# Electronic Supplementary Material (ESI) for RSC Advances # 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_agps5_0m _database_code_depnum_ccdc_archive 'CCDC 908358' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H98 Mn6 N16 O22' _chemical_formula_weight 2133.53 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 ? _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 19.4681(6) _cell_length_b 23.9169(7) _cell_length_c 21.0592(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.1360(10) _cell_angle_gamma 90.00 _cell_volume 9780.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4400.0 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9372 _exptl_absorpt_correction_T_max 0.9644 _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 ? _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 61728 _diffrn_reflns_av_R_equivalents 0.1054 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 24.76 _reflns_number_total 8354 _reflns_number_gt 5623 _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, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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^)+(0.1010P)^2^+16.7725P] 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 8354 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1826 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.35360(3) 0.30316(3) 0.18810(3) 0.0383(2) Uani 1 1 d . . . Mn2 Mn 0.5000 0.22474(4) 0.2500 0.0335(3) Uani 1 2 d S . . Mn3 Mn 0.51664(3) 0.26647(3) 0.10812(3) 0.0355(2) Uani 1 1 d . . . O2 O 0.39265(16) 0.34633(14) 0.28033(14) 0.0404(8) Uani 1 1 d . . . O10 O 0.46897(18) 0.18516(15) 0.09948(15) 0.0472(9) Uani 1 1 d . . . O1 O 0.46657(15) 0.28313(12) 0.19620(13) 0.0313(7) Uani 1 1 d . . . O11 O 0.40718(18) 0.33087(15) 0.38528(15) 0.0474(9) Uani 1 1 d . . . O7 O 0.41281(16) 0.21740(14) 0.31138(15) 0.0427(8) Uani 1 1 d . . . O6 O 0.48311(17) 0.40104(14) 0.18786(16) 0.0450(8) Uani 1 1 d . . . O3 O 0.43985(16) 0.30485(16) 0.04766(16) 0.0485(9) Uani 1 1 d . . . O8 O 0.32121(18) 0.23381(15) 0.24289(17) 0.0491(9) Uani 1 1 d . . . O5 O 0.37478(17) 0.38529(15) 0.14983(16) 0.0477(9) Uani 1 1 d . . . N7 N 0.1191(2) 0.3038(2) 0.1423(2) 0.0564(13) Uani 1 1 d . . . O9 O 0.45395(18) 0.16373(14) 0.20077(15) 0.0445(8) Uani 1 1 d . . . O4 O 0.34043(17) 0.28366(16) 0.08971(16) 0.0484(9) Uani 1 1 d . . . N1 N 0.57225(19) 0.24270(17) 0.01620(18) 0.0394(9) Uani 1 1 d . . . N5 N 0.6048(2) 0.2795(2) -0.0872(2) 0.0563(12) Uani 1 1 d . . . N2 N 0.2357(2) 0.33057(18) 0.18468(19) 0.0430(10) Uani 1 1 d . . . N3 N 0.6777(2) 0.2101(2) -0.0306(2) 0.0558(12) Uani 1 1 d . . . N4 N 0.5648(3) 0.1833(2) -0.0794(2) 0.0644(14) Uani 1 1 d . . . C022 C 0.3530(3) 0.2063(2) 0.2869(2) 0.0397(12) Uani 1 1 d . . . C023 C 0.3813(2) 0.3570(2) 0.3379(2) 0.0379(11) Uani 1 1 d . . . C024 C 0.4290(3) 0.4122(2) 0.1518(2) 0.0405(12) Uani 1 1 d . . . N6 N 0.1349(3) 0.3539(3) 0.2428(2) 0.0780(18) Uani 1 1 d . . . C026 C 0.3338(2) 0.4045(2) 0.3494(2) 0.0414(12) Uani 1 1 d . . . C027 C 0.3183(3) 0.1559(2) 0.3121(2) 0.0477(13) Uani 1 1 d . . . C028 C 0.4341(3) 0.4622(2) 0.1102(3) 0.0543(14) Uani 1 1 d . . . C029 C 0.2293(3) 0.3369(3) -0.0775(3) 0.0656(17) Uani 1 1 d . . . H29 H 0.1816 0.3334 -0.0823 0.079 Uiso 1 1 calc R . . C030 C 0.6448(3) 0.2241(2) 0.0287(2) 0.0489(13) Uani 1 1 d . . . H03A H 0.6710 0.2535 0.0509 0.059 Uiso 1 1 calc R . . H03B H 0.6460 0.1915 0.0561 0.059 Uiso 1 1 calc R . . C031 C 0.2842(4) 0.4927(3) 0.3161(4) 0.075(2) Uani 1 1 d . . . H31 H 0.2810 0.5226 0.2878 0.090 Uiso 1 1 calc R . . C032 C 0.2654(3) 0.3192(3) -0.0210(3) 0.0567(15) Uani 1 1 d . . . H32 H 0.2414 0.3050 0.0121 0.068 Uiso 1 1 calc R . . C033 C 0.3286(3) 0.4487(2) 0.3061(3) 0.0568(15) Uani 1 1 d . . . H33 H 0.3547 0.4487 0.2708 0.068 Uiso 1 1 calc R . . C034 C 0.2643(4) 0.3593(3) -0.1253(3) 0.0688(18) Uani 1 1 d . . . H34 H 0.2401 0.3720 -0.1622 0.083 Uiso 1 1 calc R . . C035 C 0.3362(2) 0.3226(2) -0.0141(2) 0.0421(12) Uani 1 1 d . . . C036 C 0.4908(7) 0.5444(5) 0.0791(6) 0.172(6) Uani 1 1 d . . . H36 H 0.5263 0.5700 0.0871 0.206 Uiso 1 1 calc R . . C037 C 0.5338(3) 0.1975(3) -0.0202(3) 0.0561(15) Uani 1 1 d . . . H03C H 0.5328 0.1644 0.0062 0.067 Uiso 1 1 calc R . . H03D H 0.4867 0.2095 -0.0301 0.067 Uiso 1 1 calc R . . C038 C 0.5741(3) 0.2919(2) -0.0268(2) 0.0510(14) Uani 1 1 d . . . H03E H 0.5275 0.3054 -0.0361 0.061 Uiso 1 1 calc R . . H03F H 0.6003 0.3215 -0.0049 0.061 Uiso 1 1 calc R . . C039 C 0.6358(3) 0.1669(3) -0.0644(3) 0.0703(18) Uani 1 1 d . . . H03G H 0.6565 0.1577 -0.1037 0.084 Uiso 1 1 calc R . . H03H H 0.6366 0.1334 -0.0384 0.084 Uiso 1 1 calc R . . C040 C 0.4363(3) 0.0752(3) 0.0620(3) 0.0690(18) Uani 1 1 d . . . H040 H 0.4346 0.1020 0.0299 0.083 Uiso 1 1 calc R . . C041 C 0.6752(3) 0.2596(3) -0.0704(3) 0.0574(15) Uani 1 1 d . . . H04A H 0.6973 0.2515 -0.1092 0.069 Uiso 1 1 calc R . . H04B H 0.7012 0.2893 -0.0483 0.069 Uiso 1 1 calc R . . C042 C 0.1914(3) 0.2881(2) 0.1491(3) 0.0507(14) Uani 1 1 d . . . H04C H 0.2079 0.2831 0.1071 0.061 Uiso 1 1 calc R . . H04D H 0.1959 0.2526 0.1712 0.061 Uiso 1 1 calc R . . C043 C 0.4436(2) 0.0913(2) 0.1252(2) 0.0431(12) Uani 1 1 d . . . N8 N 0.1533(2) 0.4018(2) 0.1425(3) 0.0724(15) Uani 1 1 d . . . C045 C 0.3855(4) 0.4711(3) 0.0620(4) 0.090(2) Uani 1 1 d . . . H45 H 0.3477 0.4474 0.0562 0.108 Uiso 1 1 calc R . . C046 C 0.1285(3) 0.4059(4) 0.2072(4) 0.093(3) Uani 1 1 d . . . H04E H 0.1545 0.4348 0.2307 0.111 Uiso 1 1 calc R . . H04F H 0.0806 0.4172 0.2037 0.111 Uiso 1 1 calc R . . C047 C 0.4556(2) 0.1513(2) 0.1417(2) 0.0381(11) Uani 1 1 d . . . C048 C 0.3751(2) 0.3020(2) 0.0458(2) 0.0408(12) Uani 1 1 d . . . C049 C 0.2945(3) 0.4050(2) 0.4015(3) 0.0510(13) Uani 1 1 d . . . H49 H 0.2987 0.3760 0.4311 0.061 Uiso 1 1 calc R . . C050 C 0.3701(3) 0.3447(3) -0.0633(3) 0.0661(17) Uani 1 1 d . . . H50 H 0.4179 0.3475 -0.0592 0.079 Uiso 1 1 calc R . . C051 C 0.4433(3) 0.0511(3) 0.1720(3) 0.0652(16) Uani 1 1 d . . . H051 H 0.4455 0.0615 0.2147 0.078 Uiso 1 1 calc R . . C052 C 0.2249(3) 0.3843(2) 0.1499(3) 0.0560(15) Uani 1 1 d . . . H05A H 0.2516 0.4132 0.1725 0.067 Uiso 1 1 calc R . . H05B H 0.2422 0.3805 0.1080 0.067 Uiso 1 1 calc R . . C053 C 0.5661(3) 0.2332(3) -0.1181(3) 0.070(2) Uani 1 1 d . . . H05C H 0.5191 0.2453 -0.1287 0.085 Uiso 1 1 calc R . . H05D H 0.5862 0.2241 -0.1576 0.085 Uiso 1 1 calc R . . C054 C 0.0944(3) 0.3119(3) 0.2062(3) 0.076(2) Uani 1 1 d . . . H05E H 0.0465 0.3235 0.2020 0.091 Uiso 1 1 calc R . . H05F H 0.0970 0.2766 0.2290 0.091 Uiso 1 1 calc R . . C055 C 0.2447(3) 0.4921(3) 0.3680(4) 0.084(2) Uani 1 1 d . . . H55 H 0.2149 0.5216 0.3745 0.101 Uiso 1 1 calc R . . C056 C 0.4354(4) -0.0207(3) 0.0935(6) 0.102(3) Uani 1 1 d . . . H056 H 0.4349 -0.0584 0.0828 0.123 Uiso 1 1 calc R . . C057 C 0.3345(4) 0.3633(3) -0.1195(3) 0.080(2) Uani 1 1 d . . . H57 H 0.3582 0.3781 -0.1523 0.096 Uiso 1 1 calc R . . C059 C 0.2548(7) 0.0628(4) 0.3616(5) 0.121(4) Uani 1 1 d . . . H59 H 0.2337 0.0319 0.3787 0.145 Uiso 1 1 calc R . . C061 C 0.1142(3) 0.3570(3) 0.1100(3) 0.0699(18) Uani 1 1 d . . . H06A H 0.0662 0.3679 0.1050 0.084 Uiso 1 1 calc R . . H06B H 0.1303 0.3525 0.0678 0.084 Uiso 1 1 calc R . . C062 C 0.2491(3) 0.4482(3) 0.4101(4) 0.0702(18) Uani 1 1 d . . . H62 H 0.2216 0.4476 0.4443 0.084 Uiso 1 1 calc R . . C063 C 0.2165(5) 0.1046(4) 0.3356(5) 0.108(3) Uani 1 1 d . . . H63 H 0.1688 0.1026 0.3354 0.130 Uiso 1 1 calc R . . C064 C 0.4869(5) 0.4989(4) 0.1189(5) 0.125(4) Uani 1 1 d . . . H64 H 0.5207 0.4934 0.1518 0.150 Uiso 1 1 calc R . . C065 C 0.2070(3) 0.3379(3) 0.2475(3) 0.0679(19) Uani 1 1 d . . . H06C H 0.2121 0.3031 0.2711 0.081 Uiso 1 1 calc R . . H06D H 0.2334 0.3663 0.2713 0.081 Uiso 1 1 calc R . . C066 C 0.3266(6) 0.0659(3) 0.3630(4) 0.108(3) Uani 1 1 d . . . H66 H 0.3537 0.0365 0.3792 0.129 Uiso 1 1 calc R . . C067 C 0.2468(3) 0.1514(3) 0.3088(3) 0.0717(18) Uani 1 1 d . . . H67 H 0.2195 0.1790 0.2890 0.086 Uiso 1 1 calc R . . C070 C 0.4397(4) -0.0050(3) 0.1556(5) 0.096(3) Uani 1 1 d . . . H070 H 0.4403 -0.0321 0.1873 0.116 Uiso 1 1 calc R . . C071 C 0.4460(7) 0.5528(4) 0.0305(6) 0.134(4) Uani 1 1 d . . . H71 H 0.4509 0.5830 0.0034 0.161 Uiso 1 1 calc R . . C072 C 0.3932(6) 0.5172(5) 0.0204(5) 0.141(4) Uani 1 1 d . . . H72 H 0.3613 0.5227 -0.0140 0.169 Uiso 1 1 calc R . . C073 C 0.3567(4) 0.1132(3) 0.3400(3) 0.0749(19) Uani 1 1 d . . . H73 H 0.4044 0.1163 0.3435 0.090 Uiso 1 1 calc R . . C456 C 0.4317(4) 0.0192(4) 0.0466(4) 0.097(3) Uani 1 1 d . . . H456 H 0.4260 0.0084 0.0041 0.116 Uiso 1 1 calc R . . Mn4 Mn 0.5000 0.34171(4) 0.2500 0.0327(3) Uani 1 2 d S . . 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 0.0343(4) 0.0475(5) 0.0326(4) 0.0053(3) -0.0017(3) -0.0022(3) Mn2 0.0400(5) 0.0343(6) 0.0257(5) 0.000 -0.0013(4) 0.000 Mn3 0.0366(4) 0.0416(5) 0.0282(4) -0.0009(3) 0.0009(3) -0.0038(3) O2 0.0426(18) 0.047(2) 0.0314(18) -0.0023(15) 0.0021(14) 0.0019(15) O10 0.060(2) 0.047(2) 0.0333(18) -0.0019(17) 0.0006(16) -0.0134(18) O1 0.0353(16) 0.0325(18) 0.0256(16) 0.0006(13) -0.0010(13) -0.0011(13) O11 0.055(2) 0.056(2) 0.0317(18) 0.0074(16) 0.0015(16) 0.0197(18) O7 0.0402(19) 0.051(2) 0.0366(18) 0.0027(16) 0.0015(15) -0.0006(16) O6 0.0440(19) 0.043(2) 0.046(2) 0.0112(16) -0.0066(16) -0.0067(16) O3 0.0358(19) 0.066(3) 0.043(2) 0.0108(18) -0.0004(15) 0.0016(17) O8 0.045(2) 0.055(2) 0.047(2) 0.0133(18) -0.0024(16) -0.0078(17) O5 0.0366(19) 0.054(2) 0.051(2) 0.0133(18) -0.0038(15) -0.0035(17) N7 0.043(3) 0.081(4) 0.044(3) -0.011(3) -0.003(2) -0.011(2) O9 0.057(2) 0.044(2) 0.0333(19) -0.0025(15) 0.0035(16) -0.0091(16) O4 0.0429(19) 0.068(3) 0.0341(19) 0.0004(17) -0.0015(15) -0.0092(17) N1 0.039(2) 0.043(3) 0.036(2) -0.0034(19) -0.0002(17) -0.0055(18) N5 0.054(3) 0.082(4) 0.034(2) 0.004(2) 0.008(2) -0.002(2) N2 0.037(2) 0.055(3) 0.036(2) -0.003(2) -0.0009(17) -0.0072(19) N3 0.046(3) 0.064(3) 0.059(3) -0.007(3) 0.010(2) 0.006(2) N4 0.061(3) 0.087(4) 0.047(3) -0.027(3) 0.013(2) -0.021(3) C022 0.044(3) 0.046(3) 0.029(3) 0.000(2) 0.007(2) -0.002(2) C023 0.037(3) 0.038(3) 0.038(3) 0.000(2) -0.001(2) 0.003(2) C024 0.048(3) 0.037(3) 0.037(3) 0.001(2) 0.004(2) 0.005(2) N6 0.047(3) 0.137(6) 0.051(3) -0.035(4) 0.010(2) -0.011(3) C026 0.036(2) 0.041(3) 0.046(3) -0.005(2) -0.009(2) 0.001(2) C027 0.060(3) 0.049(3) 0.035(3) 0.001(2) 0.006(2) -0.008(3) C028 0.060(3) 0.045(3) 0.057(3) 0.017(3) -0.002(3) 0.005(3) C029 0.054(3) 0.072(5) 0.068(4) -0.006(3) -0.015(3) 0.007(3) C030 0.046(3) 0.062(4) 0.038(3) 0.000(3) -0.002(2) 0.003(3) C031 0.078(5) 0.036(4) 0.108(6) 0.005(4) -0.008(4) 0.012(3) C032 0.047(3) 0.077(4) 0.045(3) 0.003(3) -0.004(2) 0.006(3) C033 0.060(3) 0.045(4) 0.064(4) 0.003(3) -0.001(3) 0.007(3) C034 0.083(5) 0.057(4) 0.063(4) 0.008(3) -0.023(4) 0.009(3) C035 0.040(3) 0.049(3) 0.036(3) -0.003(2) -0.005(2) 0.003(2) C036 0.219(13) 0.121(9) 0.164(11) 0.091(9) -0.060(10) -0.093(9) C037 0.051(3) 0.074(4) 0.044(3) -0.021(3) 0.010(2) -0.024(3) C038 0.053(3) 0.059(4) 0.041(3) 0.001(3) 0.003(2) 0.007(3) C039 0.079(4) 0.065(4) 0.070(4) -0.026(3) 0.025(4) 0.001(3) C040 0.078(4) 0.068(4) 0.063(4) -0.028(3) 0.017(3) -0.024(3) C041 0.044(3) 0.082(5) 0.047(3) -0.009(3) 0.014(3) -0.011(3) C042 0.043(3) 0.062(4) 0.047(3) -0.003(3) 0.004(2) -0.006(3) C043 0.037(3) 0.041(3) 0.051(3) -0.010(2) 0.004(2) -0.008(2) N8 0.046(3) 0.068(4) 0.102(4) -0.008(3) -0.008(3) 0.011(3) C045 0.073(4) 0.096(6) 0.099(6) 0.056(5) -0.017(4) 0.005(4) C046 0.049(4) 0.114(7) 0.114(7) -0.062(6) -0.001(4) 0.014(4) C047 0.034(2) 0.043(3) 0.037(3) -0.001(2) -0.003(2) -0.003(2) C048 0.041(3) 0.043(3) 0.037(3) -0.004(2) 0.000(2) 0.004(2) C049 0.048(3) 0.053(4) 0.053(3) -0.010(3) 0.004(2) 0.005(3) C050 0.049(3) 0.089(5) 0.059(4) 0.026(3) 0.001(3) -0.002(3) C051 0.069(4) 0.045(4) 0.080(4) 0.005(3) -0.001(3) -0.014(3) C052 0.046(3) 0.047(4) 0.073(4) 0.001(3) -0.006(3) 0.004(3) C053 0.053(3) 0.125(6) 0.033(3) -0.017(4) 0.001(3) -0.004(4) C054 0.045(3) 0.128(6) 0.055(4) -0.013(4) 0.010(3) -0.022(4) C055 0.058(4) 0.049(4) 0.146(7) -0.016(5) 0.016(4) 0.015(3) C056 0.088(6) 0.051(5) 0.172(10) -0.035(6) 0.038(6) -0.018(4) C057 0.080(5) 0.097(6) 0.061(4) 0.040(4) -0.002(3) -0.002(4) C059 0.172(11) 0.083(7) 0.112(7) 0.027(6) 0.038(7) -0.052(7) C061 0.045(3) 0.100(6) 0.063(4) -0.001(4) -0.012(3) 0.008(3) C062 0.055(4) 0.060(4) 0.098(5) -0.021(4) 0.018(3) 0.004(3) C063 0.095(6) 0.107(7) 0.128(7) 0.004(6) 0.040(5) -0.057(6) C064 0.136(8) 0.085(6) 0.144(8) 0.063(6) -0.056(6) -0.055(6) C065 0.047(3) 0.117(6) 0.040(3) -0.015(3) 0.000(3) -0.013(3) C066 0.159(9) 0.061(5) 0.101(6) 0.030(5) -0.003(6) -0.029(6) C067 0.068(4) 0.071(5) 0.077(4) -0.003(4) 0.013(3) -0.021(3) C070 0.089(6) 0.051(5) 0.148(8) 0.015(5) 0.002(5) -0.009(4) C071 0.170(11) 0.062(6) 0.173(11) 0.064(7) 0.038(9) 0.005(6) C072 0.127(8) 0.147(10) 0.148(9) 0.111(8) -0.008(7) 0.032(7) C073 0.091(5) 0.059(4) 0.074(4) 0.017(4) -0.001(4) -0.016(4) C456 0.092(5) 0.090(6) 0.112(7) -0.060(6) 0.032(5) -0.032(5) Mn4 0.0338(5) 0.0340(6) 0.0294(5) 0.000 -0.0033(4) 0.000 _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 2.121(3) . ? Mn1 O8 2.141(3) . ? Mn1 O5 2.174(4) . ? Mn1 O1 2.245(3) . ? Mn1 O2 2.281(3) . ? Mn1 N2 2.384(4) . ? Mn1 Mn4 3.1838(8) . ? Mn2 O1 1.884(3) . ? Mn2 O1 1.884(3) 2_655 ? Mn2 O9 1.968(3) . ? Mn2 O9 1.968(3) 2_655 ? Mn2 O7 2.213(3) 2_655 ? Mn2 O7 2.213(3) . ? Mn2 Mn4 2.7975(14) . ? Mn2 Mn3 3.1886(7) . ? Mn2 Mn3 3.1886(7) 2_655 ? Mn3 O3 2.103(3) . ? Mn3 O11 2.136(3) 2_655 ? Mn3 O10 2.157(3) . ? Mn3 O1 2.193(3) . ? Mn3 N1 2.355(4) . ? Mn3 O7 2.409(3) 2_655 ? O2 C023 1.274(5) . ? O2 Mn4 2.232(3) . ? O10 C047 1.244(6) . ? O1 Mn4 1.888(3) . ? O11 C023 1.252(6) . ? O11 Mn3 2.136(3) 2_655 ? O7 C022 1.267(6) . ? O7 Mn3 2.409(3) 2_655 ? O6 C024 1.281(6) . ? O6 Mn4 1.942(3) . ? O3 C048 1.260(6) . ? O8 C022 1.261(6) . ? O5 C024 1.236(6) . ? N7 C061 1.442(8) . ? N7 C042 1.455(7) . ? N7 C054 1.474(7) . ? O9 C047 1.281(6) . ? O4 C048 1.262(6) . ? N1 C030 1.486(6) . ? N1 C038 1.487(7) . ? N1 C037 1.494(6) . ? N5 C053 1.466(8) . ? N5 C041 1.469(7) . ? N5 C038 1.475(6) . ? N2 C065 1.482(6) . ? N2 C052 1.486(7) . ? N2 C042 1.497(7) . ? N3 C041 1.451(8) . ? N3 C039 1.468(8) . ? N3 C030 1.482(7) . ? N4 C053 1.445(8) . ? N4 C039 1.449(8) . ? N4 C037 1.464(6) . ? C022 C027 1.498(7) . ? C023 C026 1.495(7) . ? C024 C028 1.488(7) . ? N6 C065 1.450(8) . ? N6 C046 1.454(10) . ? N6 C054 1.462(8) . ? C026 C049 1.382(7) . ? C026 C033 1.397(7) . ? C027 C073 1.373(9) . ? C027 C067 1.392(8) . ? C028 C045 1.353(8) . ? C028 C064 1.354(9) . ? C029 C034 1.367(9) . ? C029 C032 1.403(8) . ? C031 C055 1.382(10) . ? C031 C033 1.386(8) . ? C032 C035 1.378(7) . ? C034 C057 1.366(9) . ? C035 C050 1.373(7) . ? C035 C048 1.508(7) . ? C036 C071 1.311(14) . ? C036 C064 1.378(11) . ? C040 C456 1.380(10) . ? C040 C043 1.383(8) . ? C043 C051 1.379(8) . ? C043 C047 1.491(7) . ? N8 C052 1.454(7) . ? N8 C061 1.457(8) . ? N8 C046 1.480(9) . ? C045 C072 1.424(10) . ? C049 C062 1.380(8) . ? C050 C057 1.399(8) . ? C051 C070 1.386(10) . ? C055 C062 1.372(10) . ? C056 C070 1.356(12) . ? C056 C456 1.371(12) . ? C059 C063 1.341(13) . ? C059 C066 1.397(13) . ? C063 C067 1.402(10) . ? C066 C073 1.378(10) . ? C071 C072 1.340(14) . ? Mn4 O1 1.888(3) 2_655 ? Mn4 O6 1.942(3) 2_655 ? Mn4 O2 2.232(3) 2_655 ? Mn4 Mn1 3.1838(8) 2_655 ? 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 O8 109.67(14) . . ? O4 Mn1 O5 81.33(14) . . ? O8 Mn1 O5 166.11(14) . . ? O4 Mn1 O1 94.36(12) . . ? O8 Mn1 O1 96.82(12) . . ? O5 Mn1 O1 90.57(12) . . ? O4 Mn1 O2 160.15(13) . . ? O8 Mn1 O2 89.13(13) . . ? O5 Mn1 O2 81.15(13) . . ? O1 Mn1 O2 76.56(11) . . ? O4 Mn1 N2 89.01(13) . . ? O8 Mn1 N2 84.77(14) . . ? O5 Mn1 N2 87.04(14) . . ? O1 Mn1 N2 175.53(13) . . ? O2 Mn1 N2 99.33(13) . . ? O4 Mn1 Mn4 120.34(9) . . ? O8 Mn1 Mn4 107.06(10) . . ? O5 Mn1 Mn4 72.66(9) . . ? O1 Mn1 Mn4 35.68(8) . . ? O2 Mn1 Mn4 44.51(8) . . ? N2 Mn1 Mn4 139.86(10) . . ? O1 Mn2 O1 84.36(18) . 2_655 ? O1 Mn2 O9 96.22(13) . . ? O1 Mn2 O9 172.12(13) 2_655 . ? O1 Mn2 O9 172.12(13) . 2_655 ? O1 Mn2 O9 96.22(13) 2_655 2_655 ? O9 Mn2 O9 84.3(2) . 2_655 ? O1 Mn2 O7 87.35(12) . 2_655 ? O1 Mn2 O7 99.43(12) 2_655 2_655 ? O9 Mn2 O7 88.45(13) . 2_655 ? O9 Mn2 O7 84.80(13) 2_655 2_655 ? O1 Mn2 O7 99.43(12) . . ? O1 Mn2 O7 87.35(12) 2_655 . ? O9 Mn2 O7 84.80(13) . . ? O9 Mn2 O7 88.45(13) 2_655 . ? O7 Mn2 O7 170.90(18) 2_655 . ? O1 Mn2 Mn4 42.18(9) . . ? O1 Mn2 Mn4 42.18(9) 2_655 . ? O9 Mn2 Mn4 137.85(10) . . ? O9 Mn2 Mn4 137.85(10) 2_655 . ? O7 Mn2 Mn4 94.55(9) 2_655 . ? O7 Mn2 Mn4 94.55(9) . . ? O1 Mn2 Mn3 42.16(9) . . ? O1 Mn2 Mn3 106.11(9) 2_655 . ? O9 Mn2 Mn3 79.15(9) . . ? O9 Mn2 Mn3 130.72(9) 2_655 . ? O7 Mn2 Mn3 48.98(9) 2_655 . ? O7 Mn2 Mn3 134.91(9) . . ? Mn4 Mn2 Mn3 71.76(2) . . ? O1 Mn2 Mn3 106.11(9) . 2_655 ? O1 Mn2 Mn3 42.16(9) 2_655 2_655 ? O9 Mn2 Mn3 130.72(9) . 2_655 ? O9 Mn2 Mn3 79.15(9) 2_655 2_655 ? O7 Mn2 Mn3 134.91(9) 2_655 2_655 ? O7 Mn2 Mn3 48.98(9) . 2_655 ? Mn4 Mn2 Mn3 71.76(2) . 2_655 ? Mn3 Mn2 Mn3 143.53(4) . 2_655 ? O3 Mn3 O11 100.63(14) . 2_655 ? O3 Mn3 O10 93.42(14) . . ? O11 Mn3 O10 161.49(15) 2_655 . ? O3 Mn3 O1 95.33(12) . . ? O11 Mn3 O1 99.37(12) 2_655 . ? O10 Mn3 O1 91.17(12) . . ? O3 Mn3 N1 87.51(14) . . ? O11 Mn3 N1 82.49(13) 2_655 . ? O10 Mn3 N1 86.19(13) . . ? O1 Mn3 N1 176.24(13) . . ? O3 Mn3 O7 169.42(12) . 2_655 ? O11 Mn3 O7 86.99(13) 2_655 2_655 ? O10 Mn3 O7 80.80(13) . 2_655 ? O1 Mn3 O7 76.05(11) . 2_655 ? N1 Mn3 O7 100.86(13) . 2_655 ? O3 Mn3 Mn2 126.02(9) . . ? O11 Mn3 Mn2 106.36(9) 2_655 . ? O10 Mn3 Mn2 74.02(9) . . ? O1 Mn3 Mn2 35.22(8) . . ? N1 Mn3 Mn2 141.13(11) . . ? O7 Mn3 Mn2 43.89(8) 2_655 . ? C023 O2 Mn4 120.8(3) . . ? C023 O2 Mn1 146.2(3) . . ? Mn4 O2 Mn1 89.73(11) . . ? C047 O10 Mn3 129.6(3) . . ? Mn2 O1 Mn4 95.74(13) . . ? Mn2 O1 Mn3 102.63(13) . . ? Mn4 O1 Mn3 119.17(14) . . ? Mn2 O1 Mn1 119.85(14) . . ? Mn4 O1 Mn1 100.41(13) . . ? Mn3 O1 Mn1 117.85(13) . . ? C023 O11 Mn3 130.5(3) . 2_655 ? C022 O7 Mn2 120.0(3) . . ? C022 O7 Mn3 148.1(3) . 2_655 ? Mn2 O7 Mn3 87.13(11) . 2_655 ? C024 O6 Mn4 130.1(3) . . ? C048 O3 Mn3 131.3(3) . . ? C022 O8 Mn1 130.7(3) . . ? C024 O5 Mn1 130.0(3) . . ? C061 N7 C042 107.6(4) . . ? C061 N7 C054 107.4(5) . . ? C042 N7 C054 108.7(4) . . ? C047 O9 Mn2 129.8(3) . . ? C048 O4 Mn1 127.3(3) . . ? C030 N1 C038 106.3(4) . . ? C030 N1 C037 107.9(4) . . ? C038 N1 C037 107.0(4) . . ? C030 N1 Mn3 114.5(3) . . ? C038 N1 Mn3 110.0(3) . . ? C037 N1 Mn3 110.7(3) . . ? C053 N5 C041 107.7(5) . . ? C053 N5 C038 107.9(4) . . ? C041 N5 C038 106.7(4) . . ? C065 N2 C052 106.8(5) . . ? C065 N2 C042 106.7(4) . . ? C052 N2 C042 106.5(4) . . ? C065 N2 Mn1 115.5(3) . . ? C052 N2 Mn1 110.7(3) . . ? C042 N2 Mn1 110.3(3) . . ? C041 N3 C039 107.5(5) . . ? C041 N3 C030 107.7(4) . . ? C039 N3 C030 108.0(4) . . ? C053 N4 C039 107.0(5) . . ? C053 N4 C037 108.3(5) . . ? C039 N4 C037 108.8(5) . . ? O8 C022 O7 125.3(4) . . ? O8 C022 C027 118.0(4) . . ? O7 C022 C027 116.7(4) . . ? O11 C023 O2 124.8(4) . . ? O11 C023 C026 117.9(4) . . ? O2 C023 C026 117.3(4) . . ? O5 C024 O6 125.1(5) . . ? O5 C024 C028 119.4(5) . . ? O6 C024 C028 115.5(5) . . ? C065 N6 C046 107.9(5) . . ? C065 N6 C054 109.7(6) . . ? C046 N6 C054 107.1(6) . . ? C049 C026 C033 119.6(5) . . ? C049 C026 C023 121.4(5) . . ? C033 C026 C023 119.1(5) . . ? C073 C027 C067 118.3(6) . . ? C073 C027 C022 120.3(5) . . ? C067 C027 C022 121.4(5) . . ? C045 C028 C064 118.8(6) . . ? C045 C028 C024 119.7(6) . . ? C064 C028 C024 121.5(6) . . ? C034 C029 C032 119.9(6) . . ? N3 C030 N1 112.4(4) . . ? C055 C031 C033 120.0(6) . . ? C035 C032 C029 120.5(5) . . ? C031 C033 C026 119.5(6) . . ? C057 C034 C029 120.6(6) . . ? C050 C035 C032 118.4(5) . . ? C050 C035 C048 121.2(5) . . ? C032 C035 C048 120.4(5) . . ? C071 C036 C064 122.2(10) . . ? N4 C037 N1 112.5(4) . . ? N5 C038 N1 113.3(4) . . ? N4 C039 N3 113.7(5) . . ? C456 C040 C043 119.8(7) . . ? N3 C041 N5 113.3(4) . . ? N7 C042 N2 113.2(4) . . ? C051 C043 C040 119.2(6) . . ? C051 C043 C047 120.9(5) . . ? C040 C043 C047 119.7(5) . . ? C052 N8 C061 107.5(5) . . ? C052 N8 C046 107.1(5) . . ? C061 N8 C046 106.7(5) . . ? C028 C045 C072 119.0(8) . . ? N6 C046 N8 113.4(5) . . ? O10 C047 O9 124.4(5) . . ? O10 C047 C043 119.8(4) . . ? O9 C047 C043 115.8(4) . . ? O3 C048 O4 125.7(5) . . ? O3 C048 C035 116.6(4) . . ? O4 C048 C035 117.6(4) . . ? C062 C049 C026 120.4(6) . . ? C035 C050 C057 121.6(6) . . ? C043 C051 C070 120.0(7) . . ? N8 C052 N2 113.7(5) . . ? N4 C053 N5 113.7(5) . . ? N6 C054 N7 111.9(5) . . ? C062 C055 C031 120.4(6) . . ? C070 C056 C456 119.9(7) . . ? C034 C057 C050 119.1(6) . . ? C063 C059 C066 119.6(8) . . ? N7 C061 N8 114.5(5) . . ? C055 C062 C049 120.0(6) . . ? C059 C063 C067 121.4(8) . . ? C028 C064 C036 120.3(8) . . ? N6 C065 N2 113.3(5) . . ? C073 C066 C059 119.1(9) . . ? C027 C067 C063 119.4(7) . . ? C056 C070 C051 120.4(8) . . ? C036 C071 C072 119.0(9) . . ? C071 C072 C045 120.6(9) . . ? C027 C073 C066 121.9(8) . . ? C056 C456 C040 120.5(8) . . ? O1 Mn4 O1 84.17(18) . 2_655 ? O1 Mn4 O6 95.95(13) . . ? O1 Mn4 O6 168.79(13) 2_655 . ? O1 Mn4 O6 168.79(13) . 2_655 ? O1 Mn4 O6 95.95(13) 2_655 2_655 ? O6 Mn4 O6 86.1(2) . 2_655 ? O1 Mn4 O2 98.88(12) . 2_655 ? O1 Mn4 O2 85.36(12) 2_655 2_655 ? O6 Mn4 O2 83.54(13) . 2_655 ? O6 Mn4 O2 92.30(13) 2_655 2_655 ? O1 Mn4 O2 85.36(12) . . ? O1 Mn4 O2 98.88(12) 2_655 . ? O6 Mn4 O2 92.30(13) . . ? O6 Mn4 O2 83.54(13) 2_655 . ? O2 Mn4 O2 174.32(18) 2_655 . ? O1 Mn4 Mn2 42.08(9) . . ? O1 Mn4 Mn2 42.08(9) 2_655 . ? O6 Mn4 Mn2 136.94(10) . . ? O6 Mn4 Mn2 136.94(10) 2_655 . ? O2 Mn4 Mn2 92.84(9) 2_655 . ? O2 Mn4 Mn2 92.84(9) . . ? O1 Mn4 Mn1 43.92(9) . . ? O1 Mn4 Mn1 106.89(9) 2_655 . ? O6 Mn4 Mn1 80.37(10) . . ? O6 Mn4 Mn1 126.20(10) 2_655 . ? O2 Mn4 Mn1 136.57(8) 2_655 . ? O2 Mn4 Mn1 45.77(8) . . ? Mn2 Mn4 Mn1 73.16(2) . . ? O1 Mn4 Mn1 106.89(9) . 2_655 ? O1 Mn4 Mn1 43.92(9) 2_655 2_655 ? O6 Mn4 Mn1 126.20(10) . 2_655 ? O6 Mn4 Mn1 80.37(10) 2_655 2_655 ? O2 Mn4 Mn1 45.77(8) 2_655 2_655 ? O2 Mn4 Mn1 136.57(8) . 2_655 ? Mn2 Mn4 Mn1 73.17(2) . 2_655 ? Mn1 Mn4 Mn1 146.33(4) . 2_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.76 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.768 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.098