# 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_1 _database_code_depnum_ccdc_archive 'CCDC 842659' #TrackingRef 'Complex 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H40 Mn3 N4 O12' _chemical_formula_weight 1173.78 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 8.1573(8) _cell_length_b 13.7300(14) _cell_length_c 13.9981(14) _cell_angle_alpha 62.583(2) _cell_angle_beta 86.744(2) _cell_angle_gamma 87.794(2) _cell_volume 1389.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7548 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 26.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 599 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7548 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.03 _reflns_number_total 5313 _reflns_number_gt 4447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0750P)^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 5313 _refine_ls_number_parameters 382 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 -1.0000 0.0000 0.5000 0.02523(12) Uani 1 2 d S . . Mn2 Mn -1.23789(3) -0.13299(2) 0.74643(2) 0.03018(11) Uani 1 1 d . . . O3 O -1.14721(18) 0.01895(12) 0.62784(12) 0.0358(3) Uani 1 1 d . . . O1 O -1.34350(19) -0.19486(13) 0.65270(13) 0.0430(4) Uani 1 1 d . . . O5 O -1.02758(19) -0.23057(15) 0.77229(14) 0.0552(5) Uani 1 1 d . . . O2 O -1.19222(19) -0.10310(13) 0.50072(12) 0.0433(4) Uani 1 1 d . . . O4 O -1.1861(2) 0.05344(14) 0.76520(14) 0.0579(5) Uani 1 1 d . . . N1 N -1.4900(2) -0.09351(15) 0.79324(14) 0.0363(4) Uani 1 1 d . . . C14 C -0.7503(3) -0.28396(19) 0.76957(18) 0.0395(5) Uani 1 1 d D . . N2 N -1.2454(2) -0.19340(16) 0.92682(15) 0.0430(5) Uani 1 1 d . . . C13 C -0.8952(3) -0.21361(18) 0.71636(17) 0.0365(5) Uani 1 1 d . . . C1 C -1.2896(3) -0.17744(17) 0.56004(18) 0.0354(5) Uani 1 1 d . . . C7 C -1.1529(2) 0.08570(17) 0.66917(18) 0.0343(5) Uani 1 1 d . . . C8 C -1.1129(3) 0.20155(19) 0.5940(2) 0.0453(6) Uani 1 1 d D . . C15 C -0.7598(3) -0.3653(2) 0.86899(19) 0.0459(6) Uani 1 1 d D . . C3 C -1.4234(3) -0.3412(2) 0.5706(2) 0.0499(6) Uani 1 1 d D . . C2 C -1.3423(3) -0.2504(2) 0.5160(2) 0.0502(6) Uani 1 1 d D . . C30 C -1.3841(3) -0.1670(2) 0.96886(18) 0.0437(5) Uani 1 1 d . . . C29 C -1.5154(3) -0.11351(19) 0.89720(17) 0.0383(5) Uani 1 1 d . . . C9 C -1.0991(4) 0.2760(2) 0.6267(2) 0.0526(6) Uani 1 1 d D . . C19 C -1.6084(3) -0.0418(2) 0.7258(2) 0.0465(6) Uani 1 1 d . . . H19A H -1.5916 -0.0265 0.6540 0.056 Uiso 1 1 calc R . . C10 C -1.0502(4) 0.3906(2) 0.5604(2) 0.0573(7) Uani 1 1 d . . . C11 C -1.0079(4) 0.4331(2) 0.4514(2) 0.0681(8) Uani 1 1 d . . . H11A H -1.0138 0.3886 0.4178 0.082 Uiso 1 1 calc R . . C12 C -0.9569(5) 0.5410(2) 0.3912(2) 0.0693(8) Uani 1 1 d . . . H12A H -0.9275 0.5676 0.3184 0.083 Uiso 1 1 calc R . . C22 C -1.6610(3) -0.0839(2) 0.9363(2) 0.0524(6) Uani 1 1 d . . . C21 C -1.7836(3) -0.0305(3) 0.8617(2) 0.0605(7) Uani 1 1 d . . . H21A H -1.8827 -0.0097 0.8838 0.073 Uiso 1 1 calc R . . C20 C -1.7562(3) -0.0094(3) 0.7575(2) 0.0581(7) Uani 1 1 d . . . H20A H -1.8359 0.0266 0.7076 0.070 Uiso 1 1 calc R . . C28 C -1.1201(4) -0.2385(3) 0.9909(2) 0.0660(8) Uani 1 1 d . . . H28A H -1.0248 -0.2576 0.9633 0.079 Uiso 1 1 calc R . . C23 C -1.6742(4) -0.1061(3) 1.0470(2) 0.0700(9) Uani 1 1 d . . . H23A H -1.7704 -0.0866 1.0734 0.084 Uiso 1 1 calc R . . C25 C -1.4011(4) -0.1858(3) 1.0765(2) 0.0644(8) Uani 1 1 d . . . C24 C -1.5514(4) -0.1542(3) 1.1134(2) 0.0768(9) Uani 1 1 d . . . H24A H -1.5639 -0.1674 1.1848 0.092 Uiso 1 1 calc R . . C26 C -1.2656(5) -0.2334(3) 1.1406(2) 0.0905(12) Uani 1 1 d . . . H26A H -1.2713 -0.2479 1.2124 0.109 Uiso 1 1 calc R . . C5 C -1.5345(6) -0.5172(3) 0.6011(3) 0.1147(18) Uani 1 1 d . . . H5A H -1.5607 -0.5319 0.6720 0.138 Uiso 1 1 calc R . . C27 C -1.1271(5) -0.2582(4) 1.0984(3) 0.0959(13) Uani 1 1 d . . . H27A H -1.0368 -0.2883 1.1407 0.115 Uiso 1 1 calc R . . C6 C -1.5688(6) -0.5947(3) 0.5679(3) 0.1148(19) Uani 1 1 d . . . H6A H -1.6165 -0.6601 0.6177 0.138 Uiso 1 1 calc R . . C4 C -1.4638(3) -0.4208(2) 0.5331(2) 0.0502(6) Uani 1 1 d . . . O6 O -0.87378(19) -0.14157(13) 0.62131(12) 0.0438(4) Uani 1 1 d . . . C17 C -0.6609(3) -0.5186(2) 1.0374(2) 0.0527(7) Uani 1 1 d . . . H17A H -0.7697 -0.5313 1.0630 0.063 Uiso 1 1 calc R . . C18 C -0.5388(3) -0.5832(2) 1.1022(2) 0.0504(7) Uani 1 1 d . . . H18A H -0.5662 -0.6389 1.1705 0.061 Uiso 1 1 calc R . . C16 C -0.6252(3) -0.43410(19) 0.93362(18) 0.0448(6) Uani 1 1 d . . . H5 H -0.6528(19) -0.265(2) 0.7288(18) 0.056(8) Uiso 1 1 d D . . H6 H -0.8646(17) -0.378(2) 0.9022(19) 0.057(8) Uiso 1 1 d D . . H4 H -1.119(3) 0.251(2) 0.7003(9) 0.058(8) Uiso 1 1 d D . . H3 H -1.090(3) 0.224(2) 0.5209(10) 0.063(8) Uiso 1 1 d D . . H1 H -1.308(3) -0.231(2) 0.4451(11) 0.069(9) Uiso 1 1 d D . . H2 H -1.447(4) -0.360(2) 0.6426(10) 0.074(9) Uiso 1 1 d 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 0.0304(2) 0.0220(2) 0.0210(2) -0.00770(17) -0.00296(15) -0.00026(16) Mn2 0.02933(18) 0.03137(19) 0.02529(18) -0.00925(14) -0.00116(12) 0.00137(12) O3 0.0444(8) 0.0309(8) 0.0352(8) -0.0184(6) 0.0062(6) -0.0040(6) O1 0.0496(9) 0.0470(9) 0.0403(9) -0.0270(8) 0.0068(7) -0.0126(7) O5 0.0409(9) 0.0567(11) 0.0437(10) -0.0037(8) -0.0009(7) 0.0190(8) O2 0.0505(9) 0.0454(9) 0.0388(9) -0.0225(7) 0.0026(7) -0.0182(8) O4 0.0871(13) 0.0483(10) 0.0405(10) -0.0237(8) 0.0173(9) -0.0132(9) N1 0.0327(9) 0.0485(11) 0.0315(10) -0.0217(8) -0.0016(7) -0.0014(8) C14 0.0360(11) 0.0401(13) 0.0334(12) -0.0095(10) -0.0063(9) 0.0120(10) N2 0.0481(11) 0.0446(11) 0.0315(10) -0.0132(8) -0.0050(8) 0.0020(9) C13 0.0392(11) 0.0352(12) 0.0305(11) -0.0111(9) -0.0079(9) 0.0095(9) C1 0.0366(11) 0.0347(12) 0.0401(12) -0.0211(10) -0.0034(9) -0.0029(9) C7 0.0343(11) 0.0311(11) 0.0384(12) -0.0170(9) 0.0017(9) 0.0008(8) C8 0.0587(15) 0.0332(12) 0.0428(14) -0.0172(11) 0.0027(11) 0.0025(10) C15 0.0359(12) 0.0456(14) 0.0386(13) -0.0048(11) -0.0056(10) 0.0107(10) C3 0.0609(15) 0.0480(15) 0.0505(16) -0.0305(13) 0.0057(12) -0.0170(12) C2 0.0652(16) 0.0512(15) 0.0447(15) -0.0307(12) 0.0082(12) -0.0212(12) C30 0.0556(14) 0.0453(14) 0.0298(12) -0.0171(10) 0.0018(10) -0.0042(11) C29 0.0400(11) 0.0449(13) 0.0341(12) -0.0219(10) 0.0041(9) -0.0062(10) C9 0.0763(18) 0.0352(13) 0.0451(15) -0.0179(12) 0.0016(13) -0.0011(12) C19 0.0361(12) 0.0670(17) 0.0451(14) -0.0333(13) -0.0065(10) 0.0057(11) C10 0.0848(19) 0.0351(13) 0.0536(16) -0.0216(12) -0.0021(14) -0.0025(13) C11 0.114(3) 0.0389(15) 0.0578(18) -0.0275(13) -0.0017(17) -0.0081(15) C12 0.120(3) 0.0376(14) 0.0501(16) -0.0196(12) -0.0019(16) -0.0068(16) C22 0.0483(14) 0.0676(17) 0.0502(15) -0.0357(14) 0.0091(11) -0.0049(12) C21 0.0364(13) 0.088(2) 0.073(2) -0.0524(17) 0.0053(12) 0.0056(13) C20 0.0375(13) 0.086(2) 0.0684(19) -0.0500(17) -0.0113(12) 0.0106(13) C28 0.0696(18) 0.077(2) 0.0444(15) -0.0222(14) -0.0225(13) 0.0240(15) C23 0.0679(19) 0.100(3) 0.0534(18) -0.0476(18) 0.0211(15) -0.0065(17) C25 0.086(2) 0.072(2) 0.0328(14) -0.0229(13) -0.0021(13) 0.0017(16) C24 0.095(2) 0.102(3) 0.0376(16) -0.0377(17) 0.0137(16) -0.003(2) C26 0.114(3) 0.116(3) 0.0320(15) -0.0262(18) -0.0189(17) 0.026(2) C5 0.211(5) 0.096(3) 0.062(2) -0.057(2) 0.054(3) -0.097(3) C27 0.101(3) 0.126(3) 0.0485(19) -0.029(2) -0.0354(18) 0.039(2) C6 0.215(5) 0.082(2) 0.066(2) -0.049(2) 0.051(3) -0.100(3) C4 0.0625(15) 0.0456(14) 0.0504(15) -0.0285(12) 0.0076(12) -0.0187(12) O6 0.0488(9) 0.0402(9) 0.0301(8) -0.0059(7) -0.0090(7) 0.0145(7) C17 0.0359(12) 0.0511(15) 0.0433(14) 0.0015(11) -0.0027(10) 0.0067(10) C18 0.0421(13) 0.0437(14) 0.0366(13) 0.0057(10) -0.0028(10) 0.0076(10) C16 0.0409(12) 0.0411(13) 0.0352(12) -0.0032(10) -0.0062(9) 0.0109(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 O2 2.1491(15) 2_356 ? Mn1 O2 2.1491(15) . ? Mn1 O6 2.1741(14) 2_356 ? Mn1 O6 2.1741(14) . ? Mn1 O3 2.2075(14) 2_356 ? Mn1 O3 2.2075(14) . ? Mn2 O5 2.0775(15) . ? Mn2 O1 2.0968(16) . ? Mn2 O3 2.1083(15) . ? Mn2 N1 2.2455(17) . ? Mn2 N2 2.2639(19) . ? O3 C7 1.288(3) . ? O1 C1 1.261(3) . ? O5 C13 1.260(3) . ? O2 C1 1.253(3) . ? O4 C7 1.223(3) . ? N1 C19 1.327(3) . ? N1 C29 1.356(3) . ? C14 C15 1.324(3) . ? C14 C13 1.495(3) . ? N2 C28 1.333(3) . ? N2 C30 1.359(3) . ? C13 O6 1.247(3) . ? C1 C2 1.483(3) . ? C7 C8 1.484(3) . ? C8 C9 1.307(4) . ? C15 C16 1.470(3) . ? C3 C2 1.306(4) . ? C3 C4 1.468(3) . ? C30 C25 1.406(3) . ? C30 C29 1.441(3) . ? C29 C22 1.403(3) . ? C9 C10 1.469(4) . ? C19 C20 1.389(3) . ? C10 C11 1.387(4) . ? C10 C12 1.393(4) 2_366 ? C11 C12 1.392(4) . ? C12 C10 1.393(4) 2_366 ? C22 C21 1.409(4) . ? C22 C23 1.433(4) . ? C21 C20 1.356(4) . ? C28 C27 1.399(4) . ? C23 C24 1.339(5) . ? C25 C26 1.404(4) . ? C25 C24 1.432(4) . ? C26 C27 1.349(5) . ? C5 C4 1.351(4) . ? C5 C6 1.385(4) . ? C6 C4 1.342(4) 2_246 ? C4 C6 1.342(4) 2_246 ? C17 C18 1.377(3) . ? C17 C16 1.402(3) . ? C18 C16 1.392(3) 2_447 ? C16 C18 1.392(3) 2_447 ? 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 O2 Mn1 O2 180.0 2_356 . ? O2 Mn1 O6 90.63(6) 2_356 2_356 ? O2 Mn1 O6 89.37(6) . 2_356 ? O2 Mn1 O6 89.37(6) 2_356 . ? O2 Mn1 O6 90.63(6) . . ? O6 Mn1 O6 180.00(13) 2_356 . ? O2 Mn1 O3 86.89(6) 2_356 2_356 ? O2 Mn1 O3 93.11(6) . 2_356 ? O6 Mn1 O3 90.15(6) 2_356 2_356 ? O6 Mn1 O3 89.85(6) . 2_356 ? O2 Mn1 O3 93.11(6) 2_356 . ? O2 Mn1 O3 86.89(6) . . ? O6 Mn1 O3 89.85(6) 2_356 . ? O6 Mn1 O3 90.15(6) . . ? O3 Mn1 O3 180.00(7) 2_356 . ? O5 Mn2 O1 94.00(8) . . ? O5 Mn2 O3 100.55(6) . . ? O1 Mn2 O3 101.87(6) . . ? O5 Mn2 N1 153.32(7) . . ? O1 Mn2 N1 89.53(6) . . ? O3 Mn2 N1 104.58(6) . . ? O5 Mn2 N2 84.91(7) . . ? O1 Mn2 N2 131.28(7) . . ? O3 Mn2 N2 126.28(7) . . ? N1 Mn2 N2 73.09(7) . . ? C7 O3 Mn2 107.65(13) . . ? C7 O3 Mn1 136.65(13) . . ? Mn2 O3 Mn1 111.38(6) . . ? C1 O1 Mn2 124.33(13) . . ? C13 O5 Mn2 130.04(14) . . ? C1 O2 Mn1 144.19(15) . . ? C19 N1 C29 117.77(19) . . ? C19 N1 Mn2 125.44(15) . . ? C29 N1 Mn2 116.34(14) . . ? C15 C14 C13 122.5(2) . . ? C28 N2 C30 118.1(2) . . ? C28 N2 Mn2 125.82(18) . . ? C30 N2 Mn2 115.45(14) . . ? O6 C13 O5 125.60(19) . . ? O6 C13 C14 117.21(19) . . ? O5 C13 C14 117.16(19) . . ? O2 C1 O1 125.4(2) . . ? O2 C1 C2 116.0(2) . . ? O1 C1 C2 118.64(19) . . ? O4 C7 O3 121.0(2) . . ? O4 C7 C8 123.0(2) . . ? O3 C7 C8 115.93(19) . . ? C9 C8 C7 122.5(2) . . ? C14 C15 C16 127.9(2) . . ? C2 C3 C4 126.7(2) . . ? C3 C2 C1 125.1(2) . . ? N2 C30 C25 122.9(2) . . ? N2 C30 C29 117.41(19) . . ? C25 C30 C29 119.6(2) . . ? N1 C29 C22 123.1(2) . . ? N1 C29 C30 117.16(19) . . ? C22 C29 C30 119.7(2) . . ? C8 C9 C10 126.8(3) . . ? N1 C19 C20 122.9(2) . . ? C11 C10 C12 118.5(3) . 2_366 ? C11 C10 C9 122.5(2) . . ? C12 C10 C9 119.0(3) 2_366 . ? C10 C11 C12 121.3(3) . . ? C11 C12 C10 120.2(3) . 2_366 ? C29 C22 C21 116.9(2) . . ? C29 C22 C23 118.8(3) . . ? C21 C22 C23 124.3(2) . . ? C20 C21 C22 119.6(2) . . ? C21 C20 C19 119.7(2) . . ? N2 C28 C27 122.2(3) . . ? C24 C23 C22 121.6(3) . . ? C26 C25 C30 116.7(3) . . ? C26 C25 C24 124.3(3) . . ? C30 C25 C24 119.0(3) . . ? C23 C24 C25 121.2(3) . . ? C27 C26 C25 120.4(3) . . ? C4 C5 C6 121.6(3) . . ? C26 C27 C28 119.7(3) . . ? C4 C6 C5 122.8(3) 2_246 . ? C5 C4 C6 115.6(3) . 2_246 ? C5 C4 C3 120.9(2) . . ? C6 C4 C3 123.5(2) 2_246 . ? C13 O6 Mn1 139.88(14) . . ? C18 C17 C16 121.6(2) . . ? C17 C18 C16 120.6(2) . 2_447 ? C18 C16 C17 117.8(2) 2_447 . ? C18 C16 C15 122.7(2) 2_447 . ? C17 C16 C15 119.4(2) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.404 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.055 data_1a _database_code_depnum_ccdc_archive 'CCDC 894709' #TrackingRef 'CP1a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H40 Mn3 N4 O12' _chemical_formula_weight 1173.78 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 8.0946(9) _cell_length_b 13.7803(14) _cell_length_c 14.0130(15) _cell_angle_alpha 61.930(2) _cell_angle_beta 86.412(2) _cell_angle_gamma 88.182(2) _cell_volume 1376.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7524 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 599 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7524 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.04 _reflns_number_total 5285 _reflns_number_gt 4493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0750P)^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 5285 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.0000 0.0000 0.01652(12) Uani 1 2 d S . . Mn2 Mn -0.24305(3) -0.13701(2) 0.24710(2) 0.01981(11) Uani 1 1 d . . . O4 O 0.14799(17) -0.01574(11) -0.12959(11) 0.0231(3) Uani 1 1 d . . . O2 O -0.35024(18) -0.19461(12) 0.15082(11) 0.0274(3) Uani 1 1 d . . . O5 O -0.12184(18) 0.14451(11) -0.12114(11) 0.0289(3) Uani 1 1 d . . . O3 O 0.1925(2) -0.05256(13) -0.26574(12) 0.0380(4) Uani 1 1 d . . . O1 O -0.19521(19) -0.10000(12) -0.00208(12) 0.0291(3) Uani 1 1 d . . . N1 N -0.2462(2) -0.19450(14) 0.42749(14) 0.0273(4) Uani 1 1 d . . . C7 C 0.1552(2) -0.08383(16) -0.16936(16) 0.0228(4) Uani 1 1 d . . . N2 N -0.4955(2) -0.09817(14) 0.29516(14) 0.0244(4) Uani 1 1 d . . . C13 C -0.0996(3) 0.21824(16) -0.21691(16) 0.0238(4) Uani 1 1 d . . . C30 C -0.5184(3) -0.11638(17) 0.39910(16) 0.0254(4) Uani 1 1 d . . . C1 C -0.2938(3) -0.17529(16) 0.05772(16) 0.0235(4) Uani 1 1 d . . . C8 C 0.1123(3) -0.19985(17) -0.09328(18) 0.0295(5) Uani 1 1 d . . . C14 C -0.2456(3) 0.28748(17) -0.26968(17) 0.0259(5) Uani 1 1 d . . . C16 C -0.3722(3) 0.43586(17) -0.43429(17) 0.0286(5) Uani 1 1 d . . . C15 C -0.2358(3) 0.36919(18) -0.37051(18) 0.0297(5) Uani 1 1 d . . . C18 C -0.3374(3) 0.52097(19) -0.53952(18) 0.0332(5) Uani 1 1 d . . . H18A H -0.2280 0.5355 -0.5664 0.040 Uiso 1 1 calc R . . C26 C -0.7889(3) -0.0339(2) 0.3647(2) 0.0392(6) Uani 1 1 d . . . H26A H -0.8878 -0.0128 0.3873 0.047 Uiso 1 1 calc R . . C2 C -0.3448(3) -0.2486(2) 0.0135(2) 0.0345(5) Uani 1 1 d . . . C17 C -0.5376(3) 0.41635(18) -0.39601(18) 0.0323(5) Uani 1 1 d . . . H17A H -0.5640 0.3606 -0.3265 0.039 Uiso 1 1 calc R . . C25 C -0.6641(3) -0.0854(2) 0.43829(19) 0.0339(5) Uani 1 1 d . . . C22 C -0.3992(3) -0.1826(2) 0.57686(19) 0.0411(6) Uani 1 1 d . . . C28 C -0.6152(3) -0.0486(2) 0.22859(18) 0.0315(5) Uani 1 1 d . . . H28A H -0.5998 -0.0354 0.1572 0.038 Uiso 1 1 calc R . . C29 C -0.3844(3) -0.16656(18) 0.46919(17) 0.0288(5) Uani 1 1 d . . . C24 C -0.6755(3) -0.1051(2) 0.5484(2) 0.0443(6) Uani 1 1 d . . . H24A H -0.7721 -0.0860 0.5753 0.053 Uiso 1 1 calc R . . C27 C -0.7641(3) -0.0151(2) 0.2606(2) 0.0380(6) Uani 1 1 d . . . H27A H -0.8452 0.0196 0.2111 0.046 Uiso 1 1 calc R . . C19 C -0.1197(3) -0.2372(2) 0.4899(2) 0.0429(6) Uani 1 1 d . . . H19A H -0.0249 -0.2566 0.4616 0.052 Uiso 1 1 calc R . . C23 C -0.5495(4) -0.1506(2) 0.6137(2) 0.0480(7) Uani 1 1 d . . . H23A H -0.5604 -0.1616 0.6846 0.058 Uiso 1 1 calc R . . C21 C -0.2610(4) -0.2278(3) 0.6397(2) 0.0585(8) Uani 1 1 d . . . H21A H -0.2642 -0.2394 0.7108 0.070 Uiso 1 1 calc R . . C20 C -0.1227(4) -0.2545(3) 0.5969(2) 0.0593(8) Uani 1 1 d . . . H20A H -0.0310 -0.2840 0.6382 0.071 Uiso 1 1 calc R . . C3 C -0.4270(3) -0.34081(19) 0.0698(2) 0.0336(5) Uani 1 1 d . . . C9 C 0.1020(3) -0.27449(18) -0.12592(19) 0.0346(5) Uani 1 1 d . . . C10 C 0.0509(3) -0.38965(18) -0.0600(2) 0.0378(6) Uani 1 1 d . . . C4 C -0.4658(3) -0.42065(19) 0.03275(19) 0.0336(5) Uani 1 1 d . . . C11 C 0.0024(4) -0.43368(19) 0.0497(2) 0.0442(7) Uani 1 1 d . . . H11A H 0.0043 -0.3900 0.0838 0.053 Uiso 1 1 calc R . . C12 C 0.0484(4) -0.45826(19) -0.1078(2) 0.0448(7) Uani 1 1 d . . . H12A H 0.0817 -0.4306 -0.1806 0.054 Uiso 1 1 calc R . . C6 C -0.5444(5) -0.5162(3) 0.1005(3) 0.0876(15) Uani 1 1 d . . . H6A H -0.5769 -0.5299 0.1706 0.105 Uiso 1 1 calc R . . C5 C -0.4225(6) -0.4064(3) -0.0680(3) 0.0920(16) Uani 1 1 d . . . H5A H -0.3685 -0.3420 -0.1172 0.110 Uiso 1 1 calc R . . O6 O 0.03513(19) 0.23716(13) -0.27341(13) 0.0357(4) Uani 1 1 d . . . H5 H -0.345(3) 0.2704(16) -0.2316(17) 0.018(5) Uiso 1 1 d . . . H6 H -0.127(3) 0.3858(19) -0.407(2) 0.036(7) Uiso 1 1 d . . . H3 H 0.090(3) -0.2179(19) -0.021(2) 0.034(6) Uiso 1 1 d . . . H4 H 0.128(3) -0.256(2) -0.195(2) 0.041(7) Uiso 1 1 d . . . H2 H -0.461(3) -0.359(2) 0.141(2) 0.037(7) Uiso 1 1 d . . . H1 H -0.297(4) -0.230(2) -0.055(3) 0.061(9) 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 0.0200(2) 0.0137(2) 0.0147(2) -0.00560(17) -0.00155(15) -0.00022(16) Mn2 0.01926(18) 0.01956(18) 0.01787(17) -0.00663(13) -0.00079(11) 0.00113(12) O4 0.0290(8) 0.0183(7) 0.0242(7) -0.0122(6) 0.0029(6) -0.0021(6) O2 0.0317(8) 0.0285(8) 0.0267(8) -0.0169(7) 0.0039(6) -0.0072(6) O5 0.0349(8) 0.0244(8) 0.0196(7) -0.0040(6) -0.0055(6) 0.0101(6) O3 0.0603(11) 0.0280(8) 0.0269(8) -0.0151(7) 0.0124(8) -0.0081(8) O1 0.0335(8) 0.0290(8) 0.0279(8) -0.0157(7) 0.0019(6) -0.0117(7) N1 0.0306(10) 0.0249(9) 0.0229(9) -0.0081(8) -0.0038(7) 0.0007(8) C7 0.0226(10) 0.0211(10) 0.0246(10) -0.0112(9) 0.0008(8) 0.0021(8) N2 0.0226(9) 0.0305(10) 0.0241(9) -0.0162(8) -0.0004(7) -0.0027(7) C13 0.0245(11) 0.0213(10) 0.0248(10) -0.0099(9) -0.0051(8) 0.0053(8) C30 0.0272(11) 0.0286(11) 0.0220(10) -0.0134(9) 0.0030(8) -0.0049(9) C1 0.0253(11) 0.0226(10) 0.0246(10) -0.0127(9) -0.0019(8) -0.0013(9) C8 0.0391(13) 0.0199(11) 0.0276(12) -0.0102(9) 0.0040(9) -0.0011(9) C14 0.0231(11) 0.0255(11) 0.0242(11) -0.0078(9) -0.0032(9) 0.0076(9) C16 0.0252(11) 0.0243(11) 0.0262(11) -0.0033(9) -0.0054(8) 0.0065(9) C15 0.0239(11) 0.0282(12) 0.0278(11) -0.0056(10) -0.0035(9) 0.0047(9) C18 0.0227(11) 0.0318(12) 0.0292(12) -0.0014(10) -0.0004(9) 0.0032(9) C26 0.0229(12) 0.0560(16) 0.0507(15) -0.0359(13) 0.0046(10) 0.0021(11) C2 0.0438(14) 0.0347(13) 0.0313(12) -0.0208(11) 0.0054(10) -0.0141(11) C17 0.0287(12) 0.0271(12) 0.0236(11) 0.0024(9) -0.0016(9) 0.0036(9) C25 0.0324(12) 0.0412(14) 0.0344(12) -0.0237(11) 0.0077(10) -0.0055(10) C22 0.0530(16) 0.0450(15) 0.0229(12) -0.0141(11) -0.0010(11) -0.0003(12) C28 0.0256(11) 0.0460(14) 0.0305(12) -0.0240(11) -0.0053(9) 0.0039(10) C29 0.0367(12) 0.0272(11) 0.0221(11) -0.0115(9) 0.0011(9) -0.0020(9) C24 0.0450(15) 0.0584(17) 0.0369(14) -0.0299(13) 0.0123(12) -0.0039(13) C27 0.0260(12) 0.0526(15) 0.0462(14) -0.0318(13) -0.0073(10) 0.0059(11) C19 0.0454(15) 0.0462(15) 0.0320(13) -0.0135(12) -0.0131(11) 0.0136(12) C23 0.0643(18) 0.0576(17) 0.0260(12) -0.0238(13) 0.0089(12) -0.0037(14) C21 0.080(2) 0.070(2) 0.0247(13) -0.0205(14) -0.0155(13) 0.0153(17) C20 0.067(2) 0.072(2) 0.0340(14) -0.0199(15) -0.0258(14) 0.0262(17) C3 0.0416(14) 0.0319(13) 0.0336(13) -0.0207(11) 0.0051(10) -0.0106(10) C9 0.0537(16) 0.0214(11) 0.0281(12) -0.0116(10) 0.0033(11) -0.0014(10) C10 0.0579(16) 0.0203(11) 0.0358(13) -0.0142(10) 0.0040(11) -0.0045(11) C4 0.0402(13) 0.0301(12) 0.0354(12) -0.0196(10) 0.0040(10) -0.0113(10) C11 0.082(2) 0.0241(12) 0.0334(13) -0.0193(11) 0.0042(13) -0.0065(12) C12 0.082(2) 0.0240(12) 0.0286(12) -0.0134(10) 0.0050(12) -0.0065(13) C6 0.165(4) 0.069(2) 0.0453(17) -0.0414(17) 0.046(2) -0.076(3) C5 0.176(4) 0.060(2) 0.0534(19) -0.0403(17) 0.051(2) -0.083(3) O6 0.0258(8) 0.0337(9) 0.0314(8) -0.0026(7) -0.0008(6) 0.0119(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 O1 2.1397(14) 2 ? Mn1 O1 2.1397(14) . ? Mn1 O5 2.1734(13) 2 ? Mn1 O5 2.1734(13) . ? Mn1 O4 2.2049(13) . ? Mn1 O4 2.2049(13) 2 ? Mn2 O6 2.0796(14) 2 ? Mn2 O2 2.0979(15) . ? Mn2 O4 2.1016(14) 2 ? Mn2 N2 2.2391(17) . ? Mn2 N1 2.2642(18) . ? O4 C7 1.296(2) . ? O4 Mn2 2.1016(14) 2 ? O2 C1 1.260(2) . ? O5 C13 1.251(2) . ? O3 C7 1.229(2) . ? O1 C1 1.252(2) . ? N1 C19 1.322(3) . ? N1 C29 1.358(3) . ? C7 C8 1.483(3) . ? N2 C28 1.322(3) . ? N2 C30 1.358(2) . ? C13 O6 1.265(3) . ? C13 C14 1.492(3) . ? C30 C25 1.409(3) . ? C30 C29 1.437(3) . ? C1 C2 1.491(3) . ? C8 C9 1.314(3) . ? C14 C15 1.329(3) . ? C16 C18 1.404(3) . ? C16 C17 1.396(3) . ? C16 C15 1.466(3) . ? C18 C17 1.382(3) 2_464 ? C26 C27 1.360(3) . ? C26 C25 1.408(3) . ? C2 C3 1.313(3) . ? C17 C18 1.382(3) 2_464 ? C25 C24 1.433(3) . ? C22 C21 1.407(4) . ? C22 C29 1.416(3) . ? C22 C23 1.429(4) . ? C28 C27 1.400(3) . ? C24 C23 1.344(4) . ? C19 C20 1.403(4) . ? C21 C20 1.358(4) . ? C3 C4 1.469(3) . ? C9 C10 1.469(3) . ? C10 C11 1.395(3) . ? C10 C12 1.394(3) . ? C4 C6 1.357(4) . ? C4 C5 1.355(4) . ? C11 C12 1.380(3) 2_545 ? C12 C11 1.380(3) 2_545 ? C6 C5 1.382(4) 2_445 ? C5 C6 1.382(4) 2_445 ? O6 Mn2 2.0796(14) 2 ? 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 O1 Mn1 O1 180.00(7) 2 . ? O1 Mn1 O5 89.38(6) 2 2 ? O1 Mn1 O5 90.62(6) . 2 ? O1 Mn1 O5 90.62(6) 2 . ? O1 Mn1 O5 89.38(6) . . ? O5 Mn1 O5 180.00(12) 2 . ? O1 Mn1 O4 87.27(5) 2 . ? O1 Mn1 O4 92.73(5) . . ? O5 Mn1 O4 90.10(5) 2 . ? O5 Mn1 O4 89.90(5) . . ? O1 Mn1 O4 92.73(5) 2 2 ? O1 Mn1 O4 87.27(5) . 2 ? O5 Mn1 O4 89.90(5) 2 2 ? O5 Mn1 O4 90.10(5) . 2 ? O4 Mn1 O4 180.00(9) . 2 ? O6 Mn2 O2 93.82(6) 2 . ? O6 Mn2 O4 101.34(6) 2 2 ? O2 Mn2 O4 101.66(6) . 2 ? O6 Mn2 N2 152.55(6) 2 . ? O2 Mn2 N2 89.74(6) . . ? O4 Mn2 N2 104.56(6) 2 . ? O6 Mn2 N1 84.79(6) 2 . ? O2 Mn2 N1 134.23(6) . . ? O4 Mn2 N1 123.53(6) 2 . ? N2 Mn2 N1 73.47(6) . . ? C7 O4 Mn2 109.06(12) . 2 ? C7 O4 Mn1 136.14(13) . . ? Mn2 O4 Mn1 111.37(6) 2 . ? C1 O2 Mn2 124.16(13) . . ? C13 O5 Mn1 140.53(13) . . ? C1 O1 Mn1 143.15(13) . . ? C19 N1 C29 118.46(19) . . ? C19 N1 Mn2 125.97(16) . . ? C29 N1 Mn2 114.83(13) . . ? O3 C7 O4 121.24(19) . . ? O3 C7 C8 122.23(18) . . ? O4 C7 C8 116.51(17) . . ? C28 N2 C30 118.14(18) . . ? C28 N2 Mn2 125.45(14) . . ? C30 N2 Mn2 115.96(13) . . ? O5 C13 O6 125.42(18) . . ? O5 C13 C14 117.14(18) . . ? O6 C13 C14 117.42(18) . . ? N2 C30 C25 122.7(2) . . ? N2 C30 C29 117.35(18) . . ? C25 C30 C29 119.97(19) . . ? O1 C1 O2 125.90(19) . . ? O1 C1 C2 115.75(18) . . ? O2 C1 C2 118.34(19) . . ? C9 C8 C7 122.1(2) . . ? C15 C14 C13 122.3(2) . . ? C18 C16 C17 118.02(19) . . ? C18 C16 C15 119.28(19) . . ? C17 C16 C15 122.68(19) . . ? C14 C15 C16 127.4(2) . . ? C17 C18 C16 121.3(2) 2_464 . ? C27 C26 C25 119.7(2) . . ? C3 C2 C1 124.5(2) . . ? C18 C17 C16 120.6(2) 2_464 . ? C30 C25 C26 117.2(2) . . ? C30 C25 C24 118.8(2) . . ? C26 C25 C24 124.0(2) . . ? C21 C22 C29 116.6(2) . . ? C21 C22 C23 124.6(2) . . ? C29 C22 C23 118.8(2) . . ? N2 C28 C27 123.1(2) . . ? N1 C29 C22 122.7(2) . . ? N1 C29 C30 117.76(18) . . ? C22 C29 C30 119.5(2) . . ? C23 C24 C25 121.3(2) . . ? C26 C27 C28 119.3(2) . . ? N1 C19 C20 122.6(2) . . ? C24 C23 C22 121.6(2) . . ? C20 C21 C22 120.2(2) . . ? C21 C20 C19 119.4(3) . . ? C2 C3 C4 126.3(2) . . ? C8 C9 C10 127.1(2) . . ? C11 C10 C12 118.0(2) . . ? C11 C10 C9 122.4(2) . . ? C12 C10 C9 119.5(2) . . ? C6 C4 C5 115.9(2) . . ? C6 C4 C3 120.9(2) . . ? C5 C4 C3 123.3(2) . . ? C12 C11 C10 120.4(2) 2_545 . ? C11 C12 C10 121.5(2) 2_545 . ? C4 C6 C5 121.6(3) . 2_445 ? C4 C5 C6 122.5(3) . 2_445 ? C13 O6 Mn2 128.88(13) . 2 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.370 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.062