) 0.0031(13) -0.0014(14) O3 0.0164(17) 0.0141(18) 0.0231(16) 0.0006(13) 0.0025(13) 0.0003(14) O4 0.0142(17) 0.0148(17) 0.0185(15) -0.0006(13) 0.0017(12) -0.0002(13) O5 0.0219(18) 0.0155(18) 0.0208(16) -0.0009(14) 0.0007(13) -0.0009(14) O6 0.0196(18) 0.0195(19) 0.0212(17) 0.0000(14) 0.0030(14) 0.0013(15) O7 0.0175(17) 0.0179(17) 0.0160(15) -0.0007(13) 0.0030(12) -0.0005(14) O8 0.034(2) 0.029(2) 0.0263(18) 0.0014(16) 0.0077(15) -0.0030(16) N1 0.019(2) 0.017(2) 0.026(2) -0.0002(17) 0.0032(17) -0.0005(17) N2 0.029(3) 0.029(3) 0.032(2) 0.001(2) 0.004(2) 0.000(2) N3 0.022(2) 0.020(2) 0.028(2) 0.0010(18) 0.0045(18) 0.0023(18) N4 0.032(3) 0.059(4) 0.039(3) 0.002(2) 0.005(2) 0.001(2) N5 0.017(2) 0.019(2) 0.024(2) -0.0018(17) 0.0031(16) 0.0008(17) N6 0.027(2) 0.029(3) 0.029(2) 0.002(2) 0.0046(18) -0.004(2) N7 0.014(2) 0.023(2) 0.028(2) -0.0016(18) 0.0043(16) -0.0007(17) N8 0.027(3) 0.027(3) 0.036(3) 0.004(2) 0.0013(19) -0.001(2) N9 0.017(2) 0.017(2) 0.021(2) -0.0024(17) 0.0031(16) 0.0014(17) N10 0.017(2) 0.018(2) 0.021(2) 0.0017(16) -0.0002(16) -0.0017(17) N11 0.015(2) 0.014(2) 0.0204(19) -0.0006(16) 0.0043(15) -0.0009(16) N12 0.025(2) 0.015(2) 0.021(2) 0.0011(16) 0.0009(17) -0.0020(17) C1 0.020(3) 0.025(3) 0.029(3) 0.001(2) 0.003(2) 0.001(2) C2 0.023(3) 0.026(3) 0.028(3) 0.001(2) 0.002(2) 0.002(2) C3 0.019(3) 0.030(3) 0.034(3) -0.001(2) 0.001(2) -0.002(2) C4 0.025(3) 0.027(3) 0.030(3) 0.001(2) 0.007(2) 0.001(2) C5 0.020(3) 0.016(3) 0.024(2) 0.002(2) 0.002(2) 0.000(2) C6 0.018(3) 0.016(3) 0.023(2) 0.0010(19) 0.0045(19) -0.002(2) C7 0.016(3) 0.021(3) 0.024(3) 0.002(2) 0.002(2) 0.001(2) C8 0.025(3) 0.022(3) 0.028(3) 0.000(2) 0.004(2) 0.001(2) C9 0.026(3) 0.027(3) 0.029(3) -0.002(2) 0.007(2) -0.002(2) C10 0.025(3) 0.031(3) 0.038(3) -0.001(2) 0.011(2) 0.001(2) C11 0.025(3) 0.024(3) 0.032(3) 0.001(2) 0.000(2) 0.000(2) C12 0.017(3) 0.017(3) 0.026(3) 0.000(2) 0.004(2) -0.004(2) C13 0.014(3) 0.017(3) 0.026(2) 0.000(2) 0.0030(19) 0.001(2) C14 0.021(3) 0.031(3) 0.026(3) 0.001(2) 0.007(2) 0.003(2) C15 0.022(3) 0.020(3) 0.026(3) 0.000(2) 0.003(2) 0.001(2) C16 0.028(3) 0.029(3) 0.029(3) -0.005(2) 0.004(2) 0.001(2) C17 0.029(3) 0.029(3) 0.029(3) -0.001(2) 0.005(2) 0.001(2) C18 0.022(3) 0.023(3) 0.025(3) 0.002(2) 0.002(2) -0.001(2) C19 0.015(2) 0.017(3) 0.023(2) 0.002(2) 0.0022(19) 0.001(2) C20 0.012(2) 0.021(3) 0.022(2) 0.003(2) 0.0031(18) 0.000(2) C21 0.022(3) 0.020(3) 0.034(3) -0.005(2) 0.004(2) -0.002(2) C22 0.028(3) 0.028(3) 0.043(3) -0.009(3) 0.000(2) 0.000(2) C23 0.030(3) 0.032(3) 0.032(3) -0.011(2) 0.003(2) -0.001(2) C24 0.025(3) 0.031(3) 0.029(3) 0.001(2) 0.001(2) -0.001(2) C25 0.016(3) 0.024(3) 0.023(2) 0.000(2) 0.0019(19) 0.001(2) C26 0.016(3) 0.020(3) 0.020(2) -0.001(2) -0.0004(18) 0.000(2) C27 0.015(3) 0.024(3) 0.023(2) -0.003(2) -0.0005(19) 0.000(2) C28 0.016(3) 0.021(3) 0.023(2) 0.002(2) 0.006(2) 0.001(2) Cl3 0.0395(9) 0.0432(9) 0.0425(8) -0.0021(7) 0.0061(6) -0.0026(7) Cl4 0.0487(10) 0.0436(10) 0.0557(9) -0.0011(7) 0.0081(7) -0.0102(7) C1W 0.045(3) 0.051(4) 0.049(3) -0.002(3) 0.003(2) -0.014(3) C2W 0.045(3) 0.051(4) 0.049(3) -0.002(3) 0.003(2) -0.014(3) Cl5 0.0584(16) 0.0460(17) 0.0488(14) -0.0070(12) 0.0066(12) -0.0026(13) Cl6 0.0584(16) 0.0460(17) 0.0488(14) -0.0070(12) 0.0066(12) -0.0026(13) Cl5' 0.0585(18) 0.081(3) 0.072(2) -0.0037(17) 0.0029(15) 0.0071(17) Cl6' 0.0585(18) 0.081(3) 0.072(2) -0.0037(17) 0.0029(15) 0.0071(17) C2W' 0.045(3) 0.051(4) 0.049(3) -0.002(3) 0.003(2) -0.014(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 O7 1.867(3) . ? Mn1 O7 1.906(3) 2_655 ? Mn1 O5 1.945(3) . ? Mn1 O2 1.963(3) . ? Mn1 O6 2.256(3) . ? Mn1 O4 2.324(3) . ? Mn1 Mn1 2.8195(13) 2_655 ? Mn1 Mn2 3.1008(10) . ? Mn1 Mn2 3.2008(10) 2_655 ? Mn2 O4 1.883(3) . ? Mn2 O4 1.900(3) 2_655 ? Mn2 O1 1.934(3) . ? Mn2 O3 1.966(3) . ? Mn2 O8 2.230(3) . ? Mn2 O7 2.343(3) . ? Mn2 Mn2 2.8204(13) 2_655 ? Mn2 Mn1 3.2008(10) 2_655 ? Mn3 O4 2.139(3) . ? Mn3 N1 2.312(4) . ? Mn3 N9 2.334(4) . ? Mn3 N10 2.344(4) . ? Mn3 N7 2.350(4) . ? Mn3 Cl1 2.4097(15) . ? Mn4 O7 2.130(3) . ? Mn4 N5 2.264(4) . ? Mn4 N12 2.284(4) . ? Mn4 N11 2.308(4) . ? Mn4 N3 2.364(4) . ? Mn4 Cl2 2.4699(14) . ? O1 N10 1.344(4) . ? O2 N12 1.349(4) . ? O3 N11 1.329(4) . ? O4 Mn2 1.900(3) 2_655 ? O5 N9 1.341(4) . ? O6 H6O 0.87(2) . ? O6 H6AO 0.89(2) . ? O7 Mn1 1.906(3) 2_655 ? O8 H8OA 0.905(10) . ? O8 H8OB 0.897(10) . ? N1 C1 1.338(5) . ? N1 C5 1.359(6) . ? N2 C7 1.146(6) . ? N3 C12 1.344(5) . ? N3 C8 1.358(6) . ? N4 C14 1.127(6) . ? N5 C15 1.327(6) . ? N5 C19 1.363(6) . ? N6 C28 1.143(6) . ? N7 C21 1.331(6) . ? N7 C25 1.353(6) . ? N8 C27 1.139(6) . ? N9 C26 1.288(5) . ? N10 C6 1.291(6) . ? N11 C20 1.308(5) . ? N12 C13 1.304(6) . ? C1 C2 1.366(6) . ? C1 H1 0.9300 . ? C2 C3 1.369(7) . ? C2 H2 0.9300 . ? C3 C4 1.390(6) . ? C3 H3 0.9300 . ? C4 C5 1.372(6) . ? C4 H4 0.9300 . ? C5 C6 1.479(6) . ? C6 C7 1.442(6) . ? C8 C9 1.371(7) . ? C8 H8 0.9300 . ? C9 C10 1.384(7) . ? C9 H9 0.9300 . ? C10 C11 1.381(7) . ? C10 H10 0.9300 . ? C11 C12 1.384(6) . ? C11 H11 0.9300 . ? C12 C13 1.471(6) . ? C13 C14 1.436(6) . ? C15 C16 1.380(6) . ? C15 H15 0.9300 . ? C16 C17 1.381(7) . ? C16 H16 0.9300 . ? C17 C18 1.371(7) . ? C17 H17 0.9300 . ? C18 C19 1.384(6) . ? C18 H18 0.9300 . ? C19 C20 1.474(6) . ? C20 C28 1.432(6) . ? C21 C22 1.374(7) . ? C21 H21 0.9300 . ? C22 C23 1.376(7) . ? C22 H22 0.9300 . ? C23 C24 1.376(7) . ? C23 H23 0.9300 . ? C24 C25 1.382(6) . ? C24 H24 0.9300 . ? C25 C26 1.462(6) . ? C26 C27 1.455(7) . ? Cl3 C1W 1.775(6) . ? Cl4 C1W 1.749(6) . ? C1W H1W1 0.9700 . ? C1W H1W2 0.9700 . ? C2W Cl5 1.709(6) . ? C2W Cl6 1.723(6) . ? C2W H2W1 0.9700 . ? C2W H2W2 0.9700 . ? Cl5' Cl5' 1.534(7) 2_656 ? Cl5' C2W' 1.702(8) . ? Cl6' C2W' 1.751(8) . ? C2W' H2W3 0.9700 . ? C2W' H2W4 0.9700 . ? 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 O7 Mn1 O7 82.93(13) . 2_655 ? O7 Mn1 O5 176.17(13) . . ? O7 Mn1 O5 95.59(12) 2_655 . ? O7 Mn1 O2 93.73(12) . . ? O7 Mn1 O2 176.59(12) 2_655 . ? O5 Mn1 O2 87.79(12) . . ? O7 Mn1 O6 101.91(12) . . ? O7 Mn1 O6 94.15(12) 2_655 . ? O5 Mn1 O6 81.70(12) . . ? O2 Mn1 O6 85.86(12) . . ? O7 Mn1 O4 85.37(12) . . ? O7 Mn1 O4 82.50(12) 2_655 . ? O5 Mn1 O4 90.95(11) . . ? O2 Mn1 O4 97.95(12) . . ? O6 Mn1 O4 171.61(11) . . ? O7 Mn1 Mn1 42.17(9) . 2_655 ? O7 Mn1 Mn1 41.11(8) 2_655 2_655 ? O5 Mn1 Mn1 136.63(10) . 2_655 ? O2 Mn1 Mn1 135.49(9) . 2_655 ? O6 Mn1 Mn1 96.46(8) . 2_655 ? O4 Mn1 Mn1 86.09(7) . 2_655 ? O7 Mn1 Mn2 48.89(9) . . ? O7 Mn1 Mn2 86.48(9) 2_655 . ? O5 Mn1 Mn2 127.59(9) . . ? O2 Mn1 Mn2 91.83(9) . . ? O6 Mn1 Mn2 150.56(8) . . ? O4 Mn1 Mn2 37.26(7) . . ? Mn1 Mn1 Mn2 65.25(2) 2_655 . ? O7 Mn1 Mn2 84.20(9) . 2_655 ? O7 Mn1 Mn2 46.56(9) 2_655 2_655 ? O5 Mn1 Mn2 92.21(9) . 2_655 ? O2 Mn1 Mn2 133.94(9) . 2_655 ? O6 Mn1 Mn2 139.69(8) . 2_655 ? O4 Mn1 Mn2 36.00(7) . 2_655 ? Mn1 Mn1 Mn2 61.617(19) 2_655 2_655 ? Mn2 Mn1 Mn2 53.15(3) . 2_655 ? O4 Mn2 O4 83.09(12) . 2_655 ? O4 Mn2 O1 92.73(12) . . ? O4 Mn2 O1 175.23(12) 2_655 . ? O4 Mn2 O3 173.44(13) . . ? O4 Mn2 O3 96.78(12) 2_655 . ? O1 Mn2 O3 87.11(12) . . ? O4 Mn2 O8 103.15(12) . . ? O4 Mn2 O8 90.80(12) 2_655 . ? O1 Mn2 O8 92.39(13) . . ? O3 Mn2 O8 83.40(12) . . ? O4 Mn2 O7 84.47(11) . . ? O4 Mn2 O7 82.11(11) 2_655 . ? O1 Mn2 O7 95.24(12) . . ? O3 Mn2 O7 89.01(11) . . ? O8 Mn2 O7 168.96(11) . . ? O4 Mn2 Mn2 42.03(9) . 2_655 ? O4 Mn2 Mn2 41.56(8) 2_655 2_655 ? O1 Mn2 Mn2 134.53(9) . 2_655 ? O3 Mn2 Mn2 138.33(9) . 2_655 ? O8 Mn2 Mn2 94.32(9) . 2_655 ? O7 Mn2 Mn2 86.00(7) . 2_655 ? O4 Mn2 Mn1 48.36(9) . . ? O4 Mn2 Mn1 86.26(9) 2_655 . ? O1 Mn2 Mn1 89.24(9) . . ? O3 Mn2 Mn1 125.09(9) . . ? O8 Mn2 Mn1 151.50(9) . . ? O7 Mn2 Mn1 36.89(7) . . ? Mn2 Mn2 Mn1 65.24(2) 2_655 . ? O4 Mn2 Mn1 83.65(9) . 2_655 ? O4 Mn2 Mn1 45.97(9) 2_655 2_655 ? O1 Mn2 Mn1 131.44(9) . 2_655 ? O3 Mn2 Mn1 91.54(9) . 2_655 ? O8 Mn2 Mn1 135.68(9) . 2_655 ? O7 Mn2 Mn1 36.21(7) . 2_655 ? Mn2 Mn2 Mn1 61.61(2) 2_655 2_655 ? Mn1 Mn2 Mn1 53.13(3) . 2_655 ? O4 Mn3 N1 139.95(12) . . ? O4 Mn3 N9 79.79(12) . . ? N1 Mn3 N9 98.97(13) . . ? O4 Mn3 N10 74.19(12) . . ? N1 Mn3 N10 70.14(13) . . ? N9 Mn3 N10 114.72(13) . . ? O4 Mn3 N7 127.79(12) . . ? N1 Mn3 N7 87.03(13) . . ? N9 Mn3 N7 69.15(13) . . ? N10 Mn3 N7 157.13(13) . . ? O4 Mn3 Cl1 102.15(9) . . ? N1 Mn3 Cl1 96.77(10) . . ? N9 Mn3 Cl1 152.30(10) . . ? N10 Mn3 Cl1 92.03(10) . . ? N7 Mn3 Cl1 89.15(10) . . ? O7 Mn4 N5 129.26(12) . . ? O7 Mn4 N12 78.61(12) . . ? N5 Mn4 N12 152.05(14) . . ? O7 Mn4 N11 79.67(12) . . ? N5 Mn4 N11 71.73(13) . . ? N12 Mn4 N11 118.17(13) . . ? O7 Mn4 N3 144.63(12) . . ? N5 Mn4 N3 82.61(13) . . ? N12 Mn4 N3 70.08(14) . . ? N11 Mn4 N3 100.67(13) . . ? O7 Mn4 Cl2 94.37(9) . . ? N5 Mn4 Cl2 90.18(10) . . ? N12 Mn4 Cl2 89.43(10) . . ? N11 Mn4 Cl2 149.40(10) . . ? N3 Mn4 Cl2 101.20(10) . . ? N10 O1 Mn2 115.3(2) . . ? N12 O2 Mn1 117.0(2) . . ? N11 O3 Mn2 115.9(2) . . ? Mn2 O4 Mn2 96.42(12) . 2_655 ? Mn2 O4 Mn3 124.70(15) . . ? Mn2 O4 Mn3 128.09(15) 2_655 . ? Mn2 O4 Mn1 94.38(12) . . ? Mn2 O4 Mn1 98.03(12) 2_655 . ? Mn3 O4 Mn1 107.62(12) . . ? N9 O5 Mn1 115.6(2) . . ? Mn1 O6 H6O 103(3) . . ? Mn1 O6 H6AO 98(3) . . ? H6O O6 H6AO 112(4) . . ? Mn1 O7 Mn1 96.72(13) . 2_655 ? Mn1 O7 Mn4 122.04(15) . . ? Mn1 O7 Mn4 130.94(14) 2_655 . ? Mn1 O7 Mn2 94.21(12) . . ? Mn1 O7 Mn2 97.23(12) 2_655 . ? Mn4 O7 Mn2 107.56(12) . . ? Mn2 O8 H8OA 96.7(8) . . ? Mn2 O8 H8OB 104(3) . . ? H8OA O8 H8OB 112.2(16) . . ? C1 N1 C5 115.3(4) . . ? C1 N1 Mn3 126.3(3) . . ? C5 N1 Mn3 117.6(3) . . ? C12 N3 C8 116.1(4) . . ? C12 N3 Mn4 115.3(3) . . ? C8 N3 Mn4 128.2(3) . . ? C15 N5 C19 117.6(4) . . ? C15 N5 Mn4 124.0(3) . . ? C19 N5 Mn4 116.3(3) . . ? C21 N7 C25 117.5(4) . . ? C21 N7 Mn3 125.0(3) . . ? C25 N7 Mn3 115.7(3) . . ? C26 N9 O5 115.2(4) . . ? C26 N9 Mn3 117.4(3) . . ? O5 N9 Mn3 127.4(2) . . ? C6 N10 O1 115.6(4) . . ? C6 N10 Mn3 117.9(3) . . ? O1 N10 Mn3 126.4(3) . . ? C20 N11 O3 116.0(3) . . ? C20 N11 Mn4 115.8(3) . . ? O3 N11 Mn4 128.1(2) . . ? C13 N12 O2 117.4(3) . . ? C13 N12 Mn4 118.9(3) . . ? O2 N12 Mn4 123.4(3) . . ? N1 C1 C2 124.9(5) . . ? N1 C1 H1 117.6 . . ? C2 C1 H1 117.5 . . ? C1 C2 C3 118.8(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 118.7(5) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118.6(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 123.7(4) . . ? N1 C5 C6 115.3(4) . . ? C4 C5 C6 120.9(4) . . ? N10 C6 C7 121.1(4) . . ? N10 C6 C5 118.1(4) . . ? C7 C6 C5 120.8(4) . . ? N2 C7 C6 178.0(5) . . ? N3 C8 C9 124.0(4) . . ? N3 C8 H8 118.0 . . ? C9 C8 H8 118.0 . . ? C8 C9 C10 118.6(5) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 118.9(5) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 118.8(4) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N3 C12 C11 123.6(4) . . ? N3 C12 C13 116.3(4) . . ? C11 C12 C13 120.1(4) . . ? N12 C13 C14 122.6(4) . . ? N12 C13 C12 117.6(4) . . ? C14 C13 C12 119.7(4) . . ? N4 C14 C13 175.1(5) . . ? N5 C15 C16 122.7(4) . . ? N5 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C15 C16 C17 119.6(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 118.7(5) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 118.9(4) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? N5 C19 C18 122.4(4) . . ? N5 C19 C20 114.9(4) . . ? C18 C19 C20 122.6(4) . . ? N11 C20 C28 122.6(4) . . ? N11 C20 C19 118.4(4) . . ? C28 C20 C19 118.9(4) . . ? N7 C21 C22 123.2(5) . . ? N7 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C23 119.5(5) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 117.9(5) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C23 C24 C25 119.8(5) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N7 C25 C24 121.9(4) . . ? N7 C25 C26 114.6(4) . . ? C24 C25 C26 123.4(4) . . ? N9 C26 C27 120.8(4) . . ? N9 C26 C25 119.0(4) . . ? C27 C26 C25 120.1(4) . . ? N8 C27 C26 178.0(5) . . ? N6 C28 C20 177.1(5) . . ? Cl4 C1W Cl3 111.5(3) . . ? Cl4 C1W H1W1 109.3 . . ? Cl3 C1W H1W1 109.3 . . ? Cl4 C1W H1W2 109.3 . . ? Cl3 C1W H1W2 109.3 . . ? H1W1 C1W H1W2 108.0 . . ? Cl5 C2W Cl6 116.3(5) . . ? Cl5 C2W H2W1 108.2 . . ? Cl6 C2W H2W1 108.2 . . ? Cl5 C2W H2W2 108.2 . . ? Cl6 C2W H2W2 108.2 . . ? H2W1 C2W H2W2 107.4 . . ? Cl5' Cl5' C2W' 163.2(6) 2_656 . ? Cl5' C2W' Cl6' 112.5(6) . . ? Cl5' C2W' H2W3 109.1 . . ? Cl6' C2W' H2W3 109.1 . . ? Cl5' C2W' H2W4 109.1 . . ? Cl6' C2W' H2W4 109.1 . . ? H2W3 C2W' H2W4 107.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.732 _refine_diff_density_min -1.539 _refine_diff_density_rms 0.119 _database_code_depnum_ccdc_archive 'CCDC 916865' ####################################################################### # # 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_af05fua1na _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H62 Mn10 N20 O28, 5(C2 H3 N), 2(H2 O)' _chemical_formula_sum 'C104 H81 Mn10 N25 O30' _chemical_formula_weight 2710.34 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.6596(3) _cell_length_b 15.8014(3) _cell_length_c 16.1286(5) _cell_angle_alpha 106.3150(10) _cell_angle_beta 115.9110(10) _cell_angle_gamma 104.1330(10) _cell_volume 2919.32(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9492 _cell_measurement_theta_min 2.179 _cell_measurement_theta_max 26.7875 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1370 _exptl_absorpt_coefficient_mu 1.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8059 _exptl_absorpt_correction_T_max 0.8956 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 1003(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 'Bruker X8 KappaAPEXII' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11432 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.02 _reflns_number_total 11432 _reflns_number_gt 10306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. The displacement parameters of some lengths in the direction of the bond are restrained to be equal within an effective standard deviation (DELU sentences) The distances of acetonitriles are restrained (DFIX sentences) ; _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^)+(0.0662P)^2^+4.4131P] 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 11432 _refine_ls_number_parameters 739 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.122 _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 0.98045(3) 0.67197(3) -0.09321(3) 0.01513(10) Uani 1 1 d . . . Mn2 Mn 0.87062(3) 0.46780(3) -0.04900(3) 0.01475(10) Uani 1 1 d U . . Mn3 Mn 0.91595(3) 0.69573(3) 0.08892(3) 0.01547(10) Uani 1 1 d U . . Mn4 Mn 0.83579(3) 0.23465(3) -0.16245(3) 0.01611(10) Uani 1 1 d U . . Mn5 Mn 1.04418(3) 0.56300(3) 0.17658(3) 0.01507(10) Uani 1 1 d . . . O1 O 0.92382(15) 0.57635(13) 0.07970(13) 0.0161(4) Uani 1 1 d . . . O2 O 0.97792(15) 0.53909(13) -0.07080(13) 0.0155(4) Uani 1 1 d . . . O3 O 0.85534(15) 0.36175(13) -0.15541(13) 0.0164(4) Uani 1 1 d . . . O4 O 1.02059(15) 0.73313(13) 0.05459(13) 0.0155(4) Uani 1 1 d . . . O5 O 1.05743(15) 0.52143(13) -0.19682(14) 0.0188(4) Uani 1 1 d . . . O6 O 0.83553(15) 0.45192(13) -0.27871(14) 0.0186(4) Uani 1 1 d . . . O7 O 1.06917(16) 0.66398(14) 0.29876(14) 0.0207(4) Uani 1 1 d . . . O8 O 1.09301(16) 0.78784(14) 0.25836(14) 0.0218(4) Uani 1 1 d U . . O9 O 0.75860(16) 0.39259(14) -0.03314(15) 0.0219(4) Uani 1 1 d . . . O10 O 0.76396(17) 0.24720(14) -0.07123(15) 0.0237(4) Uani 1 1 d . . . O11 O 0.73834(17) 0.49289(15) -0.14668(15) 0.0244(4) Uani 1 1 d U . . O12 O 0.6338(2) -0.0464(2) -0.2918(3) 0.0603(8) Uani 1 1 d . . . O13 O 0.76028(17) 0.63661(15) -0.04667(15) 0.0259(4) Uani 1 1 d U . . O14 O 0.8570(2) 0.91930(17) 0.20559(19) 0.0361(5) Uani 1 1 d . . . N1 N 1.09363(19) 0.79540(16) -0.09903(17) 0.0196(5) Uani 1 1 d . . . N2 N 1.07095(19) 0.61323(16) -0.16410(17) 0.0180(4) Uani 1 1 d . . . N3 N 1.2129(2) 0.6061(2) -0.2860(2) 0.0340(6) Uani 1 1 d . . . N4 N 0.83590(19) 0.71177(17) -0.17705(17) 0.0191(5) Uani 1 1 d . . . N5 N 0.83942(18) 0.54034(16) -0.24936(17) 0.0174(4) Uani 1 1 d . . . N6 N 0.5926(2) 0.4036(2) -0.4819(2) 0.0353(6) Uani 1 1 d . . . N7 N 0.6768(2) 0.18356(18) -0.28754(19) 0.0259(5) Uani 1 1 d U . . N8 N 0.78339(17) 0.09639(15) -0.19646(16) 0.0133(4) Uani 1 1 d U . . N9 N 0.8347(2) 0.68250(17) 0.16438(18) 0.0218(5) Uani 1 1 d U . . N10 N 0.90751(16) 0.82118(14) 0.12355(15) 0.0113(4) Uani 1 1 d U . . C1 C 1.1075(2) 0.8894(2) -0.0615(2) 0.0256(6) Uani 1 1 d . . . H1 H 1.0743 0.9070 -0.0259 0.031 Uiso 1 1 calc R . . C2 C 1.1697(3) 0.9594(2) -0.0747(3) 0.0321(7) Uani 1 1 d . . . H2 H 1.1778 1.0232 -0.0486 0.039 Uiso 1 1 calc R . . C3 C 1.2196(3) 0.9336(2) -0.1271(3) 0.0349(7) Uani 1 1 d . . . H3 H 1.2609 0.9797 -0.1375 0.042 Uiso 1 1 calc R . . C4 C 1.2077(3) 0.8388(2) -0.1641(2) 0.0283(6) Uani 1 1 d . . . H4 H 1.2417 0.8208 -0.1988 0.034 Uiso 1 1 calc R . . C5 C 1.1447(2) 0.7708(2) -0.1492(2) 0.0216(6) Uani 1 1 d . . . C6 C 1.1296(2) 0.6701(2) -0.1834(2) 0.0187(5) Uani 1 1 d . . . C7 C 1.1776(2) 0.6351(2) -0.2391(2) 0.0218(6) Uani 1 1 d . . . C8 C 0.8331(2) 0.7984(2) -0.1373(2) 0.0246(6) Uani 1 1 d . . . H8 H 0.8881 0.8429 -0.0693 0.029 Uiso 1 1 calc R . . C9 C 0.7500(2) 0.8222(2) -0.1958(2) 0.0272(6) Uani 1 1 d . . . H9 H 0.7495 0.8819 -0.1672 0.033 Uiso 1 1 calc R . . C10 C 0.6685(2) 0.7566(2) -0.2966(2) 0.0269(6) Uani 1 1 d . . . H10 H 0.6131 0.7720 -0.3368 0.032 Uiso 1 1 calc R . . C11 C 0.6694(2) 0.6677(2) -0.3378(2) 0.0236(6) Uani 1 1 d . . . H11 H 0.6142 0.6226 -0.4056 0.028 Uiso 1 1 calc R . . C12 C 0.7534(2) 0.6463(2) -0.2772(2) 0.0190(5) Uani 1 1 d . . . C13 C 0.7561(2) 0.55234(19) -0.3111(2) 0.0182(5) Uani 1 1 d . . . C14 C 0.6642(2) 0.4707(2) -0.4071(2) 0.0223(6) Uani 1 1 d . . . C15 C 1.0849(2) 0.7517(2) 0.3157(2) 0.0216(6) Uani 1 1 d . . . C16 C 1.0890(3) 0.8118(2) 0.4070(3) 0.0381(8) Uani 1 1 d . . . C17 C 1.0580(4) 0.7708(3) 0.4611(3) 0.0558(11) Uani 1 1 d . . . H17 H 1.0345 0.7042 0.4407 0.067 Uiso 1 1 calc R . . C18 C 1.0622(8) 0.8294(4) 0.5457(6) 0.108(3) Uani 1 1 d . . . H18 H 1.0414 0.8020 0.5823 0.129 Uiso 1 1 calc R . . C19 C 1.0963(9) 0.9267(5) 0.5756(6) 0.130(3) Uani 1 1 d . . . H19 H 1.0996 0.9656 0.6330 0.156 Uiso 1 1 calc R . . C20 C 1.1261(7) 0.9679(4) 0.5216(5) 0.101(2) Uani 1 1 d . . . H20 H 1.1490 1.0345 0.5422 0.122 Uiso 1 1 calc R . . C21 C 1.1220(5) 0.9108(3) 0.4372(4) 0.0590(12) Uani 1 1 d . . . H21 H 1.1414 0.9387 0.4003 0.071 Uiso 1 1 calc R . . C22 C 0.7224(2) 0.3033(2) -0.0502(2) 0.0201(5) Uani 1 1 d . . . C23 C 0.6240(2) 0.2672(2) -0.0422(2) 0.0278(6) Uani 1 1 d U . . C24 C 0.5734(3) 0.3270(2) -0.0217(3) 0.0315(7) Uani 1 1 d . . . H24 H 0.6000 0.3901 -0.0145 0.038 Uiso 1 1 calc R . . C25 C 0.4842(3) 0.2935(3) -0.0119(3) 0.0482(9) Uani 1 1 d . . . H25 H 0.4491 0.3331 -0.0007 0.058 Uiso 1 1 calc R . . C26 C 0.4473(4) 0.2011(4) -0.0188(5) 0.0693(14) Uani 1 1 d . . . H26 H 0.3890 0.1792 -0.0097 0.083 Uiso 1 1 calc R . . C27 C 0.4971(5) 0.1416(4) -0.0393(5) 0.0800(17) Uani 1 1 d . . . H27 H 0.4715 0.0791 -0.0448 0.096 Uiso 1 1 calc R . . C28 C 0.5849(3) 0.1737(3) -0.0518(4) 0.0525(10) Uani 1 1 d U . . H28 H 0.6173 0.1327 -0.0666 0.063 Uiso 1 1 calc R . . C29 C 0.6790(3) 0.0399(2) -0.2668(3) 0.0361(7) Uani 1 1 d U . . C30 C 0.6135(3) 0.0889(3) -0.3183(3) 0.0426(8) Uani 1 1 d . . . C32 C 0.6284(3) 0.2355(2) -0.3317(2) 0.0323(7) Uani 1 1 d . . . H32 H 0.6717 0.3004 -0.3102 0.039 Uiso 1 1 calc R . . C33 C 0.5159(3) 0.1930(3) -0.4079(3) 0.0479(9) Uani 1 1 d . . . H33 H 0.4839 0.2285 -0.4387 0.057 Uiso 1 1 calc R . . C34 C 0.4517(4) 0.0978(4) -0.4378(4) 0.0724(15) Uani 1 1 d . . . H34 H 0.3754 0.0689 -0.4878 0.087 Uiso 1 1 calc R . . C35 C 0.5010(4) 0.0452(4) -0.3933(5) 0.0762(17) Uani 1 1 d . . . H35 H 0.4582 -0.0196 -0.4139 0.091 Uiso 1 1 calc R . . C36 C 0.7045(2) 0.5568(2) -0.1270(2) 0.0191(5) Uani 1 1 d . . . C37 C 0.5888(2) 0.5391(2) -0.2062(2) 0.0213(5) Uani 1 1 d . . . C38 C 0.5536(3) 0.6129(2) -0.1936(2) 0.0294(6) Uani 1 1 d . . . H38 H 0.6012 0.6729 -0.1360 0.035 Uiso 1 1 calc R . . C39 C 0.4475(3) 0.5973(3) -0.2666(3) 0.0412(8) Uani 1 1 d . . . H39 H 0.4237 0.6467 -0.2577 0.049 Uiso 1 1 calc R . . C40 C 0.3775(3) 0.5093(3) -0.3521(3) 0.0434(9) Uani 1 1 d . . . H40 H 0.3064 0.4992 -0.4011 0.052 Uiso 1 1 calc R . . C41 C 0.4123(3) 0.4350(3) -0.3659(3) 0.0400(8) Uani 1 1 d . . . H41 H 0.3646 0.3754 -0.4241 0.048 Uiso 1 1 calc R . . C42 C 0.5181(3) 0.4499(2) -0.2927(2) 0.0295(6) Uani 1 1 d . . . H42 H 0.5416 0.4003 -0.3015 0.035 Uiso 1 1 calc R . . C43 C 0.8643(2) 0.8428(2) 0.1772(2) 0.0237(6) Uani 1 1 d U . . C44 C 0.8206(3) 0.7640(2) 0.2019(2) 0.0284(6) Uani 1 1 d . . . C46 C 0.7950(3) 0.6039(2) 0.1790(2) 0.0288(6) Uani 1 1 d . . . H46 H 0.8034 0.5479 0.1527 0.035 Uiso 1 1 calc R . . C47 C 0.7427(3) 0.6068(3) 0.2323(3) 0.0391(8) Uani 1 1 d . . . H47 H 0.7164 0.5531 0.2422 0.047 Uiso 1 1 calc R . . C48 C 0.7295(4) 0.6892(3) 0.2709(3) 0.0474(9) Uani 1 1 d . . . H48 H 0.6944 0.6917 0.3071 0.057 Uiso 1 1 calc R . . C49 C 0.7690(3) 0.7687(3) 0.2553(3) 0.0408(8) Uani 1 1 d . . . H49 H 0.7606 0.8248 0.2809 0.049 Uiso 1 1 calc R . . N1W N 0.6006(7) 0.1128(5) 0.2250(5) 0.0610(6) Uani 0.50 1 d PD . . C1W C 0.6272(7) 0.2126(6) 0.3921(5) 0.0454(6) Uani 0.50 1 d PD . . C2W C 0.6076(6) 0.1581(5) 0.2938(5) 0.0416(5) Uani 0.50 1 d PD . . N2W N 0.2476(3) 0.1728(3) 0.4871(3) 0.0610(6) Uani 1 1 d D . . C3W C 0.0825(3) 0.1397(3) 0.3130(3) 0.0454(6) Uani 1 1 d D . . C4W C 0.1747(3) 0.1575(3) 0.4091(3) 0.0416(5) Uani 1 1 d D . . N3W N 0.0772(3) 0.3687(3) 0.4111(3) 0.0610(6) Uani 1 1 d D . . C5W C 0.1008(3) 0.5451(3) 0.4569(3) 0.0454(6) Uani 1 1 d D . . C6W C 0.0881(3) 0.4472(3) 0.4322(3) 0.0416(5) Uani 1 1 d D . . O1W O 1.0489(2) 0.96974(17) 0.11454(18) 0.0352(5) 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 Mn1 0.0174(2) 0.0159(2) 0.01468(19) 0.00784(15) 0.00936(16) 0.00833(16) Mn2 0.0168(2) 0.01478(19) 0.01473(19) 0.00704(15) 0.00927(16) 0.00785(16) Mn3 0.0187(2) 0.0156(2) 0.01634(19) 0.00836(16) 0.01092(16) 0.00927(16) Mn4 0.0178(2) 0.01549(19) 0.01555(19) 0.00733(15) 0.00871(16) 0.00795(16) Mn5 0.0186(2) 0.0152(2) 0.01401(19) 0.00730(15) 0.00941(16) 0.00887(16) O1 0.0190(9) 0.0169(9) 0.0162(8) 0.0086(7) 0.0106(7) 0.0099(7) O2 0.0190(9) 0.0159(9) 0.0141(8) 0.0075(7) 0.0094(7) 0.0092(7) O3 0.0186(9) 0.0165(9) 0.0166(9) 0.0080(7) 0.0105(7) 0.0084(7) O4 0.0179(9) 0.0169(9) 0.0153(8) 0.0085(7) 0.0101(7) 0.0089(7) O5 0.0229(9) 0.0178(9) 0.0191(9) 0.0094(7) 0.0123(8) 0.0107(8) O6 0.0214(9) 0.0186(9) 0.0172(9) 0.0091(7) 0.0100(8) 0.0103(8) O7 0.0265(10) 0.0191(9) 0.0188(9) 0.0083(8) 0.0132(8) 0.0112(8) O8 0.0263(9) 0.0219(10) 0.0186(8) 0.0093(7) 0.0122(6) 0.0120(8) O9 0.0236(10) 0.0213(10) 0.0249(10) 0.0113(8) 0.0152(8) 0.0106(8) O10 0.0272(10) 0.0253(10) 0.0261(10) 0.0144(9) 0.0170(9) 0.0137(9) O11 0.0259(10) 0.0311(11) 0.0211(10) 0.0138(8) 0.0127(8) 0.0171(9) O12 0.0472(16) 0.0380(15) 0.071(2) 0.0230(14) 0.0165(15) 0.0138(13) O13 0.0239(9) 0.0258(11) 0.0240(9) 0.0113(8) 0.0094(7) 0.0116(8) O14 0.0484(14) 0.0303(12) 0.0434(13) 0.0181(10) 0.0315(12) 0.0217(11) N1 0.0202(11) 0.0203(11) 0.0197(11) 0.0097(9) 0.0109(9) 0.0096(9) N2 0.0202(11) 0.0198(11) 0.0172(10) 0.0097(9) 0.0106(9) 0.0105(9) N3 0.0347(15) 0.0402(16) 0.0337(14) 0.0172(13) 0.0212(13) 0.0194(13) N4 0.0201(11) 0.0208(11) 0.0192(11) 0.0103(9) 0.0113(9) 0.0097(9) N5 0.0204(11) 0.0177(11) 0.0174(10) 0.0093(9) 0.0113(9) 0.0091(9) N6 0.0314(14) 0.0349(15) 0.0323(15) 0.0140(13) 0.0124(13) 0.0140(13) N7 0.0229(10) 0.0241(12) 0.0225(11) 0.0086(10) 0.0075(8) 0.0097(10) N8 0.0163(9) 0.0129(7) 0.0150(10) 0.0075(8) 0.0096(8) 0.0088(7) N9 0.0265(12) 0.0225(12) 0.0253(12) 0.0132(10) 0.0179(10) 0.0129(10) N10 0.0137(9) 0.0106(8) 0.0122(9) 0.0065(8) 0.0076(8) 0.0062(8) C1 0.0271(15) 0.0255(15) 0.0279(15) 0.0129(12) 0.0164(13) 0.0128(12) C2 0.0344(17) 0.0256(15) 0.0382(17) 0.0144(14) 0.0203(15) 0.0138(14) C3 0.0352(17) 0.0328(17) 0.0460(19) 0.0223(15) 0.0260(16) 0.0151(14) C4 0.0288(15) 0.0292(16) 0.0334(16) 0.0158(13) 0.0202(13) 0.0131(13) C5 0.0210(13) 0.0238(14) 0.0226(13) 0.0120(11) 0.0119(11) 0.0110(11) C6 0.0203(13) 0.0216(13) 0.0195(12) 0.0112(11) 0.0124(11) 0.0112(11) C7 0.0211(13) 0.0262(14) 0.0227(13) 0.0133(11) 0.0128(12) 0.0121(12) C8 0.0253(14) 0.0238(14) 0.0246(14) 0.0099(12) 0.0143(12) 0.0102(12) C9 0.0283(15) 0.0254(15) 0.0309(15) 0.0133(13) 0.0165(13) 0.0144(13) C10 0.0255(14) 0.0280(15) 0.0316(15) 0.0167(13) 0.0149(13) 0.0148(13) C11 0.0217(13) 0.0242(14) 0.0233(14) 0.0115(12) 0.0102(12) 0.0103(12) C12 0.0198(13) 0.0204(13) 0.0198(13) 0.0108(11) 0.0117(11) 0.0088(11) C13 0.0196(13) 0.0191(13) 0.0177(12) 0.0099(11) 0.0104(11) 0.0085(11) C14 0.0230(14) 0.0237(14) 0.0220(14) 0.0117(12) 0.0115(12) 0.0118(12) C15 0.0231(13) 0.0225(14) 0.0196(13) 0.0091(11) 0.0117(11) 0.0108(11) C16 0.056(2) 0.0309(17) 0.0363(18) 0.0152(15) 0.0309(17) 0.0205(16) C17 0.096(3) 0.037(2) 0.062(3) 0.026(2) 0.060(3) 0.032(2) C18 0.215(9) 0.072(4) 0.115(5) 0.055(4) 0.135(6) 0.073(5) C19 0.255(11) 0.077(4) 0.127(6) 0.049(4) 0.150(8) 0.078(6) C20 0.188(8) 0.052(3) 0.102(5) 0.033(3) 0.108(5) 0.049(4) C21 0.099(4) 0.039(2) 0.058(3) 0.023(2) 0.057(3) 0.028(2) C22 0.0208(13) 0.0210(13) 0.0181(12) 0.0089(11) 0.0100(11) 0.0092(11) C23 0.0230(14) 0.0311(14) 0.0269(15) 0.0117(13) 0.0127(12) 0.0110(12) C24 0.0324(16) 0.0294(16) 0.0359(17) 0.0153(14) 0.0206(14) 0.0132(14) C25 0.042(2) 0.048(2) 0.061(2) 0.0227(19) 0.0318(19) 0.0216(18) C26 0.059(3) 0.058(3) 0.100(4) 0.033(3) 0.054(3) 0.020(2) C27 0.074(3) 0.060(3) 0.127(5) 0.045(3) 0.069(4) 0.027(3) C28 0.047(2) 0.0344(17) 0.080(3) 0.024(2) 0.039(2) 0.0164(17) C29 0.0237(12) 0.0280(17) 0.0383(18) 0.0119(13) 0.0071(11) 0.0069(11) C30 0.0347(18) 0.0300(17) 0.047(2) 0.0143(16) 0.0123(16) 0.0121(15) C32 0.0315(16) 0.0267(16) 0.0315(16) 0.0124(13) 0.0120(14) 0.0127(14) C33 0.041(2) 0.040(2) 0.048(2) 0.0190(17) 0.0116(17) 0.0197(17) C34 0.044(2) 0.052(3) 0.077(3) 0.024(2) 0.005(2) 0.015(2) C35 0.047(3) 0.044(2) 0.094(4) 0.028(3) 0.010(3) 0.013(2) C36 0.0188(13) 0.0217(13) 0.0210(13) 0.0117(11) 0.0119(11) 0.0097(11) C37 0.0194(13) 0.0265(14) 0.0226(13) 0.0135(12) 0.0130(11) 0.0103(11) C38 0.0294(15) 0.0325(16) 0.0325(16) 0.0170(13) 0.0185(14) 0.0158(13) C39 0.0375(19) 0.055(2) 0.048(2) 0.0316(19) 0.0262(17) 0.0276(18) C40 0.0315(18) 0.062(2) 0.043(2) 0.0309(19) 0.0200(16) 0.0210(18) C41 0.0316(17) 0.048(2) 0.0306(17) 0.0148(15) 0.0152(15) 0.0081(16) C42 0.0300(16) 0.0309(16) 0.0284(15) 0.0136(13) 0.0168(13) 0.0115(13) C43 0.0290(15) 0.0259(14) 0.0269(14) 0.0128(12) 0.0202(12) 0.0164(12) C44 0.0342(16) 0.0271(15) 0.0326(16) 0.0146(13) 0.0221(14) 0.0164(13) C46 0.0357(16) 0.0280(15) 0.0342(16) 0.0174(13) 0.0233(14) 0.0178(14) C47 0.049(2) 0.0399(19) 0.051(2) 0.0286(17) 0.0366(18) 0.0238(17) C48 0.062(2) 0.050(2) 0.062(2) 0.031(2) 0.050(2) 0.031(2) C49 0.057(2) 0.0375(19) 0.053(2) 0.0240(17) 0.042(2) 0.0283(18) N1W 0.0578(15) 0.0601(16) 0.0624(16) 0.0296(13) 0.0290(13) 0.0251(13) C1W 0.0486(14) 0.0457(14) 0.0441(14) 0.0209(12) 0.0259(12) 0.0206(12) C2W 0.0403(13) 0.0428(14) 0.0422(13) 0.0204(11) 0.0218(11) 0.0180(11) N2W 0.0578(15) 0.0601(16) 0.0624(16) 0.0296(13) 0.0290(13) 0.0251(13) C3W 0.0486(14) 0.0457(14) 0.0441(14) 0.0209(12) 0.0259(12) 0.0206(12) C4W 0.0403(13) 0.0428(14) 0.0422(13) 0.0204(11) 0.0218(11) 0.0180(11) N3W 0.0578(15) 0.0601(16) 0.0624(16) 0.0296(13) 0.0290(13) 0.0251(13) C5W 0.0486(14) 0.0457(14) 0.0441(14) 0.0209(12) 0.0259(12) 0.0206(12) C6W 0.0403(13) 0.0428(14) 0.0422(13) 0.0204(11) 0.0218(11) 0.0180(11) O1W 0.0382(12) 0.0337(12) 0.0378(13) 0.0175(10) 0.0218(11) 0.0173(10) _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 O4 2.0408(18) . ? Mn1 O2 2.2227(18) . ? Mn1 N1 2.286(2) . ? Mn1 N2 2.293(2) . ? Mn1 N4 2.311(2) . ? Mn1 N5 2.313(2) . ? Mn2 O3 1.9154(18) . ? Mn2 O2 1.9255(18) . ? Mn2 O9 1.9388(19) . ? Mn2 O1 1.9469(18) . ? Mn2 O11 2.1109(19) . ? Mn2 O2 2.2720(18) 2_765 ? Mn2 Mn5 2.8306(5) 2_765 ? Mn2 Mn5 2.9899(5) . ? Mn2 Mn2 3.1456(7) 2_765 ? Mn3 O4 1.8687(18) . ? Mn3 O1 1.8862(18) . ? Mn3 N10 1.953(2) . ? Mn3 N9 2.058(2) . ? Mn3 O13 2.077(2) . ? Mn3 O8 2.4587(19) . ? Mn3 Mn4 3.0662(5) 2_765 ? Mn4 O4 1.8698(18) 2_765 ? Mn4 O3 1.9211(18) . ? Mn4 N8 1.950(2) . ? Mn4 N7 2.053(2) . ? Mn4 O10 2.146(2) . ? Mn4 O8 2.212(2) 2_765 ? Mn4 Mn3 3.0662(5) 2_765 ? Mn5 O2 1.8259(17) 2_765 ? Mn5 O3 1.8742(18) 2_765 ? Mn5 O1 1.8859(18) . ? Mn5 O6 1.9393(18) 2_765 ? Mn5 O5 1.9504(19) 2_765 ? Mn5 O7 1.9698(19) . ? Mn5 Mn2 2.8306(5) 2_765 ? O2 Mn5 1.8259(17) 2_765 ? O2 Mn2 2.2720(18) 2_765 ? O3 Mn5 1.8742(18) 2_765 ? O4 Mn4 1.8698(18) 2_765 ? O5 N2 1.327(3) . ? O5 Mn5 1.9504(19) 2_765 ? O6 N5 1.321(3) . ? O6 Mn5 1.9393(18) 2_765 ? O7 C15 1.274(3) . ? O8 C15 1.248(3) . ? O8 Mn4 2.212(2) 2_765 ? O9 C22 1.279(3) . ? O10 C22 1.245(3) . ? O11 C36 1.253(3) . ? O12 C29 1.214(4) . ? O13 C36 1.261(3) . ? O14 C43 1.216(4) . ? N1 C1 1.362(4) . ? N1 C5 1.364(4) . ? N2 C6 1.287(4) . ? N3 C7 1.145(4) . ? N4 C8 1.357(4) . ? N4 C12 1.373(3) . ? N5 C13 1.294(3) . ? N6 C14 1.146(4) . ? N7 C30 1.359(4) . ? N7 C32 1.362(4) . ? N8 C29 1.293(4) . ? N9 C44 1.366(4) . ? N9 C46 1.366(4) . ? N10 C43 1.299(3) . ? C1 C2 1.382(4) . ? C1 H1 0.9300 . ? C2 C3 1.383(5) . ? C2 H2 0.9300 . ? C3 C4 1.382(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(4) . ? C4 H4 0.9300 . ? C5 C6 1.454(4) . ? C6 C7 1.440(4) . ? C8 C9 1.391(4) . ? C8 H8 0.9300 . ? C9 C10 1.377(4) . ? C9 H9 0.9300 . ? C10 C11 1.381(4) . ? C10 H10 0.9300 . ? C11 C12 1.387(4) . ? C11 H11 0.9300 . ? C12 C13 1.447(4) . ? C13 C14 1.443(4) . ? C15 C16 1.478(4) . ? C16 C17 1.380(5) . ? C16 C21 1.384(5) . ? C17 C18 1.384(7) . ? C17 H17 0.9300 . ? C18 C19 1.357(8) . ? C18 H18 0.9300 . ? C19 C20 1.373(9) . ? C19 H19 0.9300 . ? C20 C21 1.371(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.492(4) . ? C23 C28 1.383(5) . ? C23 C24 1.390(4) . ? C24 C25 1.380(5) . ? C24 H24 0.9300 . ? C25 C26 1.381(6) . ? C25 H25 0.9300 . ? C26 C27 1.378(7) . ? C26 H26 0.9300 . ? C27 C28 1.385(6) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.496(5) . ? C30 C35 1.376(6) . ? C32 C33 1.380(5) . ? C32 H32 0.9300 . ? C33 C34 1.373(6) . ? C33 H33 0.9300 . ? C34 C35 1.379(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.503(4) . ? C37 C38 1.386(4) . ? C37 C42 1.387(4) . ? C38 C39 1.384(5) . ? C38 H38 0.9300 . ? C39 C40 1.370(6) . ? C39 H39 0.9300 . ? C40 C41 1.390(6) . ? C40 H40 0.9300 . ? C41 C42 1.386(5) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.493(4) . ? C44 C49 1.372(5) . ? C46 C47 1.379(5) . ? C46 H46 0.9300 . ? C47 C48 1.376(5) . ? C47 H47 0.9300 . ? C48 C49 1.387(5) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? N1W C2W 1.083(7) . ? C1W C2W 1.433(7) . ? N2W C4W 1.145(4) . ? C3W C4W 1.431(5) . ? N3W C6W 1.139(4) . ? C5W C6W 1.427(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O2 85.26(7) . . ? O4 Mn1 N1 102.62(8) . . ? O2 Mn1 N1 139.09(7) . . ? O4 Mn1 N2 132.76(8) . . ? O2 Mn1 N2 74.65(7) . . ? N1 Mn1 N2 70.76(8) . . ? O4 Mn1 N4 101.65(7) . . ? O2 Mn1 N4 130.86(7) . . ? N1 Mn1 N4 87.36(8) . . ? N2 Mn1 N4 123.94(8) . . ? O4 Mn1 N5 139.07(8) . . ? O2 Mn1 N5 73.43(7) . . ? N1 Mn1 N5 116.48(8) . . ? N2 Mn1 N5 74.98(8) . . ? N4 Mn1 N5 70.08(8) . . ? O3 Mn2 O2 80.77(7) . . ? O3 Mn2 O9 97.36(8) . . ? O2 Mn2 O9 177.63(8) . . ? O3 Mn2 O1 165.26(8) . . ? O2 Mn2 O1 93.65(8) . . ? O9 Mn2 O1 88.51(8) . . ? O3 Mn2 O11 96.49(8) . . ? O2 Mn2 O11 94.88(8) . . ? O9 Mn2 O11 83.85(8) . . ? O1 Mn2 O11 97.58(8) . . ? O3 Mn2 O2 90.22(7) . 2_765 ? O2 Mn2 O2 83.27(7) . 2_765 ? O9 Mn2 O2 98.23(7) . 2_765 ? O1 Mn2 O2 75.52(7) . 2_765 ? O11 Mn2 O2 172.68(7) . 2_765 ? O3 Mn2 Mn5 41.12(5) . 2_765 ? O2 Mn2 Mn5 39.71(5) . 2_765 ? O9 Mn2 Mn5 138.34(6) . 2_765 ? O1 Mn2 Mn5 132.44(6) . 2_765 ? O11 Mn2 Mn5 95.71(6) . 2_765 ? O2 Mn2 Mn5 87.41(5) 2_765 2_765 ? O3 Mn2 Mn5 127.79(5) . . ? O2 Mn2 Mn5 89.73(5) . . ? O9 Mn2 Mn5 92.58(6) . . ? O1 Mn2 Mn5 38.01(5) . . ? O11 Mn2 Mn5 135.59(6) . . ? O2 Mn2 Mn5 37.58(4) 2_765 . ? Mn5 Mn2 Mn5 114.640(15) 2_765 . ? O3 Mn2 Mn2 84.53(6) . 2_765 ? O2 Mn2 Mn2 45.83(5) . 2_765 ? O9 Mn2 Mn2 135.65(6) . 2_765 ? O1 Mn2 Mn2 81.85(5) . 2_765 ? O11 Mn2 Mn2 140.22(6) . 2_765 ? O2 Mn2 Mn2 37.44(5) 2_765 2_765 ? Mn5 Mn2 Mn2 59.763(14) 2_765 2_765 ? Mn5 Mn2 Mn2 54.877(13) . 2_765 ? O4 Mn3 O1 94.99(8) . . ? O4 Mn3 N10 93.79(8) . . ? O1 Mn3 N10 168.26(8) . . ? O4 Mn3 N9 164.98(9) . . ? O1 Mn3 N9 89.55(9) . . ? N10 Mn3 N9 80.04(9) . . ? O4 Mn3 O13 105.41(8) . . ? O1 Mn3 O13 96.40(8) . . ? N10 Mn3 O13 88.75(8) . . ? N9 Mn3 O13 88.24(9) . . ? O4 Mn3 O8 77.71(7) . . ? O1 Mn3 O8 91.95(7) . . ? N10 Mn3 O8 82.32(7) . . ? N9 Mn3 O8 87.84(8) . . ? O13 Mn3 O8 170.75(7) . . ? O4 Mn3 Mn4 34.91(5) . 2_765 ? O1 Mn3 Mn4 83.40(6) . 2_765 ? N10 Mn3 Mn4 99.54(6) . 2_765 ? N9 Mn3 Mn4 132.25(7) . 2_765 ? O13 Mn3 Mn4 139.42(6) . 2_765 ? O8 Mn3 Mn4 45.57(5) . 2_765 ? O4 Mn4 O3 99.05(8) 2_765 . ? O4 Mn4 N8 93.62(8) 2_765 . ? O3 Mn4 N8 167.28(8) . . ? O4 Mn4 N7 173.49(9) 2_765 . ? O3 Mn4 N7 86.89(9) . . ? N8 Mn4 N7 80.40(9) . . ? O4 Mn4 O10 95.55(8) 2_765 . ? O3 Mn4 O10 92.81(8) . . ? N8 Mn4 O10 87.00(8) . . ? N7 Mn4 O10 86.77(9) . . ? O4 Mn4 O8 84.40(7) 2_765 2_765 ? O3 Mn4 O8 90.69(7) . 2_765 ? N8 Mn4 O8 89.47(8) . 2_765 ? N7 Mn4 O8 92.90(9) . 2_765 ? O10 Mn4 O8 176.46(7) . 2_765 ? O4 Mn4 Mn3 34.89(5) 2_765 2_765 ? O3 Mn4 Mn3 85.21(5) . 2_765 ? N8 Mn4 Mn3 104.86(6) . 2_765 ? N7 Mn4 Mn3 144.33(8) . 2_765 ? O10 Mn4 Mn3 128.30(6) . 2_765 ? O8 Mn4 Mn3 52.55(5) 2_765 2_765 ? O2 Mn5 O3 84.52(8) 2_765 2_765 ? O2 Mn5 O1 88.75(8) 2_765 . ? O3 Mn5 O1 91.51(8) 2_765 . ? O2 Mn5 O6 92.33(8) 2_765 2_765 ? O3 Mn5 O6 90.67(8) 2_765 2_765 ? O1 Mn5 O6 177.65(8) . 2_765 ? O2 Mn5 O5 92.74(8) 2_765 2_765 ? O3 Mn5 O5 176.57(8) 2_765 2_765 ? O1 Mn5 O5 90.50(8) . 2_765 ? O6 Mn5 O5 87.37(8) 2_765 2_765 ? O2 Mn5 O7 173.63(8) 2_765 . ? O3 Mn5 O7 99.90(8) 2_765 . ? O1 Mn5 O7 95.68(8) . . ? O6 Mn5 O7 83.09(8) 2_765 . ? O5 Mn5 O7 82.66(8) 2_765 . ? O2 Mn5 Mn2 42.36(6) 2_765 2_765 ? O3 Mn5 Mn2 42.23(5) 2_765 2_765 ? O1 Mn5 Mn2 92.04(5) . 2_765 ? O6 Mn5 Mn2 90.16(6) 2_765 2_765 ? O5 Mn5 Mn2 134.90(6) 2_765 2_765 ? O7 Mn5 Mn2 141.63(6) . 2_765 ? O2 Mn5 Mn2 49.36(6) 2_765 . ? O3 Mn5 Mn2 89.81(6) 2_765 . ? O1 Mn5 Mn2 39.47(5) . . ? O6 Mn5 Mn2 141.43(6) 2_765 . ? O5 Mn5 Mn2 89.98(6) 2_765 . ? O7 Mn5 Mn2 134.65(6) . . ? Mn2 Mn5 Mn2 65.360(15) 2_765 . ? Mn5 O1 Mn3 125.05(10) . . ? Mn5 O1 Mn2 102.52(8) . . ? Mn3 O1 Mn2 123.48(9) . . ? Mn5 O2 Mn2 97.93(8) 2_765 . ? Mn5 O2 Mn1 116.06(8) 2_765 . ? Mn2 O2 Mn1 122.67(9) . . ? Mn5 O2 Mn2 93.07(7) 2_765 2_765 ? Mn2 O2 Mn2 96.73(7) . 2_765 ? Mn1 O2 Mn2 123.86(8) . 2_765 ? Mn5 O3 Mn2 96.64(8) 2_765 . ? Mn5 O3 Mn4 125.49(9) 2_765 . ? Mn2 O3 Mn4 125.74(9) . . ? Mn3 O4 Mn4 110.20(9) . 2_765 ? Mn3 O4 Mn1 121.52(9) . . ? Mn4 O4 Mn1 119.07(9) 2_765 . ? N2 O5 Mn5 114.82(15) . 2_765 ? N5 O6 Mn5 114.65(15) . 2_765 ? C15 O7 Mn5 126.38(17) . . ? C15 O8 Mn4 132.82(18) . 2_765 ? C15 O8 Mn3 107.95(17) . . ? Mn4 O8 Mn3 81.88(6) 2_765 . ? C22 O9 Mn2 131.08(18) . . ? C22 O10 Mn4 130.57(18) . . ? C36 O11 Mn2 130.82(18) . . ? C36 O13 Mn3 133.44(18) . . ? C1 N1 C5 118.6(2) . . ? C1 N1 Mn1 124.35(19) . . ? C5 N1 Mn1 116.91(18) . . ? C6 N2 O5 117.3(2) . . ? C6 N2 Mn1 117.95(18) . . ? O5 N2 Mn1 124.31(16) . . ? C8 N4 C12 118.6(2) . . ? C8 N4 Mn1 124.36(18) . . ? C12 N4 Mn1 116.74(17) . . ? C13 N5 O6 117.2(2) . . ? C13 N5 Mn1 118.36(18) . . ? O6 N5 Mn1 124.40(15) . . ? C30 N7 C32 119.8(3) . . ? C30 N7 Mn4 112.1(2) . . ? C32 N7 Mn4 127.6(2) . . ? C29 N8 Mn4 118.0(2) . . ? C44 N9 C46 119.4(2) . . ? C44 N9 Mn3 112.96(19) . . ? C46 N9 Mn3 127.6(2) . . ? C43 N10 Mn3 118.76(18) . . ? N1 C1 C2 121.8(3) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 119.2(3) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 115.4(2) . . ? C4 C5 C6 123.3(3) . . ? N2 C6 C7 121.3(2) . . ? N2 C6 C5 118.3(2) . . ? C7 C6 C5 120.4(2) . . ? N3 C7 C6 178.1(3) . . ? N4 C8 C9 121.6(3) . . ? N4 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 119.4(3) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N4 C12 C11 121.3(2) . . ? N4 C12 C13 115.3(2) . . ? C11 C12 C13 123.2(2) . . ? N5 C13 C14 119.8(2) . . ? N5 C13 C12 118.4(2) . . ? C14 C13 C12 121.6(2) . . ? N6 C14 C13 177.4(3) . . ? O8 C15 O7 124.0(2) . . ? O8 C15 C16 118.9(3) . . ? O7 C15 C16 117.1(3) . . ? C17 C16 C21 119.5(3) . . ? C17 C16 C15 121.3(3) . . ? C21 C16 C15 119.2(3) . . ? C16 C17 C18 119.6(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 120.4(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.4(6) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 120.0(5) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C16 120.1(4) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? O10 C22 O9 124.8(3) . . ? O10 C22 C23 119.5(3) . . ? O9 C22 C23 115.8(2) . . ? C28 C23 C24 119.5(3) . . ? C28 C23 C22 119.4(3) . . ? C24 C23 C22 121.0(3) . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.9(4) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 120.9(5) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C23 C28 C27 119.5(4) . . ? C23 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? O12 C29 N8 125.0(3) . . ? O12 C29 C30 120.3(3) . . ? N8 C29 C30 114.6(3) . . ? N7 C30 C35 120.5(4) . . ? N7 C30 C29 113.7(3) . . ? C35 C30 C29 125.7(4) . . ? N7 C32 C33 120.8(3) . . ? N7 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 119.5(4) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 119.6(4) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C30 C35 C34 119.8(4) . . ? C30 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? O11 C36 O13 125.5(2) . . ? O11 C36 C37 118.0(2) . . ? O13 C36 C37 116.5(2) . . ? C38 C37 C42 119.9(3) . . ? C38 C37 C36 119.8(3) . . ? C42 C37 C36 120.3(3) . . ? C39 C38 C37 120.0(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 120.1(3) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 120.3(3) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 119.8(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C37 119.7(3) . . ? C41 C42 H42 120.1 . . ? C37 C42 H42 120.1 . . ? O14 C43 N10 124.8(3) . . ? O14 C43 C44 120.8(3) . . ? N10 C43 C44 114.5(2) . . ? N9 C44 C49 121.1(3) . . ? N9 C44 C43 113.7(3) . . ? C49 C44 C43 125.2(3) . . ? N9 C46 C47 120.6(3) . . ? N9 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C48 C47 C46 120.0(3) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 119.3(3) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? C44 C49 C48 119.6(3) . . ? C44 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? N1W C2W C1W 171.9(9) . . ? N2W C4W C3W 178.5(5) . . ? N3W C6W C5W 179.1(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.364 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.090 _database_code_depnum_ccdc_archive 'CCDC 916866' ####################################################################### # # 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_af28laz1na _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H42 Mn10 N27 O22, C4 H12 N, 6(C H4 O)' _chemical_formula_sum 'C61 H78 Mn10 N28 O28' _chemical_formula_weight 2200.91 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 13.4205(11) _cell_length_b 14.6915(10) _cell_length_c 23.2200(19) _cell_angle_alpha 78.504(4) _cell_angle_beta 81.110(4) _cell_angle_gamma 80.152(3) _cell_volume 4385.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1928 _cell_measurement_theta_min 2.335 _cell_measurement_theta_max 25.86 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2228 _exptl_absorpt_coefficient_mu 1.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 KappaAPEXII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15918 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 25.35 _reflns_number_total 15918 _reflns_number_gt 11191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER APEX2' _computing_cell_refinement 'BRUKER APEX2' _computing_data_reduction 'BRUKER APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. The displacement parameters of some lengths in the direction of the bond are restrained to be equal within an effective standard deviation (DELU sentences) The distance of methanol are restrained (DFIX sentences) ; _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^)+(0.0348P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15918 _refine_ls_number_parameters 1143 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.981 _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 0.90980(4) 0.20399(3) 0.24093(2) 0.01240(12) Uani 1 1 d . . . Mn2 Mn 1.14330(4) 0.15239(3) 0.23221(2) 0.01553(12) Uani 1 1 d . . . Mn3 Mn 1.05311(4) 0.29331(3) 0.13763(2) 0.01342(12) Uani 1 1 d . . . Mn4 Mn 0.91447(4) 0.15854(3) 0.12686(2) 0.01395(12) Uani 1 1 d . . . Mn5 Mn 0.99756(4) 0.06781(3) 0.33193(2) 0.01615(12) Uani 1 1 d . . . Mn6 Mn 1.04805(4) 0.34138(3) 0.25604(2) 0.01470(12) Uani 1 1 d . . . Mn7 Mn 0.81693(4) 0.38625(3) 0.26132(2) 0.01373(12) Uani 1 1 d . . . Mn8 Mn 0.66422(4) 0.21226(3) 0.19611(2) 0.01559(12) Uani 1 1 d . . . Mn9 Mn 0.70036(4) 0.19921(3) 0.35234(2) 0.01533(12) Uani 1 1 d . . . Mn10 Mn 0.79314(4) -0.00301(3) 0.27924(2) 0.01680(13) Uani 1 1 d . . . O1 O 1.02302(16) 0.18917(14) 0.28836(9) 0.0150(5) Uani 1 1 d . . . O2 O 1.01369(15) 0.16995(13) 0.17603(9) 0.0123(5) Uani 1 1 d . . . O3 O 0.82328(15) 0.19910(13) 0.18786(9) 0.0133(5) Uani 1 1 d . . . O4 O 0.93478(15) 0.33471(13) 0.21231(9) 0.0134(5) Uani 1 1 d . . . O5 O 1.13550(16) 0.28028(14) 0.19844(9) 0.0144(5) Uani 1 1 d . . . O6 O 0.80898(16) 0.26085(13) 0.29074(9) 0.0140(5) Uani 1 1 d . . . O7 O 0.89645(16) 0.08519(14) 0.28276(10) 0.0154(5) Uani 1 1 d . . . O8 O 0.65251(16) 0.36220(14) 0.17152(10) 0.0199(6) Uani 1 1 d . . . O9 O 0.81125(16) 0.17268(15) 0.07397(10) 0.0181(5) Uani 1 1 d . . . O10 O 0.70580(16) 0.42710(14) 0.32086(10) 0.0184(5) Uani 1 1 d . . . O11 O 0.98386(18) -0.06406(14) 0.36019(10) 0.0217(6) Uani 1 1 d . . . O12 O 0.79868(17) 0.15812(15) 0.41850(10) 0.0213(6) Uani 1 1 d . . . O13 O 0.88871(17) -0.05800(14) 0.20753(10) 0.0209(6) Uani 1 1 d . . . O14 O 1.07690(17) 0.42194(14) 0.10861(10) 0.0175(5) Uani 1 1 d . . . O15 O 1.08044(16) 0.46993(14) 0.19474(10) 0.0179(5) Uani 1 1 d . . . O16 O 1.15513(16) 0.32481(15) 0.30722(10) 0.0191(5) Uani 1 1 d U . . O17 O 1.23929(17) 0.18419(15) 0.29015(10) 0.0215(6) Uani 1 1 d . . . O18 O 1.18740(16) 0.21892(14) 0.09003(10) 0.0179(5) Uani 1 1 d . . . O19 O 1.24285(17) 0.11538(15) 0.16735(11) 0.0207(6) Uani 1 1 d . . . O20 O 1.13448(16) 0.02912(14) 0.27226(10) 0.0178(5) Uani 1 1 d . . . O21 O 0.96384(16) 0.29417(14) 0.08303(9) 0.0153(5) Uani 1 1 d . . . O22 O 0.94524(16) 0.39929(14) 0.30702(10) 0.0183(5) Uani 1 1 d . . . N1 N 0.8129(2) 0.53034(18) 0.22362(12) 0.0192(7) Uani 1 1 d . . . N2 N 0.7015(2) 0.41612(18) 0.19161(12) 0.0165(6) Uani 1 1 d . . . N3 N 0.5545(3) 0.5678(2) 0.09515(17) 0.0536(11) Uani 1 1 d . . . N4 N 0.5247(2) 0.24599(18) 0.14459(13) 0.0196(7) Uani 1 1 d . . . N5 N 0.7162(2) 0.20270(18) 0.09707(12) 0.0176(7) Uani 1 1 d . . . N6 N 0.7042(2) 0.2637(2) -0.05350(15) 0.0392(9) Uani 1 1 d . . . N7 N 0.5715(2) 0.22055(18) 0.42820(12) 0.0200(7) Uani 1 1 d . . . N8 N 0.6618(2) 0.35886(17) 0.35815(12) 0.0160(6) Uani 1 1 d . . . N9 N 0.5062(3) 0.5572(2) 0.39359(17) 0.0501(11) Uani 1 1 d . . . N10 N 0.7479(2) -0.15079(18) 0.30979(13) 0.0210(7) Uani 1 1 d . . . N11 N 0.9045(2) -0.09306(18) 0.34537(12) 0.0178(7) Uani 1 1 d . . . N12 N 1.0635(3) -0.3063(2) 0.37611(19) 0.0570(12) Uani 1 1 d . . . N13 N 1.0968(2) 0.05932(18) 0.39691(12) 0.0190(7) Uani 1 1 d . . . N14 N 0.8959(2) 0.12674(17) 0.41027(12) 0.0174(7) Uani 1 1 d . . . N15 N 0.8549(3) 0.1901(2) 0.54675(15) 0.0390(9) Uani 1 1 d . . . N16 N 1.0191(2) 0.10014(17) 0.06195(12) 0.0162(6) Uani 1 1 d . . . N17 N 0.9292(2) -0.00466(17) 0.16010(13) 0.0169(6) Uani 1 1 d . . . N18 N 1.0658(2) -0.2232(2) 0.15700(15) 0.0368(9) Uani 1 1 d . . . N19 N 0.5866(2) 0.23596(18) 0.28443(12) 0.0183(6) Uani 1 1 d U . . N20 N 0.5257(2) 0.30639(19) 0.28489(12) 0.0194(7) Uani 1 1 d U . . N21 N 0.4665(2) 0.3738(2) 0.28575(14) 0.0313(8) Uani 1 1 d . . . N22 N 0.6843(2) 0.05222(18) 0.35197(12) 0.0193(7) Uani 1 1 d . . . N23 N 0.6001(2) 0.03059(18) 0.36049(13) 0.0222(7) Uani 1 1 d . . . N24 N 0.5189(3) 0.0101(2) 0.36863(15) 0.0380(9) Uani 1 1 d . . . N25 N 0.6750(2) 0.05649(18) 0.21970(13) 0.0200(7) Uani 1 1 d . . . N26 N 0.6696(2) 0.01421(19) 0.18092(14) 0.0237(7) Uani 1 1 d . . . N27 N 0.6640(3) -0.0259(2) 0.14392(15) 0.0367(9) Uani 1 1 d . . . C1 C 0.8732(3) 0.5862(2) 0.23646(16) 0.0213(8) Uani 1 1 d . . . H1 H 0.9237 0.5591 0.2604 0.026 Uiso 1 1 calc R . . C2 C 0.8635(3) 0.6809(2) 0.21590(16) 0.0294(9) Uani 1 1 d . . . H2 H 0.9080 0.7170 0.2245 0.035 Uiso 1 1 calc R . . C3 C 0.7860(3) 0.7213(2) 0.18208(17) 0.0369(11) Uani 1 1 d . . . H3 H 0.7762 0.7858 0.1687 0.044 Uiso 1 1 calc R . . C4 C 0.7237(3) 0.6664(2) 0.16823(16) 0.0328(10) Uani 1 1 d . . . H4 H 0.6714 0.6932 0.1455 0.039 Uiso 1 1 calc R . . C5 C 0.7395(3) 0.5701(2) 0.18860(15) 0.0224(8) Uani 1 1 d . . . C6 C 0.6822(3) 0.5057(2) 0.17089(15) 0.0206(8) Uani 1 1 d . . . C7 C 0.6105(3) 0.5396(2) 0.12904(18) 0.0296(10) Uani 1 1 d . . . C8 C 0.4297(2) 0.2724(2) 0.16921(16) 0.0217(8) Uani 1 1 d . . . H8 H 0.4135 0.2546 0.2099 0.026 Uiso 1 1 calc R . . C9 C 0.3547(3) 0.3252(2) 0.13667(17) 0.0277(9) Uani 1 1 d . . . H9 H 0.2895 0.3418 0.1552 0.033 Uiso 1 1 calc R . . C10 C 0.3780(3) 0.3527(2) 0.07661(18) 0.0290(9) Uani 1 1 d . . . H10 H 0.3291 0.3894 0.0543 0.035 Uiso 1 1 calc R . . C11 C 0.4754(3) 0.3250(2) 0.04955(17) 0.0243(9) Uani 1 1 d . . . H11 H 0.4926 0.3415 0.0089 0.029 Uiso 1 1 calc R . . C12 C 0.5459(2) 0.2721(2) 0.08520(16) 0.0189(8) Uani 1 1 d . . . C13 C 0.6516(3) 0.2405(2) 0.06048(15) 0.0184(8) Uani 1 1 d . . . C14 C 0.6808(3) 0.2529(2) -0.00320(18) 0.0263(9) Uani 1 1 d . . . C15 C 0.5306(3) 0.1520(2) 0.46586(16) 0.0251(9) Uani 1 1 d . . . H15 H 0.5591 0.0903 0.4634 0.030 Uiso 1 1 calc R . . C16 C 0.4486(3) 0.1667(3) 0.50817(17) 0.0321(10) Uani 1 1 d . . . H16 H 0.4219 0.1166 0.5333 0.038 Uiso 1 1 calc R . . C17 C 0.4074(3) 0.2580(3) 0.51208(17) 0.0345(10) Uani 1 1 d . . . H17 H 0.3520 0.2704 0.5402 0.041 Uiso 1 1 calc R . . C18 C 0.4476(3) 0.3301(2) 0.47493(17) 0.0283(9) Uani 1 1 d . . . H18 H 0.4195 0.3919 0.4773 0.034 Uiso 1 1 calc R . . C19 C 0.5310(3) 0.3108(2) 0.43337(16) 0.0206(8) Uani 1 1 d . . . C20 C 0.5823(3) 0.3833(2) 0.39250(15) 0.0192(8) Uani 1 1 d . . . C21 C 0.5402(3) 0.4809(3) 0.39256(17) 0.0299(9) Uani 1 1 d . . . C22 C 0.6635(3) -0.1764(2) 0.29893(17) 0.0262(9) Uani 1 1 d . . . H22 H 0.6171 -0.1315 0.2790 0.031 Uiso 1 1 calc R . . C23 C 0.6418(3) -0.2686(2) 0.31645(16) 0.0274(9) Uani 1 1 d . . . H23 H 0.5820 -0.2846 0.3082 0.033 Uiso 1 1 calc R . . C24 C 0.7102(3) -0.3350(3) 0.34593(17) 0.0301(9) Uani 1 1 d . . . H24 H 0.6976 -0.3967 0.3578 0.036 Uiso 1 1 calc R . . C25 C 0.7985(3) -0.3086(2) 0.35773(16) 0.0255(9) Uani 1 1 d . . . H25 H 0.8461 -0.3524 0.3775 0.031 Uiso 1 1 calc R . . C26 C 0.8144(3) -0.2161(2) 0.33966(15) 0.0212(8) Uani 1 1 d . . . C27 C 0.9052(3) -0.1833(2) 0.35240(16) 0.0225(8) Uani 1 1 d . . . C28 C 0.9939(3) -0.2499(3) 0.36717(19) 0.0374(11) Uani 1 1 d . . . C29 C 1.1963(3) 0.0238(2) 0.39119(16) 0.0226(8) Uani 1 1 d . . . H29 H 1.2249 0.0025 0.3563 0.027 Uiso 1 1 calc R . . C30 C 1.2586(3) 0.0172(2) 0.43472(17) 0.0256(9) Uani 1 1 d . . . H30 H 1.3276 -0.0060 0.4285 0.031 Uiso 1 1 calc R . . C31 C 1.2162(3) 0.0456(2) 0.48740(16) 0.0275(9) Uani 1 1 d . . . H31 H 1.2552 0.0393 0.5182 0.033 Uiso 1 1 calc R . . C32 C 1.1141(3) 0.0838(2) 0.49340(16) 0.0231(8) Uani 1 1 d . . . H32 H 1.0845 0.1054 0.5280 0.028 Uiso 1 1 calc R . . C33 C 1.0566(3) 0.0900(2) 0.44843(15) 0.0179(8) Uani 1 1 d . . . C34 C 0.9482(3) 0.1273(2) 0.45310(15) 0.0191(8) Uani 1 1 d . . . C35 C 0.8974(3) 0.1624(2) 0.50532(17) 0.0246(9) Uani 1 1 d . . . C36 C 1.0584(3) 0.1508(2) 0.01156(15) 0.0202(8) Uani 1 1 d . . . H36 H 1.0357 0.2149 0.0036 0.024 Uiso 1 1 calc R . . C37 C 1.1314(3) 0.1118(2) -0.02899(16) 0.0254(9) Uani 1 1 d . . . H37 H 1.1574 0.1491 -0.0634 0.030 Uiso 1 1 calc R . . C38 C 1.1647(3) 0.0171(2) -0.01748(16) 0.0244(9) Uani 1 1 d . . . H38 H 1.2142 -0.0106 -0.0440 0.029 Uiso 1 1 calc R . . C39 C 1.1244(3) -0.0367(2) 0.03352(16) 0.0229(9) Uani 1 1 d . . . H39 H 1.1459 -0.1010 0.0416 0.027 Uiso 1 1 calc R . . C40 C 1.0512(2) 0.0061(2) 0.07283(16) 0.0180(8) Uani 1 1 d . . . C41 C 1.0031(2) -0.0470(2) 0.12672(16) 0.0180(8) Uani 1 1 d . . . C42 C 1.0373(3) -0.1455(2) 0.14361(17) 0.0240(9) Uani 1 1 d . . . C43 C 1.0876(2) 0.4825(2) 0.13956(16) 0.0177(8) Uani 1 1 d . . . C44 C 1.1107(3) 0.5745(2) 0.10386(17) 0.0344(10) Uani 1 1 d . . . H44A H 1.0918 0.5811 0.0649 0.052 Uiso 1 1 calc R . . H44B H 1.1823 0.5771 0.1011 0.052 Uiso 1 1 calc R . . H44C H 1.0729 0.6246 0.1227 0.052 Uiso 1 1 calc R . . C45 C 1.2243(3) 0.2528(2) 0.31614(15) 0.0205(8) Uani 1 1 d U . . C46 C 1.2891(3) 0.2523(2) 0.36364(16) 0.0288(9) Uani 1 1 d . . . H46A H 1.2870 0.3154 0.3698 0.043 Uiso 1 1 calc R . . H46B H 1.3581 0.2267 0.3516 0.043 Uiso 1 1 calc R . . H46C H 1.2635 0.2146 0.3998 0.043 Uiso 1 1 calc R . . C47 C 1.2498(3) 0.1526(2) 0.11252(16) 0.0196(8) Uani 1 1 d . . . C48 C 1.3384(3) 0.1105(2) 0.07360(17) 0.0312(10) Uani 1 1 d . . . H48A H 1.3857 0.0700 0.0978 0.047 Uiso 1 1 calc R . . H48B H 1.3717 0.1596 0.0486 0.047 Uiso 1 1 calc R . . H48C H 1.3143 0.0748 0.0495 0.047 Uiso 1 1 calc R . . C49 C 1.1467(3) -0.0519(2) 0.24569(16) 0.0262(9) Uani 1 1 d . . . H49A H 1.1388 -0.1061 0.2760 0.039 Uiso 1 1 calc R . . H49B H 1.2134 -0.0601 0.2238 0.039 Uiso 1 1 calc R . . H49C H 1.0962 -0.0443 0.2194 0.039 Uiso 1 1 calc R . . C50 C 0.8908(3) 0.3744(2) 0.06596(15) 0.0223(8) Uani 1 1 d . . . H50A H 0.8524 0.3612 0.0377 0.034 Uiso 1 1 calc R . . H50B H 0.9255 0.4271 0.0484 0.034 Uiso 1 1 calc R . . H50C H 0.8454 0.3887 0.1002 0.034 Uiso 1 1 calc R . . C51 C 0.9393(3) 0.3817(3) 0.36960(17) 0.0407(11) Uani 1 1 d . . . H51A H 0.8803 0.4197 0.3858 0.061 Uiso 1 1 calc R . . H51B H 0.9994 0.3970 0.3810 0.061 Uiso 1 1 calc R . . H51C H 0.9343 0.3166 0.3844 0.061 Uiso 1 1 calc R . . N28 N 0.3136(3) 0.6025(2) 0.24678(16) 0.0419(9) Uani 1 1 d . . . C52 C 0.2545(4) 0.5414(3) 0.2936(3) 0.106(3) Uani 1 1 d . . . H52A H 0.1917 0.5363 0.2803 0.159 Uiso 1 1 calc R . . H52B H 0.2399 0.5683 0.3290 0.159 Uiso 1 1 calc R . . H52C H 0.2936 0.4802 0.3018 0.159 Uiso 1 1 calc R . . C53 C 0.4095(4) 0.6115(3) 0.2654(3) 0.103(3) Uani 1 1 d . . . H53A H 0.3961 0.6400 0.3001 0.155 Uiso 1 1 calc R . . H53B H 0.4472 0.6499 0.2341 0.155 Uiso 1 1 calc R . . H53C H 0.4487 0.5504 0.2743 0.155 Uiso 1 1 calc R . . C54 C 0.3359(5) 0.5596(4) 0.1935(3) 0.116(3) Uani 1 1 d . . . H54A H 0.2733 0.5528 0.1808 0.173 Uiso 1 1 calc R . . H54B H 0.3760 0.4989 0.2022 0.173 Uiso 1 1 calc R . . H54C H 0.3732 0.5989 0.1626 0.173 Uiso 1 1 calc R . . C55 C 0.2526(4) 0.6980(3) 0.2334(3) 0.087(2) Uani 1 1 d . . . H55A H 0.1891 0.6924 0.2211 0.130 Uiso 1 1 calc R . . H55B H 0.2901 0.7366 0.2022 0.130 Uiso 1 1 calc R . . H55C H 0.2394 0.7262 0.2682 0.130 Uiso 1 1 calc R . . O1W O 0.0925(3) 0.4474(3) 0.51333(19) 0.0915(13) Uani 1 1 d D . . C1W C 0.1111(5) 0.3690(4) 0.4846(3) 0.093(2) Uani 1 1 d D . . O2W O 0.6797(3) 0.1988(2) 0.64272(16) 0.0760(11) Uani 1 1 d D . . H2OW H 0.7097 0.2448 0.6352 0.091 Uiso 1 1 calc R . . C2W C 0.6118(3) 0.2074(3) 0.6021(2) 0.0569(14) Uani 1 1 d D . . H2AW H 0.5617 0.1665 0.6177 0.068 Uiso 1 1 calc R . . H2BW H 0.6480 0.1907 0.5658 0.068 Uiso 1 1 calc R . . H2CW H 0.5786 0.2711 0.5946 0.068 Uiso 1 1 calc R . . O4W O 0.4315(2) 0.8784(2) 0.25193(15) 0.0701(10) Uani 1 1 d D . . C4W C 0.4187(3) 0.9805(3) 0.2449(2) 0.0490(12) Uani 1 1 d D . . O5W O 0.4801(4) 0.7837(3) 0.1595(2) 0.1354(18) Uani 1 1 d D . . C5W C 0.4996(5) 0.8334(4) 0.0982(3) 0.0788(13) Uani 1 1 d D . . O6W O 0.2834(5) 0.5040(5) 0.5267(3) 0.105(2) Uani 0.638(5) 1 d PD . . O6W' O 0.2285(9) 0.5635(8) 0.4587(5) 0.105(2) Uani 0.362(5) 1 d PD . . C6W C 0.2819(5) 0.5929(4) 0.4974(3) 0.0788(13) Uani 1 1 d D . . C7W C 0.8322(3) 0.6123(2) 0.03432(18) 0.0393(11) Uani 1 1 d D . . H7AW H 0.7894 0.5641 0.0416 0.047 Uiso 1 1 calc R . . H7BW H 0.8720 0.6037 0.0665 0.047 Uiso 1 1 calc R . . H7CW H 0.8769 0.6086 -0.0019 0.047 Uiso 1 1 calc R . . O7W O 0.7716(2) 0.70028(17) 0.02974(12) 0.0438(8) Uani 1 1 d D . . H7OW H 0.7861 0.7315 -0.0030 0.053 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 0.0114(3) 0.0122(2) 0.0140(3) -0.0058(2) -0.0012(2) 0.0011(2) Mn2 0.0130(3) 0.0163(3) 0.0168(3) -0.0060(2) -0.0014(2) 0.0025(2) Mn3 0.0132(3) 0.0134(2) 0.0146(3) -0.0067(2) -0.0012(2) 0.0002(2) Mn4 0.0121(3) 0.0156(3) 0.0158(3) -0.0093(2) -0.0014(2) 0.0009(2) Mn5 0.0163(3) 0.0157(3) 0.0158(3) -0.0039(2) -0.0030(2) 0.0017(2) Mn6 0.0127(3) 0.0178(3) 0.0152(3) -0.0088(2) -0.0011(2) -0.0005(2) Mn7 0.0139(3) 0.0115(2) 0.0159(3) -0.0070(2) -0.0001(2) 0.0015(2) Mn8 0.0130(3) 0.0177(3) 0.0168(3) -0.0078(2) -0.0017(2) 0.0012(2) Mn9 0.0149(3) 0.0140(3) 0.0163(3) -0.0053(2) 0.0005(2) 0.0009(2) Mn10 0.0156(3) 0.0139(3) 0.0208(3) -0.0059(2) -0.0004(2) -0.0001(2) O1 0.0159(13) 0.0163(12) 0.0141(13) -0.0067(10) -0.0011(10) -0.0016(10) O2 0.0112(12) 0.0135(11) 0.0127(13) -0.0054(9) -0.0004(10) -0.0002(9) O3 0.0085(12) 0.0161(11) 0.0166(13) -0.0078(10) -0.0020(10) 0.0007(9) O4 0.0129(12) 0.0114(11) 0.0154(13) -0.0047(10) 0.0007(10) -0.0003(9) O5 0.0123(12) 0.0162(11) 0.0153(13) -0.0057(10) -0.0030(10) 0.0007(9) O6 0.0144(13) 0.0116(11) 0.0142(13) -0.0033(9) 0.0015(10) 0.0011(9) O7 0.0155(13) 0.0145(11) 0.0161(13) -0.0044(10) -0.0008(10) -0.0007(9) O8 0.0163(13) 0.0197(12) 0.0257(15) -0.0090(11) -0.0046(11) -0.0004(10) O9 0.0098(13) 0.0269(13) 0.0198(14) -0.0146(11) -0.0018(10) 0.0033(10) O10 0.0173(13) 0.0163(12) 0.0207(14) -0.0081(11) 0.0035(11) 0.0005(10) O11 0.0252(14) 0.0193(12) 0.0211(15) -0.0004(11) -0.0068(11) -0.0044(11) O12 0.0167(14) 0.0266(13) 0.0188(14) -0.0041(11) -0.0020(11) 0.0021(11) O13 0.0241(14) 0.0157(12) 0.0214(15) -0.0056(11) 0.0046(11) -0.0030(10) O14 0.0270(14) 0.0146(11) 0.0130(13) -0.0060(10) -0.0015(11) -0.0054(10) O15 0.0186(14) 0.0199(12) 0.0175(15) -0.0102(11) 0.0010(11) -0.0036(10) O16 0.0163(13) 0.0250(12) 0.0187(14) -0.0103(11) -0.0035(11) -0.0020(9) O17 0.0190(14) 0.0264(13) 0.0208(15) -0.0098(11) -0.0038(11) -0.0001(11) O18 0.0150(13) 0.0193(12) 0.0195(14) -0.0082(10) 0.0003(11) 0.0003(10) O19 0.0195(14) 0.0205(12) 0.0204(15) -0.0062(11) 0.0005(11) 0.0024(10) O20 0.0209(13) 0.0131(11) 0.0169(14) -0.0031(10) -0.0003(11) 0.0028(10) O21 0.0156(13) 0.0150(11) 0.0154(13) -0.0054(10) -0.0037(10) 0.0021(10) O22 0.0191(13) 0.0218(12) 0.0159(14) -0.0127(10) 0.0000(11) 0.0009(10) N1 0.0191(17) 0.0183(15) 0.0186(17) -0.0092(13) 0.0071(13) 0.0005(13) N2 0.0115(15) 0.0180(15) 0.0187(17) -0.0049(13) 0.0019(13) -0.0003(12) N3 0.073(3) 0.041(2) 0.051(3) 0.0036(19) -0.036(2) -0.008(2) N4 0.0165(17) 0.0268(16) 0.0178(18) -0.0079(13) -0.0025(13) -0.0044(13) N5 0.0156(16) 0.0192(15) 0.0201(17) -0.0109(13) -0.0015(14) -0.0007(12) N6 0.031(2) 0.060(2) 0.024(2) -0.0078(18) -0.0061(17) 0.0043(17) N7 0.0227(17) 0.0195(15) 0.0178(17) -0.0059(13) -0.0012(14) -0.0011(13) N8 0.0160(16) 0.0183(15) 0.0148(17) -0.0067(13) -0.0010(13) -0.0023(12) N9 0.051(2) 0.0203(18) 0.068(3) -0.0132(18) 0.029(2) 0.0003(17) N10 0.0191(17) 0.0192(15) 0.0253(19) -0.0105(13) 0.0021(14) -0.0011(13) N11 0.0165(16) 0.0218(16) 0.0136(17) -0.0050(13) 0.0016(13) 0.0001(13) N12 0.054(3) 0.035(2) 0.084(3) -0.013(2) -0.027(2) 0.007(2) N13 0.0176(17) 0.0180(15) 0.0192(18) 0.0010(13) -0.0051(13) 0.0011(13) N14 0.0184(17) 0.0163(15) 0.0162(17) -0.0013(12) -0.0036(13) 0.0002(12) N15 0.038(2) 0.053(2) 0.029(2) -0.0194(18) -0.0095(18) 0.0047(17) N16 0.0159(16) 0.0175(14) 0.0177(17) -0.0081(13) -0.0004(13) -0.0046(12) N17 0.0148(16) 0.0166(14) 0.0214(18) -0.0101(13) -0.0028(13) 0.0004(12) N18 0.034(2) 0.0233(18) 0.050(2) -0.0127(16) 0.0055(17) 0.0022(15) N19 0.0145(16) 0.0207(14) 0.0207(17) -0.0092(13) -0.0005(13) -0.0002(10) N20 0.0155(16) 0.0232(14) 0.0200(17) -0.0087(13) -0.0004(13) -0.0004(11) N21 0.0267(19) 0.0304(18) 0.036(2) -0.0173(16) -0.0061(16) 0.0126(15) N22 0.0191(17) 0.0203(15) 0.0190(18) -0.0087(13) 0.0004(14) -0.0002(13) N23 0.027(2) 0.0171(16) 0.0221(19) -0.0073(13) 0.0047(15) -0.0041(14) N24 0.031(2) 0.039(2) 0.045(2) -0.0141(17) 0.0117(18) -0.0152(17) N25 0.0202(17) 0.0183(15) 0.0225(18) -0.0091(14) -0.0003(14) -0.0016(12) N26 0.0221(18) 0.0232(16) 0.026(2) -0.0084(15) 0.0001(15) -0.0020(13) N27 0.048(2) 0.039(2) 0.029(2) -0.0182(17) 0.0019(17) -0.0145(17) C1 0.021(2) 0.0200(18) 0.024(2) -0.0119(16) 0.0079(16) -0.0064(16) C2 0.042(3) 0.025(2) 0.022(2) -0.0106(17) 0.0143(19) -0.0166(18) C3 0.072(3) 0.0159(19) 0.018(2) 0.0001(17) 0.007(2) -0.009(2) C4 0.059(3) 0.0152(19) 0.021(2) -0.0013(17) -0.004(2) -0.0001(19) C5 0.032(2) 0.0214(19) 0.011(2) -0.0056(16) 0.0007(17) 0.0042(17) C6 0.025(2) 0.0193(19) 0.016(2) -0.0069(16) -0.0027(16) 0.0041(16) C7 0.044(3) 0.0168(19) 0.028(3) -0.0011(17) -0.013(2) 0.0006(18) C8 0.013(2) 0.030(2) 0.026(2) -0.0115(17) -0.0014(17) -0.0067(16) C9 0.011(2) 0.039(2) 0.037(3) -0.017(2) -0.0038(18) -0.0005(17) C10 0.014(2) 0.032(2) 0.041(3) -0.0064(19) -0.0121(19) 0.0016(17) C11 0.022(2) 0.030(2) 0.022(2) -0.0012(17) -0.0089(17) -0.0024(17) C12 0.0133(19) 0.0191(18) 0.026(2) -0.0075(16) -0.0025(16) -0.0025(15) C13 0.018(2) 0.0207(18) 0.017(2) -0.0063(16) -0.0031(16) -0.0023(15) C14 0.017(2) 0.033(2) 0.028(3) -0.0087(19) -0.0062(18) 0.0055(17) C15 0.030(2) 0.0214(19) 0.022(2) -0.0014(17) 0.0003(18) -0.0058(17) C16 0.037(3) 0.031(2) 0.026(2) -0.0015(18) 0.0043(19) -0.0116(19) C17 0.031(2) 0.043(2) 0.027(2) -0.014(2) 0.0164(19) -0.008(2) C18 0.028(2) 0.025(2) 0.033(3) -0.0155(18) 0.0057(19) -0.0018(17) C19 0.021(2) 0.0234(19) 0.021(2) -0.0100(16) -0.0067(17) -0.0007(16) C20 0.019(2) 0.0208(18) 0.021(2) -0.0156(16) 0.0003(16) 0.0019(15) C21 0.026(2) 0.026(2) 0.035(3) -0.0080(18) 0.0123(18) -0.0051(18) C22 0.023(2) 0.026(2) 0.030(2) -0.0127(17) 0.0003(18) 0.0014(17) C23 0.027(2) 0.026(2) 0.031(2) -0.0091(18) 0.0066(18) -0.0108(17) C24 0.031(2) 0.026(2) 0.033(3) -0.0105(18) 0.0103(19) -0.0068(18) C25 0.034(2) 0.0176(19) 0.023(2) -0.0047(16) 0.0003(18) -0.0004(17) C26 0.021(2) 0.0216(19) 0.019(2) -0.0073(16) 0.0031(16) 0.0017(16) C27 0.028(2) 0.0141(18) 0.024(2) -0.0018(16) -0.0065(17) 0.0021(16) C28 0.040(3) 0.026(2) 0.048(3) -0.008(2) -0.014(2) 0.000(2) C29 0.025(2) 0.0208(19) 0.020(2) -0.0052(16) -0.0044(17) 0.0049(16) C30 0.016(2) 0.029(2) 0.030(2) -0.0001(18) -0.0071(18) -0.0009(16) C31 0.035(2) 0.031(2) 0.017(2) 0.0020(17) -0.0081(18) -0.0087(18) C32 0.027(2) 0.0240(19) 0.018(2) -0.0030(16) -0.0032(17) -0.0040(17) C33 0.023(2) 0.0155(17) 0.015(2) -0.0033(15) -0.0009(16) -0.0029(15) C34 0.024(2) 0.0154(18) 0.017(2) -0.0018(15) -0.0023(16) -0.0022(15) C35 0.025(2) 0.031(2) 0.018(2) -0.0070(18) -0.0072(18) 0.0018(17) C36 0.019(2) 0.0249(19) 0.020(2) -0.0104(17) -0.0033(16) -0.0040(16) C37 0.025(2) 0.037(2) 0.020(2) -0.0140(18) 0.0025(17) -0.0140(18) C38 0.018(2) 0.034(2) 0.027(2) -0.0232(18) 0.0047(17) -0.0038(17) C39 0.016(2) 0.0235(19) 0.033(2) -0.0190(18) 0.0010(17) 0.0001(16) C40 0.0130(19) 0.0187(18) 0.027(2) -0.0137(16) -0.0060(16) -0.0011(15) C41 0.0157(19) 0.0166(17) 0.026(2) -0.0147(16) -0.0035(16) -0.0009(15) C42 0.019(2) 0.021(2) 0.032(2) -0.0124(17) 0.0032(17) -0.0023(16) C43 0.0144(19) 0.0159(17) 0.023(2) -0.0071(16) -0.0019(16) -0.0005(14) C44 0.057(3) 0.021(2) 0.029(3) -0.0071(18) -0.004(2) -0.0136(19) C45 0.0153(19) 0.0286(18) 0.017(2) -0.0029(17) -0.0019(16) -0.0038(12) C46 0.027(2) 0.031(2) 0.031(2) -0.0052(18) -0.0139(19) -0.0033(17) C47 0.019(2) 0.0176(18) 0.023(2) -0.0094(17) 0.0045(17) -0.0051(16) C48 0.033(2) 0.029(2) 0.028(2) -0.0118(18) 0.0055(19) 0.0044(18) C49 0.027(2) 0.0209(19) 0.030(2) -0.0098(17) -0.0009(18) 0.0029(16) C50 0.023(2) 0.0255(19) 0.015(2) 0.0018(16) -0.0067(16) 0.0024(16) C51 0.028(2) 0.071(3) 0.026(3) -0.027(2) -0.0047(19) 0.008(2) N28 0.037(2) 0.037(2) 0.048(3) -0.0061(18) -0.0111(19) 0.0076(17) C52 0.082(5) 0.040(3) 0.155(7) 0.013(4) 0.049(4) 0.012(3) C53 0.077(4) 0.054(3) 0.202(8) -0.032(4) -0.084(5) -0.003(3) C54 0.140(7) 0.128(6) 0.074(5) -0.042(4) -0.049(5) 0.056(5) C55 0.063(4) 0.056(3) 0.117(6) 0.012(3) -0.021(4) 0.035(3) O1W 0.079(3) 0.091(3) 0.113(4) -0.052(3) 0.004(3) -0.011(2) C1W 0.084(5) 0.127(5) 0.082(5) -0.065(4) -0.038(4) 0.028(4) O2W 0.077(3) 0.084(3) 0.070(3) -0.018(2) -0.015(2) -0.007(2) C2W 0.053(3) 0.041(3) 0.066(4) -0.011(3) 0.009(3) 0.011(2) O4W 0.053(2) 0.085(3) 0.068(3) -0.006(2) -0.0118(19) 0.0015(19) C4W 0.032(3) 0.048(3) 0.059(3) 0.001(2) -0.010(2) 0.009(2) O5W 0.122(4) 0.133(4) 0.154(5) -0.048(4) 0.019(4) -0.034(3) C5W 0.103(4) 0.067(3) 0.066(3) -0.006(2) -0.011(3) -0.016(2) O6W 0.123(5) 0.110(5) 0.077(4) -0.017(4) -0.012(4) -0.006(4) O6W' 0.123(5) 0.110(5) 0.077(4) -0.017(4) -0.012(4) -0.006(4) C6W 0.103(4) 0.067(3) 0.066(3) -0.006(2) -0.011(3) -0.016(2) C7W 0.049(3) 0.040(2) 0.026(3) -0.005(2) 0.002(2) -0.007(2) O7W 0.068(2) 0.0264(15) 0.0288(18) -0.0059(13) 0.0096(15) 0.0040(14) _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 O3 1.838(2) . ? Mn1 O6 1.839(2) . ? Mn1 O7 1.844(2) . ? Mn1 O2 1.969(2) . ? Mn1 O1 1.969(2) . ? Mn1 O4 1.971(2) . ? Mn1 Mn4 2.8468(7) . ? Mn1 Mn7 2.8511(7) . ? Mn1 Mn5 2.8517(7) . ? Mn1 Mn3 3.0590(7) . ? Mn1 Mn6 3.0667(7) . ? Mn1 Mn2 3.0803(7) . ? Mn2 O20 1.878(2) . ? Mn2 O5 1.878(2) . ? Mn2 O19 1.950(2) . ? Mn2 O1 1.982(2) . ? Mn2 O17 2.163(2) . ? Mn2 O2 2.282(2) . ? Mn2 Mn3 2.9540(7) . ? Mn2 Mn6 2.9714(7) . ? Mn2 Mn5 3.0026(8) . ? Mn3 O21 1.871(2) . ? Mn3 O5 1.886(2) . ? Mn3 O14 1.939(2) . ? Mn3 O2 1.974(2) . ? Mn3 O18 2.204(2) . ? Mn3 O4 2.267(2) . ? Mn3 Mn6 2.9602(7) . ? Mn3 Mn4 3.0076(7) . ? Mn4 O3 1.847(2) . ? Mn4 O2 1.930(2) . ? Mn4 O9 1.948(2) . ? Mn4 N16 2.104(3) . ? Mn4 O21 2.209(2) . ? Mn4 N17 2.352(3) . ? Mn5 O7 1.858(2) . ? Mn5 O1 1.924(2) . ? Mn5 O11 1.948(2) . ? Mn5 N13 2.134(3) . ? Mn5 O20 2.188(2) . ? Mn5 N14 2.318(3) . ? Mn6 O22 1.877(2) . ? Mn6 O5 1.899(2) . ? Mn6 O16 1.957(2) . ? Mn6 O4 1.980(2) . ? Mn6 O15 2.191(2) . ? Mn6 O1 2.277(2) . ? Mn6 Mn7 3.0472(7) . ? Mn7 O6 1.848(2) . ? Mn7 O4 1.936(2) . ? Mn7 O10 1.971(2) . ? Mn7 N1 2.118(3) . ? Mn7 O22 2.211(2) . ? Mn7 N2 2.339(3) . ? Mn8 O3 2.092(2) . ? Mn8 O8 2.147(2) . ? Mn8 N19 2.216(3) . ? Mn8 N25 2.229(3) . ? Mn8 N4 2.307(3) . ? Mn8 N5 2.323(3) . ? Mn9 O6 2.069(2) . ? Mn9 O12 2.110(2) . ? Mn9 N22 2.208(3) . ? Mn9 N19 2.287(3) . ? Mn9 N7 2.299(3) . ? Mn9 N8 2.340(3) . ? Mn10 O7 2.074(2) . ? Mn10 O13 2.143(2) . ? Mn10 N25 2.216(3) . ? Mn10 N22 2.241(3) . ? Mn10 N10 2.300(3) . ? Mn10 N11 2.359(3) . ? O8 N2 1.303(3) . ? O9 N5 1.342(3) . ? O10 N8 1.343(3) . ? O11 N11 1.328(3) . ? O12 N14 1.306(3) . ? O13 N17 1.319(3) . ? O14 C43 1.288(4) . ? O15 C43 1.249(4) . ? O16 C45 1.288(4) . ? O17 C45 1.248(4) . ? O18 C47 1.255(4) . ? O19 C47 1.278(4) . ? O20 C49 1.421(4) . ? O21 C50 1.430(3) . ? O22 C51 1.417(4) . ? N1 C1 1.347(4) . ? N1 C5 1.354(4) . ? N2 C6 1.304(4) . ? N3 C7 1.141(4) . ? N4 C8 1.340(4) . ? N4 C12 1.355(4) . ? N5 C13 1.287(4) . ? N6 C14 1.148(5) . ? N7 C15 1.331(4) . ? N7 C19 1.366(4) . ? N8 C20 1.274(4) . ? N9 C21 1.140(4) . ? N10 C22 1.327(4) . ? N10 C26 1.353(4) . ? N11 C27 1.301(4) . ? N12 C28 1.154(5) . ? N13 C29 1.345(4) . ? N13 C33 1.363(4) . ? N14 C34 1.305(4) . ? N15 C35 1.150(4) . ? N16 C36 1.341(4) . ? N16 C40 1.360(4) . ? N17 C41 1.310(4) . ? N18 C42 1.136(4) . ? N19 N20 1.205(3) . ? N20 N21 1.160(3) . ? N22 N23 1.202(4) . ? N23 N24 1.158(4) . ? N25 N26 1.209(4) . ? N26 N27 1.153(4) . ? C1 C2 1.368(4) . ? C1 H1 0.9300 . ? C2 C3 1.380(5) . ? C2 H2 0.9300 . ? C3 C4 1.368(5) . ? C3 H3 0.9300 . ? C4 C5 1.389(4) . ? C4 H4 0.9300 . ? C5 C6 1.470(5) . ? C6 C7 1.432(5) . ? C8 C9 1.386(5) . ? C8 H8 0.9300 . ? C9 C10 1.375(5) . ? C9 H9 0.9300 . ? C10 C11 1.391(5) . ? C10 H10 0.9300 . ? C11 C12 1.386(4) . ? C11 H11 0.9300 . ? C12 C13 1.479(5) . ? C13 C14 1.453(5) . ? C15 C16 1.375(5) . ? C15 H15 0.9300 . ? C16 C17 1.375(5) . ? C16 H16 0.9300 . ? C17 C18 1.358(5) . ? C17 H17 0.9300 . ? C18 C19 1.390(5) . ? C18 H18 0.9300 . ? C19 C20 1.467(5) . ? C20 C21 1.448(5) . ? C22 C23 1.402(5) . ? C22 H22 0.9300 . ? C23 C24 1.373(5) . ? C23 H23 0.9300 . ? C24 C25 1.389(5) . ? C24 H24 0.9300 . ? C25 C26 1.383(4) . ? C25 H25 0.9300 . ? C26 C27 1.476(5) . ? C27 C28 1.444(5) . ? C29 C30 1.387(5) . ? C29 H29 0.9300 . ? C30 C31 1.379(5) . ? C30 H30 0.9300 . ? C31 C32 1.386(5) . ? C31 H31 0.9300 . ? C32 C33 1.372(4) . ? C32 H32 0.9300 . ? C33 C34 1.459(5) . ? C34 C35 1.440(5) . ? C36 C37 1.383(5) . ? C36 H36 0.9300 . ? C37 C38 1.372(5) . ? C37 H37 0.9300 . ? C38 C39 1.377(5) . ? C38 H38 0.9300 . ? C39 C40 1.391(5) . ? C39 H39 0.9300 . ? C40 C41 1.457(5) . ? C41 C42 1.436(4) . ? C43 C44 1.492(5) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.504(4) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.501(5) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? N28 C53 1.455(5) . ? N28 C54 1.466(6) . ? N28 C52 1.485(6) . ? N28 C55 1.499(5) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? O1W C1W 1.412(5) . ? O2W C2W 1.384(5) . ? O2W H2OW 0.8200 . ? C2W H2AW 0.9600 . ? C2W H2BW 0.9600 . ? C2W H2CW 0.9600 . ? O4W C4W 1.460(5) . ? O5W C5W 1.469(6) . ? O6W C6W 1.345(6) . ? O6W' C6W 1.403(8) . ? C7W O7W 1.399(4) . ? C7W H7AW 0.9600 . ? C7W H7BW 0.9600 . ? C7W H7CW 0.9600 . ? O7W H7OW 0.8200 . ? 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 O3 Mn1 O6 93.99(9) . . ? O3 Mn1 O7 94.07(9) . . ? O6 Mn1 O7 93.20(9) . . ? O3 Mn1 O2 81.97(9) . . ? O6 Mn1 O2 167.44(9) . . ? O7 Mn1 O2 98.93(9) . . ? O3 Mn1 O1 167.29(9) . . ? O6 Mn1 O1 98.29(9) . . ? O7 Mn1 O1 82.04(9) . . ? O2 Mn1 O1 86.68(9) . . ? O3 Mn1 O4 97.94(9) . . ? O6 Mn1 O4 81.81(9) . . ? O7 Mn1 O4 167.28(9) . . ? O2 Mn1 O4 86.96(9) . . ? O1 Mn1 O4 87.09(8) . . ? O3 Mn1 Mn4 39.52(7) . . ? O6 Mn1 Mn4 133.04(7) . . ? O7 Mn1 Mn4 95.93(7) . . ? O2 Mn1 Mn4 42.58(6) . . ? O1 Mn1 Mn4 128.57(7) . . ? O4 Mn1 Mn4 96.01(6) . . ? O3 Mn1 Mn7 93.91(6) . . ? O6 Mn1 Mn7 39.47(6) . . ? O7 Mn1 Mn7 132.44(7) . . ? O2 Mn1 Mn7 128.62(6) . . ? O1 Mn1 Mn7 97.64(6) . . ? O4 Mn1 Mn7 42.65(6) . . ? Mn4 Mn1 Mn7 118.80(2) . . ? O3 Mn1 Mn5 133.19(6) . . ? O6 Mn1 Mn5 95.80(7) . . ? O7 Mn1 Mn5 39.81(7) . . ? O2 Mn1 Mn5 95.60(6) . . ? O1 Mn1 Mn5 42.29(6) . . ? O4 Mn1 Mn5 128.74(6) . . ? Mn4 Mn1 Mn5 119.76(2) . . ? Mn7 Mn1 Mn5 121.44(2) . . ? O3 Mn1 Mn3 88.77(7) . . ? O6 Mn1 Mn3 129.28(7) . . ? O7 Mn1 Mn3 137.16(7) . . ? O2 Mn1 Mn3 39.19(6) . . ? O1 Mn1 Mn3 85.99(7) . . ? O4 Mn1 Mn3 47.77(6) . . ? Mn4 Mn1 Mn3 61.105(17) . . ? Mn7 Mn1 Mn3 89.809(19) . . ? Mn5 Mn1 Mn3 118.19(2) . . ? O3 Mn1 Mn6 136.26(7) . . ? O6 Mn1 Mn6 88.36(7) . . ? O7 Mn1 Mn6 129.45(7) . . ? O2 Mn1 Mn6 86.45(6) . . ? O1 Mn1 Mn6 47.91(6) . . ? O4 Mn1 Mn6 39.19(6) . . ? Mn4 Mn1 Mn6 118.90(2) . . ? Mn7 Mn1 Mn6 61.858(17) . . ? Mn5 Mn1 Mn6 89.737(19) . . ? Mn3 Mn1 Mn6 57.794(16) . . ? O3 Mn1 Mn2 129.41(7) . . ? O6 Mn1 Mn2 136.23(7) . . ? O7 Mn1 Mn2 89.47(7) . . ? O2 Mn1 Mn2 47.74(6) . . ? O1 Mn1 Mn2 38.94(6) . . ? O4 Mn1 Mn2 86.17(6) . . ? Mn4 Mn1 Mn2 89.898(19) . . ? Mn7 Mn1 Mn2 119.66(2) . . ? Mn5 Mn1 Mn2 60.673(17) . . ? Mn3 Mn1 Mn2 57.521(16) . . ? Mn6 Mn1 Mn2 57.813(16) . . ? O20 Mn2 O5 172.26(10) . . ? O20 Mn2 O19 94.92(9) . . ? O5 Mn2 O19 92.47(9) . . ? O20 Mn2 O1 85.57(9) . . ? O5 Mn2 O1 86.74(9) . . ? O19 Mn2 O1 169.27(9) . . ? O20 Mn2 O17 95.58(9) . . ? O5 Mn2 O17 85.10(9) . . ? O19 Mn2 O17 102.04(9) . . ? O1 Mn2 O17 88.56(9) . . ? O20 Mn2 O2 98.70(8) . . ? O5 Mn2 O2 78.84(8) . . ? O19 Mn2 O2 91.02(9) . . ? O1 Mn2 O2 78.32(8) . . ? O17 Mn2 O2 159.73(8) . . ? O20 Mn2 Mn3 140.37(7) . . ? O5 Mn2 Mn3 38.38(6) . . ? O19 Mn2 Mn3 84.07(7) . . ? O1 Mn2 Mn3 88.72(6) . . ? O17 Mn2 Mn3 123.48(6) . . ? O2 Mn2 Mn3 41.89(5) . . ? O20 Mn2 Mn6 134.36(7) . . ? O5 Mn2 Mn6 38.36(7) . . ? O19 Mn2 Mn6 130.70(7) . . ? O1 Mn2 Mn6 50.00(6) . . ? O17 Mn2 Mn6 76.09(6) . . ? O2 Mn2 Mn6 83.64(5) . . ? Mn3 Mn2 Mn6 59.943(16) . . ? O20 Mn2 Mn5 46.57(7) . . ? O5 Mn2 Mn5 125.71(7) . . ? O19 Mn2 Mn5 139.77(7) . . ? O1 Mn2 Mn5 39.06(6) . . ? O17 Mn2 Mn5 94.22(7) . . ? O2 Mn2 Mn5 85.33(6) . . ? Mn3 Mn2 Mn5 116.77(2) . . ? Mn6 Mn2 Mn5 88.75(2) . . ? O20 Mn2 Mn1 92.42(7) . . ? O5 Mn2 Mn1 80.98(7) . . ? O19 Mn2 Mn1 130.70(7) . . ? O1 Mn2 Mn1 38.63(6) . . ? O17 Mn2 Mn1 125.64(6) . . ? O2 Mn2 Mn1 39.69(5) . . ? Mn3 Mn2 Mn1 60.877(16) . . ? Mn6 Mn2 Mn1 60.864(16) . . ? Mn5 Mn2 Mn1 55.896(16) . . ? O21 Mn3 O5 173.02(9) . . ? O21 Mn3 O14 94.87(9) . . ? O5 Mn3 O14 91.59(9) . . ? O21 Mn3 O2 86.12(9) . . ? O5 Mn3 O2 87.10(9) . . ? O14 Mn3 O2 171.55(9) . . ? O21 Mn3 O18 95.83(9) . . ? O5 Mn3 O18 85.66(9) . . ? O14 Mn3 O18 99.89(9) . . ? O2 Mn3 O18 88.34(8) . . ? O21 Mn3 O4 97.80(9) . . ? O5 Mn3 O4 79.24(8) . . ? O14 Mn3 O4 92.40(8) . . ? O2 Mn3 O4 79.15(8) . . ? O18 Mn3 O4 160.78(8) . . ? O21 Mn3 Mn2 135.60(6) . . ? O5 Mn3 Mn2 38.20(6) . . ? O14 Mn3 Mn2 129.46(7) . . ? O2 Mn3 Mn2 50.52(6) . . ? O18 Mn3 Mn2 76.36(6) . . ? O4 Mn3 Mn2 84.42(5) . . ? O21 Mn3 Mn6 139.44(7) . . ? O5 Mn3 Mn6 38.69(6) . . ? O14 Mn3 Mn6 84.40(7) . . ? O2 Mn3 Mn6 89.39(6) . . ? O18 Mn3 Mn6 124.34(6) . . ? O4 Mn3 Mn6 41.95(5) . . ? Mn2 Mn3 Mn6 60.320(17) . . ? O21 Mn3 Mn4 47.06(6) . . ? O5 Mn3 Mn4 126.10(7) . . ? O14 Mn3 Mn4 140.87(7) . . ? O2 Mn3 Mn4 39.09(6) . . ? O18 Mn3 Mn4 93.78(6) . . ? O4 Mn3 Mn4 85.71(5) . . ? Mn2 Mn3 Mn4 89.321(19) . . ? Mn6 Mn3 Mn4 117.20(2) . . ? O21 Mn3 Mn1 92.19(7) . . ? O5 Mn3 Mn1 81.47(7) . . ? O14 Mn3 Mn1 132.48(7) . . ? O2 Mn3 Mn1 39.07(6) . . ? O18 Mn3 Mn1 126.03(6) . . ? O4 Mn3 Mn1 40.08(5) . . ? Mn2 Mn3 Mn1 61.602(17) . . ? Mn6 Mn3 Mn1 61.233(17) . . ? Mn4 Mn3 Mn1 55.964(16) . . ? O3 Mn4 O2 82.81(9) . . ? O3 Mn4 O9 94.20(9) . . ? O2 Mn4 O9 169.23(9) . . ? O3 Mn4 N16 174.86(10) . . ? O2 Mn4 N16 96.49(9) . . ? O9 Mn4 N16 87.40(10) . . ? O3 Mn4 O21 98.96(8) . . ? O2 Mn4 O21 78.45(8) . . ? O9 Mn4 O21 91.87(9) . . ? N16 Mn4 O21 85.86(9) . . ? O3 Mn4 N17 99.85(10) . . ? O2 Mn4 N17 91.57(9) . . ? O9 Mn4 N17 99.14(9) . . ? N16 Mn4 N17 75.06(10) . . ? O21 Mn4 N17 157.38(9) . . ? O3 Mn4 Mn1 39.30(6) . . ? O2 Mn4 Mn1 43.65(6) . . ? O9 Mn4 Mn1 133.20(7) . . ? N16 Mn4 Mn1 139.40(7) . . ? O21 Mn4 Mn1 91.41(6) . . ? N17 Mn4 Mn1 95.23(7) . . ? O3 Mn4 Mn3 90.20(6) . . ? O2 Mn4 Mn3 40.16(6) . . ? O9 Mn4 Mn3 129.88(7) . . ? N16 Mn4 Mn3 92.52(7) . . ? O21 Mn4 Mn3 38.32(5) . . ? N17 Mn4 Mn3 129.18(7) . . ? Mn1 Mn4 Mn3 62.931(17) . . ? O7 Mn5 O1 82.90(9) . . ? O7 Mn5 O11 92.91(9) . . ? O1 Mn5 O11 167.75(10) . . ? O7 Mn5 N13 171.28(10) . . ? O1 Mn5 N13 96.46(9) . . ? O11 Mn5 N13 89.41(10) . . ? O7 Mn5 O20 101.62(9) . . ? O1 Mn5 O20 78.98(8) . . ? O11 Mn5 O20 90.68(9) . . ? N13 Mn5 O20 86.74(10) . . ? O7 Mn5 N14 96.81(10) . . ? O1 Mn5 N14 94.46(9) . . ? O11 Mn5 N14 97.47(10) . . ? N13 Mn5 N14 74.55(10) . . ? O20 Mn5 N14 159.43(9) . . ? O7 Mn5 Mn1 39.43(6) . . ? O1 Mn5 Mn1 43.53(6) . . ? O11 Mn5 Mn1 131.76(7) . . ? N13 Mn5 Mn1 138.82(7) . . ? O20 Mn5 Mn1 92.68(6) . . ? N14 Mn5 Mn1 95.83(7) . . ? O7 Mn5 Mn2 91.61(7) . . ? O1 Mn5 Mn2 40.48(6) . . ? O11 Mn5 Mn2 128.64(7) . . ? N13 Mn5 Mn2 93.51(8) . . ? O20 Mn5 Mn2 38.55(5) . . ? N14 Mn5 Mn2 132.63(7) . . ? Mn1 Mn5 Mn2 63.431(18) . . ? O22 Mn6 O5 171.20(9) . . ? O22 Mn6 O16 95.67(9) . . ? O5 Mn6 O16 92.83(9) . . ? O22 Mn6 O4 84.48(9) . . ? O5 Mn6 O4 86.74(9) . . ? O16 Mn6 O4 169.31(9) . . ? O22 Mn6 O15 96.60(9) . . ? O5 Mn6 O15 84.01(8) . . ? O16 Mn6 O15 100.76(9) . . ? O4 Mn6 O15 89.83(8) . . ? O22 Mn6 O1 99.34(9) . . ? O5 Mn6 O1 78.27(8) . . ? O16 Mn6 O1 90.55(8) . . ? O4 Mn6 O1 78.89(8) . . ? O15 Mn6 O1 159.42(8) . . ? O22 Mn6 Mn3 133.24(7) . . ? O5 Mn6 Mn3 38.38(6) . . ? O16 Mn6 Mn3 131.08(7) . . ? O4 Mn6 Mn3 49.93(6) . . ? O15 Mn6 Mn3 76.22(6) . . ? O1 Mn6 Mn3 83.37(6) . . ? O22 Mn6 Mn2 141.03(7) . . ? O5 Mn6 Mn2 37.87(6) . . ? O16 Mn6 Mn2 84.07(6) . . ? O4 Mn6 Mn2 89.09(6) . . ? O15 Mn6 Mn2 121.82(6) . . ? O1 Mn6 Mn2 41.82(5) . . ? Mn3 Mn6 Mn2 59.737(16) . . ? O22 Mn6 Mn7 46.17(7) . . ? O5 Mn6 Mn7 125.04(7) . . ? O16 Mn6 Mn7 140.08(7) . . ? O4 Mn6 Mn7 38.38(6) . . ? O15 Mn6 Mn7 95.86(6) . . ? O1 Mn6 Mn7 85.98(5) . . ? Mn3 Mn6 Mn7 88.030(19) . . ? Mn2 Mn6 Mn7 116.90(2) . . ? O22 Mn6 Mn1 91.66(7) . . ? O5 Mn6 Mn1 81.07(6) . . ? O16 Mn6 Mn1 130.41(7) . . ? O4 Mn6 Mn1 38.98(6) . . ? O15 Mn6 Mn1 127.00(6) . . ? O1 Mn6 Mn1 39.92(5) . . ? Mn3 Mn6 Mn1 60.972(16) . . ? Mn2 Mn6 Mn1 61.323(16) . . ? Mn7 Mn6 Mn1 55.591(15) . . ? O6 Mn7 O4 82.54(9) . . ? O6 Mn7 O10 92.35(9) . . ? O4 Mn7 O10 171.80(9) . . ? O6 Mn7 N1 174.32(10) . . ? O4 Mn7 N1 99.33(10) . . ? O10 Mn7 N1 86.37(10) . . ? O6 Mn7 O22 97.84(9) . . ? O4 Mn7 O22 77.14(8) . . ? O10 Mn7 O22 97.32(9) . . ? N1 Mn7 O22 87.82(9) . . ? O6 Mn7 N2 100.01(9) . . ? O4 Mn7 N2 97.61(9) . . ? O10 Mn7 N2 89.57(9) . . ? N1 Mn7 N2 74.46(10) . . ? O22 Mn7 N2 160.57(9) . . ? O6 Mn7 Mn1 39.23(7) . . ? O4 Mn7 Mn1 43.62(6) . . ? O10 Mn7 Mn1 131.58(7) . . ? N1 Mn7 Mn1 141.74(8) . . ? O22 Mn7 Mn1 91.12(5) . . ? N2 Mn7 Mn1 97.87(6) . . ? O6 Mn7 Mn6 88.79(7) . . ? O4 Mn7 Mn6 39.42(6) . . ? O10 Mn7 Mn6 134.51(7) . . ? N1 Mn7 Mn6 96.06(8) . . ? O22 Mn7 Mn6 37.78(6) . . ? N2 Mn7 Mn6 134.92(7) . . ? Mn1 Mn7 Mn6 62.552(16) . . ? O3 Mn8 O8 91.12(8) . . ? O3 Mn8 N19 114.28(9) . . ? O8 Mn8 N19 86.86(9) . . ? O3 Mn8 N25 89.39(9) . . ? O8 Mn8 N25 178.68(10) . . ? N19 Mn8 N25 94.04(10) . . ? O3 Mn8 N4 144.58(10) . . ? O8 Mn8 N4 78.79(9) . . ? N19 Mn8 N4 99.13(10) . . ? N25 Mn8 N4 100.10(10) . . ? O3 Mn8 N5 75.75(9) . . ? O8 Mn8 N5 88.15(9) . . ? N19 Mn8 N5 168.86(10) . . ? N25 Mn8 N5 90.80(10) . . ? N4 Mn8 N5 70.12(10) . . ? O6 Mn9 O12 93.45(9) . . ? O6 Mn9 N22 118.35(9) . . ? O12 Mn9 N22 92.12(9) . . ? O6 Mn9 N19 90.48(9) . . ? O12 Mn9 N19 175.86(10) . . ? N22 Mn9 N19 84.86(10) . . ? O6 Mn9 N7 145.89(9) . . ? O12 Mn9 N7 86.24(9) . . ? N22 Mn9 N7 95.73(10) . . ? N19 Mn9 N7 91.24(10) . . ? O6 Mn9 N8 75.89(9) . . ? O12 Mn9 N8 98.19(9) . . ? N22 Mn9 N8 162.01(10) . . ? N19 Mn9 N8 84.04(9) . . ? N7 Mn9 N8 70.43(10) . . ? O7 Mn10 O13 91.24(9) . . ? O7 Mn10 N25 115.54(9) . . ? O13 Mn10 N25 89.52(10) . . ? O7 Mn10 N22 92.15(9) . . ? O13 Mn10 N22 176.19(10) . . ? N25 Mn10 N22 87.45(10) . . ? O7 Mn10 N10 146.00(9) . . ? O13 Mn10 N10 86.45(9) . . ? N25 Mn10 N10 98.38(10) . . ? N22 Mn10 N10 91.71(10) . . ? O7 Mn10 N11 75.52(9) . . ? O13 Mn10 N11 89.51(9) . . ? N25 Mn10 N11 168.92(10) . . ? N22 Mn10 N11 93.02(10) . . ? N10 Mn10 N11 70.55(10) . . ? Mn5 O1 Mn1 94.19(9) . . ? Mn5 O1 Mn2 100.46(9) . . ? Mn1 O1 Mn2 102.43(10) . . ? Mn5 O1 Mn6 167.91(11) . . ? Mn1 O1 Mn6 92.17(8) . . ? Mn2 O1 Mn6 88.18(8) . . ? Mn4 O2 Mn1 93.77(9) . . ? Mn4 O2 Mn3 100.75(9) . . ? Mn1 O2 Mn3 101.74(9) . . ? Mn4 O2 Mn2 168.27(10) . . ? Mn1 O2 Mn2 92.57(8) . . ? Mn3 O2 Mn2 87.59(8) . . ? Mn1 O3 Mn4 101.18(10) . . ? Mn1 O3 Mn8 131.31(12) . . ? Mn4 O3 Mn8 126.80(11) . . ? Mn7 O4 Mn1 93.73(9) . . ? Mn7 O4 Mn6 102.19(10) . . ? Mn1 O4 Mn6 101.83(9) . . ? Mn7 O4 Mn3 166.81(11) . . ? Mn1 O4 Mn3 92.15(8) . . ? Mn6 O4 Mn3 88.12(8) . . ? Mn2 O5 Mn3 103.42(10) . . ? Mn2 O5 Mn6 103.77(11) . . ? Mn3 O5 Mn6 102.93(10) . . ? Mn1 O6 Mn7 101.30(10) . . ? Mn1 O6 Mn9 127.98(10) . . ? Mn7 O6 Mn9 129.86(11) . . ? Mn1 O7 Mn5 100.76(10) . . ? Mn1 O7 Mn10 129.97(11) . . ? Mn5 O7 Mn10 129.22(11) . . ? N2 O8 Mn8 126.07(18) . . ? N5 O9 Mn4 114.69(18) . . ? N8 O10 Mn7 116.32(17) . . ? N11 O11 Mn5 116.17(18) . . ? N14 O12 Mn9 126.05(19) . . ? N17 O13 Mn10 123.35(17) . . ? C43 O14 Mn3 127.2(2) . . ? C43 O15 Mn6 126.3(2) . . ? C45 O16 Mn6 126.4(2) . . ? C45 O17 Mn2 127.3(2) . . ? C47 O18 Mn3 126.4(2) . . ? C47 O19 Mn2 128.4(2) . . ? C49 O20 Mn2 126.1(2) . . ? C49 O20 Mn5 121.6(2) . . ? Mn2 O20 Mn5 94.88(8) . . ? C50 O21 Mn3 121.94(19) . . ? C50 O21 Mn4 120.81(19) . . ? Mn3 O21 Mn4 94.62(9) . . ? C51 O22 Mn6 124.9(2) . . ? C51 O22 Mn7 121.8(2) . . ? Mn6 O22 Mn7 96.06(9) . . ? C1 N1 C5 118.2(3) . . ? C1 N1 Mn7 123.8(2) . . ? C5 N1 Mn7 117.7(2) . . ? O8 N2 C6 115.8(3) . . ? O8 N2 Mn7 132.96(19) . . ? C6 N2 Mn7 111.2(2) . . ? C8 N4 C12 117.3(3) . . ? C8 N4 Mn8 123.3(2) . . ? C12 N4 Mn8 115.1(2) . . ? C13 N5 O9 117.2(3) . . ? C13 N5 Mn8 116.7(2) . . ? O9 N5 Mn8 125.46(19) . . ? C15 N7 C19 117.5(3) . . ? C15 N7 Mn9 125.1(2) . . ? C19 N7 Mn9 117.3(2) . . ? C20 N8 O10 117.7(3) . . ? C20 N8 Mn9 116.7(2) . . ? O10 N8 Mn9 124.52(19) . . ? C22 N10 C26 118.5(3) . . ? C22 N10 Mn10 124.8(2) . . ? C26 N10 Mn10 116.8(2) . . ? C27 N11 O11 117.1(3) . . ? C27 N11 Mn10 114.4(2) . . ? O11 N11 Mn10 125.01(19) . . ? C29 N13 C33 117.3(3) . . ? C29 N13 Mn5 124.5(2) . . ? C33 N13 Mn5 118.1(2) . . ? C34 N14 O12 116.4(3) . . ? C34 N14 Mn5 111.8(2) . . ? O12 N14 Mn5 131.8(2) . . ? C36 N16 C40 118.3(3) . . ? C36 N16 Mn4 123.7(2) . . ? C40 N16 Mn4 117.9(2) . . ? C41 N17 O13 116.2(3) . . ? C41 N17 Mn4 109.5(2) . . ? O13 N17 Mn4 133.64(19) . . ? N20 N19 Mn8 115.8(2) . . ? N20 N19 Mn9 118.5(2) . . ? Mn8 N19 Mn9 110.33(11) . . ? N21 N20 N19 179.4(4) . . ? N23 N22 Mn9 118.5(2) . . ? N23 N22 Mn10 117.3(2) . . ? Mn9 N22 Mn10 110.39(12) . . ? N24 N23 N22 179.7(4) . . ? N26 N25 Mn10 117.2(2) . . ? N26 N25 Mn8 117.6(2) . . ? Mn10 N25 Mn8 111.19(12) . . ? N27 N26 N25 179.7(4) . . ? N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.2(3) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.2(3) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 122.3(3) . . ? N2 C6 C7 120.3(3) . . ? N2 C6 C5 118.8(3) . . ? C7 C6 C5 120.8(3) . . ? N3 C7 C6 178.7(5) . . ? N4 C8 C9 122.8(3) . . ? N4 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C10 C9 C8 119.2(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 119.4(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 117.8(4) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? N4 C12 C11 123.4(3) . . ? N4 C12 C13 114.9(3) . . ? C11 C12 C13 121.6(3) . . ? N5 C13 C14 121.6(3) . . ? N5 C13 C12 117.9(3) . . ? C14 C13 C12 120.5(3) . . ? N6 C14 C13 179.2(4) . . ? N7 C15 C16 124.0(3) . . ? N7 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? C15 C16 C17 117.8(4) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 119.5(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? N7 C19 C18 121.1(3) . . ? N7 C19 C20 115.0(3) . . ? C18 C19 C20 123.9(3) . . ? N8 C20 C21 122.1(3) . . ? N8 C20 C19 119.4(3) . . ? C21 C20 C19 118.5(3) . . ? N9 C21 C20 178.8(4) . . ? N10 C22 C23 122.4(3) . . ? N10 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C24 C23 C22 119.0(3) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 119.0(3) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 118.9(3) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N10 C26 C25 122.3(3) . . ? N10 C26 C27 116.3(3) . . ? C25 C26 C27 121.4(3) . . ? N11 C27 C28 122.3(3) . . ? N11 C27 C26 117.5(3) . . ? C28 C27 C26 120.1(3) . . ? N12 C28 C27 175.4(4) . . ? N13 C29 C30 123.3(3) . . ? N13 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? C31 C30 C29 118.7(3) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C30 C31 C32 118.4(3) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? N13 C33 C32 121.9(3) . . ? N13 C33 C34 115.7(3) . . ? C32 C33 C34 122.4(3) . . ? N14 C34 C35 119.4(3) . . ? N14 C34 C33 119.8(3) . . ? C35 C34 C33 120.7(3) . . ? N15 C35 C34 178.6(4) . . ? N16 C36 C37 122.8(3) . . ? N16 C36 H36 118.6 . . ? C37 C36 H36 118.6 . . ? C38 C37 C36 118.7(3) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C37 C38 C39 119.5(3) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C39 C40 119.4(3) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? N16 C40 C39 121.2(3) . . ? N16 C40 C41 116.5(3) . . ? C39 C40 C41 122.3(3) . . ? N17 C41 C42 119.9(3) . . ? N17 C41 C40 120.0(3) . . ? C42 C41 C40 120.1(3) . . ? N18 C42 C41 178.9(4) . . ? O15 C43 O14 125.8(3) . . ? O15 C43 C44 119.8(3) . . ? O14 C43 C44 114.4(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O17 C45 O16 125.7(3) . . ? O17 C45 C46 118.7(3) . . ? O16 C45 C46 115.6(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O18 C47 O19 124.6(3) . . ? O18 C47 C48 119.6(3) . . ? O19 C47 C48 115.8(3) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O20 C49 H49A 109.5 . . ? O20 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O20 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O21 C50 H50A 109.5 . . ? O21 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O21 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O22 C51 H51A 109.5 . . ? O22 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O22 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 N28 C54 108.5(4) . . ? C53 N28 C52 110.9(4) . . ? C54 N28 C52 108.5(4) . . ? C53 N28 C55 109.2(4) . . ? C54 N28 C55 109.9(4) . . ? C52 N28 C55 109.8(4) . . ? N28 C52 H52A 109.5 . . ? N28 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N28 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N28 C53 H53A 109.5 . . ? N28 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N28 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N28 C54 H54A 109.5 . . ? N28 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N28 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N28 C55 H55A 109.5 . . ? N28 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N28 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C2W O2W H2OW 109.5 . . ? O2W C2W H2AW 109.5 . . ? O2W C2W H2BW 109.5 . . ? H2AW C2W H2BW 109.5 . . ? O2W C2W H2CW 109.5 . . ? H2AW C2W H2CW 109.5 . . ? H2BW C2W H2CW 109.5 . . ? O6W C6W O6W' 84.1(6) . . ? O7W C7W H7AW 109.5 . . ? O7W C7W H7BW 109.5 . . ? H7AW C7W H7BW 109.5 . . ? O7W C7W H7CW 109.5 . . ? H7AW C7W H7CW 109.5 . . ? H7BW C7W H7CW 109.5 . . ? C7W O7W H7OW 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.062 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 927000'