Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_ast _database_code_CSD 160800 # B101607P _publ_requested_journal Chemical communications #=========================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 182 _publ_contact_author # Name and address of author for correspondence ; Dr Christine J. McKenzie Department of Chemistry University of Southern Denmark, Main Campus: Odense University Campusvej 55 DK-5230 Odense M Denmark ; _publ_contact_author_phone '+45 6550 2518' _publ_contact_author_fax '+45 6615 8780' _publ_contact_author_email chk@chem.sdu.dk #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Air oxidation of alcohols and ketones by a dimanganese complex and structural characterisation of a dimanganese complex containing the unprecedented [Mn^II^(OH~2~)~2~...(OCH~3~)~2~Mn^III^] motif. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Astrid Boisen ' ; Department of Chemistry University of Southern Denmark, Main Campus: Odense University Campusvej 55 DK-5230 Odense M Denmark ; 'Alan Hazell ' ; Department of Chemistry Aarhus University DK-8000 \%Arhus C Denmark ; 'Kenneth Bendix Jensen ' ;Department of Chemistry University of Southern Denmark, Main Campus: Odense University Campusvej 55 DK-5230 Odense M Denmark ; 'Edel Johansen ' ;Department of Chemistry University of Southern Denmark, Main Campus: Odense University Campusvej 55 DK-5230 Odense M Denmark ; 'Christine J. McKenzie ' ;Department of Chemistry University of Southern Denmark, Main Campus: Odense University Campusvej 55 DK-5230 Odense M Denmark ; #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_sum 'C38 H51 N6 O14 Cl2 Mn2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_weight 996.67 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pna21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,-y,1/2+z' '1/2+x,1/2-y,+z' '1/2-x,1/2+y,1/2+z' _cell_length_a 22.331(1) _cell_length_b 18.351(1) _cell_length_c 10.9217(7) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 4475.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 5467 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 29.8 _exptl_crystal_description ellipsoid _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type 'multi-scan, SADABS' _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 0.872 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 40601 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 29.8 _diffrn_reflns_reduction_process 40601 _reflns_number_total 11470 _reflns_number_observed 6869 _reflns_observed_criterion I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^ ; _refine_ls_hydrogen_treatment ; H-atoms of ligand and of methoxy groups constrained to have C-H = 0.95 \%A and Uiso 1.2 * Ueq of the atom to which it is attached. The methyl hydrogens were disordered over two sites. Hydrogen atoms of the coordinated water molecules were kept fixed at the positions found from a difference map. ; _refine_ls_extinction_method ; B-C type 1 Lorentzian isotropic Becker and Coppens (1974) ; _refine_ls_extinction_coef 59(17) _refine_ls_abs_structure_details ; refine Rogere factor ; _refine_ls_abs_structure_Rogers 0.90(4) _refine_ls_number_reflns 6869 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.043 _refine_ls_wR_factor_obs 0.048 _refine_ls_goodness_of_fit_obs 1.344 _refine_ls_shift/esd_max 0.0013 _refine_ls_shift/esd_mean 0.0001 _refine_diff_density_max 1.0(1) _refine_diff_density_min -1.1(1) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Mn1 0.29541(3) 0.17120(3) 0.80200 0.0191(3) Uij 1. Mn1A 0.23923(3) -0.00652(3) 0.67102(10) 0.0197(3) Uij 1. O1 0.2365(1) 0.1106(1) 0.6853(3) 0.018(1) Uij 1. O2 0.3661(1) 0.1183(2) 0.6975(4) 0.036(2) Uij 1. O3 0.2874(1) 0.0992(2) 0.9544(3) 0.029(2) Uij 1. O4 0.3207(1) -0.0135(2) 0.6423(3) 0.031(2) Uij 1. O5 0.2415(1) -0.0109(2) 0.8448(3) 0.027(2) Uij 1. C4 0.3606(3) -0.0552(3) 0.7180(7) 0.056(4) Uij 1. C5 0.2519(3) -0.0696(3) 0.9217(6) 0.043(3) Uij 1. N1 0.2914(1) 0.2661(2) 0.6706(4) 0.021(2) Uij 1. N1A 0.1442(1) -0.0088(2) 0.6695(4) 0.019(2) Uij 1. N2 0.3694(2) 0.2457(2) 0.8611(4) 0.023(2) Uij 1. N2A 0.2114(2) -0.1277(2) 0.6641(4) 0.026(2) Uij 1. N3 0.2147(2) 0.2346(2) 0.8625(4) 0.020(2) Uij 1. N3A 0.2245(2) 0.0063(2) 0.4856(4) 0.022(2) Uij 1. C1 0.2683(2) 0.2382(2) 0.5494(5) 0.024(2) Uij 1. C1A 0.1188(2) 0.0611(2) 0.7190(4) 0.018(2) Uij 1. C2 0.3539(2) 0.2919(2) 0.6549(5) 0.024(2) Uij 1. C2A 0.1236(2) -0.0697(2) 0.7480(4) 0.022(2) Uij 1. C3 0.2534(2) 0.3249(2) 0.7216(5) 0.024(2) Uij 1. C3A 0.1229(2) -0.0207(2) 0.5424(5) 0.023(2) Uij 1. C10 0.1925(2) 0.1480(2) 0.6273(4) 0.017(2) Uij 1. C11 0.2051(2) 0.2112(2) 0.5588(4) 0.021(2) Uij 1. C11A 0.1332(2) 0.1250(2) 0.6392(4) 0.017(2) Uij 1. C12 0.1589(2) 0.2472(2) 0.5009(5) 0.025(3) Uij 1. C12A 0.0877(2) 0.1634(2) 0.5797(4) 0.024(3) Uij 1. C13 0.0990(2) 0.2257(3) 0.5092(5) 0.026(3) Uij 1. C14 0.0497(2) 0.2674(3) 0.4420(5) 0.034(3) Uij 1. C15 0.0564(3) 0.3496(3) 0.4669(7) 0.060(5) Uij 1. C16 -0.0121(2) 0.2484(3) 0.4880(7) 0.058(4) Uij 1. C17 0.0549(3) 0.2546(4) 0.3078(8) 0.077(5) Uij 1. C20 0.4015(2) 0.2426(3) 0.9645(5) 0.028(3) Uij 1. C20A 0.2466(2) -0.1870(3) 0.6433(5) 0.035(3) Uij 1. C21 0.4520(2) 0.2854(3) 0.9865(5) 0.029(3) Uij 1. C21A 0.2316(2) -0.2553(2) 0.6840(6) 0.039(3) Uij 1. C22 0.4686(2) 0.3352(3) 0.8982(5) 0.031(3) Uij 1. C22A 0.1788(2) -0.2652(2) 0.7464(5) 0.034(3) Uij 1. C23 0.4352(2) 0.3402(2) 0.7908(6) 0.026(2) Uij 1. C23A 0.1411(2) -0.2049(2) 0.7651(5) 0.030(3) Uij 1. C24 0.3867(2) 0.2941(2) 0.7742(5) 0.024(3) Uij 1. C24A 0.1600(2) -0.1372(2) 0.7219(4) 0.023(2) Uij 1. C30 0.1715(2) 0.2085(2) 0.9365(5) 0.024(3) Uij 1. C30A 0.2674(2) 0.0242(2) 0.4033(5) 0.027(3) Uij 1. C31 0.1176(2) 0.2422(3) 0.9533(5) 0.038(3) Uij 1. C31A 0.2542(2) 0.0408(3) 0.2835(5) 0.033(3) Uij 1. C32 0.1062(2) 0.3065(3) 0.8912(6) 0.048(4) Uij 1. C32A 0.1947(2) 0.0411(3) 0.2464(5) 0.034(3) Uij 1. C33 0.1498(2) 0.3339(3) 0.8130(6) 0.039(3) Uij 1. C33A 0.1511(2) 0.0236(3) 0.3296(5) 0.030(3) Uij 1. C34 0.2034(2) 0.2964(2) 0.8005(5) 0.025(2) Uij 1. C34A 0.1673(2) 0.0051(2) 0.4484(4) 0.021(2) Uij 1. CL1 0.05685(4) 0.00739(6) 1.04629(13) 0.022(1) Uij 1. O6 0.0839(1) 0.0785(2) 1.0387(4) 0.035(2) Uij 1. O7 0.0198(1) -0.0049(2) 0.9401(3) 0.032(2) Uij 1. O8 0.0208(1) 0.0030(2) 1.1554(4) 0.036(2) Uij 1. O9 0.1033(1) -0.0463(2) 1.0514(4) 0.038(2) Uij 1. CL2 0.42586(7) 0.05215(9) 1.1706(3) 0.075(1) Uij 1. O10 0.4203(4) 0.1113(5) 1.2213(12) 0.247(12) Uij 1. O11 0.3851(3) 0.0469(6) 1.0777(10) 0.215(10) Uij 1. O12 0.4152(5) -0.0008(6) 1.2387(13) 0.270(14) Uij 1. O13 0.4821(3) 0.0402(6) 1.1337(12) 0.224(11) Uij 1. O14 0.5260(2) -0.0915(3) 1.3102(9) 0.140(6) Uij 1. HO2a 0.4036 0.1190 0.7396 0.040 Uiso 1. HO2b 0.3605 0.0661 0.6923 0.040 Uiso 1. HO3a 0.2619 0.0613 0.9249 0.040 Uiso 1. HO3b 0.3211 0.0850 1.0022 0.040 Uiso 1. H1a 0.2932 0.1993 0.5228 0.028 Uiso 1. H1b 0.2697 0.2766 0.4913 0.028 Uiso 1. H1Aa 0.1349 0.0695 0.7982 0.021 Uiso 1. H1Ab 0.0765 0.0565 0.7246 0.021 Uiso 1. H2a 0.3532 0.3395 0.6208 0.029 Uiso 1. H2b 0.3742 0.2598 0.6008 0.029 Uiso 1. H2Aa 0.0826 -0.0793 0.7316 0.026 Uiso 1. H2Ab 0.1283 -0.0565 0.8315 0.026 Uiso 1. H3a 0.2365 0.3517 0.6557 0.029 Uiso 1. H3b 0.2778 0.3562 0.7697 0.029 Uiso 1. H3Aa 0.0864 0.0051 0.5313 0.028 Uiso 1. H3Ab 0.1160 -0.0713 0.5306 0.028 Uiso 1. H4a 0.3441 -0.0603 0.7977 0.068 Uiso 0.5 H4b 0.3982 -0.0312 0.7235 0.068 Uiso 0.5 H4c 0.3659 -0.1020 0.6822 0.068 Uiso 0.5 H4a' 0.3910 -0.0766 0.6687 0.068 Uiso 0.5 H4b' 0.3389 -0.0925 0.7589 0.068 Uiso 0.5 H4c' 0.3784 -0.0236 0.7766 0.068 Uiso 0.5 H5a 0.2416 -0.1136 0.8809 0.051 Uiso 0.5 H5b 0.2283 -0.0648 0.9936 0.051 Uiso 0.5 H5c 0.2931 -0.0705 0.9430 0.051 Uiso 0.5 H5a' 0.2733 -0.0538 0.9919 0.051 Uiso 0.5 H5b' 0.2745 -0.1056 0.8797 0.051 Uiso 0.5 H5c' 0.2144 -0.0896 0.9460 0.051 Uiso 0.5 H12 0.1682 0.2889 0.4529 0.029 Uiso 1. H12A 0.0476 0.1467 0.5872 0.029 Uiso 1. H15a 0.0258 0.3755 0.4251 0.072 Uiso 1. H15b 0.0944 0.3657 0.4387 0.072 Uiso 1. H15c 0.0532 0.3584 0.5524 0.072 Uiso 1. H16a -0.0427 0.2743 0.4462 0.070 Uiso 1. H16b -0.0143 0.2597 0.5727 0.070 Uiso 1. H16c -0.0184 0.1976 0.4768 0.070 Uiso 1. H17a 0.0243 0.2805 0.2660 0.092 Uiso 1. H17b 0.0510 0.2039 0.2915 0.092 Uiso 1. H17c 0.0929 0.2710 0.2802 0.092 Uiso 1. H20 0.3892 0.2093 1.0263 0.033 Uiso 1. H20A 0.2829 -0.1808 0.5990 0.041 Uiso 1. H21 0.4743 0.2804 1.0601 0.035 Uiso 1. H21A 0.2575 -0.2954 0.6691 0.046 Uiso 1. H22 0.5024 0.3658 0.9105 0.038 Uiso 1. H22A 0.1680 -0.3120 0.7763 0.041 Uiso 1. H23 0.4456 0.3747 0.7296 0.031 Uiso 1. H23A 0.1038 -0.2101 0.8060 0.036 Uiso 1. H30 0.1789 0.1643 0.9792 0.029 Uiso 1. H30A 0.3080 0.0253 0.4293 0.033 Uiso 1. H31 0.0885 0.2220 1.0067 0.046 Uiso 1. H31A 0.2853 0.0519 0.2271 0.039 Uiso 1. H32 0.0693 0.3314 0.9019 0.057 Uiso 1. H32A 0.1843 0.0533 0.1645 0.041 Uiso 1. H33 0.1430 0.3776 0.7686 0.046 Uiso 1. H33A 0.1101 0.0241 0.3062 0.036 Uiso 1. loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn1A 0.0188(3) 0.0202(3) 0.0201(3) -0.0005(3) -0.0020(3) 0.0009(4) Mn1 0.0168(3) 0.0202(3) 0.0204(3) -0.0036(3) -0.0025(3) 0.0033(3) O1 0.015(1) 0.021(1) 0.019(2) -0.001(1) -0.002(1) -0.001(1) O2 0.021(2) 0.031(2) 0.056(3) 0.000(1) 0.001(2) 0.002(2) O3 0.032(2) 0.027(2) 0.027(2) -0.005(1) -0.010(2) 0.002(2) O4 0.024(2) 0.033(2) 0.036(3) 0.006(1) -0.001(1) 0.001(2) O5 0.035(2) 0.021(2) 0.024(2) -0.002(1) -0.003(1) 0.007(1) N1A 0.020(2) 0.018(2) 0.019(2) -0.005(1) 0.000(2) 0.005(2) N1 0.016(2) 0.022(2) 0.024(2) -0.005(1) -0.002(2) 0.000(2) N2A 0.031(2) 0.019(2) 0.029(2) -0.001(2) 0.004(2) -0.001(2) N2 0.019(2) 0.028(2) 0.021(2) -0.004(2) -0.001(2) 0.002(2) N3A 0.026(2) 0.017(2) 0.023(2) -0.001(2) 0.001(2) 0.000(2) N3 0.019(2) 0.020(2) 0.022(2) -0.005(1) -0.002(2) -0.001(2) C1A 0.018(2) 0.020(2) 0.015(2) -0.004(2) -0.001(2) 0.000(2) C1 0.020(2) 0.031(3) 0.020(3) -0.007(2) -0.003(2) 0.008(2) C2A 0.026(2) 0.018(2) 0.021(3) -0.004(2) 0.002(2) 0.007(2) C2 0.025(2) 0.026(2) 0.022(3) -0.013(2) -0.001(2) 0.007(2) C3A 0.022(2) 0.019(2) 0.030(3) -0.008(2) -0.005(2) -0.003(2) C3 0.028(2) 0.018(2) 0.027(3) -0.001(2) -0.005(2) 0.005(2) C4 0.036(3) 0.041(4) 0.092(6) 0.007(3) -0.007(3) 0.015(3) C5 0.059(4) 0.031(3) 0.038(4) 0.001(3) -0.011(3) 0.009(3) C10 0.019(2) 0.019(2) 0.014(2) -0.002(2) -0.003(2) 0.001(2) C11A 0.018(2) 0.018(2) 0.016(3) -0.002(2) -0.001(2) 0.004(2) C11 0.019(2) 0.026(2) 0.019(3) -0.006(2) -0.001(2) 0.000(2) C12A 0.015(2) 0.034(3) 0.024(3) -0.005(2) -0.003(2) 0.008(2) C12 0.027(2) 0.023(2) 0.023(3) -0.005(2) -0.003(2) 0.012(2) C13 0.019(2) 0.030(3) 0.029(3) -0.002(2) -0.008(2) 0.008(2) C14 0.022(2) 0.038(3) 0.042(4) -0.004(2) -0.012(2) 0.019(3) C15 0.042(3) 0.044(4) 0.093(6) 0.003(3) -0.024(4) 0.014(4) C16 0.023(3) 0.066(4) 0.085(6) 0.004(3) -0.016(3) 0.040(4) C17 0.072(5) 0.111(6) 0.046(4) 0.036(4) -0.024(4) 0.016(5) C20A 0.035(3) 0.029(3) 0.040(4) 0.000(2) 0.002(2) -0.008(2) C20 0.027(2) 0.030(3) 0.026(3) 0.000(2) -0.003(2) 0.003(2) C21A 0.050(3) 0.022(2) 0.044(4) 0.004(2) 0.006(3) -0.007(3) C21 0.025(2) 0.034(3) 0.029(3) 0.002(2) -0.010(2) -0.009(2) C22A 0.055(3) 0.018(3) 0.029(3) -0.006(2) -0.007(3) 0.004(2) C22 0.020(2) 0.025(3) 0.049(4) -0.002(2) -0.004(2) -0.012(3) C23A 0.036(3) 0.022(3) 0.032(3) -0.007(2) -0.006(2) 0.003(2) C23 0.022(2) 0.019(2) 0.037(3) -0.004(2) 0.004(2) -0.005(2) C24A 0.029(2) 0.025(3) 0.016(3) -0.007(2) -0.004(2) -0.003(2) C24 0.018(2) 0.021(2) 0.033(3) -0.002(2) -0.001(2) 0.002(2) C30A 0.026(2) 0.026(3) 0.030(3) -0.002(2) 0.002(2) 0.000(2) C30 0.028(2) 0.025(3) 0.020(3) -0.008(2) -0.004(2) 0.004(2) C31A 0.036(3) 0.034(3) 0.028(3) -0.008(2) 0.010(2) 0.003(2) C31 0.029(3) 0.050(4) 0.037(4) -0.007(2) 0.009(3) -0.004(3) C32A 0.044(3) 0.032(3) 0.026(3) -0.008(2) -0.005(2) 0.009(2) C32 0.026(3) 0.051(4) 0.066(5) 0.015(3) 0.003(3) 0.001(3) C33A 0.029(2) 0.036(3) 0.025(3) -0.003(2) -0.004(2) -0.002(2) C33 0.027(2) 0.038(3) 0.051(4) 0.007(2) 0.001(3) 0.014(3) C34A 0.023(2) 0.016(2) 0.022(3) -0.001(2) -0.001(2) -0.003(2) C34 0.024(2) 0.023(2) 0.028(3) -0.004(2) -0.004(2) -0.003(3) CL1 0.0193(5) 0.0276(6) 0.0196(6) 0.0027(4) 0.0023(4) 0.0054(5) O6 0.031(2) 0.030(2) 0.044(2) -0.005(1) -0.007(2) 0.011(2) O7 0.027(2) 0.044(2) 0.025(2) 0.003(2) -0.003(1) -0.003(2) O8 0.030(2) 0.055(2) 0.024(2) -0.003(2) 0.009(2) -0.001(2) O9 0.040(2) 0.038(2) 0.036(2) 0.019(2) 0.004(2) 0.010(2) CL2 0.041(1) 0.048(1) 0.136(2) 0.004(1) -0.036(1) 0.026(1) O10 0.172(8) 0.178(8) 0.391(17) 0.111(7) -0.119(9) -0.202(10) O11 0.103(6) 0.301(11) 0.241(12) 0.014(6) -0.128(7) 0.079(9) O12 0.242(12) 0.244(11) 0.324(17) -0.114(9) -0.045(11) 0.222(12) O13 0.053(4) 0.328(12) 0.290(15) 0.049(6) -0.032(6) -0.106(11) O14 0.052(3) 0.082(4) 0.287(10) -0.007(3) -0.006(5) 0.082(6) # 2_654 1-x, -y, -0.5-z #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mn1 Mn1A 3.776(1) Mn1A O1 2.155(3) Mn1A O4 1.849(3) Mn1A O5 1.900(4) Mn1A N1A 2.123(3) Mn1A N2A 2.310(3) Mn1A N3A 2.065(4) Mn1 O1 2.143(3) Mn1 O2 2.176(3) Mn1 O3 2.132(3) Mn1 N1 2.258(4) Mn1 N2 2.239(4) Mn1 N3 2.244(4) O1 C10 1.355(5) O4 C4 1.438(7) O5 C5 1.385(6) N1A C1A 1.504(5) N1A C2A 1.481(5) N1A C3A 1.483(6) N1 C1 1.510(6) N1 C2 1.483(5) N1 C3 1.482(6) N2A C20A 1.362(6) N2A C24A 1.322(6) N3A C30A 1.354(6) N3A C34A 1.342(5) N2 C20 1.339(6) N2 C24 1.356(6) N3 C30 1.347(6) N3 C34 1.345(6) C20A C21A 1.372(7) C21A C22A 1.374(7) C22A C23A 1.406(7) C23A C24A 1.393(6) C24A C2A 1.508(6) C20 C21 1.396(6) C21 C22 1.380(7) C22 C23 1.393(7) C23 C24 1.386(6) C24 C2 1.495(7) C30A C31A 1.375(8) C31A C32A 1.391(7) C32A C33A 1.370(7) C33A C34A 1.390(7) C34A C3A 1.504(7) C30 C31 1.365(7) C31 C32 1.383(8) C32 C33 1.389(8) C33 C34 1.387(6) C34 C3 1.504(7) C1A C11A 1.496(6) C10 C11A 1.396(5) C11A C12A 1.398(6) C1 C11 1.498(6) C11 C12 1.380(6) C11 C10 1.409(6) C12 C13A 1.396(6) C12A C13A 1.401(6) C13 C14 1.530(6) C14 C15 1.541(7) C14 C16 1.509(7) C14 C17 1.488(9) CL1 O6 1.439(3) CL1 O7 1.442(4) CL1 O8 1.440(4) CL1 O9 1.432(3) CL2 O10 1.225(7) CL2 O11 1.367(8) CL2 O12 1.246(7) CL2 O13 1.337(8) O2 HO2a 0.955 O2 HO2b 0.968 O3 HO3a 0.956 O3 HO3b 0.954 C4 H4a 0.950 C4 H4b 0.950 C4 H4c 0.950 C4 H4c' 0.950 C4 H4a' 0.950 C4 H4b' 0.950 C5 H5a 0.950 C5 H5b 0.950 C5 H5c 0.950 C5 H5a' 0.950 C5 H5b' 0.950 C5 H5c' 0.950 C2 H2a 0.950 C2 H2b 0.950 C3 H3a 0.950 C3 H3b 0.950 C20 H20 0.950 C21 H21 0.950 C22 H22 0.950 C23 H23 0.950 C30 H30 0.950 C31 H31 0.950 C32 H32 0.950 C33 H33 0.950 C2A H2Aa 0.950 C2A H2Ab 0.950 C3A H3Aa 0.950 C3A H3Ab 0.950 C30A H30A 0.950 C31A H31A 0.950 C32A H32A 0.950 C33A H33A 0.950 C20A H20A 0.950 C21A H21A 0.950 C22A H22A 0.950 C23A H23A 0.950 C1A H1Aa 0.950 C1A H1Ab 0.950 C1 H1a 0.950 C1 H1b 0.950 C12A H12A 0.950 C12 H12 0.950 C15 H15a 0.950 C15 H15b 0.950 C15 H15c 0.950 C16 H16a 0.950 C16 H16b 0.950 C16 H16c 0.950 C17 H17a 0.950 C17 H17b 0.950 C17 H17c 0.950 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Mn1A O4 96.2(1) O1 Mn1A O5 88.4(1) O1 Mn1A N1A 89.6(1) O1 Mn1A N2A 162.6(1) O1 Mn1A N3A 87.3(1) O4 Mn1A O5 98.0(1) O4 Mn1A N1A 168.6(2) O4 Mn1A N2A 101.1(1) O4 Mn1A N3A 89.9(1) O5 Mn1A N1A 92.0(2) O5 Mn1A N2A 89.9(2) O5 Mn1A N3A 171.3(1) N1A Mn1A N2A 73.2(1) N1A Mn1A N3A 80.5(2) N2A Mn1A N3A 92.0(2) O1 Mn1 O2 84.4(1) O1 Mn1 O3 95.2(1) O1 Mn1 N1 89.9(1) O1 Mn1 N2 160.2(1) O1 Mn1 N3 87.2(1) O2 Mn1 O3 101.2(1) O2 Mn1 N1 92.3(1) O2 Mn1 N2 83.6(1) O2 Mn1 N3 165.5(1) O3 Mn1 N1 166.0(1) O3 Mn1 N2 102.4(1) O3 Mn1 N3 91.4(1) N1 Mn1 N2 75.0(1) N1 Mn1 N3 75.8(1) N2 Mn1 N3 101.0(1) Mn1A O1 Mn1 122.9(1) Mn1A O1 C10 119.4(2) Mn1A O4 C4 123.3(3) Mn1A O5 C5 130.0(3) Mn1A N1A C1 111.0(2) Mn1A N1A C2A 108.7(2) Mn1A N1A C3A 109.3(3) Mn1A N2A C20A 128.2(3) Mn1A N2A C24A 110.2(3) Mn1A N3A C30A 124.5(3) Mn1A N3A C34A 116.5(3) Mn1 O1 C10 117.4(2) Mn1 N1 C1 108.0(2) Mn1 N1 C2 106.4(2) Mn1 N1 C3 110.2(3) Mn1 N2 C20 127.7(3) Mn1 N2 C24 114.1(3) Mn1 N3 C30 124.6(3) Mn1 N3 C34 116.1(3) C20 N2 C24 117.7(4) C30 N3 C34 117.9(4) C30A N3A C34A 118.5(4) C20A N2A C24A 118.5(4) C2 N1 C3 110.5(3) C3 N1 C1 112.4(3) C2 N1 C1 109.2(4) C3A N1A C2A 109.4(3) C2A N1A C1A 108.6(3) C3A N1A C1A 109.9(3) N2 C20 C21 123.7(5) C20 C21 C22 118.0(5) C21 C22 C23 119.3(4) C22 C23 C24 119.3(5) N2 C24 C23 122.1(5) N2 C24 C2 116.9(4) C23 C24 C2 120.9(4) N1 C2 C24 111.6(4) N3 C30 C31 123.4(4) C30 C31 C32 118.8(5) C31 C32 C33 118.8(5) C32 C33 C34 119.0(5) N3 C34 C33 122.1(5) N3 C34 C3 116.2(4) C33 C34 C3 121.6(4) N1 C3 C34 112.8(3) N3A C30A C31A 122.2(4) C30A C31A C32A 118.9(5) C31A C32A C33A 119.1(5) C32A C33A C34A 119.4(4) N3A C34A C33A 121.8(4) N3A C34A C3A 115.3(4) C33A C34A C3A 122.9(4) N1A C3A C34A 112.4(3) N2A C20A C21A 122.3(5) C20A C21A C22A 119.5(4) C21A C22A C23A 118.8(4) C22A C23A C24A 118.2(5) N2A C24A C23A 122.8(4) N2A C24A C2A 116.7(4) C23A C24A C2A 120.4(4) N1A C2A C24A 110.1(4) N1 C1 C11 112.0(4) C12 C11 C10 119.2(4) C1 C11 C12 121.0(4) C1 C11 C10 119.8(4) C11 C12 C13 123.4(4) C12 C13 C12 116.1(4) C12 C13 C14 121.1(4) C14 C13 C12 122.8(4) C17 C14 C16 111.3(5) C13 C14 C17 109.7(4) C15 C14 C17 108.8(5) C13 C14 C16 112.5(4) C15 C14 C16 104.9(5) C13 C14 C15 109.6(4) N1A C1A C11A 112.2(3) C12A C11A C10 119.6(4) C1A C11A C10 119.7(4) C1A C11A C12A 120.6(4) C13 C12 C11 122.3(4) O1 C10 C11 119.4(4) O1 C10 C11 121.3(3) C11A C10 C11 119.2(4) O6 CL1 O9 108.8(2) O8 CL1 O9 109.5(2) O7 CL1 O9 109.8(2) O6 CL1 O8 109.4(2) O6 CL1 O7 109.6(2) O7 CL1 O8 109.7(2) O10 CL2 O12 113.7(10) O10 CL2 O13 112.2(6) O10 CL2 O11 109.2(6) O12 CL2 O13 103.4(8) O11 CL2 O12 105.2(7) O11 CL2 O13 113.0(7) HO2a O2 HO2b 98.8 HO3a O3 HO3b 117.0 H5a C5 H5c 109.6 H5b C5 H5c 109.6 O5 C5 H5c 108.8 H5a' C5 H5b' 109.5 H5a' C5 H5c' 109.6 O5 C5 H5a' 109.6 H5a C5 H5b 109.5 O5 C5 H5a 109.6 O5 C5 H5b 109.6 H5b' C5 H5c' 109.6 O5 C5 H5b' 109.6 O5 C5 H5c' 108.8 H4a C4 H4b 109.5 H4a C4 H4c 109.6 O4 C4 H4a 109.7 H4b C4 H4c 109.6 O4 C4 H4b 109.7 H4a' C4 H4c' 109.7 H4b' C4 H4c' 109.7 O4 C4 H4c' 108.7 O4 C4 H4c 108.7 H4a' C4 H4b' 109.4 O4 C4 H4a' 109.7 O4 C4 H4b' 109.7 N2 C20 H20 118.2 C21 C20 H20 118.2 C22 C21 H21 121.0 C20 C21 H21 121.0 C21 C22 H22 120.4 C23 C22 H22 120.4 C24 C23 H23 120.4 C22 C23 H23 120.4 H2a C2 H2b 109.5 N1 C2 H2a 108.9 C24 C2 H2a 108.9 N1 C2 H2b 108.9 C24 C2 H2b 108.9 N3 C30 H30 118.3 C31 C30 H30 118.3 C30 C31 H31 120.6 C32 C31 H31 120.6 C31 C32 H32 120.6 C33 C32 H32 120.6 C34 C33 H33 120.5 C32 C33 H33 120.5 H3a C3 H3b 109.5 N1 C3 H3a 108.6 C34 C3 H3a 108.6 N1 C3 H3b 108.6 C34 C3 H3b 108.6 N3A C30A H30A 118.9 C31A C30A H30A 118.9 C30A C31A H31A 120.6 C32A C31A H31A 120.6 C33A C32A H32A 120.5 C31A C32A H32A 120.5 C32A C33A H33A 120.3 C34A C33A H33A 120.3 H3Aa C3A H3Ab 109.5 N1A C3A H3Aa 108.7 C34A C3A H3Aa 108.7 N1A C3A H3Ab 108.7 C34A C3A H3Ab 108.7 N2A C20A H20A 118.9 C21A C20A H20A 118.9 C20A C21A H21A 120.3 C22A C21A H21A 120.3 C21A C22A H22A 120.6 C23A C22A H22A 120.6 C24A C23A H23A 120.9 C22A C23A H23A 120.9 H2Aa C2A H2Ab 109.5 N1A C2A H2Aa 109.3 C24A C2A H2Aa 109.3 N1A C2A H2Ab 109.3 C24A C2A H2Ab 109.3 H1a C1 H1b 109.5 C11 C1 H1a 108.8 N1 C1 H1a 108.8 C11 C1 H1b 108.8 N1 C1 H1b 108.8 C11 C12 H12 118.3 C13 C12 H12 118.3 H15a C15 H15b 109.5 H15a C15 H15c 109.5 C14 C15 H15a 109.6 H15b C15 H15c 109.5 C14 C15 H15b 109.4 C14 C15 H15c 109.5 H17a C17 H17b 109.4 H17a C17 H17c 109.4 C14 C17 H17a 109.7 H17b C17 H17c 109.5 C14 C17 H17b 109.4 C14 C17 H17c 109.4 H16a C16 H16b 108.7 H16b C16 H16c 109.5 C14 C16 H16b 108.7 H16a C16 H16c 108.7 C14 C16 H16a 112.5 C14 C16 H16c 108.7 H1Aa C1A H1Ab 109.5 C11A C1A H1Aa 108.8 N1A C1A H1Aa 108.8 C11A C1A H1Ab 108.8 N1A C1A H1Ab 108.8 C11A C12A H12A 118.8 C13A C12A H12A 118.8 loop_ _publ_manuscript_incl_extra_item '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A O2 HO2a O14 0.955 1.823 2.750(7) 163.0 2_654 O2 HO2b O4 0.968 1.796 2.691(5) 152.5 . O3 HO3a O5 0.956 1.652 2.563(4) 158.0 . O3 HO3b O11 0.954 1.791 2.738(7) 171.7 .