data_c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Mn N3.33 O6' _chemical_formula_weight 425.92 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 7.570(7) _cell_length_b 10.630(10) _cell_length_c 16.062(15) _cell_angle_alpha 97.955(10) _cell_angle_beta 94.363(11) _cell_angle_gamma 103.286(10) _cell_volume 1238(2) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3706 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.90 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 649 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7228 _exptl_absorpt_correction_T_max 0.7913 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4523 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4523 _reflns_number_gt 3913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+1.5145P] 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 4523 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1627 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _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 1.15301(10) 1.16370(7) 0.49674(5) 0.0226(2) Uani 1 1 d . . . Mn2 Mn 1.0000 1.0000 1.0000 0.0207(3) Uani 1 2 d S . . N1 N 0.8760(6) 0.8938(4) 1.0957(3) 0.0254(9) Uani 1 1 d . . . N2 N 0.7264(6) 0.7376(4) 1.1591(3) 0.0266(10) Uani 1 1 d . . . N3 N 0.4555(6) 0.3971(5) 1.1068(3) 0.0328(11) Uani 1 1 d . . . N4 N 0.3756(6) 0.4458(4) 1.3313(3) 0.0275(9) Uani 1 1 d . . . N5 N 0.2619(6) 0.3290(4) 1.4284(3) 0.0301(10) Uani 1 1 d . . . O1 O 1.2744(7) 1.0489(5) 0.4033(3) 0.0431(11) Uani 1 1 d . . . O2 O 1.6875(6) 1.1580(4) 0.8822(2) 0.0332(9) Uani 1 1 d . . . H2 H 1.7286 1.1932 0.9306 0.050 Uiso 1 1 calc R . . O3 O 1.7205(5) 0.9713(4) 0.9249(2) 0.0314(9) Uani 1 1 d . . . O4 O 1.0197(5) 0.8202(4) 0.9162(2) 0.0306(8) Uani 1 1 d . . . O5 O 1.1450(6) 0.6953(4) 0.9919(2) 0.0434(11) Uani 1 1 d . . . O6 O 1.0876(6) 0.3044(4) 0.5876(2) 0.0375(9) Uani 1 1 d . . . O7 O 0.8264(6) 0.2079(4) 0.6333(3) 0.0437(11) Uani 1 1 d . . . O8 O 1.3425(6) 1.1200(4) 0.5965(2) 0.0368(10) Uani 1 1 d . . . O9 O 1.1049(5) 0.9528(4) 0.5608(2) 0.0386(10) Uani 1 1 d . . . C1 C 0.7517(8) 0.7816(5) 1.0842(3) 0.0276(11) Uani 1 1 d . . . H1A H 0.6898 0.7385 1.0321 0.033 Uiso 1 1 calc R . . C2 C 0.8442(7) 0.8294(5) 1.2211(3) 0.0260(11) Uani 1 1 d . . . H2A H 0.8592 0.8264 1.2788 0.031 Uiso 1 1 calc R . . C3 C 0.9319(8) 0.9233(5) 1.1803(3) 0.0253(10) Uani 1 1 d . . . H3 H 1.0189 0.9980 1.2062 0.030 Uiso 1 1 calc R . . C4 C 0.6122(7) 0.6154(5) 1.1707(3) 0.0264(11) Uani 1 1 d . . . C5 C 0.5689(8) 0.5121(5) 1.1038(3) 0.0312(12) Uani 1 1 d . . . H5 H 0.6218 0.5238 1.0541 0.037 Uiso 1 1 calc R . . C6 C 0.3883(8) 0.3795(5) 1.1811(3) 0.0296(12) Uani 1 1 d . . . H6 H 0.3044 0.3017 1.1842 0.036 Uiso 1 1 calc R . . C7 C 0.4408(7) 0.4740(5) 1.2529(3) 0.0256(11) Uani 1 1 d . . . C8 C 0.5493(7) 0.5969(5) 1.2481(3) 0.0263(11) Uani 1 1 d . . . H8 H 0.5784 0.6636 1.2946 0.032 Uiso 1 1 calc R . . C9 C 0.3225(8) 0.3247(5) 1.3536(4) 0.0337(13) Uani 1 1 d . . . H9 H 0.3285 0.2477 1.3197 0.040 Uiso 1 1 calc R . . C10 C 0.2760(8) 0.4610(5) 1.4563(4) 0.0324(12) Uani 1 1 d . . . H10 H 0.2419 0.4953 1.5073 0.039 Uiso 1 1 calc R . . C11 C 0.3476(7) 0.5322(5) 1.3972(3) 0.0299(12) Uani 1 1 d . . . H11 H 0.3727 0.6228 1.4011 0.036 Uiso 1 1 calc R . . C12 C 1.0768(7) 0.7204(5) 0.9246(3) 0.0237(11) Uani 1 1 d . . . C13 C 1.0551(7) 0.6151(5) 0.8477(3) 0.0213(10) Uani 1 1 d . . . C14 C 1.1270(7) 0.6399(5) 0.7722(3) 0.0214(10) Uani 1 1 d . . . C15 C 1.0976(7) 0.5361(5) 0.7053(3) 0.0232(11) Uani 1 1 d . . . H15 H 1.1500 0.5503 0.6558 0.028 Uiso 1 1 calc R . . C16 C 0.9925(7) 0.4122(5) 0.7102(3) 0.0217(10) Uani 1 1 d . . . C17 C 0.9202(7) 0.3894(5) 0.7848(3) 0.0251(11) Uani 1 1 d . . . H17 H 0.8483 0.3072 0.7887 0.030 Uiso 1 1 calc R . . C18 C 0.9549(7) 0.4893(5) 0.8541(3) 0.0242(11) Uani 1 1 d . . . H18 H 0.9112 0.4724 0.9051 0.029 Uiso 1 1 calc R . . C19 C 1.2421(7) 0.7703(5) 0.7624(3) 0.0202(10) Uani 1 1 d . . . C20 C 1.3851(6) 0.8401(5) 0.8229(3) 0.0197(10) Uani 1 1 d . . . H20 H 1.4086 0.8062 0.8717 0.024 Uiso 1 1 calc R . . C21 C 1.4947(6) 0.9611(5) 0.8113(3) 0.0211(10) Uani 1 1 d . . . C22 C 1.4568(7) 1.0146(5) 0.7392(3) 0.0216(10) Uani 1 1 d . . . H22 H 1.5273 1.0956 0.7319 0.026 Uiso 1 1 calc R . . C23 C 1.3131(7) 0.9465(5) 0.6781(3) 0.0212(10) Uani 1 1 d . . . C24 C 1.2078(7) 0.8236(5) 0.6900(3) 0.0238(10) Uani 1 1 d . . . H24 H 1.1137 0.7773 0.6488 0.029 Uiso 1 1 calc R . . C25 C 1.6458(7) 1.0324(5) 0.8787(3) 0.0226(10) Uani 1 1 d . . . C26 C 1.2519(7) 1.0094(5) 0.6067(3) 0.0244(11) Uani 1 1 d . . . C27 C 0.9640(7) 0.2994(5) 0.6374(3) 0.0274(11) Uani 1 1 d . . . H2W H 1.36(2) 1.079(15) 0.441(9) 0.17(7) Uiso 1 1 d . . . H1W H 1.233(9) 0.976(8) 0.391(4) 0.04(2) Uiso 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 0.0276(4) 0.0171(4) 0.0213(4) 0.0057(3) 0.0032(3) 0.0003(3) Mn2 0.0256(5) 0.0143(5) 0.0230(5) 0.0077(4) 0.0060(4) 0.0023(4) N1 0.028(2) 0.021(2) 0.027(2) 0.0078(18) 0.0071(18) 0.0030(18) N2 0.031(2) 0.023(2) 0.025(2) 0.0080(18) 0.0039(18) 0.0031(19) N3 0.034(3) 0.026(2) 0.036(3) 0.007(2) 0.005(2) 0.002(2) N4 0.031(2) 0.022(2) 0.030(2) 0.0115(18) 0.0050(19) 0.0029(19) N5 0.037(2) 0.023(2) 0.029(2) 0.0080(18) 0.0071(19) 0.0025(19) O1 0.054(3) 0.022(2) 0.050(3) 0.002(2) 0.022(2) 0.000(2) O2 0.042(2) 0.024(2) 0.0277(19) 0.0058(15) -0.0083(17) -0.0023(17) O3 0.032(2) 0.0246(19) 0.034(2) 0.0115(16) -0.0089(16) 0.0001(16) O4 0.043(2) 0.0194(18) 0.0290(19) -0.0004(15) 0.0054(17) 0.0079(17) O5 0.074(3) 0.0182(19) 0.029(2) 0.0024(16) -0.014(2) 0.000(2) O6 0.051(2) 0.026(2) 0.034(2) -0.0016(16) 0.0171(19) 0.0068(18) O7 0.048(2) 0.020(2) 0.053(3) -0.0081(18) 0.008(2) -0.0044(18) O8 0.049(2) 0.023(2) 0.034(2) 0.0149(16) -0.0051(18) -0.0032(18) O9 0.031(2) 0.046(3) 0.033(2) 0.0175(18) -0.0094(17) -0.0039(18) C1 0.034(3) 0.023(3) 0.025(3) 0.007(2) 0.002(2) 0.004(2) C2 0.035(3) 0.019(3) 0.023(3) 0.004(2) 0.003(2) 0.005(2) C3 0.029(3) 0.016(2) 0.028(3) 0.002(2) 0.005(2) 0.000(2) C4 0.026(3) 0.024(3) 0.030(3) 0.010(2) 0.003(2) 0.004(2) C5 0.033(3) 0.030(3) 0.028(3) 0.009(2) 0.006(2) -0.001(2) C6 0.033(3) 0.021(3) 0.034(3) 0.012(2) 0.001(2) 0.001(2) C7 0.021(2) 0.025(3) 0.032(3) 0.012(2) 0.004(2) 0.005(2) C8 0.027(3) 0.022(3) 0.030(3) 0.009(2) 0.003(2) 0.002(2) C9 0.045(3) 0.019(3) 0.039(3) 0.009(2) 0.010(3) 0.007(2) C10 0.038(3) 0.022(3) 0.035(3) 0.009(2) 0.007(2) 0.001(2) C11 0.034(3) 0.023(3) 0.034(3) 0.009(2) 0.006(2) 0.005(2) C12 0.023(2) 0.018(3) 0.024(3) 0.0031(19) 0.000(2) -0.005(2) C13 0.025(3) 0.017(3) 0.022(2) 0.0022(19) 0.0018(19) 0.007(2) C14 0.024(3) 0.015(2) 0.025(3) 0.0057(19) 0.0008(19) 0.004(2) C15 0.029(3) 0.017(2) 0.022(2) 0.0047(19) 0.001(2) 0.002(2) C16 0.026(2) 0.010(2) 0.028(3) 0.0023(18) 0.001(2) 0.0037(19) C17 0.024(2) 0.012(2) 0.037(3) 0.003(2) 0.003(2) 0.0000(19) C18 0.028(3) 0.016(2) 0.029(3) 0.006(2) 0.009(2) 0.003(2) C19 0.022(2) 0.013(2) 0.025(2) 0.0033(18) 0.0033(19) 0.0042(19) C20 0.025(3) 0.015(2) 0.019(2) 0.0050(17) 0.0030(18) 0.003(2) C21 0.018(2) 0.017(2) 0.028(3) 0.0045(19) 0.0023(19) 0.004(2) C22 0.022(2) 0.016(2) 0.026(3) 0.0038(19) 0.004(2) 0.003(2) C23 0.024(2) 0.016(2) 0.025(2) 0.0058(19) 0.0058(19) 0.0066(19) C24 0.026(2) 0.019(3) 0.024(3) 0.0038(19) 0.001(2) 0.000(2) C25 0.025(2) 0.016(2) 0.022(2) 0.0051(18) 0.001(2) -0.004(2) C26 0.025(3) 0.023(3) 0.026(3) 0.004(2) 0.001(2) 0.008(2) C27 0.036(3) 0.018(3) 0.027(3) 0.004(2) -0.001(2) 0.005(2) _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 2.112(4) 1_565 ? Mn1 O9 2.120(4) 2_776 ? Mn1 O1 2.192(5) . ? Mn1 N5 2.231(5) 1_664 ? Mn1 O8 2.237(4) . ? Mn1 H2W 2.14(15) . ? Mn2 N1 2.175(4) 2_777 ? Mn2 N1 2.175(4) . ? Mn2 O4 2.221(4) 2_777 ? Mn2 O4 2.221(4) . ? Mn2 O3 2.288(4) 1_455 ? Mn2 O3 2.288(4) 2_877 ? N1 C1 1.318(7) . ? N1 C3 1.363(7) . ? N2 C1 1.361(7) . ? N2 C2 1.391(7) . ? N2 C4 1.430(6) . ? N3 C5 1.332(7) . ? N3 C6 1.352(7) . ? N4 C9 1.364(7) . ? N4 C11 1.366(7) . ? N4 C7 1.432(7) . ? N5 C9 1.318(7) . ? N5 C10 1.389(7) . ? N5 Mn1 2.231(5) 1_446 ? O1 H2W 0.80(15) . ? O1 H1W 0.76(8) . ? O2 C25 1.291(6) . ? O2 H2 0.8200 . ? O3 C25 1.238(6) . ? O3 Mn2 2.288(4) 1_655 ? O4 C12 1.254(6) . ? O5 C12 1.252(6) . ? O6 C27 1.274(7) . ? O6 Mn1 2.112(4) 1_545 ? O7 C27 1.241(7) . ? O8 C26 1.257(6) . ? O9 C26 1.261(6) . ? O9 Mn1 2.120(4) 2_776 ? C1 H1A 0.9300 . ? C2 C3 1.346(7) . ? C2 H2A 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.387(8) . ? C4 C8 1.387(7) . ? C5 H5 0.9300 . ? C6 C7 1.386(8) . ? C6 H6 0.9300 . ? C7 C8 1.390(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.362(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.518(7) . ? C13 C18 1.399(7) . ? C13 C14 1.400(7) . ? C14 C15 1.394(7) . ? C14 C19 1.494(7) . ? C15 C16 1.390(7) . ? C15 H15 0.9300 . ? C16 C17 1.384(7) . ? C16 C27 1.518(7) . ? C17 C18 1.392(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.392(7) . ? C19 C24 1.394(7) . ? C20 C21 1.406(7) . ? C20 H20 0.9300 . ? C21 C22 1.398(7) . ? C21 C25 1.497(7) . ? C22 C23 1.396(7) . ? C22 H22 0.9300 . ? C23 C24 1.412(7) . ? C23 C26 1.500(7) . ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Mn1 O9 103.98(18) 1_565 2_776 ? O6 Mn1 O1 167.98(18) 1_565 . ? O9 Mn1 O1 86.9(2) 2_776 . ? O6 Mn1 N5 86.65(18) 1_565 1_664 ? O9 Mn1 N5 112.60(16) 2_776 1_664 ? O1 Mn1 N5 84.47(18) . 1_664 ? O6 Mn1 O8 89.37(17) 1_565 . ? O9 Mn1 O8 128.48(15) 2_776 . ? O1 Mn1 O8 87.61(19) . . ? N5 Mn1 O8 117.76(17) 1_664 . ? O6 Mn1 H2W 149(4) 1_565 . ? O9 Mn1 H2W 107(4) 2_776 . ? O1 Mn1 H2W 21(4) . . ? N5 Mn1 H2W 84(4) 1_664 . ? O8 Mn1 H2W 69(4) . . ? N1 Mn2 N1 180.000(2) 2_777 . ? N1 Mn2 O4 94.05(17) 2_777 2_777 ? N1 Mn2 O4 85.95(17) . 2_777 ? N1 Mn2 O4 85.95(17) 2_777 . ? N1 Mn2 O4 94.05(17) . . ? O4 Mn2 O4 180.000(2) 2_777 . ? N1 Mn2 O3 88.85(16) 2_777 1_455 ? N1 Mn2 O3 91.15(16) . 1_455 ? O4 Mn2 O3 94.44(15) 2_777 1_455 ? O4 Mn2 O3 85.56(15) . 1_455 ? N1 Mn2 O3 91.15(16) 2_777 2_877 ? N1 Mn2 O3 88.85(16) . 2_877 ? O4 Mn2 O3 85.56(15) 2_777 2_877 ? O4 Mn2 O3 94.44(15) . 2_877 ? O3 Mn2 O3 180.000(1) 1_455 2_877 ? C1 N1 C3 106.3(4) . . ? C1 N1 Mn2 128.0(4) . . ? C3 N1 Mn2 125.2(4) . . ? C1 N2 C2 106.7(4) . . ? C1 N2 C4 126.5(4) . . ? C2 N2 C4 126.6(4) . . ? C5 N3 C6 117.3(5) . . ? C9 N4 C11 106.1(4) . . ? C9 N4 C7 126.1(5) . . ? C11 N4 C7 127.8(4) . . ? C9 N5 C10 104.9(4) . . ? C9 N5 Mn1 128.7(4) . 1_446 ? C10 N5 Mn1 126.4(4) . 1_446 ? Mn1 O1 H2W 76(10) . . ? Mn1 O1 H1W 119(5) . . ? H2W O1 H1W 123(10) . . ? C25 O2 H2 109.5 . . ? C25 O3 Mn2 137.1(3) . 1_655 ? C12 O4 Mn2 136.4(3) . . ? C27 O6 Mn1 133.3(4) . 1_545 ? C26 O8 Mn1 99.7(3) . . ? C26 O9 Mn1 168.7(4) . 2_776 ? N1 C1 N2 110.6(5) . . ? N1 C1 H1A 124.7 . . ? N2 C1 H1A 124.7 . . ? C3 C2 N2 105.6(4) . . ? C3 C2 H2A 127.2 . . ? N2 C2 H2A 127.2 . . ? C2 C3 N1 110.7(5) . . ? C2 C3 H3 124.6 . . ? N1 C3 H3 124.6 . . ? C5 C4 C8 119.5(5) . . ? C5 C4 N2 119.0(5) . . ? C8 C4 N2 121.4(5) . . ? N3 C5 C4 123.5(5) . . ? N3 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? N3 C6 C7 122.0(5) . . ? N3 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C8 120.4(5) . . ? C6 C7 N4 119.4(4) . . ? C8 C7 N4 120.2(5) . . ? C4 C8 C7 116.8(5) . . ? C4 C8 H8 121.6 . . ? C7 C8 H8 121.6 . . ? N5 C9 N4 112.4(5) . . ? N5 C9 H9 123.8 . . ? N4 C9 H9 123.8 . . ? C11 C10 N5 109.4(5) . . ? C11 C10 H10 125.3 . . ? N5 C10 H10 125.3 . . ? N4 C11 C10 107.2(5) . . ? N4 C11 H11 126.4 . . ? C10 C11 H11 126.4 . . ? O5 C12 O4 126.2(5) . . ? O5 C12 C13 115.4(5) . . ? O4 C12 C13 118.3(4) . . ? C18 C13 C14 120.0(4) . . ? C18 C13 C12 117.0(4) . . ? C14 C13 C12 123.0(4) . . ? C15 C14 C13 118.2(5) . . ? C15 C14 C19 119.0(4) . . ? C13 C14 C19 122.7(4) . . ? C16 C15 C14 122.1(5) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C17 C16 C15 119.1(5) . . ? C17 C16 C27 119.2(4) . . ? C15 C16 C27 121.6(5) . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.4(5) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C20 C19 C24 118.6(4) . . ? C20 C19 C14 122.1(4) . . ? C24 C19 C14 119.3(4) . . ? C19 C20 C21 121.1(4) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 119.8(4) . . ? C22 C21 C25 121.4(4) . . ? C20 C21 C25 118.8(4) . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 119.3(4) . . ? C22 C23 C26 121.1(4) . . ? C24 C23 C26 119.0(4) . . ? C19 C24 C23 121.3(4) . . ? C19 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? O3 C25 O2 125.4(4) . . ? O3 C25 C21 120.4(4) . . ? O2 C25 C21 114.2(4) . . ? O8 C26 O9 121.3(5) . . ? O8 C26 C23 119.6(4) . . ? O9 C26 C23 119.0(5) . . ? O7 C27 O6 125.5(5) . . ? O7 C27 C16 117.5(5) . . ? O6 C27 C16 116.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Mn2 N1 C1 21(100) 2_777 . . . ? O4 Mn2 N1 C1 140.5(5) 2_777 . . . ? O4 Mn2 N1 C1 -39.5(5) . . . . ? O3 Mn2 N1 C1 46.2(5) 1_455 . . . ? O3 Mn2 N1 C1 -133.8(5) 2_877 . . . ? N1 Mn2 N1 C3 -169(100) 2_777 . . . ? O4 Mn2 N1 C3 -49.0(4) 2_777 . . . ? O4 Mn2 N1 C3 131.0(4) . . . . ? O3 Mn2 N1 C3 -143.4(4) 1_455 . . . ? O3 Mn2 N1 C3 36.6(4) 2_877 . . . ? N1 Mn2 O4 C12 130.9(5) 2_777 . . . ? N1 Mn2 O4 C12 -49.1(5) . . . . ? O4 Mn2 O4 C12 -102(100) 2_777 . . . ? O3 Mn2 O4 C12 -140.0(5) 1_455 . . . ? O3 Mn2 O4 C12 40.0(5) 2_877 . . . ? O6 Mn1 O8 C26 107.8(4) 1_565 . . . ? O9 Mn1 O8 C26 0.3(4) 2_776 . . . ? O1 Mn1 O8 C26 -83.9(4) . . . . ? N5 Mn1 O8 C26 -166.3(3) 1_664 . . . ? C3 N1 C1 N2 -0.2(6) . . . . ? Mn2 N1 C1 N2 171.6(4) . . . . ? C2 N2 C1 N1 -0.1(6) . . . . ? C4 N2 C1 N1 -175.4(5) . . . . ? C1 N2 C2 C3 0.5(6) . . . . ? C4 N2 C2 C3 175.7(5) . . . . ? N2 C2 C3 N1 -0.6(6) . . . . ? C1 N1 C3 C2 0.6(6) . . . . ? Mn2 N1 C3 C2 -171.6(4) . . . . ? C1 N2 C4 C5 23.4(8) . . . . ? C2 N2 C4 C5 -150.9(5) . . . . ? C1 N2 C4 C8 -158.8(5) . . . . ? C2 N2 C4 C8 26.8(8) . . . . ? C6 N3 C5 C4 -3.7(8) . . . . ? C8 C4 C5 N3 6.1(8) . . . . ? N2 C4 C5 N3 -176.1(5) . . . . ? C5 N3 C6 C7 -3.1(8) . . . . ? N3 C6 C7 C8 7.4(8) . . . . ? N3 C6 C7 N4 -175.3(5) . . . . ? C9 N4 C7 C6 25.8(8) . . . . ? C11 N4 C7 C6 -151.7(5) . . . . ? C9 N4 C7 C8 -156.9(5) . . . . ? C11 N4 C7 C8 25.5(8) . . . . ? C5 C4 C8 C7 -1.6(7) . . . . ? N2 C4 C8 C7 -179.3(4) . . . . ? C6 C7 C8 C4 -4.8(7) . . . . ? N4 C7 C8 C4 178.0(5) . . . . ? C10 N5 C9 N4 0.2(7) . . . . ? Mn1 N5 C9 N4 178.8(4) 1_446 . . . ? C11 N4 C9 N5 0.6(7) . . . . ? C7 N4 C9 N5 -177.4(5) . . . . ? C9 N5 C10 C11 -0.8(6) . . . . ? Mn1 N5 C10 C11 -179.5(4) 1_446 . . . ? C9 N4 C11 C10 -1.0(6) . . . . ? C7 N4 C11 C10 176.9(5) . . . . ? N5 C10 C11 N4 1.2(6) . . . . ? Mn2 O4 C12 O5 0.4(8) . . . . ? Mn2 O4 C12 C13 177.3(3) . . . . ? O5 C12 C13 C18 55.8(6) . . . . ? O4 C12 C13 C18 -121.5(5) . . . . ? O5 C12 C13 C14 -125.5(5) . . . . ? O4 C12 C13 C14 57.2(7) . . . . ? C18 C13 C14 C15 -0.8(7) . . . . ? C12 C13 C14 C15 -179.5(5) . . . . ? C18 C13 C14 C19 -177.2(5) . . . . ? C12 C13 C14 C19 4.1(7) . . . . ? C13 C14 C15 C16 3.2(7) . . . . ? C19 C14 C15 C16 179.8(4) . . . . ? C14 C15 C16 C17 -2.4(8) . . . . ? C14 C15 C16 C27 -179.0(5) . . . . ? C15 C16 C17 C18 -0.8(8) . . . . ? C27 C16 C17 C18 175.8(5) . . . . ? C16 C17 C18 C13 3.2(8) . . . . ? C14 C13 C18 C17 -2.4(7) . . . . ? C12 C13 C18 C17 176.4(5) . . . . ? C15 C14 C19 C20 -130.1(5) . . . . ? C13 C14 C19 C20 46.2(7) . . . . ? C15 C14 C19 C24 48.9(7) . . . . ? C13 C14 C19 C24 -134.7(5) . . . . ? C24 C19 C20 C21 -0.8(7) . . . . ? C14 C19 C20 C21 178.3(5) . . . . ? C19 C20 C21 C22 1.9(7) . . . . ? C19 C20 C21 C25 179.6(4) . . . . ? C20 C21 C22 C23 -1.5(7) . . . . ? C25 C21 C22 C23 -179.0(4) . . . . ? C21 C22 C23 C24 -0.2(7) . . . . ? C21 C22 C23 C26 171.1(4) . . . . ? C20 C19 C24 C23 -0.9(7) . . . . ? C14 C19 C24 C23 -180.0(4) . . . . ? C22 C23 C24 C19 1.4(7) . . . . ? C26 C23 C24 C19 -170.1(5) . . . . ? Mn2 O3 C25 O2 -26.8(9) 1_655 . . . ? Mn2 O3 C25 C21 152.6(4) 1_655 . . . ? C22 C21 C25 O3 -154.5(5) . . . . ? C20 C21 C25 O3 28.0(7) . . . . ? C22 C21 C25 O2 25.0(7) . . . . ? C20 C21 C25 O2 -152.5(5) . . . . ? Mn1 O8 C26 O9 4.9(6) . . . . ? Mn1 O8 C26 C23 -171.3(4) . . . . ? Mn1 O9 C26 O8 -159.6(18) 2_776 . . . ? Mn1 O9 C26 C23 17(2) 2_776 . . . ? C22 C23 C26 O8 7.3(7) . . . . ? C24 C23 C26 O8 178.5(5) . . . . ? C22 C23 C26 O9 -169.0(5) . . . . ? C24 C23 C26 O9 2.3(7) . . . . ? Mn1 O6 C27 O7 -13.4(9) 1_545 . . . ? Mn1 O6 C27 C16 163.6(3) 1_545 . . . ? C17 C16 C27 O7 27.0(7) . . . . ? C15 C16 C27 O7 -156.4(5) . . . . ? C17 C16 C27 O6 -150.3(5) . . . . ? C15 C16 C27 O6 26.3(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O5 0.82 1.66 2.441(5) 158.3 2_877 O1 H2W O8 0.80(15) 2.49(14) 3.066(7) 129(13) . O1 H1W O7 0.76(8) 1.88(8) 2.629(7) 170(7) 2_766 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.217 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.110