# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email vlpec@umich.edu _publ_contact_author_name 'Prof. Vincent L. Pecoraro' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name T.M.Rajendiran M.L.Kirk I.A.Setyawati M.T.Caudle 'Jeff W.Kampf' ; V.L.Pecoraro ; data_mnbig _database_code_CSD 191509 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H130 Mn2 N6 O8' _chemical_formula_weight 1641.97 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.1300(14) _cell_length_b 35.455(3) _cell_length_c 20.564(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.856(8) _cell_angle_gamma 90.00 _cell_volume 9401.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 178(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.80 _cell_measurement_theta_max 12.49 _exptl_crystal_description irregular _exptl_crystal_colour 'dark green?' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 178(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.61 _diffrn_reflns_number 10872 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9251 _reflns_number_gt 5430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; The lattice contains a total of 8 toluene solvent molecules, two per Mn complex, all of which are disordered. They have been located on a difference electron density map and refined as rigid groups at relative occupancies of 0.65/0.35. One of the t-butyl groups (C26-C28) is also disordered and refined at occupancies of 0.58 and 0.42 for 2 orientations rotated approx. 60 deg. with respect to one another. All hydrogens were placed in calculated positions except for the hydrogen on O4 which was refined isotropically. 04-H4OX, 0.86(2) A; O4A..H4OX, 1.61A. 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^)+(0.1046P)^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 9251 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1672 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 0.45998(4) 0.567514(13) 0.59252(2) 0.02487(16) Uani 1 1 d . . . N1 N 0.4422(2) 0.55833(7) 0.49390(13) 0.0283(6) Uani 1 1 d . . . N2 N 0.3057(2) 0.56879(7) 0.58195(13) 0.0291(6) Uani 1 1 d . . . N3 N 0.4817(2) 0.55999(7) 0.69471(12) 0.0243(6) Uani 1 1 d . . . O1 O 0.60328(17) 0.56590(6) 0.59597(10) 0.0268(5) Uani 1 1 d . . . O2 O 0.45707(18) 0.62397(6) 0.60137(10) 0.0281(5) Uani 1 1 d . . . O3 O 0.45576(19) 0.50138(6) 0.60756(10) 0.0320(6) Uani 1 1 d . . . O4 O 0.4840(2) 0.45841(6) 0.68864(11) 0.0354(6) Uani 1 1 d . . . H4OX H 0.497(6) 0.4580(16) 0.729(3) 0.02(2) Uiso 0.50 1 d P . . C1 C 0.6460(3) 0.58888(9) 0.55747(15) 0.0263(7) Uani 1 1 d . . . C2 C 0.7461(3) 0.60410(10) 0.57977(16) 0.0325(8) Uani 1 1 d . . . C3 C 0.7801(3) 0.63117(10) 0.53978(18) 0.0394(9) Uani 1 1 d . . . H3 H 0.8442 0.6433 0.5565 0.034(3) Uiso 1 1 calc R . . C4 C 0.7279(3) 0.64188(10) 0.47714(18) 0.0382(9) Uani 1 1 d . A . C5 C 0.6378(3) 0.62266(10) 0.45293(16) 0.0350(8) Uani 1 1 d . . . H5 H 0.6038 0.6270 0.4086 0.034(3) Uiso 1 1 calc R . . C6 C 0.5944(3) 0.59674(9) 0.49170(15) 0.0277(7) Uani 1 1 d . . . C7 C 0.5037(3) 0.57549(9) 0.46187(15) 0.0288(8) Uani 1 1 d . . . H7 H 0.4882 0.5741 0.4149 0.034(3) Uiso 1 1 calc R . . C8 C 0.3621(3) 0.53318(10) 0.45732(17) 0.0374(9) Uani 1 1 d . . . H8A H 0.3807 0.5067 0.4695 0.034(3) Uiso 1 1 calc R . . H8B H 0.3607 0.5360 0.4093 0.034(3) Uiso 1 1 calc R . . C9 C 0.2546(3) 0.54128(11) 0.47127(18) 0.0406(9) Uani 1 1 d . . . H9A H 0.2045 0.5237 0.4450 0.034(3) Uiso 1 1 calc R . . H9B H 0.2342 0.5672 0.4563 0.034(3) Uiso 1 1 calc R . . C10 C 0.2472(3) 0.53756(10) 0.54424(18) 0.0375(9) Uani 1 1 d . . . H10A H 0.1737 0.5386 0.5491 0.034(3) Uiso 1 1 calc R . . H10B H 0.2764 0.5130 0.5617 0.034(3) Uiso 1 1 calc R . . C11 C 0.2520(3) 0.59653(9) 0.59883(16) 0.0317(8) Uani 1 1 d . . . H11 H 0.1802 0.5917 0.5959 0.034(3) Uiso 1 1 calc R . . C12 C 0.2861(3) 0.63318(9) 0.62106(16) 0.0296(8) Uani 1 1 d . . . C13 C 0.2096(3) 0.65839(10) 0.63544(16) 0.0334(8) Uani 1 1 d . . . H13 H 0.1427 0.6489 0.6376 0.034(3) Uiso 1 1 calc R . . C14 C 0.2290(3) 0.69594(10) 0.64630(17) 0.0339(8) Uani 1 1 d . . . C15 C 0.3308(3) 0.70839(9) 0.64389(16) 0.0339(8) Uani 1 1 d . . . H15 H 0.3456 0.7344 0.6518 0.034(3) Uiso 1 1 calc R . . C16 C 0.4102(3) 0.68574(9) 0.63102(15) 0.0294(8) Uani 1 1 d . . . C17 C 0.3872(3) 0.64643(9) 0.61791(15) 0.0273(7) Uani 1 1 d . . . C18 C 0.5000 0.58091(13) 0.7500 0.0251(10) Uani 1 2 d S . . H18 H 0.5000 0.6077 0.7500 0.034(3) Uiso 1 2 calc SR . . C19 C 0.4887(2) 0.52324(9) 0.71603(14) 0.0244(7) Uani 1 1 d . . . C20 C 0.4751(3) 0.49289(9) 0.66715(16) 0.0279(7) Uani 1 1 d . . . C21 C 0.8157(3) 0.58946(11) 0.64359(18) 0.0398(9) Uani 1 1 d . . . C22 C 0.8286(3) 0.54686(12) 0.6367(2) 0.0521(11) Uani 1 1 d . . . H22A H 0.8736 0.5370 0.6766 0.067(3) Uiso 1 1 calc R . . H22B H 0.8600 0.5416 0.5980 0.067(3) Uiso 1 1 calc R . . H22C H 0.7606 0.5346 0.6310 0.067(3) Uiso 1 1 calc R . . C23 C 0.7706(3) 0.59729(12) 0.70578(17) 0.0497(11) Uani 1 1 d . . . H23A H 0.7634 0.6246 0.7111 0.067(3) Uiso 1 1 calc R . . H23B H 0.8172 0.5870 0.7446 0.067(3) Uiso 1 1 calc R . . H23C H 0.7024 0.5853 0.7014 0.067(3) Uiso 1 1 calc R . . C24 C 0.9242(3) 0.60701(15) 0.6544(2) 0.0689(15) Uani 1 1 d . . . H24A H 0.9190 0.6343 0.6608 0.067(3) Uiso 1 1 calc R . . H24B H 0.9557 0.6022 0.6156 0.067(3) Uiso 1 1 calc R . . H24C H 0.9675 0.5958 0.6937 0.067(3) Uiso 1 1 calc R . . C25 C 0.7705(3) 0.67274(11) 0.43733(19) 0.0460(10) Uani 1 1 d . . . C26 C 0.8546(8) 0.6969(3) 0.4812(5) 0.070(3) Uani 0.58 1 d P A 1 H26A H 0.8781 0.7167 0.4542 0.067(3) Uiso 0.58 1 calc PR A 1 H26B H 0.9135 0.6809 0.5002 0.067(3) Uiso 0.58 1 calc PR A 1 H26C H 0.8256 0.7085 0.5170 0.067(3) Uiso 0.58 1 calc PR A 1 C27 C 0.8140(9) 0.6558(3) 0.3827(4) 0.061(3) Uani 0.58 1 d P A 1 H27A H 0.7603 0.6410 0.3542 0.067(3) Uiso 0.58 1 calc PR A 1 H27B H 0.8723 0.6393 0.4011 0.067(3) Uiso 0.58 1 calc PR A 1 H27C H 0.8383 0.6759 0.3566 0.067(3) Uiso 0.58 1 calc PR A 1 C28 C 0.6829(7) 0.6999(2) 0.4089(5) 0.062(2) Uani 0.58 1 d P A 1 H28A H 0.6282 0.6862 0.3793 0.067(3) Uiso 0.58 1 calc PR A 1 H28B H 0.7101 0.7199 0.3841 0.067(3) Uiso 0.58 1 calc PR A 1 H28C H 0.6543 0.7111 0.4452 0.067(3) Uiso 0.58 1 calc PR A 1 C26A C 0.7003(15) 0.6769(7) 0.3661(9) 0.145(9) Uani 0.42 1 d P A 2 H26D H 0.6924 0.6522 0.3444 0.218 Uiso 0.42 1 calc PR A 2 H26E H 0.7332 0.6944 0.3395 0.218 Uiso 0.42 1 calc PR A 2 H26F H 0.6320 0.6866 0.3703 0.218 Uiso 0.42 1 calc PR A 2 C27A C 0.8769(13) 0.6590(4) 0.4237(9) 0.089(5) Uani 0.42 1 d P A 2 H27D H 0.9041 0.6776 0.3961 0.133 Uiso 0.42 1 calc PR A 2 H27E H 0.8680 0.6347 0.4007 0.133 Uiso 0.42 1 calc PR A 2 H27F H 0.9256 0.6562 0.4658 0.133 Uiso 0.42 1 calc PR A 2 C28A C 0.7813(18) 0.7082(5) 0.4718(10) 0.116(9) Uani 0.42 1 d P A 2 H28D H 0.8108 0.7038 0.5187 0.174 Uiso 0.42 1 calc PR A 2 H28E H 0.7131 0.7201 0.4679 0.174 Uiso 0.42 1 calc PR A 2 H28F H 0.8274 0.7247 0.4525 0.174 Uiso 0.42 1 calc PR A 2 C29 C 0.1464(3) 0.72447(10) 0.6572(2) 0.0433(10) Uani 1 1 d . . . C30 C 0.1210(4) 0.74970(14) 0.5950(3) 0.0803(17) Uani 1 1 d . . . H30A H 0.0986 0.7339 0.5558 0.067(3) Uiso 1 1 calc R . . H30B H 0.1830 0.7639 0.5898 0.067(3) Uiso 1 1 calc R . . H30C H 0.0654 0.7673 0.5998 0.067(3) Uiso 1 1 calc R . . C31 C 0.1834(4) 0.74878(14) 0.7184(3) 0.0750(16) Uani 1 1 d . . . H31A H 0.1290 0.7668 0.7236 0.067(3) Uiso 1 1 calc R . . H31B H 0.2462 0.7625 0.7131 0.067(3) Uiso 1 1 calc R . . H31C H 0.1989 0.7326 0.7576 0.067(3) Uiso 1 1 calc R . . C32 C 0.0451(4) 0.70559(13) 0.6650(3) 0.0678(14) Uani 1 1 d . . . H32A H 0.0168 0.6915 0.6247 0.067(3) Uiso 1 1 calc R . . H32B H -0.0048 0.7249 0.6726 0.067(3) Uiso 1 1 calc R . . H32C H 0.0581 0.6883 0.7028 0.067(3) Uiso 1 1 calc R . . C33 C 0.5179(3) 0.70135(9) 0.62899(17) 0.0330(8) Uani 1 1 d . . . C34 C 0.5286(3) 0.74292(10) 0.6486(2) 0.0494(11) Uani 1 1 d . . . H34A H 0.6000 0.7512 0.6494 0.067(3) Uiso 1 1 calc R . . H34B H 0.5114 0.7462 0.6926 0.067(3) Uiso 1 1 calc R . . H34C H 0.4811 0.7580 0.6162 0.067(3) Uiso 1 1 calc R . . C35 C 0.5398(3) 0.69759(11) 0.55816(18) 0.0485(11) Uani 1 1 d . . . H35A H 0.5348 0.6710 0.5448 0.067(3) Uiso 1 1 calc R . . H35B H 0.6096 0.7070 0.5571 0.067(3) Uiso 1 1 calc R . . H35C H 0.4887 0.7124 0.5276 0.067(3) Uiso 1 1 calc R . . C36 C 0.5996(3) 0.67938(10) 0.67714(18) 0.0445(10) Uani 1 1 d . . . H36A H 0.5930 0.6524 0.6668 0.067(3) Uiso 1 1 calc R . . H36B H 0.5893 0.6836 0.7226 0.067(3) Uiso 1 1 calc R . . H36C H 0.6689 0.6881 0.6730 0.067(3) Uiso 1 1 calc R . . C37 C 0.2613(5) 0.02942(11) 0.2505(3) 0.0841(7) Uiso 0.65 1 d PR B 1 H37A H 0.2984 0.0128 0.2249 0.126 Uiso 0.65 1 calc PR C 1 H37B H 0.2565 0.0548 0.2311 0.126 Uiso 0.65 1 calc PR D 1 H37C H 0.1914 0.0195 0.2496 0.126 Uiso 0.65 1 calc PR E 1 C38 C 0.3171(4) 0.03123(18) 0.3187(2) 0.0841(7) Uiso 0.65 1 d PG B 1 C39 C 0.2795(4) 0.05342(17) 0.3646(3) 0.0841(7) Uiso 0.65 1 d PG B 1 H39 H 0.2145 0.0658 0.3526 0.101 Uiso 0.65 1 calc PR B 1 C40 C 0.3371(5) 0.05754(16) 0.4283(3) 0.0841(7) Uiso 0.65 1 d PG B 1 H40 H 0.3114 0.0727 0.4597 0.101 Uiso 0.65 1 calc PR B 1 C41 C 0.4322(4) 0.03947(17) 0.4459(2) 0.0841(7) Uiso 0.65 1 d PG B 1 H41 H 0.4715 0.0423 0.4894 0.101 Uiso 0.65 1 calc PR B 1 C42 C 0.4698(4) 0.01728(16) 0.4000(3) 0.0841(7) Uiso 0.65 1 d PG B 1 H42 H 0.5348 0.0049 0.4120 0.101 Uiso 0.65 1 calc PR B 1 C43 C 0.4122(5) 0.01316(15) 0.3363(3) 0.0841(7) Uiso 0.65 1 d PG B 1 H43 H 0.4379 -0.0020 0.3049 0.101 Uiso 0.65 1 calc PR B 1 C44 C 0.8747(7) 0.1317(2) 0.2965(4) 0.0841(7) Uiso 0.65 1 d P F 1 H44A H 0.9453 0.1364 0.3206 0.126 Uiso 0.65 1 calc PR F 1 H44B H 0.8577 0.1498 0.2601 0.126 Uiso 0.65 1 calc PR F 1 H44C H 0.8701 0.1060 0.2786 0.126 Uiso 0.65 1 calc PR F 1 C45 C 0.8012(4) 0.13598(17) 0.3417(3) 0.0841(7) Uiso 0.65 1 d PG F 1 C46 C 0.6958(5) 0.13068(16) 0.3182(2) 0.0841(7) Uiso 0.65 1 d PG F 1 H46 H 0.6722 0.1218 0.2744 0.101 Uiso 0.65 1 calc PR F 1 C47 C 0.6249(3) 0.13843(14) 0.3588(2) 0.0841(7) Uiso 0.65 1 d PG F 1 H47 H 0.5529 0.1348 0.3428 0.101 Uiso 0.65 1 calc PR F 1 C48 C 0.6594(4) 0.15147(14) 0.4229(3) 0.0841(7) Uiso 0.65 1 d PG F 1 H48 H 0.6109 0.1568 0.4507 0.101 Uiso 0.65 1 calc PR F 1 C49 C 0.7648(5) 0.15677(19) 0.4464(2) 0.0841(7) Uiso 0.65 1 d PG F 1 H49 H 0.7884 0.1657 0.4903 0.101 Uiso 0.65 1 calc PR F 1 C50 C 0.8357(3) 0.14903(19) 0.4058(3) 0.0841(7) Uiso 0.65 1 d PG F 1 H50 H 0.9077 0.1526 0.4219 0.101 Uiso 0.65 1 calc PR F 1 C37A C 0.4216(8) 0.0541(3) 0.4560(6) 0.0963(16) Uiso 0.35 1 d PG F 2 H37D H 0.4967 0.0560 0.4717 0.144 Uiso 0.35 1 calc PR F 2 H37E H 0.3953 0.0317 0.4754 0.144 Uiso 0.35 1 calc PR F 2 H37F H 0.3876 0.0766 0.4694 0.144 Uiso 0.35 1 calc PR F 2 C38A C 0.4009(10) 0.0511(4) 0.3881(4) 0.0963(16) Uiso 0.35 1 d PG F 2 C39A C 0.2988(9) 0.0475(4) 0.3551(6) 0.0963(16) Uiso 0.35 1 d PG F 2 H39A H 0.2441 0.0470 0.3795 0.116 Uiso 0.35 1 calc PR F 2 C40A C 0.2766(7) 0.0447(4) 0.2865(6) 0.0963(16) Uiso 0.35 1 d PG F 2 H40A H 0.2068 0.0422 0.2640 0.116 Uiso 0.35 1 calc PR F 2 C41A C 0.3566(10) 0.0454(3) 0.2508(4) 0.0963(16) Uiso 0.35 1 d PG F 2 H41A H 0.3415 0.0435 0.2039 0.116 Uiso 0.35 1 calc PR F 2 C42A C 0.4588(8) 0.0491(4) 0.2838(6) 0.0963(16) Uiso 0.35 1 d PG . 2 H42A H 0.5134 0.0496 0.2594 0.116 Uiso 0.35 1 calc PR F 2 C43A C 0.4809(7) 0.0519(4) 0.3524(6) 0.0963(16) Uiso 0.35 1 d PG F 2 H43A H 0.5507 0.0544 0.3750 0.116 Uiso 0.35 1 calc PR F 2 C44A C 0.5517(13) 0.1548(5) 0.2773(8) 0.0963(16) Uiso 0.35 1 d P G 2 H44D H 0.4882 0.1630 0.2917 0.144 Uiso 0.35 1 calc PR G 2 H44E H 0.5418 0.1293 0.2587 0.144 Uiso 0.35 1 calc PR G 2 H44F H 0.5674 0.1722 0.2435 0.144 Uiso 0.35 1 calc PR G 2 C45A C 0.6365(8) 0.1546(4) 0.3332(6) 0.0963(16) Uiso 0.35 1 d PG G 2 C46A C 0.7308(11) 0.1435(4) 0.3181(5) 0.0963(16) Uiso 0.35 1 d PG G 2 H46A H 0.7355 0.1376 0.2737 0.116 Uiso 0.35 1 calc PR G 2 C47A C 0.8182(8) 0.1409(4) 0.3679(7) 0.0963(16) Uiso 0.35 1 d PG G 2 H47A H 0.8827 0.1333 0.3575 0.116 Uiso 0.35 1 calc PR G 2 C48A C 0.8114(9) 0.1496(4) 0.4329(6) 0.0963(16) Uiso 0.35 1 d PG G 2 H48A H 0.8711 0.1478 0.4669 0.116 Uiso 0.35 1 calc PR G 2 C49A C 0.7171(11) 0.1607(4) 0.4480(5) 0.0963(16) Uiso 0.35 1 d PG G 2 H49A H 0.7124 0.1666 0.4924 0.116 Uiso 0.35 1 calc PR G 2 C50A C 0.6297(8) 0.1633(3) 0.3982(7) 0.0963(16) Uiso 0.35 1 d PG G 2 H50A H 0.5652 0.1709 0.4085 0.116 Uiso 0.35 1 calc PR G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0321(3) 0.0232(3) 0.0184(2) 0.0009(2) 0.0024(2) -0.0087(2) N1 0.0332(16) 0.0267(15) 0.0227(13) -0.0039(11) -0.0004(12) -0.0075(12) N2 0.0329(16) 0.0246(14) 0.0288(14) 0.0001(12) 0.0031(12) -0.0120(13) N3 0.0323(15) 0.0220(14) 0.0202(13) 0.0010(10) 0.0091(11) -0.0025(12) O1 0.0305(12) 0.0296(12) 0.0192(10) 0.0028(9) 0.0024(9) -0.0069(11) O2 0.0338(13) 0.0246(11) 0.0263(12) 0.0004(9) 0.0061(10) -0.0066(11) O3 0.0454(15) 0.0284(12) 0.0219(12) -0.0022(9) 0.0056(11) -0.0086(11) O4 0.0596(18) 0.0225(13) 0.0237(13) -0.0005(10) 0.0068(13) -0.0043(12) C1 0.039(2) 0.0239(17) 0.0171(15) -0.0014(12) 0.0071(14) -0.0067(15) C2 0.038(2) 0.0339(19) 0.0255(17) -0.0044(14) 0.0072(15) -0.0135(16) C3 0.042(2) 0.038(2) 0.038(2) -0.0035(16) 0.0071(18) -0.0174(18) C4 0.048(2) 0.0321(19) 0.038(2) 0.0028(16) 0.0161(18) -0.0126(18) C5 0.048(2) 0.0352(19) 0.0229(17) 0.0039(14) 0.0108(16) -0.0046(18) C6 0.037(2) 0.0267(17) 0.0192(15) -0.0009(13) 0.0061(14) -0.0032(15) C7 0.042(2) 0.0262(17) 0.0165(15) -0.0011(13) 0.0013(15) 0.0005(15) C8 0.044(2) 0.034(2) 0.0303(19) -0.0107(15) -0.0026(17) -0.0121(17) C9 0.037(2) 0.038(2) 0.042(2) -0.0106(17) -0.0043(18) -0.0132(18) C10 0.034(2) 0.0293(19) 0.048(2) -0.0063(16) 0.0039(17) -0.0167(16) C11 0.0319(19) 0.0287(18) 0.0338(18) 0.0047(15) 0.0040(16) -0.0081(16) C12 0.0344(19) 0.0279(17) 0.0256(17) 0.0049(14) 0.0028(15) -0.0057(15) C13 0.0326(19) 0.0312(19) 0.0351(19) 0.0041(15) 0.0030(16) -0.0044(16) C14 0.037(2) 0.0319(19) 0.0310(18) 0.0079(15) 0.0014(16) 0.0010(17) C15 0.050(2) 0.0223(17) 0.0289(18) 0.0037(14) 0.0054(17) -0.0024(17) C16 0.044(2) 0.0263(17) 0.0184(15) 0.0027(13) 0.0064(15) -0.0081(16) C17 0.036(2) 0.0262(17) 0.0188(15) 0.0041(13) 0.0022(14) -0.0079(16) C18 0.029(3) 0.024(2) 0.023(2) 0.000 0.008(2) 0.000 C19 0.0279(18) 0.0251(16) 0.0213(15) -0.0009(13) 0.0074(14) -0.0039(14) C20 0.0338(19) 0.0252(17) 0.0254(17) -0.0006(13) 0.0072(15) -0.0056(15) C21 0.038(2) 0.046(2) 0.0319(19) 0.0001(17) -0.0025(17) -0.0140(18) C22 0.046(3) 0.061(3) 0.044(2) 0.005(2) -0.005(2) 0.003(2) C23 0.062(3) 0.057(3) 0.0255(19) -0.0018(18) -0.0045(19) -0.006(2) C24 0.055(3) 0.091(4) 0.051(3) 0.013(3) -0.013(2) -0.029(3) C25 0.058(3) 0.042(2) 0.043(2) 0.0098(18) 0.020(2) -0.014(2) C26 0.096(8) 0.065(8) 0.049(5) 0.008(5) 0.010(6) -0.052(7) C27 0.084(8) 0.057(5) 0.052(5) 0.010(4) 0.039(5) -0.018(5) C28 0.073(6) 0.052(5) 0.069(6) 0.034(4) 0.035(5) -0.004(5) C26A 0.127(16) 0.20(2) 0.125(16) 0.109(16) 0.054(13) -0.025(16) C27A 0.118(14) 0.049(7) 0.126(14) 0.005(9) 0.088(12) -0.020(9) C28A 0.20(2) 0.051(10) 0.129(18) -0.011(10) 0.12(2) -0.047(14) C29 0.041(2) 0.0291(19) 0.056(2) 0.0061(18) 0.0013(19) 0.0024(18) C30 0.080(4) 0.063(3) 0.093(4) 0.034(3) 0.004(3) 0.024(3) C31 0.054(3) 0.067(3) 0.097(4) -0.033(3) -0.001(3) 0.021(3) C32 0.058(3) 0.051(3) 0.097(4) 0.002(3) 0.022(3) 0.013(2) C33 0.047(2) 0.0234(17) 0.0313(18) -0.0064(14) 0.0148(17) -0.0138(16) C34 0.063(3) 0.032(2) 0.060(3) -0.0114(18) 0.028(2) -0.020(2) C35 0.074(3) 0.041(2) 0.038(2) 0.0005(17) 0.029(2) -0.016(2) C36 0.042(2) 0.048(2) 0.044(2) -0.0083(18) 0.0083(19) -0.0174(19) _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 1.870(2) . ? Mn1 N2 1.996(3) . ? Mn1 O2 2.011(2) . ? Mn1 N1 2.024(3) . ? Mn1 N3 2.084(2) . ? Mn1 O3 2.367(2) . ? N1 C7 1.287(4) . ? N1 C8 1.473(4) . ? N2 C11 1.295(4) . ? N2 C10 1.481(4) . ? N3 C18 1.341(3) . ? N3 C19 1.372(4) . ? O1 C1 1.332(4) . ? O2 C17 1.307(4) . ? O3 C20 1.241(4) . ? O4 C20 1.298(4) . ? C1 C2 1.414(5) . ? C1 C6 1.421(4) . ? C2 C3 1.391(5) . ? C2 C21 1.541(5) . ? C3 C4 1.393(5) . ? C4 C5 1.375(5) . ? C4 C25 1.534(5) . ? C5 C6 1.406(4) . ? C6 C7 1.445(5) . ? C8 C9 1.520(5) . ? C9 C10 1.527(5) . ? C11 C12 1.421(5) . ? C12 C13 1.417(5) . ? C12 C17 1.422(5) . ? C13 C14 1.366(5) . ? C14 C15 1.418(5) . ? C14 C29 1.531(5) . ? C15 C16 1.381(5) . ? C16 C17 1.441(4) . ? C16 C33 1.526(5) . ? C18 N3 1.341(3) 2_656 ? C19 C19 1.372(6) 2_656 ? C19 C20 1.460(4) . ? C21 C22 1.529(6) . ? C21 C23 1.532(5) . ? C21 C24 1.533(5) . ? C25 C28A 1.436(18) . ? C25 C27 1.480(10) . ? C25 C28 1.530(10) . ? C25 C26 1.547(11) . ? C25 C27A 1.553(16) . ? C25 C26A 1.583(19) . ? C29 C32 1.524(6) . ? C29 C31 1.526(6) . ? C29 C30 1.546(6) . ? C33 C34 1.527(5) . ? C33 C36 1.529(5) . ? C33 C35 1.542(5) . ? C37 C38 1.456(6) . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C44 C45 1.469(9) . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C37A C38A 1.376(14) . ? C38A C39A 1.3900 . ? C38A C43A 1.3900 . ? C39A C40A 1.3900 . ? C40A C41A 1.3900 . ? C41A C42A 1.3900 . ? C42A C43A 1.3900 . ? C42A C42A 1.917(18) 2_655 ? C44A C45A 1.442(16) . ? C45A C46A 1.3900 . ? C45A C50A 1.3900 . ? C46A C47A 1.3900 . ? C47A C48A 1.3900 . ? C48A C49A 1.3900 . ? C49A C50A 1.3900 . ? 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 N2 175.98(10) . . ? O1 Mn1 O2 93.62(10) . . ? N2 Mn1 O2 87.20(10) . . ? O1 Mn1 N1 87.60(10) . . ? N2 Mn1 N1 88.38(11) . . ? O2 Mn1 N1 104.50(10) . . ? O1 Mn1 N3 90.70(10) . . ? N2 Mn1 N3 93.21(11) . . ? O2 Mn1 N3 92.14(9) . . ? N1 Mn1 N3 163.34(10) . . ? O1 Mn1 O3 90.74(9) . . ? N2 Mn1 O3 89.33(10) . . ? O2 Mn1 O3 166.62(8) . . ? N1 Mn1 O3 88.31(9) . . ? N3 Mn1 O3 75.14(9) . . ? C7 N1 C8 118.8(3) . . ? C7 N1 Mn1 118.2(2) . . ? C8 N1 Mn1 123.1(2) . . ? C11 N2 C10 117.0(3) . . ? C11 N2 Mn1 125.5(2) . . ? C10 N2 Mn1 117.1(2) . . ? C18 N3 C19 105.3(3) . . ? C18 N3 Mn1 138.8(2) . . ? C19 N3 Mn1 115.59(19) . . ? C1 O1 Mn1 119.5(2) . . ? C17 O2 Mn1 131.0(2) . . ? C20 O3 Mn1 111.3(2) . . ? O1 C1 C2 120.7(3) . . ? O1 C1 C6 120.4(3) . . ? C2 C1 C6 118.8(3) . . ? C3 C2 C1 117.0(3) . . ? C3 C2 C21 122.1(3) . . ? C1 C2 C21 120.9(3) . . ? C2 C3 C4 125.3(3) . . ? C5 C4 C3 116.1(3) . . ? C5 C4 C25 122.4(3) . . ? C3 C4 C25 121.5(3) . . ? C4 C5 C6 122.1(3) . . ? C5 C6 C1 119.7(3) . . ? C5 C6 C7 119.3(3) . . ? C1 C6 C7 120.6(3) . . ? N1 C7 C6 125.1(3) . . ? N1 C8 C9 112.9(3) . . ? C8 C9 C10 113.7(3) . . ? N2 C10 C9 109.1(3) . . ? N2 C11 C12 128.8(3) . . ? C13 C12 C11 116.9(3) . . ? C13 C12 C17 120.4(3) . . ? C11 C12 C17 121.8(3) . . ? C14 C13 C12 122.1(3) . . ? C13 C14 C15 116.5(3) . . ? C13 C14 C29 123.6(3) . . ? C15 C14 C29 119.9(3) . . ? C16 C15 C14 125.2(3) . . ? C15 C16 C17 117.4(3) . . ? C15 C16 C33 122.1(3) . . ? C17 C16 C33 120.5(3) . . ? O2 C17 C12 121.2(3) . . ? O2 C17 C16 120.4(3) . . ? C12 C17 C16 118.4(3) . . ? N3 C18 N3 112.8(4) 2_656 . ? C19 C19 N3 108.28(16) 2_656 . ? C19 C19 C20 132.51(18) 2_656 . ? N3 C19 C20 119.2(3) . . ? O3 C20 O4 123.6(3) . . ? O3 C20 C19 118.5(3) . . ? O4 C20 C19 117.9(3) . . ? C22 C21 C23 108.9(3) . . ? C22 C21 C24 107.3(4) . . ? C23 C21 C24 107.5(3) . . ? C22 C21 C2 108.2(3) . . ? C23 C21 C2 112.9(3) . . ? C24 C21 C2 111.9(3) . . ? C28A C25 C27 135.5(8) . . ? C28A C25 C28 68.6(10) . . ? C27 C25 C28 109.6(6) . . ? C28A C25 C4 111.8(7) . . ? C27 C25 C4 110.3(4) . . ? C28 C25 C4 109.3(4) . . ? C28A C25 C26 40.0(9) . . ? C27 C25 C26 109.4(7) . . ? C28 C25 C26 106.0(6) . . ? C4 C25 C26 112.1(5) . . ? C28A C25 C27A 110.8(11) . . ? C27 C25 C27A 41.2(6) . . ? C28 C25 C27A 139.9(7) . . ? C4 C25 C27A 107.7(6) . . ? C26 C25 C27A 73.2(8) . . ? C28A C25 C26A 111.3(13) . . ? C27 C25 C26A 64.9(9) . . ? C28 C25 C26A 47.5(9) . . ? C4 C25 C26A 110.6(7) . . ? C26 C25 C26A 135.7(9) . . ? C27A C25 C26A 104.4(11) . . ? C32 C29 C31 108.1(4) . . ? C32 C29 C14 112.4(3) . . ? C31 C29 C14 111.7(3) . . ? C32 C29 C30 106.6(4) . . ? C31 C29 C30 109.9(4) . . ? C14 C29 C30 108.0(4) . . ? C16 C33 C34 112.5(3) . . ? C16 C33 C36 109.8(3) . . ? C34 C33 C36 107.6(3) . . ? C16 C33 C35 109.4(3) . . ? C34 C33 C35 108.0(3) . . ? C36 C33 C35 109.6(3) . . ? C39 C38 C43 120.0 . . ? C39 C38 C37 120.1(5) . . ? C43 C38 C37 119.7(5) . . ? C40 C39 C38 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C38 120.0 . . ? C46 C45 C50 120.0 . . ? C46 C45 C44 119.7(5) . . ? C50 C45 C44 120.0(5) . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C50 C49 C48 120.0 . . ? C49 C50 C45 120.0 . . ? C37A C38A C39A 119.4(10) . . ? C37A C38A C43A 120.6(10) . . ? C39A C38A C43A 120.0 . . ? C38A C39A C40A 120.0 . . ? C41A C40A C39A 120.0 . . ? C40A C41A C42A 120.0 . . ? C43A C42A C41A 120.0 . . ? C43A C42A C42A 134.3(14) . 2_655 ? C41A C42A C42A 105.7(14) . 2_655 ? C42A C43A C38A 120.0 . . ? C46A C45A C50A 120.0 . . ? C46A C45A C44A 114.2(12) . . ? C50A C45A C44A 125.8(12) . . ? C47A C46A C45A 120.0 . . ? C48A C47A C46A 120.0 . . ? C49A C48A C47A 120.0 . . ? C48A C49A C50A 120.0 . . ? C49A C50A C45A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.730 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.068 data_mn43 _database_code_CSD 195449 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Mn2III/IV(dtsalpn)2DCBI) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H109 Mn2 N10 O8' _chemical_formula_weight 1436.64 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.6699(8) _cell_length_b 21.6736(11) _cell_length_c 24.3289(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.814(2) _cell_angle_gamma 90.00 _cell_volume 8603.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 6437 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.36 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3068 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8735 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; hemisphere of 1321 frames x 30 sec. @ 4.109 cm; 0.3 deg. steps in omega & phi ; _diffrn_ambient_temperature 158(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55447 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.41 _reflns_number_total 17626 _reflns_number_gt 10096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Use of the PLATON/SQUEEZE subroutine revealed the presence of six solvent accessible voids of total volume 1392.3 A^3 and containing an extimated 222 electrons per unit cell due to diffuse solvent scattering. This has been included in all derived crystal quantities as 10 additional acetonitrile solvate molecules per unit cell. 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^)+(0.1276P)^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 SHELXL _refine_ls_extinction_coef 0.00057(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17626 _refine_ls_number_parameters 924 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2277 _refine_ls_wR_factor_gt 0.2029 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.02727(3) 0.38891(2) 0.42436(2) 0.03275(16) Uani 1 1 d . . . Mn2 Mn 0.09065(3) 0.10403(2) 0.45122(2) 0.04233(17) Uani 1 1 d . . . O1 O 0.12423(13) 0.40236(9) 0.47646(9) 0.0326(5) Uani 1 1 d . . . O2 O 0.08545(13) 0.38744(9) 0.36493(9) 0.0353(5) Uani 1 1 d . . . O3 O -0.03397(15) 0.37991(11) 0.48629(10) 0.0444(6) Uani 1 1 d . . . O4 O -0.07261(18) 0.31611(13) 0.54815(12) 0.0609(8) Uani 1 1 d . . . O5 O -0.0289(2) 0.17760(13) 0.56891(12) 0.0667(8) Uani 1 1 d . . . O6 O -0.00959(14) 0.09583(10) 0.40049(10) 0.0403(6) Uani 1 1 d . . . O7 O 0.15127(16) 0.11270(10) 0.39052(11) 0.0487(6) Uani 1 1 d . . . O8 O 0.03284(16) 0.11316(11) 0.51904(11) 0.0484(6) Uani 1 1 d . . . N1 N 0.00460(17) 0.47960(14) 0.42220(11) 0.0392(7) Uani 1 1 d . . . N2 N -0.07723(16) 0.37912(13) 0.36902(12) 0.0387(7) Uani 1 1 d . . . N3 N 0.03979(16) 0.29717(12) 0.43886(11) 0.0327(6) Uani 1 1 d . . . N4 N 0.07126(17) 0.19880(12) 0.45343(11) 0.0353(6) Uani 1 1 d . . . N5 N 0.0948(2) 0.01183(16) 0.45966(15) 0.0563(9) Uani 1 1 d . . . N6 N 0.1983(2) 0.10616(15) 0.50535(13) 0.0556(9) Uani 1 1 d . . . C1 C 0.17671(19) 0.44752(15) 0.47253(12) 0.0323(7) Uani 1 1 d . . . C2 C 0.2601(2) 0.43953(16) 0.49841(15) 0.0390(8) Uani 1 1 d . . . C3 C 0.3121(2) 0.48715(17) 0.49270(16) 0.0471(9) Uani 1 1 d . . . H3A H 0.3688 0.4814 0.5079 0.057 Uiso 1 1 calc R . . C4 C 0.2880(2) 0.54394(17) 0.46607(16) 0.0460(9) Uani 1 1 d . . . C5 C 0.2062(2) 0.55152(16) 0.44415(14) 0.0396(8) Uani 1 1 d . . . H5A H 0.1871 0.5898 0.4273 0.048 Uiso 1 1 calc R . . C6 C 0.1500(2) 0.50344(15) 0.44614(13) 0.0350(7) Uani 1 1 d . . . C7 C 0.0640(2) 0.51826(16) 0.42814(13) 0.0386(8) Uani 1 1 d . . . H7A H 0.0504 0.5603 0.4200 0.046 Uiso 1 1 calc R . . C8 C -0.0789(2) 0.5050(2) 0.4183(2) 0.0672(13) Uani 1 1 d . . . H8A H -0.0930 0.5019 0.4558 0.081 Uiso 1 1 calc R . . H8B H -0.0777 0.5494 0.4089 0.081 Uiso 1 1 calc R . . C9 C -0.1448(3) 0.4755(2) 0.3771(2) 0.0789(15) Uani 1 1 d . . . H9A H -0.1361 0.4850 0.3390 0.095 Uiso 1 1 calc R . . H9B H -0.1977 0.4942 0.3807 0.095 Uiso 1 1 calc R . . C10 C -0.1517(2) 0.4051(2) 0.38258(18) 0.0576(11) Uani 1 1 d . . . H10A H -0.1560 0.3938 0.4213 0.069 Uiso 1 1 calc R . . H10B H -0.2008 0.3895 0.3562 0.069 Uiso 1 1 calc R . . C11 C -0.0822(2) 0.35876(16) 0.31819(15) 0.0419(8) Uani 1 1 d . . . H11A H -0.1359 0.3507 0.2973 0.050 Uiso 1 1 calc R . . C12 C -0.0164(2) 0.34706(15) 0.29019(14) 0.0365(8) Uani 1 1 d . . . C13 C -0.0386(2) 0.32621(15) 0.23430(14) 0.0401(8) Uani 1 1 d . . . H13A H -0.0935 0.3137 0.2199 0.048 Uiso 1 1 calc R . . C14 C 0.0166(2) 0.32365(15) 0.20065(15) 0.0421(9) Uani 1 1 d . . . C15 C 0.0976(2) 0.34219(15) 0.22377(15) 0.0433(8) Uani 1 1 d . . . H15A H 0.1369 0.3400 0.2005 0.052 Uiso 1 1 calc R . . C16 C 0.1237(2) 0.36328(15) 0.27814(15) 0.0403(8) Uani 1 1 d . . . C17 C 0.0652(2) 0.36526(14) 0.31301(14) 0.0351(8) Uani 1 1 d . . . C18 C 0.07797(19) 0.24831(14) 0.42281(13) 0.0321(7) Uani 1 1 d . . . H18A H 0.1067 0.2490 0.3929 0.038 Uiso 1 1 calc R . . C19 C 0.0259(2) 0.21650(15) 0.49217(14) 0.0380(8) Uani 1 1 d . . . C20 C 0.0066(2) 0.27770(15) 0.48381(13) 0.0364(8) Uani 1 1 d . . . C21 C -0.0368(2) 0.32533(17) 0.50961(16) 0.0444(9) Uani 1 1 d . . . C22 C 0.0079(2) 0.16689(17) 0.53089(16) 0.0476(9) Uani 1 1 d . . . C23 C -0.0226(2) 0.05525(17) 0.35880(15) 0.0444(9) Uani 1 1 d . . . C24 C -0.0807(2) 0.06907(19) 0.30897(17) 0.0589(11) Uani 1 1 d . . . C25 C -0.0852(3) 0.0298(2) 0.2644(2) 0.109(2) Uani 1 1 d . . . H25A H -0.1198 0.0421 0.2301 0.131 Uiso 1 1 calc R . . C26 C -0.0464(8) -0.0238(6) 0.2638(6) 0.142(7) Uani 1 1 d . . . C27 C 0.0051(2) -0.0424(2) 0.3199(2) 0.0883(18) Uani 1 1 d . . . H27A H 0.0296 -0.0821 0.3242 0.106 Uiso 1 1 calc R . . C28 C 0.0172(2) -0.00232(16) 0.36513(17) 0.0469(9) Uani 1 1 d . . . C29 C 0.0663(3) -0.0218(3) 0.4174(3) 0.0566(17) Uani 1 1 d . . . H29A H 0.0790 -0.0646 0.4210 0.068 Uiso 1 1 calc R . . C30 C 0.1199(4) -0.0194(3) 0.5145(3) 0.113(2) Uani 1 1 d . . . H30A H 0.1377 -0.0619 0.5080 0.136 Uiso 1 1 calc R . . H30B H 0.0717 -0.0225 0.5323 0.136 Uiso 1 1 calc R . . C31 C 0.1877(5) 0.0125(4) 0.5543(3) 0.145(3) Uani 1 1 d . . . H31A H 0.1836 -0.0025 0.5921 0.174 Uiso 1 1 calc R . . H31B H 0.2389 -0.0053 0.5465 0.174 Uiso 1 1 calc R . . C32 C 0.2025(3) 0.0765(3) 0.5607(2) 0.0905(18) Uani 1 1 d . . . H32A H 0.2574 0.0834 0.5846 0.109 Uiso 1 1 calc R . . H32B H 0.1613 0.0953 0.5796 0.109 Uiso 1 1 calc R . . C33 C 0.2646(3) 0.12657(19) 0.49442(16) 0.0555(11) Uani 1 1 d . . . H33A H 0.3097 0.1289 0.5254 0.067 Uiso 1 1 calc R . . C34 C 0.2807(2) 0.14680(16) 0.44120(15) 0.0462(9) Uani 1 1 d . . . C35 C 0.3600(3) 0.16950(17) 0.44078(17) 0.0537(10) Uani 1 1 d . . . H35A H 0.3966 0.1768 0.4756 0.064 Uiso 1 1 calc R . . C36 C 0.3858(3) 0.18133(18) 0.39213(17) 0.0569(11) Uani 1 1 d . . . C37 C 0.3277(3) 0.17067(18) 0.34201(17) 0.0605(11) Uani 1 1 d . . . H37A H 0.3442 0.1790 0.3076 0.073 Uiso 1 1 calc R . . C38 C 0.2493(3) 0.14923(17) 0.33888(16) 0.0530(10) Uani 1 1 d . . . C39 C 0.2241(2) 0.13610(15) 0.39042(15) 0.0465(9) Uani 1 1 d . . . C40 C 0.2897(2) 0.38097(16) 0.53332(16) 0.0431(9) Uani 1 1 d . . . C41 C 0.2751(2) 0.32294(18) 0.49728(17) 0.0570(11) Uani 1 1 d . . . H41A H 0.2876 0.2865 0.5213 0.086 Uiso 1 1 calc R . . H41B H 0.3106 0.3236 0.4698 0.086 Uiso 1 1 calc R . . H41C H 0.2176 0.3215 0.4776 0.086 Uiso 1 1 calc R . . C42 C 0.2457(3) 0.37565(19) 0.58183(16) 0.0578(11) Uani 1 1 d . . . H42A H 0.2569 0.4124 0.6056 0.087 Uiso 1 1 calc R . . H42B H 0.2651 0.3389 0.6041 0.087 Uiso 1 1 calc R . . H42C H 0.1866 0.3722 0.5672 0.087 Uiso 1 1 calc R . . C43 C 0.3820(3) 0.3849(2) 0.5587(2) 0.0827(17) Uani 1 1 d . . . H43A H 0.3932 0.4223 0.5816 0.124 Uiso 1 1 calc R . . H43B H 0.4127 0.3863 0.5284 0.124 Uiso 1 1 calc R . . H43C H 0.3988 0.3486 0.5823 0.124 Uiso 1 1 calc R . . C44 C 0.3516(3) 0.59281(19) 0.46093(19) 0.0582(11) Uani 1 1 d . . . C45 C 0.4110(3) 0.6026(2) 0.5166(2) 0.0948(19) Uani 1 1 d . . . H45A H 0.3806 0.6155 0.5451 0.142 Uiso 1 1 calc R . . H45B H 0.4507 0.6347 0.5122 0.142 Uiso 1 1 calc R . . H45C H 0.4401 0.5640 0.5283 0.142 Uiso 1 1 calc R . . C46 C 0.3996(3) 0.5722(2) 0.4168(2) 0.0736(14) Uani 1 1 d . . . H46A H 0.4274 0.5331 0.4285 0.110 Uiso 1 1 calc R . . H46B H 0.4403 0.6036 0.4130 0.110 Uiso 1 1 calc R . . H46C H 0.3617 0.5665 0.3806 0.110 Uiso 1 1 calc R . . C47 C 0.3100(3) 0.6548(2) 0.4411(2) 0.0818(15) Uani 1 1 d . . . H47A H 0.2735 0.6668 0.4661 0.123 Uiso 1 1 calc R . . H47B H 0.2782 0.6503 0.4027 0.123 Uiso 1 1 calc R . . H47C H 0.3520 0.6866 0.4419 0.123 Uiso 1 1 calc R . . C48 C -0.0066(2) 0.30516(18) 0.13838(15) 0.0514(10) Uani 1 1 d . . . C49 C 0.0419(3) 0.2487(2) 0.12772(19) 0.0758(14) Uani 1 1 d . . . H49A H 0.1006 0.2574 0.1390 0.114 Uiso 1 1 calc R . . H49B H 0.0285 0.2384 0.0877 0.114 Uiso 1 1 calc R . . H49C H 0.0278 0.2139 0.1496 0.114 Uiso 1 1 calc R . . C50 C -0.0982(3) 0.2885(2) 0.12123(17) 0.0629(12) Uani 1 1 d . . . H50A H -0.1314 0.3246 0.1260 0.094 Uiso 1 1 calc R . . H50B H -0.1107 0.2548 0.1450 0.094 Uiso 1 1 calc R . . H50C H -0.1107 0.2754 0.0818 0.094 Uiso 1 1 calc R . . C51 C 0.0098(3) 0.3599(2) 0.10282(18) 0.0774(14) Uani 1 1 d . . . H51A H 0.0678 0.3714 0.1132 0.116 Uiso 1 1 calc R . . H51B H -0.0241 0.3950 0.1094 0.116 Uiso 1 1 calc R . . H51C H -0.0037 0.3486 0.0630 0.116 Uiso 1 1 calc R . . C52 C 0.2112(2) 0.3857(2) 0.29913(18) 0.0593(11) Uani 1 1 d . . . C53 C 0.2107(3) 0.4550(2) 0.31293(19) 0.0753(15) Uani 1 1 d . . . H53A H 0.1854 0.4780 0.2791 0.113 Uiso 1 1 calc R . . H53B H 0.2670 0.4693 0.3262 0.113 Uiso 1 1 calc R . . H53C H 0.1792 0.4618 0.3423 0.113 Uiso 1 1 calc R . . C54 C 0.2646(3) 0.3779(3) 0.2552(2) 0.0939(19) Uani 1 1 d . . . H54A H 0.2401 0.4007 0.2211 0.141 Uiso 1 1 calc R . . H54B H 0.2681 0.3340 0.2461 0.141 Uiso 1 1 calc R . . H54C H 0.3196 0.3939 0.2702 0.141 Uiso 1 1 calc R . . C55 C 0.2511(3) 0.3507(3) 0.3524(2) 0.0875(17) Uani 1 1 d . . . H55A H 0.2532 0.3066 0.3439 0.131 Uiso 1 1 calc R . . H55B H 0.2188 0.3569 0.3813 0.131 Uiso 1 1 calc R . . H55C H 0.3069 0.3662 0.3659 0.131 Uiso 1 1 calc R . . C56 C -0.1363(2) 0.12583(18) 0.30375(17) 0.0521(10) Uani 1 1 d . . . C57 C -0.1912(3) 0.1198(2) 0.3450(2) 0.0756(14) Uani 1 1 d . . . H57A H -0.2172 0.0790 0.3411 0.113 Uiso 1 1 calc R . . H57B H -0.2336 0.1518 0.3376 0.113 Uiso 1 1 calc R . . H57C H -0.1589 0.1246 0.3832 0.113 Uiso 1 1 calc R . . C58 C -0.0883(3) 0.1870(2) 0.3153(2) 0.0832(16) Uani 1 1 d . . . H58A H -0.1268 0.2217 0.3105 0.125 Uiso 1 1 calc R . . H58B H -0.0514 0.1913 0.2889 0.125 Uiso 1 1 calc R . . H58C H -0.0561 0.1869 0.3539 0.125 Uiso 1 1 calc R . . C59 C -0.1924(3) 0.1311(3) 0.2454(2) 0.105(2) Uani 1 1 d . . . H59A H -0.2313 0.0966 0.2397 0.157 Uiso 1 1 calc R . . H59B H -0.1592 0.1299 0.2165 0.157 Uiso 1 1 calc R . . H59C H -0.2226 0.1701 0.2427 0.157 Uiso 1 1 calc R . . C60 C -0.0493(4) -0.0672(3) 0.2142(3) 0.130(3) Uani 1 1 d . . . C61 C -0.0233(6) -0.1354(3) 0.2338(4) 0.236(6) Uani 1 1 d . . . H61A H -0.0319 -0.1627 0.2010 0.354 Uiso 1 1 calc R . . H61B H -0.0567 -0.1497 0.2601 0.354 Uiso 1 1 calc R . . H61C H 0.0347 -0.1360 0.2523 0.354 Uiso 1 1 calc R . . C62 C -0.1329(3) -0.0673(4) 0.1798(3) 0.135(3) Uani 1 1 d . . . H62A H -0.1567 -0.0259 0.1798 0.203 Uiso 1 1 calc R . . H62B H -0.1668 -0.0969 0.1953 0.203 Uiso 1 1 calc R . . H62C H -0.1310 -0.0791 0.1412 0.203 Uiso 1 1 calc R . . C63 C 0.0040(6) -0.0386(5) 0.1752(4) 0.118(4) Uani 1 1 d . . . H63A H -0.0202 0.0006 0.1601 0.176 Uiso 1 1 calc R . . H63B H 0.0060 -0.0671 0.1442 0.176 Uiso 1 1 calc R . . H63C H 0.0596 -0.0314 0.1968 0.176 Uiso 1 1 calc R . . C64 C 0.4708(3) 0.2047(2) 0.39130(19) 0.0678(12) Uani 1 1 d . . . C65 C 0.5261(8) 0.1531(7) 0.4157(8) 0.096(6) Uani 0.400(9) 1 d P B 1 H65A H 0.5138 0.1165 0.3918 0.144 Uiso 0.400(9) 1 calc PR B 1 H65B H 0.5176 0.1436 0.4534 0.144 Uiso 0.400(9) 1 calc PR B 1 H65C H 0.5832 0.1653 0.4178 0.144 Uiso 0.400(9) 1 calc PR B 1 C65A C 0.5283(5) 0.2118(5) 0.4522(3) 0.078(3) Uani 0.600(9) 1 d P B 2 H65D H 0.5334 0.1718 0.4714 0.117 Uiso 0.600(9) 1 calc PR B 2 H65E H 0.5042 0.2419 0.4741 0.117 Uiso 0.600(9) 1 calc PR B 2 H65F H 0.5827 0.2260 0.4483 0.117 Uiso 0.600(9) 1 calc PR B 2 C66 C 0.4822(8) 0.2624(6) 0.4229(7) 0.090(5) Uani 0.400(9) 1 d P B 1 H66A H 0.4711 0.2555 0.4605 0.134 Uiso 0.400(9) 1 calc PR B 1 H66B H 0.4443 0.2936 0.4033 0.134 Uiso 0.400(9) 1 calc PR B 1 H66C H 0.5387 0.2767 0.4262 0.134 Uiso 0.400(9) 1 calc PR B 1 C66A C 0.4667(6) 0.2707(5) 0.3674(5) 0.109(5) Uani 0.600(9) 1 d P B 2 H66D H 0.4338 0.2708 0.3291 0.164 Uiso 0.600(9) 1 calc PR B 2 H66E H 0.5222 0.2852 0.3669 0.164 Uiso 0.600(9) 1 calc PR B 2 H66F H 0.4414 0.2981 0.3910 0.164 Uiso 0.600(9) 1 calc PR B 2 C67 C 0.4773(11) 0.2144(9) 0.3265(6) 0.096(6) Uani 0.400(9) 1 d P B 1 H67A H 0.4656 0.1754 0.3062 0.143 Uiso 0.400(9) 1 calc PR B 1 H67B H 0.5327 0.2282 0.3248 0.143 Uiso 0.400(9) 1 calc PR B 1 H67C H 0.4375 0.2456 0.3093 0.143 Uiso 0.400(9) 1 calc PR B 1 C67A C 0.5181(7) 0.1644(9) 0.3582(7) 0.143(7) Uani 0.600(9) 1 d P B 2 H67D H 0.5251 0.1232 0.3750 0.214 Uiso 0.600(9) 1 calc PR B 2 H67E H 0.5720 0.1828 0.3589 0.214 Uiso 0.600(9) 1 calc PR B 2 H67F H 0.4879 0.1613 0.3193 0.214 Uiso 0.600(9) 1 calc PR B 2 C68 C 0.1908(3) 0.1374(2) 0.28245(17) 0.0672(12) Uani 1 1 d . . . C69 C 0.2259(4) 0.1565(3) 0.2327(2) 0.107(2) Uani 1 1 d . . . H69A H 0.2362 0.2011 0.2342 0.161 Uiso 1 1 calc R . . H69B H 0.1869 0.1464 0.1979 0.161 Uiso 1 1 calc R . . H69C H 0.2775 0.1345 0.2335 0.161 Uiso 1 1 calc R . . C70 C 0.1101(3) 0.1719(2) 0.27978(18) 0.0796(15) Uani 1 1 d . . . H70A H 0.0840 0.1574 0.3100 0.119 Uiso 1 1 calc R . . H70B H 0.0736 0.1641 0.2434 0.119 Uiso 1 1 calc R . . H70C H 0.1210 0.2162 0.2842 0.119 Uiso 1 1 calc R . . C71 C 0.1721(3) 0.0667(2) 0.2774(2) 0.0882(17) Uani 1 1 d . . . H71A H 0.1413 0.0545 0.3059 0.132 Uiso 1 1 calc R . . H71B H 0.2237 0.0436 0.2831 0.132 Uiso 1 1 calc R . . H71C H 0.1395 0.0576 0.2400 0.132 Uiso 1 1 calc R . . N7 N 0.2506(6) 0.8557(6) 0.4007(5) 0.113(4) Uani 0.50 1 d P . . C72 C 0.1004(13) 0.5154(6) 0.7919(5) 0.107(6) Uani 0.50 1 d P . . C73 C 0.0238(9) 0.5012(4) 0.7860(6) 0.093(4) Uani 0.50 1 d P . . H73A H -0.0087 0.5389 0.7858 0.139 Uiso 0.50 1 calc PR . . H73B H 0.0162 0.4748 0.8173 0.139 Uiso 0.50 1 calc PR . . H73C H 0.0056 0.4791 0.7505 0.139 Uiso 0.50 1 calc PR . . N8 N 0.2246(5) 0.2199(4) 0.8911(4) 0.080(2) Uani 0.50 1 d P . . C74 C 0.2063(7) 0.8180(6) 0.3805(4) 0.070(3) Uani 0.50 1 d P . . C75 C 0.1524(6) 0.7729(4) 0.3599(3) 0.057(2) Uani 0.50 1 d P . . H75A H 0.1271 0.7569 0.3900 0.086 Uiso 0.50 1 calc PR . . H75B H 0.1812 0.7394 0.3450 0.086 Uiso 0.50 1 calc PR . . H75C H 0.1098 0.7896 0.3297 0.086 Uiso 0.50 1 calc PR . . N9 N 0.1685(10) 0.5358(6) 0.7961(6) 0.142(6) Uani 0.50 1 d P . . C76 C 0.2513(4) 0.2489(4) 0.9275(4) 0.0499(19) Uani 0.50 1 d P . . C77 C 0.2876(5) 0.2889(4) 0.9752(3) 0.0521(19) Uani 0.50 1 d P . . H77A H 0.3315 0.2665 1.0003 0.078 Uiso 0.50 1 calc PR . . H77B H 0.2453 0.3007 0.9959 0.078 Uiso 0.50 1 calc PR . . H77C H 0.3102 0.3261 0.9612 0.078 Uiso 0.50 1 calc PR . . 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 0.0330(3) 0.0344(3) 0.0292(3) -0.0026(2) 0.0026(2) 0.0015(2) Mn2 0.0502(3) 0.0347(3) 0.0356(3) 0.0105(2) -0.0063(2) -0.0108(2) O1 0.0356(12) 0.0332(12) 0.0272(12) 0.0011(9) 0.0024(9) -0.0023(10) O2 0.0386(12) 0.0314(12) 0.0320(12) -0.0043(9) -0.0019(10) -0.0057(10) O3 0.0483(14) 0.0386(14) 0.0452(15) -0.0042(11) 0.0066(12) 0.0035(11) O4 0.081(2) 0.0596(18) 0.0508(17) -0.0019(13) 0.0332(16) 0.0009(15) O5 0.106(2) 0.0529(17) 0.0542(18) 0.0093(14) 0.0473(18) 0.0016(16) O6 0.0468(14) 0.0292(12) 0.0387(13) 0.0069(10) -0.0057(11) -0.0093(10) O7 0.0546(16) 0.0329(13) 0.0485(15) -0.0014(11) -0.0132(12) -0.0023(12) O8 0.0664(17) 0.0323(14) 0.0481(15) 0.0061(11) 0.0154(13) -0.0072(12) N1 0.0370(16) 0.0495(18) 0.0292(15) -0.0059(13) 0.0024(12) 0.0057(14) N2 0.0350(15) 0.0396(16) 0.0388(17) -0.0056(13) 0.0014(13) 0.0009(12) N3 0.0358(15) 0.0304(14) 0.0318(15) 0.0002(11) 0.0067(12) -0.0049(12) N4 0.0484(17) 0.0262(14) 0.0284(14) -0.0022(11) 0.0011(12) -0.0051(12) N5 0.066(2) 0.047(2) 0.050(2) 0.0217(16) -0.0034(17) -0.0073(17) N6 0.054(2) 0.061(2) 0.0417(18) 0.0226(15) -0.0135(15) -0.0218(16) C1 0.0377(18) 0.0376(18) 0.0220(15) -0.0040(13) 0.0065(13) 0.0018(15) C2 0.0385(19) 0.0361(19) 0.040(2) 0.0022(15) 0.0031(15) -0.0022(15) C3 0.040(2) 0.047(2) 0.051(2) 0.0030(17) 0.0009(17) -0.0040(17) C4 0.047(2) 0.041(2) 0.048(2) 0.0035(17) 0.0074(18) -0.0064(17) C5 0.051(2) 0.0351(19) 0.0321(18) -0.0005(14) 0.0069(16) 0.0012(16) C6 0.0392(19) 0.0352(18) 0.0296(17) -0.0045(14) 0.0050(14) 0.0016(15) C7 0.046(2) 0.041(2) 0.0264(17) -0.0051(14) 0.0023(15) 0.0109(17) C8 0.038(2) 0.078(3) 0.083(3) -0.014(3) 0.006(2) 0.016(2) C9 0.047(3) 0.082(3) 0.098(4) -0.033(3) -0.009(2) 0.022(2) C10 0.0299(19) 0.081(3) 0.058(3) -0.017(2) 0.0004(18) 0.0043(19) C11 0.0380(19) 0.041(2) 0.041(2) -0.0025(16) -0.0052(16) 0.0017(16) C12 0.0422(19) 0.0292(17) 0.0335(18) -0.0011(14) -0.0032(15) 0.0001(14) C13 0.049(2) 0.0298(17) 0.0361(19) -0.0027(14) -0.0044(16) 0.0000(15) C14 0.057(2) 0.0239(17) 0.040(2) -0.0035(14) -0.0010(17) 0.0041(15) C15 0.058(2) 0.0359(19) 0.0360(19) -0.0012(15) 0.0091(17) -0.0003(17) C16 0.046(2) 0.0329(18) 0.041(2) -0.0026(15) 0.0051(16) -0.0034(15) C17 0.048(2) 0.0201(15) 0.0344(18) -0.0003(13) 0.0013(15) 0.0023(14) C18 0.0361(17) 0.0291(17) 0.0313(17) -0.0046(13) 0.0072(14) -0.0057(14) C19 0.047(2) 0.0340(18) 0.0329(18) -0.0018(14) 0.0073(15) -0.0057(15) C20 0.044(2) 0.0363(18) 0.0289(17) 0.0001(14) 0.0084(15) -0.0106(15) C21 0.047(2) 0.044(2) 0.042(2) -0.0009(17) 0.0073(17) -0.0060(17) C22 0.064(3) 0.038(2) 0.040(2) 0.0056(16) 0.0091(19) -0.0081(18) C23 0.043(2) 0.042(2) 0.045(2) -0.0024(17) 0.0006(17) -0.0102(16) C24 0.051(2) 0.059(3) 0.057(3) -0.016(2) -0.012(2) 0.012(2) C25 0.103(4) 0.096(4) 0.099(4) -0.050(3) -0.050(3) 0.045(3) C26 0.126(11) 0.081(7) 0.181(12) -0.053(7) -0.055(8) 0.002(7) C27 0.054(3) 0.070(3) 0.122(5) -0.042(3) -0.025(3) 0.018(2) C28 0.037(2) 0.038(2) 0.060(2) -0.0033(17) -0.0024(18) -0.0053(16) C29 0.053(3) 0.033(3) 0.084(4) 0.022(3) 0.015(2) -0.004(2) C30 0.117(5) 0.105(4) 0.100(4) 0.057(3) -0.022(4) -0.019(4) C31 0.168(6) 0.133(5) 0.097(5) 0.059(4) -0.064(4) -0.081(5) C32 0.084(3) 0.113(4) 0.060(3) 0.051(3) -0.020(3) -0.035(3) C33 0.059(3) 0.057(2) 0.039(2) 0.0135(18) -0.0154(19) -0.013(2) C34 0.057(2) 0.0333(19) 0.041(2) 0.0084(15) -0.0082(17) -0.0096(17) C35 0.069(3) 0.038(2) 0.046(2) 0.0028(17) -0.005(2) -0.0135(19) C36 0.075(3) 0.046(2) 0.046(2) 0.0010(18) 0.004(2) -0.010(2) C37 0.088(3) 0.047(2) 0.044(2) -0.0035(18) 0.008(2) -0.010(2) C38 0.075(3) 0.036(2) 0.042(2) -0.0070(16) -0.001(2) -0.0057(19) C39 0.068(3) 0.0206(17) 0.042(2) -0.0029(14) -0.0104(18) -0.0021(17) C40 0.0384(19) 0.039(2) 0.046(2) 0.0055(16) -0.0030(16) 0.0015(15) C41 0.059(2) 0.043(2) 0.061(3) -0.0031(19) -0.006(2) 0.0149(19) C42 0.073(3) 0.057(3) 0.038(2) 0.0072(18) -0.003(2) 0.017(2) C43 0.049(3) 0.063(3) 0.120(5) 0.032(3) -0.022(3) 0.002(2) C44 0.053(2) 0.049(2) 0.069(3) 0.008(2) 0.004(2) -0.0105(19) C45 0.108(4) 0.088(4) 0.074(4) 0.013(3) -0.015(3) -0.056(3) C46 0.052(3) 0.084(3) 0.084(4) 0.018(3) 0.012(2) -0.014(2) C47 0.078(3) 0.051(3) 0.118(4) 0.014(3) 0.024(3) -0.017(2) C48 0.069(3) 0.046(2) 0.034(2) -0.0074(16) -0.0010(18) 0.0046(19) C49 0.094(3) 0.076(3) 0.050(3) -0.027(2) -0.001(2) 0.017(3) C50 0.072(3) 0.066(3) 0.041(2) -0.014(2) -0.010(2) -0.001(2) C51 0.115(4) 0.074(3) 0.036(2) 0.001(2) 0.000(2) -0.020(3) C52 0.049(2) 0.075(3) 0.053(3) -0.017(2) 0.008(2) -0.015(2) C53 0.093(3) 0.082(3) 0.057(3) -0.025(2) 0.029(3) -0.051(3) C54 0.058(3) 0.148(5) 0.084(4) -0.049(4) 0.033(3) -0.029(3) C55 0.042(3) 0.131(5) 0.079(4) -0.016(3) -0.012(2) -0.006(3) C56 0.052(2) 0.048(2) 0.047(2) 0.0030(18) -0.0099(18) 0.0046(18) C57 0.070(3) 0.067(3) 0.092(4) 0.028(3) 0.022(3) 0.020(2) C58 0.072(3) 0.061(3) 0.106(4) 0.041(3) -0.006(3) -0.010(2) C59 0.101(4) 0.127(5) 0.065(3) -0.022(3) -0.033(3) 0.057(4) C60 0.117(5) 0.094(5) 0.155(7) -0.057(5) -0.030(5) 0.019(4) C61 0.176(7) 0.163(7) 0.306(11) -0.174(8) -0.098(7) 0.089(6) C62 0.104(5) 0.165(7) 0.126(6) -0.088(5) -0.001(4) -0.037(4) C63 0.092(7) 0.151(10) 0.097(7) -0.076(7) -0.011(6) 0.008(6) C64 0.070(3) 0.077(3) 0.057(3) 0.004(2) 0.015(2) -0.018(3) C65 0.076(9) 0.078(10) 0.134(16) -0.003(10) 0.024(10) -0.007(8) C65A 0.062(5) 0.101(8) 0.067(6) 0.005(5) 0.005(4) -0.033(5) C66 0.075(9) 0.071(9) 0.112(13) -0.008(9) -0.006(8) -0.038(7) C66A 0.092(7) 0.130(9) 0.096(9) 0.048(7) -0.007(6) -0.060(6) C67 0.100(12) 0.111(14) 0.075(10) -0.007(9) 0.016(9) -0.047(10) C67A 0.090(8) 0.223(19) 0.124(13) -0.080(13) 0.042(9) -0.024(10) C68 0.088(3) 0.070(3) 0.038(2) -0.010(2) 0.000(2) -0.014(3) C69 0.126(5) 0.154(6) 0.038(3) -0.020(3) 0.005(3) -0.030(4) C70 0.109(4) 0.077(3) 0.039(2) 0.000(2) -0.018(2) 0.016(3) C71 0.103(4) 0.078(4) 0.079(4) -0.041(3) 0.007(3) -0.019(3) N7 0.089(7) 0.163(11) 0.090(8) 0.047(7) 0.027(6) -0.034(7) C72 0.151(13) 0.071(9) 0.077(8) 0.004(6) -0.031(11) 0.079(11) C73 0.143(11) 0.027(5) 0.113(10) 0.016(5) 0.037(9) 0.020(6) N8 0.087(6) 0.052(5) 0.096(7) -0.012(5) 0.005(5) -0.007(4) C74 0.070(6) 0.100(7) 0.051(5) 0.030(5) 0.039(5) 0.013(5) C75 0.077(5) 0.061(5) 0.045(4) 0.010(4) 0.036(4) 0.022(4) N9 0.163(12) 0.108(10) 0.127(10) -0.005(7) -0.033(10) 0.093(10) C76 0.036(4) 0.038(4) 0.075(6) 0.009(4) 0.009(4) 0.006(3) C77 0.046(4) 0.053(5) 0.052(5) 0.013(4) -0.002(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.861(2) . ? Mn1 O2 1.899(2) . ? Mn1 N2 1.983(3) . ? Mn1 O3 1.995(3) . ? Mn1 N1 2.000(3) . ? Mn1 N3 2.023(3) . ? Mn2 O6 1.871(2) . ? Mn2 O7 1.962(3) . ? Mn2 N6 1.997(3) . ? Mn2 N5 2.009(3) . ? Mn2 N4 2.082(3) . ? Mn2 O8 2.084(3) . ? O1 C1 1.329(4) . ? O2 C17 1.329(4) . ? O3 C21 1.317(4) . ? O4 C21 1.227(4) . ? O5 C22 1.232(4) . ? O6 C23 1.326(4) . ? O7 C39 1.316(4) . ? O8 C22 1.289(4) . ? N1 C7 1.283(4) . ? N1 C8 1.482(4) . ? N2 C11 1.299(4) . ? N2 C10 1.461(4) . ? N3 C18 1.334(4) . ? N3 C20 1.389(4) . ? N4 C18 1.324(4) . ? N4 C19 1.378(4) . ? N5 C29 1.271(7) . ? N5 C30 1.478(6) . ? N6 C33 1.268(5) . ? N6 C32 1.482(5) . ? C1 C6 1.401(4) . ? C1 C2 1.415(4) . ? C2 C3 1.372(5) . ? C2 C40 1.550(5) . ? C3 C4 1.410(5) . ? C4 C5 1.368(5) . ? C4 C44 1.522(5) . ? C5 C6 1.409(5) . ? C6 C7 1.446(5) . ? C8 C9 1.473(6) . ? C9 C10 1.538(6) . ? C11 C12 1.428(5) . ? C12 C13 1.409(4) . ? C12 C17 1.415(5) . ? C13 C14 1.353(5) . ? C14 C15 1.411(5) . ? C14 C48 1.538(5) . ? C15 C16 1.383(5) . ? C16 C17 1.418(5) . ? C16 C52 1.523(5) . ? C19 C20 1.371(5) . ? C19 C22 1.500(5) . ? C20 C21 1.472(5) . ? C23 C28 1.406(5) . ? C23 C24 1.420(5) . ? C24 C25 1.368(6) . ? C24 C56 1.530(5) . ? C25 C26 1.331(17) . ? C26 C27 1.511(18) . ? C26 C60 1.523(7) . ? C27 C28 1.383(6) . ? C28 C29 1.428(7) . ? C30 C31 1.497(8) . ? C31 C32 1.412(9) . ? C33 C34 1.443(5) . ? C34 C39 1.412(5) . ? C34 C35 1.412(5) . ? C35 C36 1.364(5) . ? C36 C37 1.412(6) . ? C36 C64 1.508(6) . ? C37 C38 1.374(6) . ? C38 C39 1.431(5) . ? C38 C68 1.534(5) . ? C40 C42 1.516(5) . ? C40 C41 1.524(5) . ? C40 C43 1.539(5) . ? C44 C45 1.520(6) . ? C44 C46 1.531(6) . ? C44 C47 1.542(6) . ? C48 C49 1.518(5) . ? C48 C51 1.526(6) . ? C48 C50 1.541(6) . ? C52 C55 1.530(7) . ? C52 C54 1.534(6) . ? C52 C53 1.540(6) . ? C56 C57 1.496(6) . ? C56 C59 1.537(6) . ? C56 C58 1.544(6) . ? C60 C62 1.472(6) . ? C60 C63 1.555(7) . ? C60 C61 1.586(7) . ? C64 C66 1.460(14) . ? C64 C65 1.492(15) . ? C64 C67A 1.513(12) . ? C64 C66A 1.541(11) . ? C64 C65A 1.598(9) . ? C64 C67 1.616(15) . ? C68 C69 1.507(7) . ? C68 C70 1.528(7) . ? C68 C71 1.564(7) . ? N7 C74 1.143(14) . ? C72 N9 1.20(2) . ? C72 C73 1.29(2) . ? N8 C76 1.103(10) . ? C74 C75 1.353(15) . ? C76 C77 1.476(12) . ? 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 O2 90.77(9) . . ? O1 Mn1 N2 177.10(11) . . ? O2 Mn1 N2 89.76(11) . . ? O1 Mn1 O3 90.48(10) . . ? O2 Mn1 O3 173.42(9) . . ? N2 Mn1 O3 89.31(11) . . ? O1 Mn1 N1 89.84(10) . . ? O2 Mn1 N1 96.87(10) . . ? N2 Mn1 N1 87.27(11) . . ? O3 Mn1 N1 89.59(11) . . ? O1 Mn1 N3 89.48(10) . . ? O2 Mn1 N3 93.77(10) . . ? N2 Mn1 N3 93.33(11) . . ? O3 Mn1 N3 79.78(10) . . ? N1 Mn1 N3 169.35(11) . . ? O6 Mn2 O7 92.34(10) . . ? O6 Mn2 N6 175.86(12) . . ? O7 Mn2 N6 87.84(13) . . ? O6 Mn2 N5 88.88(12) . . ? O7 Mn2 N5 99.20(12) . . ? N6 Mn2 N5 87.01(13) . . ? O6 Mn2 N4 89.34(10) . . ? O7 Mn2 N4 91.81(10) . . ? N6 Mn2 N4 94.79(12) . . ? N5 Mn2 N4 168.90(13) . . ? O6 Mn2 O8 92.06(11) . . ? O7 Mn2 O8 168.54(10) . . ? N6 Mn2 O8 88.54(13) . . ? N5 Mn2 O8 91.46(12) . . ? N4 Mn2 O8 77.66(10) . . ? C1 O1 Mn1 123.98(19) . . ? C17 O2 Mn1 131.3(2) . . ? C21 O3 Mn1 118.8(2) . . ? C23 O6 Mn2 123.4(2) . . ? C39 O7 Mn2 131.0(2) . . ? C22 O8 Mn2 119.1(2) . . ? C7 N1 C8 117.3(3) . . ? C7 N1 Mn1 120.1(2) . . ? C8 N1 Mn1 122.5(3) . . ? C11 N2 C10 117.0(3) . . ? C11 N2 Mn1 124.0(2) . . ? C10 N2 Mn1 118.3(2) . . ? C18 N3 C20 106.3(3) . . ? C18 N3 Mn1 140.1(2) . . ? C20 N3 Mn1 113.1(2) . . ? C18 N4 C19 106.3(3) . . ? C18 N4 Mn2 138.9(2) . . ? C19 N4 Mn2 113.7(2) . . ? C29 N5 C30 117.2(4) . . ? C29 N5 Mn2 119.3(3) . . ? C30 N5 Mn2 123.0(4) . . ? C33 N6 C32 117.4(3) . . ? C33 N6 Mn2 125.0(3) . . ? C32 N6 Mn2 117.3(3) . . ? O1 C1 C6 121.2(3) . . ? O1 C1 C2 118.6(3) . . ? C6 C1 C2 120.1(3) . . ? C3 C2 C1 116.5(3) . . ? C3 C2 C40 122.4(3) . . ? C1 C2 C40 121.1(3) . . ? C2 C3 C4 125.2(3) . . ? C5 C4 C3 116.8(3) . . ? C5 C4 C44 122.7(3) . . ? C3 C4 C44 120.5(3) . . ? C4 C5 C6 121.0(3) . . ? C1 C6 C5 120.3(3) . . ? C1 C6 C7 122.2(3) . . ? C5 C6 C7 116.8(3) . . ? N1 C7 C6 125.7(3) . . ? C9 C8 N1 116.2(4) . . ? C8 C9 C10 115.5(4) . . ? N2 C10 C9 106.3(3) . . ? N2 C11 C12 127.5(3) . . ? C13 C12 C17 120.7(3) . . ? C13 C12 C11 116.2(3) . . ? C17 C12 C11 122.3(3) . . ? C14 C13 C12 121.3(3) . . ? C13 C14 C15 117.5(3) . . ? C13 C14 C48 122.8(3) . . ? C15 C14 C48 119.6(3) . . ? C16 C15 C14 124.3(3) . . ? C15 C16 C17 117.6(3) . . ? C15 C16 C52 121.2(3) . . ? C17 C16 C52 121.2(3) . . ? O2 C17 C12 120.7(3) . . ? O2 C17 C16 120.5(3) . . ? C12 C17 C16 118.7(3) . . ? N4 C18 N3 112.2(3) . . ? C20 C19 N4 108.3(3) . . ? C20 C19 C22 135.7(3) . . ? N4 C19 C22 116.0(3) . . ? C19 C20 N3 106.9(3) . . ? C19 C20 C21 137.5(3) . . ? N3 C20 C21 115.6(3) . . ? O4 C21 O3 122.8(3) . . ? O4 C21 C20 124.7(3) . . ? O3 C21 C20 112.5(3) . . ? O5 C22 O8 124.8(3) . . ? O5 C22 C19 122.1(3) . . ? O8 C22 C19 113.1(3) . . ? O6 C23 C28 120.3(3) . . ? O6 C23 C24 119.3(3) . . ? C28 C23 C24 120.3(3) . . ? C25 C24 C23 117.6(4) . . ? C25 C24 C56 120.0(4) . . ? C23 C24 C56 122.4(3) . . ? C26 C25 C24 127.1(7) . . ? C25 C26 C27 114.3(7) . . ? C25 C26 C60 127.6(14) . . ? C27 C26 C60 118.1(12) . . ? C28 C27 C26 120.9(6) . . ? C27 C28 C23 118.8(4) . . ? C27 C28 C29 119.1(4) . . ? C23 C28 C29 122.1(4) . . ? N5 C29 C28 127.0(5) . . ? N5 C30 C31 114.2(5) . . ? C32 C31 C30 128.1(6) . . ? C31 C32 N6 110.6(5) . . ? N6 C33 C34 128.6(4) . . ? C39 C34 C35 120.7(4) . . ? C39 C34 C33 121.4(3) . . ? C35 C34 C33 117.3(3) . . ? C36 C35 C34 122.3(4) . . ? C35 C36 C37 115.8(4) . . ? C35 C36 C64 122.6(4) . . ? C37 C36 C64 121.6(4) . . ? C38 C37 C36 125.4(4) . . ? C37 C38 C39 117.8(4) . . ? C37 C38 C68 122.0(4) . . ? C39 C38 C68 120.2(4) . . ? O7 C39 C34 120.9(3) . . ? O7 C39 C38 121.0(3) . . ? C34 C39 C38 118.0(4) . . ? C42 C40 C41 109.8(3) . . ? C42 C40 C43 107.1(4) . . ? C41 C40 C43 107.8(3) . . ? C42 C40 C2 109.8(3) . . ? C41 C40 C2 111.4(3) . . ? C43 C40 C2 110.7(3) . . ? C45 C44 C4 111.2(4) . . ? C45 C44 C46 109.1(4) . . ? C4 C44 C46 109.1(4) . . ? C45 C44 C47 109.0(4) . . ? C4 C44 C47 110.8(3) . . ? C46 C44 C47 107.5(4) . . ? C49 C48 C51 111.5(4) . . ? C49 C48 C14 110.1(3) . . ? C51 C48 C14 108.5(3) . . ? C49 C48 C50 107.3(3) . . ? C51 C48 C50 108.2(4) . . ? C14 C48 C50 111.3(3) . . ? C16 C52 C55 110.3(4) . . ? C16 C52 C54 112.6(3) . . ? C55 C52 C54 108.8(4) . . ? C16 C52 C53 109.6(4) . . ? C55 C52 C53 108.6(4) . . ? C54 C52 C53 106.8(4) . . ? C57 C56 C24 108.5(3) . . ? C57 C56 C59 106.6(4) . . ? C24 C56 C59 112.4(4) . . ? C57 C56 C58 108.6(4) . . ? C24 C56 C58 113.1(3) . . ? C59 C56 C58 107.5(4) . . ? C62 C60 C26 109.0(8) . . ? C62 C60 C63 104.2(6) . . ? C26 C60 C63 107.9(5) . . ? C62 C60 C61 109.8(6) . . ? C26 C60 C61 112.1(8) . . ? C63 C60 C61 113.5(7) . . ? C66 C64 C65 115.4(10) . . ? C66 C64 C36 107.5(7) . . ? C65 C64 C36 104.4(6) . . ? C66 C64 C67A 138.4(8) . . ? C65 C64 C67A 55.4(9) . . ? C36 C64 C67A 114.1(6) . . ? C66 C64 C66A 52.7(7) . . ? C65 C64 C66A 145.2(7) . . ? C36 C64 C66A 110.3(5) . . ? C67A C64 C66A 108.8(9) . . ? C66 C64 C65A 56.0(7) . . ? C65 C64 C65A 60.0(8) . . ? C36 C64 C65A 114.1(4) . . ? C67A C64 C65A 105.6(8) . . ? C66A C64 C65A 103.4(6) . . ? C66 C64 C67 112.0(9) . . ? C65 C64 C67 109.0(11) . . ? C36 C64 C67 107.9(6) . . ? C67A C64 C67 53.9(8) . . ? C66A C64 C67 61.1(8) . . ? C65A C64 C67 138.0(7) . . ? C69 C68 C70 108.4(4) . . ? C69 C68 C38 113.1(4) . . ? C70 C68 C38 110.5(4) . . ? C69 C68 C71 108.1(4) . . ? C70 C68 C71 108.4(4) . . ? C38 C68 C71 108.3(4) . . ? N9 C72 C73 172.1(13) . . ? N7 C74 C75 176.1(10) . . ? N8 C76 C77 178.5(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.638 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.080