Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'George Christou' _publ_contact_author_address ; Department of Chemistry University of Florida Gainesville FL 32611-7200 UNITED STATES OF AMERICA ; _publ_contact_author_email CHRISTOU@CHEM.UFL.EDU _publ_section_title ; New Mn12 single-molecule magnets from edge-sharing bioctahedra ; loop_ _publ_author_name 'George Christou' 'Khalil Abboud' 'Euan Brechin' 'Muralee Murugesu' 'Wolfgang Wernsdorfer' data_xm49 _database_code_depnum_ccdc_archive 'CCDC 290612' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C176 H178 Mn12 N6 O42' _chemical_formula_weight 3708.52 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 28.4275(19) _cell_length_b 20.2935(14) _cell_length_c 29.446(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16987(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 277 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description prisms _exptl_crystal_colour brown _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7648 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7415 _exptl_absorpt_correction_T_max 0.8866 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 104881 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19342 _reflns_number_gt 13619 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit consists of a half Mn12 cluster and three acetonitrile molecules of crystallization. One of the acetonitrile molecules is disordered against one of the phenyl groups and refines to 0.833(5) occupancy, but used as a whole molecule in calculating the formula weight, diffraction density and absorption coefficient. ; _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^)+(0.0379P)^2^+47.2910P] 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 19342 _refine_ls_number_parameters 1152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _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 0.45847(2) 0.53955(3) 0.49925(2) 0.02216(14) Uani 1 1 d . . . Mn2 Mn 0.48799(2) 0.48171(3) 0.59234(2) 0.02278(14) Uani 1 1 d . . . Mn3 Mn 0.40807(2) 0.44625(3) 0.42924(2) 0.02603(15) Uani 1 1 d . . . Mn4 Mn 0.46387(2) 0.41601(3) 0.33584(2) 0.02830(16) Uani 1 1 d . . . Mn5 Mn 0.43368(2) 0.36353(3) 0.54586(2) 0.02515(15) Uani 1 1 d . . . Mn6 Mn 0.50550(2) 0.35256(3) 0.42944(2) 0.02804(16) Uani 1 1 d . . . O1 O 0.42480(11) 0.35158(15) 0.61833(11) 0.0316(7) Uani 1 1 d . . . O2 O 0.46341(11) 0.43257(15) 0.65340(11) 0.0312(7) Uani 1 1 d . . . O3 O 0.49779(12) 0.32828(17) 0.31608(12) 0.0397(8) Uani 1 1 d . . . O4 O 0.52361(12) 0.27962(16) 0.38093(12) 0.0386(8) Uani 1 1 d . . . O5 O 0.35324(12) 0.34335(19) 0.54430(12) 0.0452(9) Uani 1 1 d . . . O6 O 0.51671(9) 0.53615(13) 0.53247(9) 0.0206(6) Uani 1 1 d . . . O7 O 0.49722(13) 0.48307(18) 0.28689(12) 0.0389(8) Uani 1 1 d . . . H7 H 0.511(2) 0.515(3) 0.302(2) 0.06(2) Uiso 1 1 d . . . O8 O 0.38649(10) 0.38941(15) 0.48590(10) 0.0291(7) Uani 1 1 d . . . O9 O 0.44069(10) 0.36615(14) 0.39724(10) 0.0276(7) Uani 1 1 d . . . O10 O 0.47155(10) 0.56515(14) 0.61878(10) 0.0253(6) Uani 1 1 d . . . O11 O 0.43746(10) 0.61442(14) 0.53333(10) 0.0250(6) Uani 1 1 d . . . O12 O 0.43036(9) 0.47455(13) 0.55833(10) 0.0230(6) Uani 1 1 d . . . O13 O 0.33443(13) 0.64346(18) 0.63413(15) 0.0522(11) Uani 1 1 d . . . H13 H 0.3060 0.6532 0.6378 0.078 Uiso 1 1 calc R . . O14 O 0.39273(11) 0.42624(16) 0.31528(11) 0.0350(8) Uani 1 1 d . . . O15 O 0.35281(11) 0.44290(16) 0.38044(11) 0.0333(7) Uani 1 1 d . . . O16 O 0.45151(10) 0.50823(14) 0.37937(10) 0.0253(6) Uani 1 1 d . . . O17 O 0.49391(10) 0.59668(13) 0.44079(10) 0.0227(6) Uani 1 1 d . . . O18 O 0.40218(10) 0.53598(14) 0.46339(10) 0.0245(6) Uani 1 1 d . . . O19 O 0.47538(11) 0.30638(15) 0.48610(11) 0.0334(7) Uani 1 1 d . . . O20 O 0.44731(13) 0.25579(16) 0.54537(13) 0.0442(9) Uani 1 1 d . . . O22' O 0.3504(2) 0.6607(3) 0.3569(2) 0.040(2) Uani 0.543(7) 1 d P A 11 H22D H 0.3404 0.6938 0.3428 0.059 Uiso 0.543(7) 1 calc PR A 11 O22 O 0.4180(3) 0.7035(4) 0.3473(3) 0.048(3) Uani 0.457(7) 1 d P A 12 H22C H 0.4041 0.7369 0.3371 0.071 Uiso 0.457(7) 1 calc PR A 12 C1 C 0.43729(16) 0.3813(2) 0.65310(16) 0.0300(10) Uani 1 1 d . . . C2 C 0.41896(17) 0.3572(3) 0.69900(17) 0.0377(11) Uani 1 1 d . . . H2A H 0.4389 0.3779 0.7230 0.045 Uiso 1 1 calc R . . C3 C 0.4246(2) 0.2825(3) 0.70321(18) 0.0437(13) Uani 1 1 d . . . C4 C 0.3912(2) 0.2426(3) 0.7231(2) 0.0642(18) Uani 1 1 d . . . H4A H 0.3628 0.2613 0.7341 0.077 Uiso 1 1 calc R . . C5 C 0.3988(3) 0.1750(4) 0.7270(3) 0.085(3) Uani 1 1 d . . . H5A H 0.3755 0.1478 0.7405 0.102 Uiso 1 1 calc R . . C6 C 0.4389(4) 0.1481(4) 0.7119(3) 0.096(3) Uani 1 1 d . . . H6A H 0.4435 0.1019 0.7146 0.116 Uiso 1 1 calc R . . C7 C 0.4733(3) 0.1863(4) 0.6927(3) 0.091(3) Uani 1 1 d . . . H7A H 0.5019 0.1670 0.6825 0.109 Uiso 1 1 calc R . . C8 C 0.4657(3) 0.2536(3) 0.6884(2) 0.0660(19) Uani 1 1 d . . . H8A H 0.4893 0.2803 0.6749 0.079 Uiso 1 1 calc R . . C9 C 0.36915(18) 0.3842(3) 0.70468(18) 0.0416(12) Uani 1 1 d . . . C10 C 0.3590(2) 0.4264(3) 0.7399(2) 0.0590(17) Uani 1 1 d . . . H10A H 0.3829 0.4375 0.7611 0.071 Uiso 1 1 calc R . . C11 C 0.3144(3) 0.4530(4) 0.7450(3) 0.078(2) Uani 1 1 d . . . H11A H 0.3077 0.4808 0.7701 0.094 Uiso 1 1 calc R . . C12 C 0.2800(3) 0.4391(4) 0.7139(3) 0.081(2) Uani 1 1 d . . . H12A H 0.2497 0.4582 0.7169 0.097 Uiso 1 1 calc R . . C13 C 0.2896(2) 0.3974(4) 0.6784(2) 0.071(2) Uani 1 1 d . . . H13A H 0.2657 0.3873 0.6568 0.085 Uiso 1 1 calc R . . C14 C 0.3338(2) 0.3699(3) 0.6739(2) 0.0557(16) Uani 1 1 d . . . H14A H 0.3401 0.3408 0.6493 0.067 Uiso 1 1 calc R . . C15 C 0.35014(17) 0.3676(2) 0.50603(17) 0.0335(11) Uani 1 1 d . . . C16 C 0.30277(17) 0.3761(3) 0.48200(18) 0.0421(13) Uani 1 1 d . . . H16A H 0.3099 0.3908 0.4503 0.051 Uiso 1 1 calc R . . C17 C 0.27659(19) 0.4317(3) 0.5045(2) 0.0472(14) Uani 1 1 d . . . C18 C 0.2609(2) 0.4284(4) 0.5478(3) 0.073(2) Uani 1 1 d . . . H18A H 0.2656 0.3892 0.5649 0.087 Uiso 1 1 calc R . . C19 C 0.2380(3) 0.4821(5) 0.5679(3) 0.103(3) Uani 1 1 d . . . H19A H 0.2272 0.4791 0.5984 0.123 Uiso 1 1 calc R . . C20 C 0.2312(4) 0.5372(5) 0.5443(4) 0.117(5) Uani 1 1 d . . . H20A H 0.2152 0.5734 0.5576 0.141 Uiso 1 1 calc R . . C21 C 0.2479(4) 0.5412(5) 0.5002(5) 0.129(5) Uani 1 1 d . . . H21A H 0.2432 0.5806 0.4834 0.155 Uiso 1 1 calc R . . C22 C 0.2711(3) 0.4897(3) 0.4803(3) 0.083(2) Uani 1 1 d . . . H22A H 0.2831 0.4937 0.4503 0.100 Uiso 1 1 calc R . . C23 C 0.27367(18) 0.3142(3) 0.4781(2) 0.0484(14) Uani 1 1 d . . . C24 C 0.2643(3) 0.2735(3) 0.5151(3) 0.084(2) Uani 1 1 d . . . H24A H 0.2778 0.2828 0.5440 0.101 Uiso 1 1 calc R . . C25 C 0.2346(3) 0.2185(4) 0.5094(5) 0.132(5) Uani 1 1 d . . . H25A H 0.2276 0.1906 0.5344 0.158 Uiso 1 1 calc R . . C26 C 0.2161(4) 0.2055(5) 0.4671(6) 0.140(6) Uani 1 1 d . . . H26A H 0.1975 0.1671 0.4627 0.168 Uiso 1 1 calc R . . C27 C 0.2235(3) 0.2453(6) 0.4330(4) 0.115(4) Uani 1 1 d . . . H27A H 0.2095 0.2365 0.4043 0.138 Uiso 1 1 calc R . . C28 C 0.2518(2) 0.3002(4) 0.4385(3) 0.083(2) Uani 1 1 d . . . H28A H 0.2561 0.3292 0.4135 0.099 Uiso 1 1 calc R . . C29 C 0.51370(17) 0.2801(3) 0.33859(18) 0.0373(12) Uani 1 1 d . . . C30 C 0.52123(19) 0.2162(3) 0.31231(19) 0.0420(12) Uani 1 1 d . B . H30A H 0.5072 0.2231 0.2816 0.050 Uiso 1 1 calc R . . C31 C 0.5727(2) 0.2000(3) 0.3048(2) 0.0500(15) Uani 1 1 d . . . C32 C 0.6068(7) 0.2157(10) 0.3351(8) 0.068(6) Uani 0.76(2) 1 d P B 1 H32A H 0.5983 0.2418 0.3606 0.082 Uiso 0.76(2) 1 calc PR B 1 C32' C 0.611(3) 0.204(3) 0.338(2) 0.052(15) Uiso 0.24(2) 1 d P B 2 H32B H 0.6093 0.2108 0.3695 0.062 Uiso 0.24(2) 1 calc PR B 2 C33 C 0.6551(4) 0.1952(6) 0.3308(6) 0.066(3) Uani 0.76(2) 1 d P B 1 H33A H 0.6768 0.1994 0.3552 0.079 Uiso 0.76(2) 1 calc PR B 1 C33' C 0.6502(19) 0.197(3) 0.3110(16) 0.070(15) Uiso 0.24(2) 1 d P B 2 H33B H 0.6748 0.2288 0.3127 0.083 Uiso 0.24(2) 1 calc PR B 2 C34 C 0.6680(5) 0.1694(8) 0.2898(6) 0.095(5) Uani 0.76(2) 1 d P B 1 H34A H 0.6998 0.1573 0.2846 0.114 Uiso 0.76(2) 1 calc PR B 1 C34' C 0.6541(18) 0.144(2) 0.2816(18) 0.075(14) Uiso 0.24(2) 1 d P B 2 H34B H 0.6846 0.1264 0.2763 0.091 Uiso 0.24(2) 1 calc PR B 2 C35 C 0.6351(5) 0.1608(10) 0.2561(5) 0.114(7) Uani 0.76(2) 1 d P B 1 H35A H 0.6439 0.1430 0.2275 0.137 Uiso 0.76(2) 1 calc PR B 1 C35' C 0.6171(12) 0.1156(19) 0.2600(12) 0.066(10) Uiso 0.24(2) 1 d P B 2 H35B H 0.6213 0.0787 0.2405 0.079 Uiso 0.24(2) 1 calc PR B 2 C36 C 0.5892(4) 0.1785(7) 0.2645(4) 0.080(4) Uani 0.76(2) 1 d P B 1 H36A H 0.5674 0.1753 0.2400 0.096 Uiso 0.76(2) 1 calc PR B 1 C36' C 0.5737(10) 0.1423(15) 0.2674(9) 0.040(7) Uiso 0.24(2) 1 d P B 2 H36B H 0.5464 0.1280 0.2518 0.048 Uiso 0.24(2) 1 calc PR B 2 C37 C 0.4936(2) 0.1600(3) 0.3343(2) 0.0489(14) Uani 1 1 d . . . C38 C 0.4453(2) 0.1558(4) 0.3278(2) 0.0669(19) Uani 1 1 d . B . H38A H 0.4300 0.1875 0.3092 0.080 Uiso 1 1 calc R . . C39 C 0.4192(3) 0.1067(5) 0.3477(3) 0.091(3) Uani 1 1 d . . . H39A H 0.3863 0.1045 0.3424 0.109 Uiso 1 1 calc R B . C40 C 0.4402(3) 0.0610(5) 0.3751(3) 0.100(3) Uani 1 1 d . B . H40A H 0.4220 0.0269 0.3884 0.120 Uiso 1 1 calc R . . C41 C 0.4882(3) 0.0645(4) 0.3833(3) 0.094(3) Uani 1 1 d . . . H41A H 0.5029 0.0338 0.4031 0.112 Uiso 1 1 calc R B . C42 C 0.5145(3) 0.1138(3) 0.3622(3) 0.072(2) Uani 1 1 d . B . H42A H 0.5475 0.1156 0.3671 0.086 Uiso 1 1 calc R . . C43 C 0.35548(16) 0.4348(2) 0.33775(16) 0.0290(10) Uani 1 1 d . C . C44 C 0.30918(17) 0.4343(2) 0.30994(18) 0.0370(12) Uani 1 1 d . . . C45 C 0.3159(10) 0.4521(14) 0.2654(7) 0.068(6) Uiso 0.167(5) 1 d PG C 12 C46 C 0.2887(9) 0.4163(13) 0.2348(10) 0.068(6) Uiso 0.167(5) 1 d PG C 12 H46A H 0.2659 0.3860 0.2457 0.082 Uiso 0.167(5) 1 calc PR C 12 C47 C 0.2949(10) 0.4250(15) 0.1884(9) 0.068(6) Uiso 0.167(5) 1 d PG C 12 H47A H 0.2763 0.4006 0.1675 0.082 Uiso 0.167(5) 1 calc PR C 12 C48 C 0.3283(12) 0.4693(18) 0.1725(7) 0.068(6) Uiso 0.167(5) 1 d PG C 12 H48A H 0.3325 0.4752 0.1407 0.082 Uiso 0.167(5) 1 calc PR C 12 C49 C 0.3555(10) 0.5051(15) 0.2030(10) 0.068(6) Uiso 0.167(5) 1 d PG C 12 H49A H 0.3783 0.5354 0.1921 0.082 Uiso 0.167(5) 1 calc PR C 12 C50 C 0.3493(9) 0.4964(13) 0.2494(9) 0.068(6) Uiso 0.167(5) 1 d PG C 12 H50A H 0.3679 0.5208 0.2703 0.082 Uiso 0.167(5) 1 calc PR C 12 C45' C 0.2960(2) 0.3628(3) 0.2985(2) 0.0395(15) Uani 0.833(5) 1 d P C 11 C46' C 0.3033(2) 0.3121(4) 0.3289(3) 0.0533(19) Uani 0.833(5) 1 d P C 11 H46B H 0.3167 0.3216 0.3576 0.064 Uiso 0.833(5) 1 calc PR C 11 C47' C 0.2915(3) 0.2476(4) 0.3186(3) 0.064(2) Uani 0.833(5) 1 d P C 11 H47B H 0.2980 0.2136 0.3399 0.076 Uiso 0.833(5) 1 calc PR C 11 C48' C 0.2714(3) 0.2328(4) 0.2797(4) 0.075(3) Uani 0.833(5) 1 d P C 11 H48B H 0.2620 0.1888 0.2737 0.090 Uiso 0.833(5) 1 calc PR C 11 C49' C 0.2641(3) 0.2808(5) 0.2477(3) 0.082(3) Uani 0.833(5) 1 d P C 11 H49B H 0.2508 0.2693 0.2191 0.098 Uiso 0.833(5) 1 calc PR C 11 C50' C 0.2759(3) 0.3474(4) 0.2565(3) 0.061(2) Uani 0.833(5) 1 d P C 11 H50B H 0.2704 0.3808 0.2345 0.074 Uiso 0.833(5) 1 calc PR C 11 C51 C 0.27073(18) 0.4727(3) 0.33413(18) 0.0402(12) Uani 1 1 d . C . C52 C 0.2769(2) 0.5389(3) 0.3416(2) 0.0597(17) Uani 1 1 d . . . H52A H 0.3048 0.5598 0.3313 0.072 Uiso 1 1 calc R C . C53 C 0.2429(3) 0.5761(4) 0.3639(3) 0.084(3) Uani 1 1 d . C . H53A H 0.2476 0.6218 0.3691 0.100 Uiso 1 1 calc R . . C54 C 0.2021(3) 0.5457(5) 0.3783(3) 0.091(3) Uani 1 1 d . . . H54A H 0.1787 0.5706 0.3938 0.109 Uiso 1 1 calc R C . C55 C 0.1950(3) 0.4802(5) 0.3706(3) 0.082(2) Uani 1 1 d . C . H55A H 0.1667 0.4597 0.3802 0.098 Uiso 1 1 calc R . . C56 C 0.2294(2) 0.4438(3) 0.3488(2) 0.0583(16) Uani 1 1 d . . . H56A H 0.2244 0.3981 0.3438 0.070 Uiso 1 1 calc R C . C57 C 0.46753(16) 0.2536(2) 0.50833(18) 0.0337(11) Uani 1 1 d . E . C58 C 0.48535(18) 0.1883(2) 0.4882(2) 0.0407(12) Uani 1 1 d . . . H58A H 0.4849 0.1971 0.4548 0.049 Uiso 1 1 calc R D 3 C59 C 0.4492(2) 0.1342(3) 0.4934(2) 0.0562(16) Uani 1 1 d . E . C60 C 0.4015(2) 0.1498(3) 0.4818(2) 0.0647(18) Uani 1 1 d . . . H60A H 0.3935 0.1935 0.4734 0.078 Uiso 1 1 calc R E . C61 C 0.3671(3) 0.1017(4) 0.4827(3) 0.083(2) Uani 1 1 d . E . H61A H 0.3353 0.1124 0.4761 0.100 Uiso 1 1 calc R . . C62 C 0.3801(3) 0.0365(4) 0.4938(3) 0.093(3) Uani 1 1 d . . . H62A H 0.3568 0.0029 0.4942 0.112 Uiso 1 1 calc R E . C63 C 0.4235(3) 0.0218(3) 0.5033(3) 0.080(2) Uani 1 1 d . E . H63A H 0.4319 -0.0220 0.5113 0.096 Uiso 1 1 calc R . . C64 C 0.4576(3) 0.0713(3) 0.5017(3) 0.074(2) Uani 1 1 d . . . H64A H 0.4894 0.0587 0.5069 0.089 Uiso 1 1 calc R E . C65 C 0.5375(5) 0.1779(8) 0.4979(7) 0.013(5) Uiso 0.24(3) 1 d PG E 3 C66 C 0.5526(7) 0.1727(14) 0.5427(6) 0.061(12) Uiso 0.24(3) 1 d PG E 3 H66A H 0.5305 0.1755 0.5668 0.074 Uiso 0.24(3) 1 calc PR E 3 C67 C 0.6000(8) 0.1633(17) 0.5522(8) 0.065(12) Uiso 0.24(3) 1 d PG E 3 H67A H 0.6103 0.1598 0.5828 0.078 Uiso 0.24(3) 1 calc PR E 3 C68 C 0.6324(6) 0.1592(16) 0.5169(10) 0.080(17) Uiso 0.24(3) 1 d PG E 3 H68A H 0.6648 0.1528 0.5234 0.096 Uiso 0.24(3) 1 calc PR E 3 C69 C 0.6173(6) 0.1644(15) 0.4722(9) 0.075(13) Uiso 0.24(3) 1 d PG E 3 H69A H 0.6395 0.1616 0.4481 0.090 Uiso 0.24(3) 1 calc PR E 3 C70 C 0.5699(7) 0.1738(12) 0.4626(7) 0.049(10) Uiso 0.24(3) 1 d PG E 3 H70A H 0.5596 0.1773 0.4320 0.059 Uiso 0.24(3) 1 calc PR E 3 C65' C 0.5323(3) 0.1733(5) 0.5110(4) 0.046(3) Uiso 0.76(3) 1 d P E 4 C66' C 0.5369(6) 0.1605(5) 0.5549(5) 0.071(3) Uani 0.76(3) 1 d P E 4 H66B H 0.5097 0.1604 0.5736 0.085 Uiso 0.76(3) 1 calc PR E 4 C67' C 0.5803(6) 0.1473(5) 0.5741(7) 0.102(7) Uani 0.76(3) 1 d P E 4 H67B H 0.5827 0.1369 0.6054 0.123 Uiso 0.76(3) 1 calc PR E 4 C68' C 0.6204(6) 0.1496(6) 0.5467(9) 0.115(10) Uani 0.76(3) 1 d P E 4 H68B H 0.6504 0.1415 0.5597 0.138 Uiso 0.76(3) 1 calc PR E 4 C69' C 0.6169(5) 0.1628(7) 0.5029(10) 0.115(8) Uani 0.76(3) 1 d P E 4 H69B H 0.6443 0.1639 0.4846 0.139 Uiso 0.76(3) 1 calc PR E 4 C70' C 0.5719(3) 0.1756(5) 0.4830(7) 0.070(3) Uani 0.76(3) 1 d P E 4 H70B H 0.5690 0.1854 0.4516 0.084 Uiso 0.76(3) 1 calc PR E 4 C71 C 0.38527(15) 0.5917(2) 0.43899(16) 0.0294(10) Uani 1 1 d . F . H71A H 0.3796 0.6279 0.4608 0.035 Uiso 1 1 calc R . . H71B H 0.3546 0.5800 0.4251 0.035 Uiso 1 1 calc R . . C72 C 0.46341(15) 0.6458(2) 0.42096(16) 0.0278(10) Uani 1 1 d . F . H72A H 0.4806 0.6688 0.3964 0.033 Uiso 1 1 calc R . . H72B H 0.4554 0.6788 0.4444 0.033 Uiso 1 1 calc R . . C73 C 0.42751(16) 0.5667(2) 0.36391(16) 0.0292(10) Uani 1 1 d . F . H73A H 0.3972 0.5536 0.3501 0.035 Uiso 1 1 calc R . . H73B H 0.4467 0.5879 0.3400 0.035 Uiso 1 1 calc R . . C74 C 0.41791(15) 0.6172(2) 0.40150(16) 0.0273(9) Uani 1 1 d . . . C75 C 0.39276(18) 0.6769(2) 0.37919(18) 0.0371(12) Uani 1 1 d . A . H75D H 0.3860 0.7101 0.4030 0.044 Uiso 0.543(7) 1 calc PR A 11 H75C H 0.4144 0.6974 0.3570 0.044 Uiso 0.457(7) 1 calc PR A 11 H75A H 0.3625 0.6620 0.3662 0.044 Uiso 0.543(7) 1 d PR A 12 H75B H 0.3857 0.7100 0.4029 0.044 Uiso 0.457(7) 1 d PR A 12 C76 C 0.39290(15) 0.6166(2) 0.55580(16) 0.0286(10) Uani 1 1 d . . . H76A H 0.3679 0.6083 0.5331 0.034 Uiso 1 1 calc R . . H76B H 0.3881 0.6616 0.5679 0.034 Uiso 1 1 calc R . . C77 C 0.38627(14) 0.4964(2) 0.57717(16) 0.0283(10) Uani 1 1 d . . . H77A H 0.3775 0.4667 0.6025 0.034 Uiso 1 1 calc R . . H77B H 0.3616 0.4927 0.5536 0.034 Uiso 1 1 calc R . . C78 C 0.42347(15) 0.5754(2) 0.63288(16) 0.0293(10) Uani 1 1 d . . . H78A H 0.4206 0.6204 0.6456 0.035 Uiso 1 1 calc R . . H78B H 0.4160 0.5438 0.6574 0.035 Uiso 1 1 calc R . . C79 C 0.38718(15) 0.5673(2) 0.59477(15) 0.0262(9) Uani 1 1 d . . . C80 C 0.33793(16) 0.5782(2) 0.61596(18) 0.0375(12) Uani 1 1 d . . . H80A H 0.3134 0.5716 0.5925 0.045 Uiso 1 1 calc R . . H80B H 0.3326 0.5456 0.6404 0.045 Uiso 1 1 calc R . . C81' C 0.5245(7) 0.4707(10) 0.2465(5) 0.110(9) Uani 0.568(19) 1 d P F 7 H81F H 0.5126 0.4982 0.2216 0.165 Uiso 0.568(19) 1 calc PR F 7 H81D H 0.5218 0.4241 0.2381 0.165 Uiso 0.568(19) 1 calc PR F 7 H81E H 0.5575 0.4814 0.2523 0.165 Uiso 0.568(19) 1 calc PR F 7 C81 C 0.4792(9) 0.5149(9) 0.2499(7) 0.089(9) Uani 0.432(19) 1 d P F 8 H81A H 0.4822 0.5626 0.2542 0.133 Uiso 0.432(19) 1 calc PR F 8 H81B H 0.4459 0.5033 0.2464 0.133 Uiso 0.432(19) 1 calc PR F 8 H81C H 0.4966 0.5016 0.2227 0.133 Uiso 0.432(19) 1 calc PR F 8 C82 C 0.41287(18) 0.3077(2) 0.39194(19) 0.0409(12) Uani 1 1 d . F . H82A H 0.3863 0.3090 0.4132 0.061 Uiso 1 1 calc R . . H82B H 0.4323 0.2689 0.3983 0.061 Uiso 1 1 calc R . . H82C H 0.4010 0.3053 0.3607 0.061 Uiso 1 1 calc R . . N1 N 0.3236(7) 0.4692(9) 0.1846(6) 0.196(8) Uani 0.833(5) 1 d P C 11 C83 C 0.3537(6) 0.4858(7) 0.1621(6) 0.131(5) Uani 0.833(5) 1 d P C 11 C84 C 0.3901(8) 0.4963(13) 0.1238(9) 0.309(16) Uani 0.833(5) 1 d P C 11 H84A H 0.4133 0.5292 0.1335 0.464 Uiso 0.833(5) 1 calc PR C 11 H84B H 0.3740 0.5118 0.0964 0.464 Uiso 0.833(5) 1 calc PR C 11 H84C H 0.4061 0.4545 0.1174 0.464 Uiso 0.833(5) 1 calc PR C 11 N2' N 0.3523(14) 0.792(3) 0.316(2) 0.09(2) Uani 0.19(4) 1 d P G 5 N2 N 0.3647(13) 0.8167(17) 0.3181(6) 0.226(13) Uani 0.81(4) 1 d P G 6 C85 C 0.3642(4) 0.8342(6) 0.2837(4) 0.115(4) Uani 1 1 d . . . C86 C 0.3597(13) 0.8599(9) 0.2410(6) 0.125(9) Uani 0.81(4) 1 d P G 6 H86A H 0.3343 0.8925 0.2407 0.187 Uiso 0.81(4) 1 calc PR G 6 H86B H 0.3524 0.8244 0.2195 0.187 Uiso 0.81(4) 1 calc PR G 6 H86C H 0.3893 0.8811 0.2321 0.187 Uiso 0.81(4) 1 calc PR G 6 C86' C 0.391(3) 0.870(4) 0.247(2) 0.11(2) Uani 0.19(4) 1 d P G 5 H86'A H 0.4164 0.8956 0.2610 0.164 Uiso 0.19(4) 1 calc PR G 5 H86'B H 0.3695 0.9001 0.2312 0.164 Uiso 0.19(4) 1 calc PR G 5 H86'C H 0.4039 0.8383 0.2257 0.164 Uiso 0.19(4) 1 calc PR G 5 N3 N 0.2324(3) 0.6856(4) 0.6263(3) 0.116(3) Uani 1 1 d . . . C87 C 0.1936(3) 0.6919(4) 0.6163(3) 0.077(2) Uani 1 1 d . . . C88 C 0.1451(3) 0.6976(4) 0.6044(3) 0.076(2) Uani 1 1 d . . . H88A H 0.1382 0.6681 0.5789 0.114 Uiso 1 1 calc R . . H88B H 0.1383 0.7432 0.5956 0.114 Uiso 1 1 calc R . . H88C H 0.1256 0.6854 0.6305 0.114 Uiso 1 1 calc R . . 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 0.0202(3) 0.0207(3) 0.0256(3) -0.0040(3) 0.0012(3) 0.0012(2) Mn2 0.0209(3) 0.0214(3) 0.0261(3) -0.0035(3) 0.0004(3) 0.0003(2) Mn3 0.0256(3) 0.0243(3) 0.0282(4) -0.0040(3) 0.0011(3) -0.0013(3) Mn4 0.0277(3) 0.0280(3) 0.0292(4) -0.0054(3) 0.0014(3) 0.0003(3) Mn5 0.0246(3) 0.0215(3) 0.0293(4) -0.0015(3) 0.0000(3) -0.0015(3) Mn6 0.0266(3) 0.0266(3) 0.0310(4) -0.0038(3) -0.0011(3) -0.0016(3) O1 0.0341(17) 0.0315(17) 0.0293(18) 0.0007(14) 0.0006(14) -0.0069(14) O2 0.0328(17) 0.0290(16) 0.0317(18) 0.0021(13) 0.0033(14) -0.0052(14) O3 0.043(2) 0.0353(18) 0.041(2) -0.0107(16) 0.0005(16) 0.0057(16) O4 0.0348(18) 0.0371(18) 0.044(2) -0.0116(16) -0.0015(16) 0.0026(15) O5 0.0338(19) 0.062(2) 0.040(2) 0.0156(19) -0.0049(16) -0.0155(17) O6 0.0204(14) 0.0185(14) 0.0230(15) -0.0055(11) 0.0008(12) 0.0001(11) O7 0.049(2) 0.041(2) 0.0266(19) -0.0007(16) 0.0026(16) -0.0054(18) O8 0.0267(15) 0.0298(16) 0.0308(18) 0.0007(14) 0.0017(13) -0.0041(13) O9 0.0286(16) 0.0228(15) 0.0312(17) -0.0044(13) -0.0028(13) -0.0040(13) O10 0.0203(14) 0.0262(15) 0.0295(17) -0.0064(13) 0.0042(12) 0.0008(12) O11 0.0255(15) 0.0210(14) 0.0285(17) -0.0052(12) 0.0025(13) 0.0042(12) O12 0.0208(14) 0.0236(14) 0.0245(16) -0.0046(12) 0.0035(12) -0.0001(12) O13 0.0351(19) 0.047(2) 0.075(3) -0.025(2) 0.016(2) 0.0058(17) O14 0.0328(17) 0.0379(18) 0.0342(19) -0.0070(15) -0.0015(15) -0.0009(14) O15 0.0290(16) 0.0350(17) 0.036(2) -0.0041(15) -0.0031(14) 0.0003(14) O16 0.0226(15) 0.0250(15) 0.0283(17) -0.0010(13) -0.0007(12) 0.0034(12) O17 0.0228(14) 0.0178(13) 0.0274(16) -0.0006(12) -0.0009(12) 0.0031(11) O18 0.0221(14) 0.0237(15) 0.0278(17) -0.0028(12) -0.0011(12) 0.0029(12) O19 0.0393(18) 0.0229(15) 0.0381(19) 0.0001(14) -0.0006(15) -0.0051(14) O20 0.058(2) 0.0259(17) 0.048(2) -0.0003(16) 0.0186(19) 0.0018(16) O22' 0.036(4) 0.032(3) 0.051(4) 0.009(3) -0.015(3) 0.004(3) O22 0.050(5) 0.045(5) 0.048(5) 0.023(4) 0.003(4) 0.016(4) C1 0.027(2) 0.028(2) 0.035(3) 0.003(2) 0.002(2) -0.0004(19) C2 0.039(3) 0.047(3) 0.027(3) 0.000(2) 0.000(2) -0.009(2) C3 0.049(3) 0.050(3) 0.032(3) 0.014(2) -0.008(2) -0.008(3) C4 0.061(4) 0.069(4) 0.062(4) 0.030(4) 0.000(3) -0.012(3) C5 0.104(7) 0.067(5) 0.085(6) 0.046(4) -0.007(5) -0.023(5) C6 0.122(8) 0.065(5) 0.102(7) 0.041(5) -0.014(6) 0.006(5) C7 0.112(7) 0.082(6) 0.078(6) 0.033(5) 0.011(5) 0.035(5) C8 0.074(4) 0.064(4) 0.060(4) 0.031(3) 0.007(4) 0.012(4) C9 0.040(3) 0.051(3) 0.033(3) 0.007(2) 0.012(2) -0.011(2) C10 0.060(4) 0.066(4) 0.050(4) -0.006(3) 0.013(3) -0.008(3) C11 0.072(5) 0.077(5) 0.086(6) -0.011(4) 0.034(4) 0.005(4) C12 0.053(4) 0.096(6) 0.093(6) 0.024(5) 0.027(4) 0.013(4) C13 0.044(3) 0.109(6) 0.059(4) 0.012(4) 0.009(3) 0.004(4) C14 0.042(3) 0.083(5) 0.041(3) 0.005(3) 0.007(3) -0.005(3) C15 0.035(2) 0.029(2) 0.036(3) -0.001(2) -0.004(2) -0.008(2) C16 0.031(3) 0.059(3) 0.036(3) 0.010(3) -0.006(2) -0.008(2) C17 0.039(3) 0.045(3) 0.058(4) -0.001(3) -0.020(3) -0.004(2) C18 0.070(5) 0.075(5) 0.073(5) -0.011(4) -0.004(4) 0.025(4) C19 0.079(6) 0.130(8) 0.099(7) -0.046(6) -0.026(5) 0.038(6) C20 0.106(7) 0.107(8) 0.139(9) -0.077(8) -0.065(7) 0.065(6) C21 0.110(8) 0.065(6) 0.212(14) -0.024(8) -0.069(9) 0.025(5) C22 0.079(5) 0.053(4) 0.116(7) 0.019(4) -0.020(5) 0.005(4) C23 0.033(3) 0.056(3) 0.056(4) -0.018(3) -0.009(3) -0.004(3) C24 0.077(5) 0.058(4) 0.117(7) 0.014(4) -0.030(5) -0.028(4) C25 0.086(6) 0.074(6) 0.235(14) 0.035(7) -0.056(8) -0.042(5) C26 0.075(6) 0.079(7) 0.266(18) -0.045(9) -0.078(9) -0.020(5) C27 0.077(6) 0.125(9) 0.142(10) -0.073(8) -0.034(7) -0.017(7) C28 0.059(4) 0.112(6) 0.077(5) -0.031(5) -0.017(4) -0.009(4) C29 0.028(2) 0.042(3) 0.042(3) -0.009(2) 0.003(2) -0.003(2) C30 0.047(3) 0.039(3) 0.040(3) -0.011(2) -0.002(2) 0.005(2) C31 0.057(4) 0.042(3) 0.051(4) -0.005(3) 0.015(3) 0.014(3) C32 0.039(7) 0.040(8) 0.126(13) -0.025(7) 0.019(6) 0.004(6) C33 0.040(5) 0.066(6) 0.091(11) 0.007(7) 0.007(6) 0.013(4) C34 0.064(8) 0.089(10) 0.132(14) 0.001(9) 0.048(9) 0.033(8) C35 0.098(11) 0.172(18) 0.072(9) -0.029(10) 0.034(8) 0.055(12) C36 0.081(8) 0.097(10) 0.063(6) -0.022(6) 0.015(6) 0.022(7) C37 0.054(3) 0.046(3) 0.047(3) -0.018(3) 0.000(3) -0.002(3) C38 0.058(4) 0.088(5) 0.055(4) -0.022(4) 0.000(3) -0.010(4) C39 0.070(5) 0.122(8) 0.080(6) -0.024(6) 0.010(5) -0.039(5) C40 0.096(7) 0.098(7) 0.106(8) -0.002(6) 0.012(6) -0.049(6) C41 0.105(7) 0.078(5) 0.098(7) 0.015(5) 0.003(5) -0.026(5) C42 0.073(5) 0.055(4) 0.087(5) 0.005(4) -0.002(4) -0.010(4) C43 0.032(2) 0.022(2) 0.033(3) -0.0039(19) -0.004(2) -0.0024(18) C44 0.031(2) 0.038(3) 0.043(3) -0.007(2) -0.008(2) 0.001(2) C45' 0.028(3) 0.048(4) 0.042(4) -0.007(3) -0.001(3) -0.001(3) C46' 0.048(4) 0.054(4) 0.058(5) -0.001(4) -0.009(4) -0.009(3) C47' 0.064(5) 0.046(4) 0.081(6) 0.003(4) -0.005(5) -0.007(4) C48' 0.073(6) 0.044(5) 0.108(8) -0.011(5) 0.008(6) -0.010(4) C49' 0.081(6) 0.091(7) 0.074(6) -0.044(6) -0.006(5) -0.023(5) C50' 0.058(5) 0.073(5) 0.053(5) -0.015(4) -0.008(4) -0.010(4) C51 0.036(3) 0.046(3) 0.039(3) -0.001(2) -0.015(2) 0.011(2) C52 0.054(4) 0.052(4) 0.073(5) -0.008(3) -0.024(3) 0.015(3) C53 0.086(6) 0.074(5) 0.091(6) -0.029(4) -0.038(5) 0.038(4) C54 0.079(6) 0.128(8) 0.065(5) -0.020(5) -0.007(4) 0.065(6) C55 0.055(4) 0.112(7) 0.078(5) 0.015(5) 0.014(4) 0.036(4) C56 0.048(3) 0.065(4) 0.061(4) 0.012(3) 0.004(3) 0.019(3) C57 0.030(2) 0.026(2) 0.044(3) -0.009(2) -0.002(2) 0.0005(19) C58 0.041(3) 0.025(2) 0.055(3) -0.008(2) 0.004(3) 0.006(2) C59 0.054(3) 0.032(3) 0.082(5) -0.015(3) 0.016(3) -0.005(3) C60 0.066(4) 0.046(3) 0.082(5) -0.002(3) -0.001(4) -0.009(3) C61 0.066(5) 0.074(5) 0.110(7) -0.021(5) 0.001(4) -0.015(4) C62 0.099(6) 0.053(4) 0.128(8) -0.017(5) 0.022(6) -0.027(4) C63 0.065(4) 0.025(3) 0.149(8) -0.006(4) 0.003(5) 0.000(3) C64 0.076(5) 0.038(3) 0.109(6) -0.003(4) 0.018(4) -0.003(3) C66' 0.085(8) 0.034(5) 0.093(8) -0.010(5) -0.030(8) 0.015(5) C67' 0.116(12) 0.041(5) 0.149(15) -0.008(7) -0.068(12) 0.005(7) C68' 0.070(9) 0.055(7) 0.22(3) -0.023(10) -0.065(14) 0.011(7) C69' 0.053(8) 0.056(7) 0.24(3) -0.013(11) 0.002(12) -0.002(5) C70' 0.052(6) 0.042(5) 0.115(12) -0.011(6) 0.007(6) 0.002(4) C71 0.025(2) 0.030(2) 0.034(3) -0.002(2) -0.0016(19) 0.0080(19) C72 0.030(2) 0.019(2) 0.034(3) -0.0026(18) 0.002(2) 0.0024(18) C73 0.027(2) 0.028(2) 0.033(3) -0.0006(19) -0.006(2) 0.0027(18) C74 0.025(2) 0.026(2) 0.031(2) -0.0014(19) -0.0052(19) 0.0025(18) C75 0.038(3) 0.029(2) 0.044(3) -0.003(2) -0.008(2) 0.009(2) C76 0.024(2) 0.026(2) 0.035(3) -0.0019(19) 0.0028(19) 0.0061(18) C77 0.020(2) 0.030(2) 0.035(3) -0.001(2) 0.0049(19) -0.0009(18) C78 0.027(2) 0.031(2) 0.030(3) -0.008(2) 0.0057(19) 0.0016(19) C79 0.025(2) 0.025(2) 0.029(2) -0.0074(19) 0.0011(19) 0.0024(17) C80 0.027(2) 0.041(3) 0.045(3) -0.007(2) 0.006(2) 0.001(2) C81' 0.131(18) 0.116(15) 0.082(11) -0.037(10) 0.033(11) -0.061(14) C81 0.12(2) 0.055(11) 0.091(15) 0.013(10) -0.032(13) -0.037(12) C82 0.037(3) 0.037(3) 0.049(3) -0.010(2) -0.004(2) -0.002(2) N1 0.200(17) 0.195(16) 0.193(16) 0.081(13) 0.077(13) 0.083(14) C83 0.133(13) 0.110(10) 0.150(15) 0.025(10) 0.009(11) -0.012(9) C84 0.21(2) 0.39(4) 0.32(3) 0.09(3) 0.02(2) -0.16(3) N2' 0.04(2) 0.09(3) 0.13(5) 0.08(3) -0.03(2) 0.00(2) N2 0.38(3) 0.22(2) 0.071(10) 0.024(12) 0.006(15) 0.21(2) C85 0.148(10) 0.123(9) 0.073(7) -0.001(6) -0.019(7) 0.060(7) C86 0.21(3) 0.089(9) 0.077(9) 0.018(7) -0.006(13) 0.001(13) C86' 0.12(5) 0.17(6) 0.04(3) 0.05(4) -0.01(3) -0.04(5) N3 0.086(5) 0.142(7) 0.118(7) -0.017(6) -0.015(5) 0.049(5) C87 0.077(5) 0.076(5) 0.078(5) -0.007(4) 0.001(4) 0.031(4) C88 0.081(5) 0.068(5) 0.078(5) 0.012(4) -0.003(4) 0.020(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 O11 1.916(3) . ? Mn1 O18 1.918(3) . ? Mn1 O6 1.924(3) . ? Mn1 O6 1.931(3) 5_666 ? Mn1 O17 2.307(3) . ? Mn1 O12 2.325(3) . ? Mn1 Mn1 2.8554(12) 5_666 ? Mn1 Mn2 3.0978(10) . ? Mn1 Mn2 3.1265(9) 5_666 ? Mn1 Mn3 3.1445(9) . ? Mn1 Mn6 3.2018(9) 5_666 ? Mn2 O10 1.922(3) . ? Mn2 O16 1.922(3) 5_666 ? Mn2 O12 1.926(3) . ? Mn2 O17 1.936(3) 5_666 ? Mn2 O2 2.172(3) . ? Mn2 O6 2.235(3) . ? Mn2 Mn1 3.1265(9) 5_666 ? Mn2 Mn5 3.1636(9) . ? Mn3 O18 2.087(3) . ? Mn3 O9 2.095(3) . ? Mn3 O8 2.119(3) . ? Mn3 O15 2.130(3) . ? Mn3 O16 2.294(3) . ? Mn3 O6 2.444(3) 5_666 ? Mn3 Mn4 3.2336(10) . ? Mn4 O3 2.107(3) . ? Mn4 O14 2.121(3) . ? Mn4 O9 2.174(3) . ? Mn4 O7 2.197(4) . ? Mn4 O16 2.295(3) . ? Mn4 O10 2.303(3) 5_666 ? Mn5 O1 2.163(3) . ? Mn5 O20 2.220(3) . ? Mn5 O17 2.246(3) 5_666 ? Mn5 O8 2.279(3) . ? Mn5 O12 2.285(3) . ? Mn5 O5 2.323(3) . ? Mn5 O19 2.418(3) . ? Mn6 O11 2.069(3) 5_666 ? Mn6 O9 2.090(3) . ? Mn6 O19 2.096(3) . ? Mn6 O4 2.120(3) . ? Mn6 O10 2.287(3) 5_666 ? Mn6 Mn1 3.2018(9) 5_666 ? O1 C1 1.240(5) . ? O2 C1 1.278(5) . ? O3 C29 1.266(6) . ? O4 C29 1.278(6) . ? O5 C15 1.233(6) . ? O6 Mn1 1.931(3) 5_666 ? O6 Mn3 2.444(3) 5_666 ? O7 C81 1.366(18) . ? O7 C81' 1.441(15) . ? O7 H7 0.87(6) . ? O8 C15 1.270(5) . ? O9 C82 1.434(5) . ? O10 C78 1.444(5) . ? O10 Mn6 2.287(3) 5_666 ? O10 Mn4 2.303(3) 5_666 ? O11 C76 1.430(5) . ? O11 Mn6 2.069(3) 5_666 ? O12 C77 1.441(5) . ? O13 C80 1.432(6) . ? O13 H13 0.8400 . ? O14 C43 1.261(5) . ? O15 C43 1.270(5) . ? O16 C73 1.442(5) . ? O16 Mn2 1.922(3) 5_666 ? O17 C72 1.444(5) . ? O17 Mn2 1.936(3) 5_666 ? O17 Mn5 2.246(3) 5_666 ? O18 C71 1.423(5) . ? O19 C57 1.276(6) . ? O20 C57 1.234(6) . ? O22' C75 1.409(7) . ? O22' H22D 0.8400 . ? O22' H75A 0.4381 . ? O22 C75 1.300(9) . ? O22 H22C 0.8400 . ? C1 C2 1.529(7) . ? C2 C9 1.528(7) . ? C2 C3 1.530(7) . ? C2 H2A 1.0000 . ? C3 C8 1.377(8) . ? C3 C4 1.379(8) . ? C4 C5 1.394(10) . ? C4 H4A 0.9500 . ? C5 C6 1.338(12) . ? C5 H5A 0.9500 . ? C6 C7 1.370(12) . ? C6 H6A 0.9500 . ? C7 C8 1.389(10) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C10 1.375(8) . ? C9 C14 1.384(8) . ? C10 C11 1.385(9) . ? C10 H10A 0.9500 . ? C11 C12 1.368(11) . ? C11 H11A 0.9500 . ? C12 C13 1.373(11) . ? C12 H12A 0.9500 . ? C13 C14 1.383(9) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.531(7) . ? C16 C17 1.505(8) . ? C16 C23 1.508(8) . ? C16 H16A 1.0000 . ? C17 C18 1.354(9) . ? C17 C22 1.385(9) . ? C18 C19 1.401(10) . ? C18 H18A 0.9500 . ? C19 C20 1.331(14) . ? C19 H19A 0.9500 . ? C20 C21 1.386(16) . ? C20 H20A 0.9500 . ? C21 C22 1.367(13) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C28 1.352(8) . ? C23 C24 1.394(10) . ? C24 C25 1.410(10) . ? C24 H24A 0.9500 . ? C25 C26 1.377(16) . ? C25 H25A 0.9500 . ? C26 C27 1.306(15) . ? C26 H26A 0.9500 . ? C27 C28 1.385(12) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.525(7) . ? C30 C31 1.516(8) . ? C30 C37 1.528(8) . ? C30 H30A 1.0000 . ? C31 C36 1.348(10) . ? C31 C32 1.36(2) . ? C31 C32' 1.46(7) . ? C31 C36' 1.61(3) . ? C32 C33 1.44(2) . ? C32 H32A 0.9500 . ? C32' C33' 1.37(9) . ? C32' H32B 0.9500 . ? C33 C34 1.37(2) . ? C33 H33A 0.9500 . ? C33' C34' 1.39(7) . ? C33' H33B 0.9500 . ? C34 C35 1.38(2) . ? C34 H34A 0.9500 . ? C34' C35' 1.36(6) . ? C34' H34B 0.9500 . ? C35 C36 1.376(15) . ? C35 H35A 0.9500 . ? C35' C36' 1.37(4) . ? C35' H35B 0.9500 . ? C36 H36A 0.9500 . ? C36' H36B 0.9500 . ? C37 C42 1.379(9) . ? C37 C38 1.390(8) . ? C38 C39 1.374(11) . ? C38 H38A 0.9500 . ? C39 C40 1.366(12) . ? C39 H39A 0.9500 . ? C40 C41 1.386(12) . ? C40 H40A 0.9500 . ? C41 C42 1.395(10) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C44 1.550(6) . ? C44 C45 1.37(2) . ? C44 C51 1.519(7) . ? C44 C45' 1.537(8) . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C46 H46A 0.9500 . ? C47 C48 1.3900 . ? C47 H47A 0.9500 . ? C48 C49 1.3900 . ? C48 H48A 0.9500 . ? C49 C50 1.3900 . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C45' C46' 1.378(9) . ? C45' C50' 1.397(9) . ? C46' C47' 1.384(10) . ? C46' H46B 0.9500 . ? C47' C48' 1.314(12) . ? C47' H47B 0.9500 . ? C48' C49' 1.372(13) . ? C48' H48B 0.9500 . ? C49' C50' 1.417(11) . ? C49' H49B 0.9500 . ? C50' H50B 0.9500 . ? C51 C52 1.373(8) . ? C51 C56 1.383(8) . ? C52 C53 1.391(9) . ? C52 H52A 0.9500 . ? C53 C54 1.381(12) . ? C53 H53A 0.9500 . ? C54 C55 1.362(12) . ? C54 H54A 0.9500 . ? C55 C56 1.381(9) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C58 1.537(6) . ? C58 C59 1.511(7) . ? C58 C65' 1.525(10) . ? C58 C65 1.525(15) . ? C58 H58A 1.0000 . ? C59 C64 1.321(8) . ? C59 C60 1.434(9) . ? C60 C61 1.382(9) . ? C60 H60A 0.9500 . ? C61 C62 1.413(11) . ? C61 H61A 0.9500 . ? C62 C63 1.300(11) . ? C62 H62A 0.9500 . ? C63 C64 1.397(9) . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C66 C67 1.3900 . ? C66 H66A 0.9500 . ? C67 C68 1.3900 . ? C67 H67A 0.9500 . ? C68 C69 1.3900 . ? C68 H68A 0.9500 . ? C69 C70 1.3900 . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? C65' C66' 1.323(14) . ? C65' C70' 1.396(13) . ? C66' C67' 1.382(15) . ? C66' H66B 0.9500 . ? C67' C68' 1.40(2) . ? C67' H67B 0.9500 . ? C68' C69' 1.32(2) . ? C68' H68B 0.9500 . ? C69' C70' 1.43(2) . ? C69' H69B 0.9500 . ? C70' H70B 0.9500 . ? C71 C74 1.532(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C74 1.529(6) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.533(6) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.553(6) . ? C75 H75D 0.9900 . ? C75 H75C 0.9900 . ? C75 H75A 0.9902 . ? C75 H75B 0.9899 . ? C76 C79 1.532(6) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C79 1.528(6) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.533(6) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.549(6) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81' H81F 0.9800 . ? C81' H81D 0.9800 . ? C81' H81E 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? N1 C83 1.133(18) . ? C83 C84 1.54(2) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? N2' C85 1.31(5) . ? N2 C85 1.08(2) . ? C85 C86 1.367(18) . ? C85 C86' 1.50(6) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C86' H86'A 0.9800 . ? C86' H86'B 0.9800 . ? C86' H86'C 0.9800 . ? N3 C87 1.149(9) . ? C87 C88 1.427(10) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? 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 O11 Mn1 O18 93.34(12) . . ? O11 Mn1 O6 91.74(12) . . ? O18 Mn1 O6 174.91(12) . . ? O11 Mn1 O6 176.16(12) . 5_666 ? O18 Mn1 O6 90.49(12) . 5_666 ? O6 Mn1 O6 84.43(12) . 5_666 ? O11 Mn1 O17 97.39(11) . . ? O18 Mn1 O17 88.43(11) . . ? O6 Mn1 O17 91.24(11) . . ? O6 Mn1 O17 83.07(11) 5_666 . ? O11 Mn1 O12 87.18(11) . . ? O18 Mn1 O12 95.95(11) . . ? O6 Mn1 O12 83.97(11) . . ? O6 Mn1 O12 92.07(11) 5_666 . ? O17 Mn1 O12 173.50(10) . . ? O11 Mn1 Mn1 134.05(10) . 5_666 ? O18 Mn1 Mn1 132.61(9) . 5_666 ? O6 Mn1 Mn1 42.31(8) . 5_666 ? O6 Mn1 Mn1 42.12(8) 5_666 5_666 ? O17 Mn1 Mn1 86.16(7) . 5_666 ? O12 Mn1 Mn1 87.34(7) . 5_666 ? O11 Mn1 Mn2 85.49(9) . . ? O18 Mn1 Mn2 134.31(9) . . ? O6 Mn1 Mn2 45.85(8) . . ? O6 Mn1 Mn2 91.57(9) 5_666 . ? O17 Mn1 Mn2 137.09(7) . . ? O12 Mn1 Mn2 38.37(7) . . ? Mn1 Mn1 Mn2 63.20(3) 5_666 . ? O11 Mn1 Mn2 135.47(9) . 5_666 ? O18 Mn1 Mn2 85.76(9) . 5_666 ? O6 Mn1 Mn2 90.85(8) . 5_666 ? O6 Mn1 Mn2 45.20(8) 5_666 5_666 ? O17 Mn1 Mn2 38.11(7) . 5_666 ? O12 Mn1 Mn2 137.26(7) . 5_666 ? Mn1 Mn1 Mn2 62.18(3) 5_666 5_666 ? Mn2 Mn1 Mn2 125.39(2) . 5_666 ? O11 Mn1 Mn3 132.74(9) . . ? O18 Mn1 Mn3 40.22(8) . . ? O6 Mn1 Mn3 134.73(8) . . ? O6 Mn1 Mn3 50.99(8) 5_666 . ? O17 Mn1 Mn3 90.71(7) . . ? O12 Mn1 Mn3 89.56(7) . . ? Mn1 Mn1 Mn3 92.77(3) 5_666 . ? Mn2 Mn1 Mn3 118.38(3) . . ? Mn2 Mn1 Mn3 64.74(2) 5_666 . ? O11 Mn1 Mn6 38.20(9) . 5_666 ? O18 Mn1 Mn6 130.81(9) . 5_666 ? O6 Mn1 Mn6 54.26(8) . 5_666 ? O6 Mn1 Mn6 138.09(8) 5_666 5_666 ? O17 Mn1 Mn6 90.35(7) . 5_666 ? O12 Mn1 Mn6 90.41(7) . 5_666 ? Mn1 Mn1 Mn6 96.30(3) 5_666 5_666 ? Mn2 Mn1 Mn6 65.93(2) . 5_666 ? Mn2 Mn1 Mn6 120.29(3) 5_666 5_666 ? Mn3 Mn1 Mn6 170.91(3) . 5_666 ? O10 Mn2 O16 87.04(12) . 5_666 ? O10 Mn2 O12 94.03(12) . . ? O16 Mn2 O12 174.16(13) 5_666 . ? O10 Mn2 O17 173.26(13) . 5_666 ? O16 Mn2 O17 93.90(12) 5_666 5_666 ? O12 Mn2 O17 84.38(12) . 5_666 ? O10 Mn2 O2 89.48(12) . . ? O16 Mn2 O2 88.73(12) 5_666 . ? O12 Mn2 O2 97.02(12) . . ? O17 Mn2 O2 97.21(12) 5_666 . ? O10 Mn2 O6 88.44(11) . . ? O16 Mn2 O6 87.86(11) 5_666 . ? O12 Mn2 O6 86.43(11) . . ? O17 Mn2 O6 84.93(11) 5_666 . ? O2 Mn2 O6 176.09(11) . . ? O10 Mn2 Mn1 87.63(9) . . ? O16 Mn2 Mn1 125.86(9) 5_666 . ? O12 Mn2 Mn1 48.54(9) . . ? O17 Mn2 Mn1 86.41(9) 5_666 . ? O2 Mn2 Mn1 145.04(9) . . ? O6 Mn2 Mn1 38.15(7) . . ? O10 Mn2 Mn1 126.12(9) . 5_666 ? O16 Mn2 Mn1 87.31(9) 5_666 5_666 ? O12 Mn2 Mn1 87.43(9) . 5_666 ? O17 Mn2 Mn1 47.35(8) 5_666 5_666 ? O2 Mn2 Mn1 143.85(9) . 5_666 ? O6 Mn2 Mn1 37.82(7) . 5_666 ? Mn1 Mn2 Mn1 54.61(2) . 5_666 ? O10 Mn2 Mn5 136.44(9) . . ? O16 Mn2 Mn5 134.82(9) 5_666 . ? O12 Mn2 Mn5 45.78(8) . . ? O17 Mn2 Mn5 44.66(8) 5_666 . ? O2 Mn2 Mn5 81.55(8) . . ? O6 Mn2 Mn5 102.22(7) . . ? Mn1 Mn2 Mn5 76.84(2) . . ? Mn1 Mn2 Mn5 76.10(2) 5_666 . ? O18 Mn3 O9 158.30(12) . . ? O18 Mn3 O8 94.14(12) . . ? O9 Mn3 O8 93.43(12) . . ? O18 Mn3 O15 107.09(12) . . ? O9 Mn3 O15 89.90(12) . . ? O8 Mn3 O15 107.47(12) . . ? O18 Mn3 O16 82.73(11) . . ? O9 Mn3 O16 84.22(11) . . ? O8 Mn3 O16 163.37(11) . . ? O15 Mn3 O16 89.01(12) . . ? O18 Mn3 O6 73.76(10) . 5_666 ? O9 Mn3 O6 86.19(10) . 5_666 ? O8 Mn3 O6 88.25(11) . 5_666 ? O15 Mn3 O6 164.01(12) . 5_666 ? O16 Mn3 O6 75.18(10) . 5_666 ? O18 Mn3 Mn1 36.41(8) . . ? O9 Mn3 Mn1 124.07(8) . . ? O8 Mn3 Mn1 86.76(9) . . ? O15 Mn3 Mn1 142.90(9) . . ? O16 Mn3 Mn1 81.04(8) . . ? O6 Mn3 Mn1 37.89(6) 5_666 . ? O18 Mn3 Mn4 127.94(9) . . ? O9 Mn3 Mn4 41.69(8) . . ? O8 Mn3 Mn4 135.10(9) . . ? O15 Mn3 Mn4 77.41(9) . . ? O16 Mn3 Mn4 45.22(7) . . ? O6 Mn3 Mn4 89.48(7) 5_666 . ? Mn1 Mn3 Mn4 116.64(3) . . ? O3 Mn4 O14 116.13(13) . . ? O3 Mn4 O9 88.58(13) . . ? O14 Mn4 O9 89.66(12) . . ? O3 Mn4 O7 98.32(14) . . ? O14 Mn4 O7 99.41(14) . . ? O9 Mn4 O7 164.68(13) . . ? O3 Mn4 O16 155.97(12) . . ? O14 Mn4 O16 86.19(11) . . ? O9 Mn4 O16 82.45(11) . . ? O7 Mn4 O16 85.83(12) . . ? O3 Mn4 O10 86.31(12) . 5_666 ? O14 Mn4 O10 155.43(12) . 5_666 ? O9 Mn4 O10 80.57(11) . 5_666 ? O7 Mn4 O10 86.21(13) . 5_666 ? O16 Mn4 O10 70.28(10) . 5_666 ? O3 Mn4 Mn3 128.30(10) . . ? O14 Mn4 Mn3 75.90(9) . . ? O9 Mn4 Mn3 39.86(8) . . ? O7 Mn4 Mn3 130.69(10) . . ? O16 Mn4 Mn3 45.19(7) . . ? O10 Mn4 Mn3 82.30(7) 5_666 . ? O1 Mn5 O20 85.20(13) . . ? O1 Mn5 O17 88.54(11) . 5_666 ? O20 Mn5 O17 101.26(12) . 5_666 ? O1 Mn5 O8 136.19(12) . . ? O20 Mn5 O8 108.95(13) . . ? O17 Mn5 O8 126.32(11) 5_666 . ? O1 Mn5 O12 86.97(11) . . ? O20 Mn5 O12 168.30(13) . . ? O17 Mn5 O12 69.83(10) 5_666 . ? O8 Mn5 O12 82.70(11) . . ? O1 Mn5 O5 83.39(12) . . ? O20 Mn5 O5 89.89(14) . . ? O17 Mn5 O5 165.66(13) 5_666 . ? O8 Mn5 O5 56.35(12) . . ? O12 Mn5 O5 97.83(12) . . ? O1 Mn5 O19 136.19(12) . . ? O20 Mn5 O19 55.77(12) . . ? O17 Mn5 O19 81.40(10) 5_666 . ? O8 Mn5 O19 80.52(11) . . ? O12 Mn5 O19 127.61(10) . . ? O5 Mn5 O19 112.56(13) . . ? O1 Mn5 Mn2 73.44(8) . . ? O20 Mn5 Mn2 131.61(11) . . ? O17 Mn5 Mn2 37.29(7) 5_666 . ? O8 Mn5 Mn2 116.60(8) . . ? O12 Mn5 Mn2 37.16(7) . . ? O5 Mn5 Mn2 128.49(10) . . ? O19 Mn5 Mn2 116.05(8) . . ? O11 Mn6 O9 152.68(11) 5_666 . ? O11 Mn6 O19 92.48(12) 5_666 . ? O9 Mn6 O19 93.44(12) . . ? O11 Mn6 O4 113.12(12) 5_666 . ? O9 Mn6 O4 90.03(12) . . ? O19 Mn6 O4 108.86(13) . . ? O11 Mn6 O10 82.46(11) 5_666 5_666 ? O9 Mn6 O10 82.73(11) . 5_666 ? O19 Mn6 O10 159.56(11) . 5_666 ? O4 Mn6 O10 91.27(12) . 5_666 ? O11 Mn6 Mn1 34.95(8) 5_666 5_666 ? O9 Mn6 Mn1 119.29(8) . 5_666 ? O19 Mn6 Mn1 85.08(9) . 5_666 ? O4 Mn6 Mn1 147.29(9) . 5_666 ? O10 Mn6 Mn1 79.43(8) 5_666 5_666 ? C1 O1 Mn5 136.6(3) . . ? C1 O2 Mn2 123.7(3) . . ? C29 O3 Mn4 132.3(3) . . ? C29 O4 Mn6 126.8(3) . . ? C15 O5 Mn5 91.0(3) . . ? Mn1 O6 Mn1 95.57(12) . 5_666 ? Mn1 O6 Mn2 96.00(11) . . ? Mn1 O6 Mn2 96.98(11) 5_666 . ? Mn1 O6 Mn3 169.18(14) . 5_666 ? Mn1 O6 Mn3 91.13(10) 5_666 5_666 ? Mn2 O6 Mn3 91.59(10) . 5_666 ? C81 O7 C81' 68.0(11) . . ? C81 O7 Mn4 130.9(10) . . ? C81' O7 Mn4 131.7(8) . . ? C81 O7 H7 103(4) . . ? C81' O7 H7 108(4) . . ? Mn4 O7 H7 108(4) . . ? C15 O8 Mn3 142.4(3) . . ? C15 O8 Mn5 92.1(3) . . ? Mn3 O8 Mn5 124.41(14) . . ? C82 O9 Mn6 115.2(3) . . ? C82 O9 Mn3 116.5(3) . . ? Mn6 O9 Mn3 106.77(13) . . ? C82 O9 Mn4 117.5(3) . . ? Mn6 O9 Mn4 99.88(12) . . ? Mn3 O9 Mn4 98.46(12) . . ? C78 O10 Mn2 118.3(2) . . ? C78 O10 Mn6 110.1(2) . 5_666 ? Mn2 O10 Mn6 108.82(13) . 5_666 ? C78 O10 Mn4 124.3(2) . 5_666 ? Mn2 O10 Mn4 100.81(12) . 5_666 ? Mn6 O10 Mn4 90.67(10) 5_666 5_666 ? C76 O11 Mn1 122.9(3) . . ? C76 O11 Mn6 116.0(3) . 5_666 ? Mn1 O11 Mn6 106.85(13) . 5_666 ? C77 O12 Mn2 121.1(3) . . ? C77 O12 Mn5 113.7(2) . . ? Mn2 O12 Mn5 97.05(12) . . ? C77 O12 Mn1 114.4(2) . . ? Mn2 O12 Mn1 93.09(11) . . ? Mn5 O12 Mn1 115.15(12) . . ? C80 O13 H13 109.5 . . ? C43 O14 Mn4 131.6(3) . . ? C43 O15 Mn3 128.9(3) . . ? C73 O16 Mn2 118.2(2) . 5_666 ? C73 O16 Mn3 113.5(2) . . ? Mn2 O16 Mn3 105.21(13) 5_666 . ? C73 O16 Mn4 124.5(3) . . ? Mn2 O16 Mn4 101.06(12) 5_666 . ? Mn3 O16 Mn4 89.59(10) . . ? C72 O17 Mn2 121.5(2) . 5_666 ? C72 O17 Mn5 111.9(2) . 5_666 ? Mn2 O17 Mn5 98.06(11) 5_666 5_666 ? C72 O17 Mn1 112.7(2) . . ? Mn2 O17 Mn1 94.54(11) 5_666 . ? Mn5 O17 Mn1 116.77(12) 5_666 . ? C71 O18 Mn1 122.0(3) . . ? C71 O18 Mn3 118.5(3) . . ? Mn1 O18 Mn3 103.37(12) . . ? C57 O19 Mn6 148.8(3) . . ? C57 O19 Mn5 86.8(3) . . ? Mn6 O19 Mn5 124.40(14) . . ? C57 O20 Mn5 97.1(3) . . ? C75 O22' H22D 109.5 . . ? C75 O22' H75A 14.2 . . ? H22D O22' H75A 121.7 . . ? C75 O22 H22C 109.5 . . ? O1 C1 O2 124.6(4) . . ? O1 C1 C2 118.5(4) . . ? O2 C1 C2 116.9(4) . . ? C9 C2 C1 107.3(4) . . ? C9 C2 C3 116.4(4) . . ? C1 C2 C3 110.7(4) . . ? C9 C2 H2A 107.4 . . ? C1 C2 H2A 107.4 . . ? C3 C2 H2A 107.4 . . ? C8 C3 C4 118.0(6) . . ? C8 C3 C2 119.1(5) . . ? C4 C3 C2 122.9(6) . . ? C3 C4 C5 120.3(7) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 120.5(7) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 120.9(8) . . ? C5 C6 H6A 119.6 . . ? C7 C6 H6A 119.6 . . ? C6 C7 C8 118.9(8) . . ? C6 C7 H7A 120.6 . . ? C8 C7 H7A 120.6 . . ? C3 C8 C7 121.4(7) . . ? C3 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C10 C9 C14 118.2(6) . . ? C10 C9 C2 120.1(5) . . ? C14 C9 C2 121.7(5) . . ? C9 C10 C11 121.1(7) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C12 C11 C10 120.0(7) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 119.8(7) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C12 C13 C14 120.1(7) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 C9 120.9(6) . . ? C13 C14 H14A 119.6 . . ? C9 C14 H14A 119.6 . . ? O5 C15 O8 120.5(4) . . ? O5 C15 C16 122.0(4) . . ? O8 C15 C16 117.4(4) . . ? C17 C16 C23 112.7(4) . . ? C17 C16 C15 108.4(4) . . ? C23 C16 C15 115.1(4) . . ? C17 C16 H16A 106.7 . . ? C23 C16 H16A 106.7 . . ? C15 C16 H16A 106.7 . . ? C18 C17 C22 119.4(7) . . ? C18 C17 C16 122.6(6) . . ? C22 C17 C16 117.9(6) . . ? C17 C18 C19 120.8(8) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C20 C19 C18 120.0(10) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 119.3(9) . . ? C19 C20 H20A 120.4 . . ? C21 C20 H20A 120.4 . . ? C22 C21 C20 121.5(10) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C17 118.9(10) . . ? C21 C22 H22A 120.5 . . ? C17 C22 H22A 120.5 . . ? C28 C23 C24 117.6(6) . . ? C28 C23 C16 119.5(7) . . ? C24 C23 C16 122.6(5) . . ? C23 C24 C25 119.3(9) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? C26 C25 C24 119.3(11) . . ? C26 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C27 C26 C25 121.1(9) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C28 120.0(10) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C23 C28 C27 122.5(9) . . ? C23 C28 H28A 118.7 . . ? C27 C28 H28A 118.7 . . ? O3 C29 O4 126.5(5) . . ? O3 C29 C30 116.2(5) . . ? O4 C29 C30 117.3(5) . . ? C31 C30 C29 113.2(4) . . ? C31 C30 C37 113.3(5) . . ? C29 C30 C37 110.3(4) . . ? C31 C30 H30A 106.5 . . ? C29 C30 H30A 106.5 . . ? C37 C30 H30A 106.5 . . ? C36 C31 C32 114.1(11) . . ? C36 C31 C32' 110(3) . . ? C32 C31 C32' 10(3) . . ? C36 C31 C30 122.3(7) . . ? C32 C31 C30 122.8(9) . . ? C32' C31 C30 128(3) . . ? C36 C31 C36' 32.4(9) . . ? C32 C31 C36' 127.6(12) . . ? C32' C31 C36' 119(3) . . ? C30 C31 C36' 106.0(11) . . ? C31 C32 C33 123.7(16) . . ? C31 C32 H32A 118.1 . . ? C33 C32 H32A 118.1 . . ? C33' C32' C31 103(4) . . ? C33' C32' H32B 128.5 . . ? C31 C32' H32B 128.5 . . ? C34 C33 C32 116.4(15) . . ? C34 C33 H33A 121.8 . . ? C32 C33 H33A 121.8 . . ? C32' C33' C34' 120(5) . . ? C32' C33' H33B 119.8 . . ? C34' C33' H33B 119.8 . . ? C33 C34 C35 120.3(11) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C35' C34' C33' 124(5) . . ? C35' C34' H34B 118.0 . . ? C33' C34' H34B 118.0 . . ? C36 C35 C34 118.8(11) . . ? C36 C35 H35A 120.6 . . ? C34 C35 H35A 120.6 . . ? C34' C35' C36' 117(3) . . ? C34' C35' H35B 121.5 . . ? C36' C35' H35B 121.5 . . ? C31 C36 C35 124.9(11) . . ? C31 C36 H36A 117.6 . . ? C35 C36 H36A 117.6 . . ? C35' C36' C31 115(2) . . ? C35' C36' H36B 122.7 . . ? C31 C36' H36B 122.7 . . ? C42 C37 C38 117.7(6) . . ? C42 C37 C30 122.6(6) . . ? C38 C37 C30 119.7(6) . . ? C39 C38 C37 121.3(8) . . ? C39 C38 H38A 119.4 . . ? C37 C38 H38A 119.4 . . ? C40 C39 C38 120.5(8) . . ? C40 C39 H39A 119.8 . . ? C38 C39 H39A 119.8 . . ? C39 C40 C41 119.9(8) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C40 C41 C42 119.0(9) . . ? C40 C41 H41A 120.5 . . ? C42 C41 H41A 120.5 . . ? C37 C42 C41 121.5(7) . . ? C37 C42 H42A 119.3 . . ? C41 C42 H42A 119.3 . . ? O14 C43 O15 126.0(4) . . ? O14 C43 C44 115.8(4) . . ? O15 C43 C44 118.2(4) . . ? C45 C44 C51 114.5(13) . . ? C45 C44 C45' 94.2(13) . . ? C51 C44 C45' 114.3(4) . . ? C45 C44 C43 112.6(13) . . ? C51 C44 C43 111.1(4) . . ? C45' C44 C43 109.1(4) . . ? C44 C45 C46 113.8(19) . . ? C44 C45 C50 125.9(19) . . ? C46 C45 C50 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 H50A 120.0 . . ? C45 C50 H50A 120.0 . . ? C46' C45' C50' 117.9(7) . . ? C46' C45' C44 121.9(6) . . ? C50' C45' C44 120.2(6) . . ? C45' C46' C47' 121.9(7) . . ? C45' C46' H46B 119.1 . . ? C47' C46' H46B 119.1 . . ? C48' C47' C46' 120.7(8) . . ? C48' C47' H47B 119.7 . . ? C46' C47' H47B 119.7 . . ? C47' C48' C49' 120.3(8) . . ? C47' C48' H48B 119.9 . . ? C49' C48' H48B 119.9 . . ? C48' C49' C50' 121.0(8) . . ? C48' C49' H49B 119.5 . . ? C50' C49' H49B 119.5 . . ? C45' C50' C49' 118.2(8) . . ? C45' C50' H50B 120.9 . . ? C49' C50' H50B 120.9 . . ? C52 C51 C56 118.2(6) . . ? C52 C51 C44 119.0(5) . . ? C56 C51 C44 122.8(5) . . ? C51 C52 C53 121.2(7) . . ? C51 C52 H52A 119.4 . . ? C53 C52 H52A 119.4 . . ? C54 C53 C52 119.1(7) . . ? C54 C53 H53A 120.5 . . ? C52 C53 H53A 120.5 . . ? C55 C54 C53 120.6(7) . . ? C55 C54 H54A 119.7 . . ? C53 C54 H54A 119.7 . . ? C54 C55 C56 119.6(8) . . ? C54 C55 H55A 120.2 . . ? C56 C55 H55A 120.2 . . ? C55 C56 C51 121.3(7) . . ? C55 C56 H56A 119.4 . . ? C51 C56 H56A 119.4 . . ? O20 C57 O19 120.3(4) . . ? O20 C57 C58 121.7(4) . . ? O19 C57 C58 117.9(4) . . ? C59 C58 C65' 113.8(6) . . ? C59 C58 C65 122.8(8) . . ? C65' C58 C65 16.0(7) . . ? C59 C58 C57 111.3(4) . . ? C65' C58 C57 106.9(5) . . ? C65 C58 C57 111.6(7) . . ? C59 C58 H58A 102.8 . . ? C65' C58 H58A 118.7 . . ? C65 C58 H58A 102.8 . . ? C57 C58 H58A 102.8 . . ? C64 C59 C60 115.3(6) . . ? C64 C59 C58 126.7(6) . . ? C60 C59 C58 117.2(5) . . ? C61 C60 C59 120.6(6) . . ? C61 C60 H60A 119.7 . . ? C59 C60 H60A 119.7 . . ? C60 C61 C62 118.7(8) . . ? C60 C61 H61A 120.6 . . ? C62 C61 H61A 120.6 . . ? C63 C62 C61 120.8(7) . . ? C63 C62 H62A 119.6 . . ? C61 C62 H62A 119.6 . . ? C62 C63 C64 119.2(7) . . ? C62 C63 H63A 120.4 . . ? C64 C63 H63A 120.4 . . ? C59 C64 C63 125.1(7) . . ? C59 C64 H64A 117.4 . . ? C63 C64 H64A 117.4 . . ? C66 C65 C70 120.0 . . ? C66 C65 C58 119.2(12) . . ? C70 C65 C58 120.9(12) . . ? C67 C66 C65 120.0 . . ? C67 C66 H66A 120.0 . . ? C65 C66 H66A 120.0 . . ? C66 C67 C68 120.0 . . ? C66 C67 H67A 120.0 . . ? C68 C67 H67A 120.0 . . ? C69 C68 C67 120.0 . . ? C69 C68 H68A 120.0 . . ? C67 C68 H68A 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H69A 120.0 . . ? C70 C69 H69A 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 H70A 120.0 . . ? C65 C70 H70A 120.0 . . ? C66' C65' C70' 120.2(11) . . ? C66' C65' C58 123.8(9) . . ? C70' C65' C58 116.0(9) . . ? C65' C66' C67' 121.7(15) . . ? C65' C66' H66B 119.1 . . ? C67' C66' H66B 119.1 . . ? C66' C67' C68' 119.0(15) . . ? C66' C67' H67B 120.5 . . ? C68' C67' H67B 120.5 . . ? C69' C68' C67' 120.5(15) . . ? C69' C68' H68B 119.7 . . ? C67' C68' H68B 119.7 . . ? C68' C69' C70' 120.2(16) . . ? C68' C69' H69B 119.9 . . ? C70' C69' H69B 119.9 . . ? C65' C70' C69' 118.2(14) . . ? C65' C70' H70B 120.9 . . ? C69' C70' H70B 120.9 . . ? O18 C71 C74 115.3(3) . . ? O18 C71 H71A 108.4 . . ? C74 C71 H71A 108.4 . . ? O18 C71 H71B 108.4 . . ? C74 C71 H71B 108.4 . . ? H71A C71 H71B 107.5 . . ? O17 C72 C74 113.4(3) . . ? O17 C72 H72A 108.9 . . ? C74 C72 H72A 108.9 . . ? O17 C72 H72B 108.9 . . ? C74 C72 H72B 108.9 . . ? H72A C72 H72B 107.7 . . ? O16 C73 C74 114.0(4) . . ? O16 C73 H73A 108.8 . . ? C74 C73 H73A 108.8 . . ? O16 C73 H73B 108.8 . . ? C74 C73 H73B 108.8 . . ? H73A C73 H73B 107.7 . . ? C72 C74 C71 111.8(4) . . ? C72 C74 C73 112.0(4) . . ? C71 C74 C73 113.7(4) . . ? C72 C74 C75 104.6(4) . . ? C71 C74 C75 106.8(4) . . ? C73 C74 C75 107.3(4) . . ? O22 C75 O22' 103.4(6) . . ? O22 C75 C74 112.1(5) . . ? O22' C75 C74 114.1(4) . . ? O22 C75 H75D 109.6 . . ? O22' C75 H75D 108.7 . . ? C74 C75 H75D 108.7 . . ? O22 C75 H75C 5.3 . . ? O22' C75 H75C 108.7 . . ? C74 C75 H75C 108.7 . . ? H75D C75 H75C 107.6 . . ? O22 C75 H75A 109.2 . . ? O22' C75 H75A 6.2 . . ? C74 C75 H75A 109.0 . . ? H75D C75 H75A 108.2 . . ? H75C C75 H75A 114.5 . . ? O22 C75 H75B 109.8 . . ? O22' C75 H75B 108.3 . . ? C74 C75 H75B 108.9 . . ? H75D C75 H75B 0.4 . . ? H75C C75 H75B 107.8 . . ? H75A C75 H75B 107.8 . . ? O11 C76 C79 114.8(3) . . ? O11 C76 H76A 108.6 . . ? C79 C76 H76A 108.6 . . ? O11 C76 H76B 108.6 . . ? C79 C76 H76B 108.6 . . ? H76A C76 H76B 107.5 . . ? O12 C77 C79 113.9(3) . . ? O12 C77 H77A 108.8 . . ? C79 C77 H77A 108.8 . . ? O12 C77 H77B 108.8 . . ? C79 C77 H77B 108.8 . . ? H77A C77 H77B 107.7 . . ? O10 C78 C79 114.3(4) . . ? O10 C78 H78A 108.7 . . ? C79 C78 H78A 108.7 . . ? O10 C78 H78B 108.7 . . ? C79 C78 H78B 108.7 . . ? H78A C78 H78B 107.6 . . ? C77 C79 C76 111.3(4) . . ? C77 C79 C78 111.2(4) . . ? C76 C79 C78 114.0(4) . . ? C77 C79 C80 104.8(3) . . ? C76 C79 C80 107.7(4) . . ? C78 C79 C80 107.3(4) . . ? O13 C80 C79 110.2(4) . . ? O13 C80 H80A 109.6 . . ? C79 C80 H80A 109.6 . . ? O13 C80 H80B 109.6 . . ? C79 C80 H80B 109.6 . . ? H80A C80 H80B 108.1 . . ? O7 C81' H81F 109.5 . . ? O7 C81' H81D 109.5 . . ? O7 C81' H81E 109.5 . . ? O7 C81 H81A 109.5 . . ? O7 C81 H81B 109.5 . . ? O7 C81 H81C 109.5 . . ? O9 C82 H82A 109.5 . . ? O9 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O9 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N1 C83 C84 167(2) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N2 C85 N2' 27(4) . . ? N2 C85 C86 174.4(18) . . ? N2' C85 C86 152(3) . . ? N2 C85 C86' 146(3) . . ? N2' C85 C86' 163(4) . . ? C86 C85 C86' 37(2) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? C85 C86' H86'A 109.5 . . ? C85 C86' H86'B 109.5 . . ? C85 C86' H86'C 109.5 . . ? N3 C87 C88 178.1(10) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.780 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.091 # Attachment 'Mn12 thme Muralee CIF 2 (Dalton).txt' data_xm54 _database_code_depnum_ccdc_archive 'CCDC 290613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C184 H198 Mn12 N12 O42' _chemical_formula_weight 3908.82 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.5435(15) _cell_length_b 18.8989(14) _cell_length_c 25.3111(19) _cell_angle_alpha 90.00 _cell_angle_beta 111.180(2) _cell_angle_gamma 90.00 _cell_volume 9163.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4044 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8438 _exptl_absorpt_correction_T_max 0.9596 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 81055 _diffrn_reflns_av_R_equivalents 0.1240 _diffrn_reflns_av_sigmaI/netI 0.1636 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.50 _reflns_number_total 20946 _reflns_number_gt 9314 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^] 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 20946 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1420 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1969 _refine_ls_wR_factor_gt 0.1770 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 1.01369(4) 0.02229(4) 0.45110(3) 0.0188(2) Uani 1 1 d . . . Mn2 Mn 1.03502(4) -0.13666(4) 0.48276(3) 0.0190(2) Uani 1 1 d . . . Mn3 Mn 0.86055(4) 0.07736(5) 0.38922(3) 0.0239(2) Uani 1 1 d . . . Mn4 Mn 0.80431(5) 0.18977(5) 0.45886(4) 0.0262(2) Uani 1 1 d . . . Mn5 Mn 1.17375(5) -0.02718(5) 0.49571(4) 0.0265(2) Uani 1 1 d . . . Mn6 Mn 0.87272(4) -0.12727(5) 0.41323(3) 0.0235(2) Uani 1 1 d . . . O1 O 0.95959(18) 0.07330(18) 0.38442(14) 0.0205(8) Uani 1 1 d . . . O2 O 1.04663(18) 0.13129(18) 0.49597(13) 0.0197(8) Uani 1 1 d . . . O3 O 1.11736(18) -0.13267(18) 0.46351(14) 0.0202(8) Uani 1 1 d . . . O4 O 0.97700(18) -0.08958(18) 0.41447(13) 0.0202(8) Uani 1 1 d . . . O5 O 1.09153(18) 0.01149(18) 0.42675(14) 0.0205(8) Uani 1 1 d . . . O6 O 1.06035(17) -0.02883(18) 0.52002(14) 0.0191(8) Uani 1 1 d . . . O7 O 0.7544(2) 0.2249(2) 0.37369(16) 0.0358(10) Uani 1 1 d . . . O8 O 0.7940(2) 0.1462(2) 0.32593(15) 0.0333(10) Uani 1 1 d . . . O10 O 0.78744(19) 0.08208(19) 0.42883(14) 0.0246(9) Uani 1 1 d . . . O11 O 0.7325(2) 0.1780(2) 0.49971(17) 0.0362(11) Uani 1 1 d . . . O12 O 0.8502(2) 0.2903(2) 0.49661(18) 0.0367(11) Uani 1 1 d . . . H12A H 0.8929 0.2846 0.5153 0.055 Uiso 1 1 calc R . . H12B H 0.834(3) 0.327(4) 0.513(3) 0.06(2) Uiso 1 1 d . . . O13 O 0.9012(2) -0.2365(2) 0.40226(15) 0.0301(10) Uani 1 1 d . . . O14 O 1.01647(19) -0.24287(19) 0.45011(15) 0.0250(9) Uani 1 1 d . . . O15 O 0.8147(2) -0.1271(2) 0.31247(16) 0.0372(11) Uani 1 1 d . . . O16 O 0.83487(19) -0.0278(2) 0.36023(15) 0.0279(9) Uani 1 1 d . . . O17 O 0.7752(2) -0.1724(2) 0.42051(18) 0.0428(12) Uani 1 1 d . . . O18 O 1.09365(18) -0.17344(18) 0.55462(14) 0.0194(8) Uani 1 1 d . . . O19 O 1.2582(2) -0.0635(2) 0.47322(17) 0.0373(11) Uani 1 1 d . . . O20 O 1.1918(2) 0.0738(2) 0.53371(17) 0.0396(11) Uani 1 1 d . . . O21 O 0.9712(2) 0.2850(2) 0.32529(15) 0.0344(10) Uani 1 1 d . . . H21A H 0.9888 0.2890 0.3002 0.052 Uiso 1 1 calc R . . O22 O 1.0331(2) -0.1833(2) 0.28786(16) 0.0351(11) Uani 1 1 d . . . H22A H 1.0318 -0.1926 0.2551 0.053 Uiso 1 1 calc R . . C1 C 1.1095(3) -0.1460(3) 0.4054(2) 0.0244(13) Uani 1 1 d . . . H1A H 1.0919 -0.1948 0.3953 0.029 Uiso 1 1 calc R . . H1B H 1.1560 -0.1431 0.4021 0.029 Uiso 1 1 calc R . . C2 C 0.9847(3) -0.1019(3) 0.3604(2) 0.0231(13) Uani 1 1 d . . . H2A H 0.9552 -0.0677 0.3324 0.028 Uiso 1 1 calc R . . H2B H 0.9675 -0.1500 0.3470 0.028 Uiso 1 1 calc R . . C3 C 1.0847(3) -0.0175(3) 0.3730(2) 0.0229(13) Uani 1 1 d . . . H3A H 1.1305 -0.0139 0.3685 0.028 Uiso 1 1 calc R . . H3B H 1.0512 0.0119 0.3431 0.028 Uiso 1 1 calc R . . C4 C 1.0604(3) -0.0949(3) 0.3633(2) 0.0214(13) Uani 1 1 d . . . C5 C 1.0601(3) -0.1140(3) 0.3032(2) 0.0275(14) Uani 1 1 d . . . H5A H 1.0311 -0.0795 0.2751 0.033 Uiso 1 1 calc R . . H5B H 1.1083 -0.1115 0.3032 0.033 Uiso 1 1 calc R . . C7 C 1.0606(3) 0.1846(3) 0.4608(2) 0.0227(13) Uani 1 1 d . . . H7A H 1.1016 0.1698 0.4518 0.027 Uiso 1 1 calc R . . H7B H 1.0728 0.2293 0.4826 0.027 Uiso 1 1 calc R . . C8 C 0.9850(3) 0.1354(3) 0.3651(2) 0.0230(13) Uani 1 1 d . . . H8A H 0.9503 0.1496 0.3280 0.028 Uiso 1 1 calc R . . H8B H 1.0287 0.1230 0.3592 0.028 Uiso 1 1 calc R . . C9 C 0.9993(3) 0.1987(3) 0.4052(2) 0.0204(12) Uani 1 1 d . . . C10 C 1.0228(3) 0.2611(3) 0.3764(2) 0.0259(13) Uani 1 1 d . . . H10A H 1.0368 0.3011 0.4034 0.031 Uiso 1 1 calc R . . H10B H 1.0645 0.2462 0.3684 0.031 Uiso 1 1 calc R . . C12 C 1.0658(3) -0.2244(3) 0.5838(2) 0.0227(13) Uani 1 1 d . . . H12D H 1.1026 -0.2363 0.6206 0.027 Uiso 1 1 calc R . . H12C H 1.0538 -0.2684 0.5610 0.027 Uiso 1 1 calc R . . C13 C 0.7664(3) -0.1264(3) 0.4522(2) 0.0307(14) Uani 1 1 d . . . C14 C 0.7091(3) -0.1299(4) 0.4771(3) 0.0394(16) Uani 1 1 d . . . H14A H 0.7030 -0.0807 0.4891 0.047 Uiso 1 1 calc R . . C15 C 0.7338(4) -0.1748(4) 0.5311(3) 0.050(2) Uani 1 1 d . . . C16 C 0.6382(3) -0.1531(4) 0.4357(3) 0.0386(17) Uani 1 1 d . . . C17 C 0.6254(4) -0.2185(4) 0.4096(3) 0.069(3) Uani 1 1 d . . . H17A H 0.6631 -0.2509 0.4175 0.083 Uiso 1 1 calc R . . C18 C 0.5826(4) -0.1059(5) 0.4243(3) 0.066(2) Uani 1 1 d . . . H18A H 0.5891 -0.0607 0.4419 0.079 Uiso 1 1 calc R . . C19 C 0.7640(4) -0.2408(4) 0.5340(4) 0.062(2) Uani 1 1 d . . . H19A H 0.7701 -0.2603 0.5015 0.074 Uiso 1 1 calc R . . C20 C 0.8104(3) -0.0616(3) 0.3129(2) 0.0252(13) Uani 1 1 d . . . C21 C 0.7799(3) -0.0164(3) 0.2594(2) 0.0265(14) Uani 1 1 d . . . H21B H 0.7691 0.0311 0.2717 0.032 Uiso 1 1 calc R . . C22 C 0.7124(3) -0.0448(4) 0.2163(2) 0.0329(15) Uani 1 1 d . . . C23 C 0.7045(4) -0.1136(4) 0.1956(3) 0.056(2) Uani 1 1 d . . . H23A H 0.7423 -0.1460 0.2092 0.068 Uiso 1 1 calc R . . C24 C 0.6420(5) -0.1353(5) 0.1554(3) 0.081(3) Uani 1 1 d . . . H24A H 0.6379 -0.1827 0.1421 0.098 Uiso 1 1 calc R . . C25 C 0.5861(5) -0.0914(6) 0.1341(4) 0.078(3) Uani 1 1 d . . . H25A H 0.5437 -0.1078 0.1065 0.094 Uiso 1 1 calc R . . C26 C 0.5924(4) -0.0232(6) 0.1534(3) 0.072(3) Uani 1 1 d . . . H26A H 0.5538 0.0082 0.1390 0.087 Uiso 1 1 calc R . . C27 C 0.6549(4) 0.0011(4) 0.1943(3) 0.055(2) Uani 1 1 d . . . H27A H 0.6585 0.0487 0.2070 0.066 Uiso 1 1 calc R . . C28 C 0.8356(3) -0.0049(3) 0.2331(2) 0.0296(14) Uani 1 1 d . . . C29 C 0.8538(3) 0.0649(3) 0.2256(3) 0.0407(17) Uani 1 1 d . . . H29A H 0.8328 0.1034 0.2376 0.049 Uiso 1 1 calc R . . C30 C 0.9030(4) 0.0774(4) 0.2003(3) 0.0515(19) Uani 1 1 d . . . H30A H 0.9157 0.1246 0.1954 0.062 Uiso 1 1 calc R . . C31 C 0.9329(4) 0.0222(4) 0.1826(3) 0.051(2) Uani 1 1 d . . . H31A H 0.9656 0.0312 0.1647 0.061 Uiso 1 1 calc R . . C32 C 0.9156(3) -0.0481(4) 0.1906(2) 0.0427(18) Uani 1 1 d . . . H32A H 0.9368 -0.0863 0.1785 0.051 Uiso 1 1 calc R . . C33 C 0.8678(3) -0.0612(4) 0.2160(2) 0.0373(16) Uani 1 1 d . . . H33A H 0.8567 -0.1086 0.2220 0.045 Uiso 1 1 calc R . . C34 C 0.7518(3) 0.1939(3) 0.3294(2) 0.0320(15) Uani 1 1 d . . . C35 C 0.6922(3) 0.2093(4) 0.2739(3) 0.0396(17) Uani 1 1 d . . . H35A H 0.6624 0.1659 0.2658 0.048 Uiso 1 1 calc R . . C36 C 0.6454(3) 0.2682(4) 0.2784(3) 0.0408(17) Uani 1 1 d . . . C37 C 0.5867(4) 0.2555(5) 0.2905(3) 0.072(3) Uani 1 1 d . . . H37A H 0.5759 0.2079 0.2964 0.086 Uiso 1 1 calc R . . C38 C 0.5428(5) 0.3081(6) 0.2947(4) 0.090(3) Uani 1 1 d . . . H38A H 0.5014 0.2970 0.3015 0.108 Uiso 1 1 calc R . . C39 C 0.5600(5) 0.3767(6) 0.2887(4) 0.081(3) Uani 1 1 d . . . H39A H 0.5314 0.4140 0.2934 0.097 Uiso 1 1 calc R . . C40 C 0.6183(5) 0.3928(5) 0.2761(4) 0.094(3) Uani 1 1 d . . . H40A H 0.6297 0.4404 0.2712 0.113 Uiso 1 1 calc R . . C41 C 0.6597(4) 0.3373(4) 0.2707(4) 0.069(2) Uani 1 1 d . . . H41A H 0.6995 0.3476 0.2614 0.083 Uiso 1 1 calc R . . C42 C 0.7161(3) 0.2167(3) 0.2239(2) 0.0360(16) Uani 1 1 d . . . C43 C 0.6720(4) 0.1942(3) 0.1708(3) 0.0424(17) Uani 1 1 d . . . H43A H 0.6272 0.1761 0.1661 0.051 Uiso 1 1 calc R . . C44 C 0.6926(4) 0.1979(4) 0.1251(3) 0.0469(19) Uani 1 1 d . . . H44A H 0.6620 0.1819 0.0891 0.056 Uiso 1 1 calc R . . C45 C 0.7576(4) 0.2248(4) 0.1308(3) 0.051(2) Uani 1 1 d . . . H45A H 0.7716 0.2271 0.0989 0.061 Uiso 1 1 calc R . . C46 C 0.8019(4) 0.2484(4) 0.1833(3) 0.0459(18) Uani 1 1 d . . . H46A H 0.8462 0.2676 0.1875 0.055 Uiso 1 1 calc R . . C47 C 0.7812(4) 0.2437(3) 0.2298(3) 0.0399(17) Uani 1 1 d . . . H47A H 0.8119 0.2592 0.2659 0.048 Uiso 1 1 calc R . . C48 C 0.7135(3) 0.1249(4) 0.5197(3) 0.0360(16) Uani 1 1 d . . . C49 C 0.6514(3) 0.1374(4) 0.5390(3) 0.0391(16) Uani 1 1 d . . . H49A H 0.6639 0.1793 0.5649 0.047 Uiso 1 1 calc R . . C50 C 0.5874(3) 0.1580(4) 0.4896(3) 0.0402(17) Uani 1 1 d . . . C51 C 0.5782(4) 0.1389(4) 0.4337(3) 0.054(2) Uani 1 1 d . . . H51A H 0.6119 0.1106 0.4259 0.065 Uiso 1 1 calc R . . C52 C 0.5181(5) 0.1624(5) 0.3894(4) 0.076(3) Uani 1 1 d . . . H52A H 0.5116 0.1506 0.3514 0.091 Uiso 1 1 calc R . . C53 C 0.4695(5) 0.2018(5) 0.4003(6) 0.094(4) Uani 1 1 d . . . H53A H 0.4292 0.2168 0.3698 0.113 Uiso 1 1 calc R . . C54 C 0.4771(5) 0.2202(5) 0.4542(5) 0.082(3) Uani 1 1 d . . . H54A H 0.4423 0.2479 0.4611 0.099 Uiso 1 1 calc R . . C55 C 0.5351(4) 0.1987(4) 0.4983(4) 0.065(2) Uani 1 1 d . . . H55A H 0.5402 0.2118 0.5358 0.078 Uiso 1 1 calc R . . C56 C 0.6408(3) 0.0761(3) 0.5739(3) 0.0321(15) Uani 1 1 d . . . C57 C 0.5940(4) 0.0230(4) 0.5504(3) 0.0449(18) Uani 1 1 d . . . H57A H 0.5663 0.0246 0.5111 0.054 Uiso 1 1 calc R . . C58 C 0.5861(4) -0.0332(4) 0.5829(3) 0.055(2) Uani 1 1 d . . . H58A H 0.5541 -0.0701 0.5657 0.066 Uiso 1 1 calc R . . C59 C 0.6246(4) -0.0356(4) 0.6405(3) 0.052(2) Uani 1 1 d . . . H59A H 0.6180 -0.0730 0.6631 0.063 Uiso 1 1 calc R . . C60 C 0.6718(4) 0.0162(5) 0.6643(3) 0.068(2) Uani 1 1 d . . . H60A H 0.6997 0.0141 0.7034 0.082 Uiso 1 1 calc R . . C61 C 0.6799(4) 0.0738(4) 0.6308(3) 0.0513(19) Uani 1 1 d . . . H61A H 0.7122 0.1106 0.6479 0.062 Uiso 1 1 calc R . . C62 C 0.9582(3) -0.2692(3) 0.4213(2) 0.0271(14) Uani 1 1 d . . . C63 C 0.9577(3) -0.3494(3) 0.4118(2) 0.0340(15) Uani 1 1 d . . . H63A H 1.0077 -0.3643 0.4236 0.041 Uiso 1 1 calc R . . C64 C 0.9233(3) -0.3697(3) 0.3502(2) 0.0323(15) Uani 1 1 d . . . C65 C 0.9318(4) -0.3270(4) 0.3080(3) 0.0498(19) Uani 1 1 d . . . H65A H 0.9558 -0.2832 0.3186 0.060 Uiso 1 1 calc R . . C66 C 0.9067(5) -0.3459(4) 0.2522(3) 0.066(2) Uani 1 1 d . . . H66A H 0.9127 -0.3158 0.2243 0.079 Uiso 1 1 calc R . . C67 C 0.8725(5) -0.4098(5) 0.2374(3) 0.075(3) Uani 1 1 d . . . H67A H 0.8547 -0.4234 0.1986 0.090 Uiso 1 1 calc R . . C68 C 0.8635(4) -0.4542(4) 0.2768(3) 0.064(2) Uani 1 1 d . . . H68A H 0.8401 -0.4982 0.2658 0.077 Uiso 1 1 calc R . . C69 C 0.8891(3) -0.4338(3) 0.3331(3) 0.0443(18) Uani 1 1 d . . . H69A H 0.8830 -0.4643 0.3607 0.053 Uiso 1 1 calc R . . C70 C 0.9296(4) -0.3833(3) 0.4533(3) 0.0404(17) Uani 1 1 d . . . C71 C 0.9769(4) -0.4115(4) 0.5036(3) 0.058(2) Uani 1 1 d . . . H71A H 1.0255 -0.4112 0.5103 0.070 Uiso 1 1 calc R . . C72 C 0.8819(6) -0.4402(4) 0.5341(4) 0.075(3) Uani 1 1 d . . . H72A H 0.8650 -0.4599 0.5612 0.090 Uiso 1 1 calc R . . C73 C 0.8371(5) -0.4124(5) 0.4863(4) 0.073(3) Uani 1 1 d . . . H73A H 0.7885 -0.4128 0.4795 0.088 Uiso 1 1 calc R . . C74 C 0.8609(4) -0.3827(4) 0.4461(3) 0.056(2) Uani 1 1 d . . . H74A H 0.8283 -0.3616 0.4131 0.067 Uiso 1 1 calc R . . C75 C 0.9524(6) -0.4404(4) 0.5442(3) 0.074(3) Uani 1 1 d . . . H75A H 0.9842 -0.4598 0.5784 0.089 Uiso 1 1 calc R . . C80 C 0.7258(4) -0.1480(5) 0.5783(3) 0.071(3) Uani 1 1 d . . . H80A H 0.7058 -0.1025 0.5776 0.085 Uiso 1 1 calc R . . C81 C 0.7471(5) -0.1881(7) 0.6277(4) 0.098(4) Uani 1 1 d . . . H81A H 0.7396 -0.1699 0.6600 0.117 Uiso 1 1 calc R . . C82 C 0.7776(5) -0.2513(7) 0.6315(5) 0.106(4) Uani 1 1 d . . . H82A H 0.7934 -0.2767 0.6663 0.127 Uiso 1 1 calc R . . C83 C 0.7853(5) -0.2783(5) 0.5843(5) 0.082(3) Uani 1 1 d . . . H83A H 0.8057 -0.3237 0.5859 0.098 Uiso 1 1 calc R . . C84 C 0.5616(5) -0.2388(6) 0.3734(4) 0.083(3) Uani 1 1 d . . . H84A H 0.5548 -0.2842 0.3561 0.099 Uiso 1 1 calc R . . C85 C 0.5088(5) -0.1938(7) 0.3626(4) 0.083(3) Uani 1 1 d . . . H85A H 0.4640 -0.2083 0.3376 0.100 Uiso 1 1 calc R . . C86 C 0.5157(4) -0.1273(7) 0.3857(3) 0.082(3) Uani 1 1 d . . . H86A H 0.4769 -0.0961 0.3762 0.098 Uiso 1 1 calc R . . N1 N 0.7890(3) 0.1014(3) 0.0388(3) 0.0595(18) Uani 1 1 d . . . C87 C 0.7618(4) 0.0632(4) 0.0570(3) 0.0488(19) Uani 1 1 d . . . C88 C 0.7247(5) 0.0133(5) 0.0799(3) 0.083(3) Uani 1 1 d . . . H88A H 0.6798 0.0338 0.0774 0.124 Uiso 1 1 calc R . . H88B H 0.7528 0.0034 0.1196 0.124 Uiso 1 1 calc R . . H88C H 0.7165 -0.0308 0.0580 0.124 Uiso 1 1 calc R . . N2 N 0.1288(4) 0.8773(3) 0.1512(3) 0.0605(19) Uani 1 1 d . . . C89 C 0.1666(5) 0.8956(4) 0.1307(3) 0.056(2) Uani 1 1 d . . . C90 C 0.2159(5) 0.9194(5) 0.1054(4) 0.083(3) Uani 1 1 d . . . H90A H 0.1906 0.9342 0.0662 0.124 Uiso 1 1 calc R . . H90B H 0.2478 0.8806 0.1058 0.124 Uiso 1 1 calc R . . H90C H 0.2428 0.9594 0.1271 0.124 Uiso 1 1 calc R . . N3 N 0.3444(4) 0.5281(5) 0.1565(3) 0.090(3) Uani 1 1 d . . . C91 C 0.3585(4) 0.4723(6) 0.1746(3) 0.066(3) Uani 1 1 d . . . C92 C 0.3726(4) 0.3991(5) 0.1971(3) 0.073(3) Uani 1 1 d . . . H92A H 0.3879 0.4002 0.2385 0.110 Uiso 1 1 calc R . . H92B H 0.4093 0.3780 0.1860 0.110 Uiso 1 1 calc R . . H92C H 0.3299 0.3708 0.1817 0.110 Uiso 1 1 calc R . . 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 0.0214(5) 0.0201(5) 0.0154(4) 0.0005(3) 0.0072(4) 0.0009(4) Mn2 0.0217(5) 0.0215(5) 0.0142(4) 0.0012(4) 0.0068(4) 0.0005(4) Mn3 0.0240(5) 0.0267(5) 0.0201(4) -0.0015(4) 0.0069(4) 0.0008(4) Mn4 0.0263(5) 0.0291(5) 0.0231(5) 0.0015(4) 0.0090(4) 0.0046(4) Mn5 0.0261(5) 0.0290(5) 0.0219(5) 0.0005(4) 0.0057(4) -0.0005(4) Mn6 0.0237(5) 0.0254(5) 0.0199(4) 0.0013(4) 0.0061(4) -0.0017(4) O1 0.023(2) 0.021(2) 0.0163(19) -0.0003(16) 0.0065(16) -0.0033(17) O2 0.022(2) 0.022(2) 0.0144(18) 0.0010(16) 0.0052(16) 0.0005(17) O3 0.023(2) 0.022(2) 0.0167(18) -0.0001(16) 0.0089(16) 0.0020(17) O4 0.025(2) 0.023(2) 0.0127(18) -0.0008(16) 0.0066(16) 0.0040(17) O5 0.024(2) 0.022(2) 0.0155(19) -0.0009(16) 0.0074(17) 0.0002(17) O6 0.021(2) 0.019(2) 0.0173(19) 0.0024(16) 0.0068(17) -0.0010(16) O7 0.043(3) 0.035(3) 0.029(2) 0.004(2) 0.012(2) 0.009(2) O8 0.037(3) 0.039(3) 0.022(2) 0.0036(19) 0.0085(19) 0.007(2) O10 0.026(2) 0.026(2) 0.023(2) -0.0032(17) 0.0091(17) -0.0003(18) O11 0.033(3) 0.041(3) 0.041(3) 0.002(2) 0.021(2) 0.004(2) O12 0.035(3) 0.031(3) 0.043(3) -0.006(2) 0.013(2) 0.003(2) O13 0.034(3) 0.024(2) 0.029(2) -0.0013(18) 0.007(2) -0.0012(19) O14 0.021(2) 0.025(2) 0.026(2) -0.0054(18) 0.0056(18) -0.0020(18) O15 0.049(3) 0.028(3) 0.028(2) -0.001(2) 0.006(2) -0.002(2) O16 0.032(2) 0.030(2) 0.020(2) -0.0032(18) 0.0070(18) -0.0038(19) O17 0.049(3) 0.042(3) 0.046(3) -0.012(2) 0.028(2) -0.005(2) O18 0.020(2) 0.023(2) 0.0159(19) 0.0047(16) 0.0087(16) 0.0043(16) O19 0.036(3) 0.045(3) 0.035(2) -0.004(2) 0.018(2) -0.002(2) O20 0.036(3) 0.035(3) 0.043(3) -0.003(2) 0.008(2) -0.006(2) O21 0.048(3) 0.039(3) 0.019(2) 0.0153(19) 0.015(2) 0.002(2) O22 0.054(3) 0.033(3) 0.023(2) -0.0123(19) 0.020(2) -0.010(2) C1 0.027(3) 0.029(3) 0.019(3) -0.006(2) 0.010(3) 0.000(3) C2 0.023(3) 0.032(3) 0.014(3) -0.001(2) 0.006(2) 0.001(3) C3 0.030(3) 0.027(3) 0.014(3) -0.002(2) 0.012(3) 0.001(3) C4 0.029(3) 0.023(3) 0.016(3) -0.002(2) 0.012(3) 0.000(3) C5 0.035(4) 0.032(4) 0.019(3) 0.000(3) 0.014(3) 0.002(3) C7 0.029(3) 0.027(3) 0.014(3) 0.003(2) 0.011(3) -0.005(3) C8 0.034(3) 0.026(3) 0.009(3) 0.002(2) 0.009(2) 0.000(3) C9 0.026(3) 0.020(3) 0.018(3) 0.002(2) 0.011(2) 0.000(2) C10 0.035(4) 0.021(3) 0.026(3) 0.002(3) 0.016(3) 0.001(3) C12 0.026(3) 0.023(3) 0.018(3) 0.007(2) 0.008(3) 0.004(3) C13 0.025(3) 0.035(4) 0.030(3) 0.001(3) 0.008(3) -0.006(3) C14 0.031(4) 0.048(4) 0.039(4) -0.006(3) 0.013(3) 0.002(3) C15 0.034(4) 0.076(6) 0.042(4) 0.013(4) 0.017(4) -0.003(4) C16 0.032(4) 0.056(5) 0.032(4) -0.001(3) 0.017(3) -0.014(3) C17 0.071(6) 0.058(6) 0.064(5) 0.000(4) 0.006(5) -0.030(5) C18 0.064(6) 0.093(7) 0.051(5) -0.004(5) 0.034(5) 0.013(5) C19 0.060(5) 0.063(6) 0.064(6) 0.007(5) 0.024(4) -0.013(5) C20 0.017(3) 0.036(4) 0.024(3) -0.001(3) 0.008(3) -0.003(3) C21 0.030(3) 0.026(3) 0.021(3) -0.001(3) 0.006(3) -0.001(3) C22 0.033(4) 0.049(4) 0.018(3) 0.002(3) 0.009(3) -0.010(3) C23 0.053(5) 0.061(5) 0.042(4) -0.006(4) 0.001(4) -0.008(4) C24 0.064(6) 0.103(8) 0.056(5) -0.022(5) -0.004(5) -0.038(6) C25 0.044(6) 0.118(9) 0.057(6) -0.005(6) -0.001(4) -0.029(6) C26 0.029(5) 0.117(8) 0.055(5) 0.030(6) -0.004(4) 0.008(5) C27 0.051(5) 0.068(5) 0.045(4) 0.017(4) 0.015(4) 0.010(4) C28 0.031(4) 0.037(4) 0.015(3) 0.003(3) 0.002(3) 0.001(3) C29 0.052(5) 0.036(4) 0.038(4) 0.003(3) 0.020(3) -0.005(3) C30 0.061(5) 0.053(5) 0.044(4) 0.005(4) 0.023(4) -0.008(4) C31 0.043(5) 0.082(6) 0.031(4) 0.015(4) 0.017(3) -0.003(4) C32 0.043(4) 0.065(5) 0.021(3) -0.001(3) 0.012(3) 0.008(4) C33 0.042(4) 0.039(4) 0.028(3) -0.001(3) 0.008(3) -0.003(3) C34 0.034(4) 0.040(4) 0.022(3) 0.009(3) 0.010(3) 0.008(3) C35 0.037(4) 0.044(4) 0.033(4) 0.007(3) 0.007(3) 0.007(3) C36 0.040(4) 0.051(5) 0.026(3) 0.006(3) 0.006(3) 0.007(4) C37 0.062(6) 0.096(7) 0.069(6) 0.028(5) 0.037(5) 0.021(5) C38 0.081(7) 0.108(9) 0.102(8) 0.045(7) 0.060(6) 0.050(7) C39 0.066(7) 0.096(8) 0.087(7) 0.010(6) 0.037(5) 0.039(6) C40 0.078(7) 0.083(8) 0.125(9) 0.016(6) 0.042(7) 0.026(6) C41 0.057(6) 0.054(6) 0.092(7) -0.006(5) 0.022(5) 0.012(4) C42 0.037(4) 0.044(4) 0.021(3) 0.011(3) 0.003(3) 0.014(3) C43 0.041(4) 0.044(4) 0.039(4) 0.009(3) 0.011(3) 0.001(3) C44 0.068(5) 0.039(4) 0.029(4) 0.003(3) 0.012(4) 0.000(4) C45 0.084(6) 0.040(4) 0.040(4) 0.011(3) 0.035(4) 0.004(4) C46 0.045(4) 0.043(4) 0.051(5) 0.007(4) 0.019(4) -0.007(4) C47 0.047(4) 0.041(4) 0.024(3) 0.003(3) 0.003(3) 0.003(3) C48 0.031(4) 0.044(5) 0.031(4) -0.003(3) 0.009(3) -0.004(3) C49 0.032(4) 0.046(4) 0.047(4) -0.005(3) 0.023(3) -0.002(3) C50 0.028(4) 0.046(4) 0.049(4) 0.006(3) 0.017(3) 0.004(3) C51 0.041(5) 0.071(6) 0.049(5) 0.008(4) 0.014(4) 0.002(4) C52 0.069(6) 0.093(7) 0.053(5) 0.026(5) 0.007(5) -0.030(6) C53 0.053(6) 0.062(7) 0.148(11) 0.050(7) 0.013(7) 0.010(5) C54 0.050(6) 0.072(7) 0.117(9) 0.014(7) 0.022(6) 0.022(5) C55 0.055(5) 0.054(5) 0.092(7) 0.000(5) 0.033(5) -0.002(4) C56 0.023(3) 0.046(4) 0.033(3) -0.005(3) 0.016(3) -0.003(3) C57 0.049(5) 0.053(5) 0.039(4) 0.001(4) 0.022(4) 0.000(4) C58 0.054(5) 0.059(5) 0.053(5) 0.010(4) 0.020(4) -0.006(4) C59 0.050(5) 0.061(5) 0.055(5) 0.023(4) 0.030(4) 0.004(4) C60 0.061(6) 0.101(7) 0.044(5) 0.014(5) 0.020(4) 0.010(5) C61 0.047(5) 0.061(5) 0.044(4) -0.003(4) 0.016(4) -0.010(4) C62 0.044(4) 0.019(3) 0.025(3) 0.002(3) 0.020(3) 0.004(3) C63 0.040(4) 0.023(3) 0.035(4) -0.002(3) 0.010(3) -0.001(3) C64 0.042(4) 0.026(4) 0.032(3) -0.008(3) 0.018(3) -0.001(3) C65 0.080(6) 0.034(4) 0.043(4) -0.007(3) 0.031(4) -0.004(4) C66 0.118(8) 0.046(5) 0.037(4) -0.012(4) 0.031(5) -0.001(5) C67 0.113(8) 0.079(7) 0.035(4) -0.015(5) 0.030(5) 0.022(6) C68 0.075(6) 0.050(5) 0.054(5) -0.030(4) 0.009(5) 0.002(4) C69 0.053(5) 0.038(4) 0.039(4) -0.012(3) 0.013(3) -0.010(3) C70 0.063(5) 0.023(4) 0.031(4) -0.008(3) 0.013(4) -0.006(3) C71 0.080(6) 0.043(5) 0.042(4) -0.005(4) 0.012(4) 0.001(4) C72 0.119(9) 0.056(6) 0.068(6) -0.003(5) 0.055(7) -0.028(6) C73 0.084(7) 0.084(7) 0.052(5) 0.009(5) 0.025(5) -0.020(5) C74 0.069(6) 0.050(5) 0.048(5) 0.002(4) 0.021(4) -0.010(4) C75 0.127(9) 0.046(5) 0.041(5) 0.015(4) 0.021(6) -0.004(6) C80 0.056(5) 0.120(8) 0.043(5) 0.005(5) 0.025(4) 0.019(5) C81 0.065(7) 0.199(13) 0.033(5) 0.021(7) 0.022(5) 0.018(7) C82 0.065(7) 0.160(12) 0.092(9) 0.081(9) 0.025(6) 0.011(7) C83 0.061(6) 0.074(7) 0.101(8) 0.040(6) 0.019(6) 0.002(5) C84 0.054(6) 0.095(8) 0.090(7) -0.012(6) 0.015(6) -0.030(6) C85 0.053(6) 0.142(10) 0.054(6) -0.012(6) 0.019(5) -0.038(7) C86 0.038(5) 0.171(11) 0.040(5) 0.016(6) 0.020(4) 0.016(6) N1 0.075(5) 0.047(4) 0.068(4) 0.014(3) 0.040(4) -0.003(4) C87 0.053(5) 0.055(5) 0.042(4) 0.013(4) 0.022(4) -0.002(4) C88 0.096(7) 0.096(7) 0.058(6) 0.021(5) 0.031(5) -0.031(6) N2 0.076(5) 0.029(4) 0.073(5) -0.014(3) 0.022(4) -0.010(3) C89 0.073(6) 0.039(5) 0.054(5) -0.010(4) 0.020(5) -0.005(4) C90 0.105(8) 0.078(7) 0.086(7) -0.017(5) 0.060(6) -0.015(6) N3 0.075(6) 0.121(8) 0.069(5) 0.016(5) 0.021(4) 0.032(5) C91 0.046(5) 0.114(9) 0.038(5) 0.001(5) 0.016(4) 0.030(6) C92 0.064(6) 0.114(8) 0.045(5) -0.002(5) 0.022(4) 0.026(5) _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 1.912(3) . ? Mn1 O6 1.915(3) 3_756 ? Mn1 O6 1.920(3) . ? Mn1 O5 1.921(3) . ? Mn1 O4 2.322(4) . ? Mn1 O2 2.332(4) . ? Mn1 Mn1 2.8566(15) 3_756 ? Mn1 Mn2 3.0991(12) . ? Mn1 Mn2 3.1124(11) 3_756 ? Mn1 Mn3 3.1422(12) . ? Mn1 Mn5 3.2060(12) . ? Mn2 O18 1.913(3) . ? Mn2 O3 1.924(3) . ? Mn2 O4 1.926(3) . ? Mn2 O2 1.941(3) 3_756 ? Mn2 O14 2.152(4) . ? Mn2 O6 2.227(4) . ? Mn2 Mn1 3.1124(11) 3_756 ? Mn2 Mn6 3.1632(12) . ? Mn3 O1 2.083(4) . ? Mn3 O10 2.087(4) . ? Mn3 O16 2.118(4) . ? Mn3 O8 2.132(4) . ? Mn3 O18 2.288(4) 3_756 ? Mn3 O6 2.462(3) 3_756 ? Mn3 Mn4 3.2293(12) . ? Mn4 O11 2.097(4) . ? Mn4 O7 2.131(4) . ? Mn4 O10 2.156(4) . ? Mn4 O12 2.181(4) . ? Mn4 O18 2.264(3) 3_756 ? Mn4 O3 2.309(3) 3_756 ? Mn5 O10 2.064(4) 3_756 ? Mn5 O5 2.074(3) . ? Mn5 O20 2.109(4) . ? Mn5 O19 2.126(4) . ? Mn5 O3 2.302(4) . ? Mn6 O13 2.190(4) . ? Mn6 O17 2.245(4) . ? Mn6 O4 2.247(4) . ? Mn6 O16 2.277(4) . ? Mn6 O2 2.298(3) 3_756 ? Mn6 O15 2.393(4) . ? Mn6 O20 2.422(4) 3_756 ? O1 C8 1.439(6) . ? O2 C7 1.439(6) . ? O2 Mn2 1.941(3) 3_756 ? O2 Mn6 2.298(3) 3_756 ? O3 C1 1.443(6) . ? O3 Mn4 2.309(3) 3_756 ? O4 C2 1.451(6) . ? O5 C3 1.425(6) . ? O6 Mn1 1.915(3) 3_756 ? O6 Mn3 2.462(3) 3_756 ? O7 C34 1.249(7) . ? O8 C34 1.275(7) . ? O10 Mn5 2.064(4) 3_756 ? O11 C48 1.248(7) . ? O12 H12A 0.8400 . ? O12 H12B 0.94(7) . ? O13 C62 1.256(7) . ? O14 C62 1.258(7) . ? O15 C20 1.242(7) . ? O16 C20 1.288(6) . ? O17 C13 1.240(7) . ? O18 C12 1.452(6) . ? O18 Mn4 2.264(3) 3_756 ? O18 Mn3 2.288(4) 3_756 ? O19 C48 1.281(7) 3_756 ? O20 C13 1.278(7) 3_756 ? O20 Mn6 2.422(4) 3_756 ? O21 C10 1.419(6) . ? O21 H21A 0.8400 . ? O22 C5 1.420(6) . ? O22 H22A 0.8400 . ? C1 C4 1.520(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C4 1.536(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.537(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.562(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C9 1.536(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.526(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.539(7) 3_756 ? C9 C10 1.550(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 C9 1.539(7) 3_756 ? C12 H12D 0.9900 . ? C12 H12C 0.9900 . ? C13 O20 1.278(7) 3_756 ? C13 C14 1.525(8) . ? C14 C16 1.519(8) . ? C14 C15 1.529(9) . ? C14 H14A 1.0000 . ? C15 C80 1.364(10) . ? C15 C19 1.382(10) . ? C16 C17 1.381(10) . ? C16 C18 1.395(10) . ? C17 C84 1.356(10) . ? C17 H17A 0.9500 . ? C18 C86 1.427(11) . ? C18 H18A 0.9500 . ? C19 C83 1.384(11) . ? C19 H19A 0.9500 . ? C20 C21 1.530(7) . ? C21 C22 1.520(8) . ? C21 C28 1.532(8) . ? C21 H21B 1.0000 . ? C22 C23 1.390(9) . ? C22 C27 1.408(9) . ? C23 C24 1.381(9) . ? C23 H23A 0.9500 . ? C24 C25 1.360(12) . ? C24 H24A 0.9500 . ? C25 C26 1.369(12) . ? C25 H25A 0.9500 . ? C26 C27 1.404(10) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C33 1.401(8) . ? C28 C29 1.403(8) . ? C29 C30 1.399(9) . ? C29 H29A 0.9500 . ? C30 C31 1.367(10) . ? C30 H30A 0.9500 . ? C31 C32 1.408(10) . ? C31 H31A 0.9500 . ? C32 C33 1.375(8) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.521(8) . ? C35 C36 1.501(9) . ? C35 C42 1.521(8) . ? C35 H35A 1.0000 . ? C36 C41 1.366(10) . ? C36 C37 1.369(9) . ? C37 C38 1.372(11) . ? C37 H37A 0.9500 . ? C38 C39 1.368(12) . ? C38 H38A 0.9500 . ? C39 C40 1.380(12) . ? C39 H39A 0.9500 . ? C40 C41 1.389(11) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C43 1.387(8) . ? C42 C47 1.389(9) . ? C43 C44 1.370(9) . ? C43 H43A 0.9500 . ? C44 C45 1.387(9) . ? C44 H44A 0.9500 . ? C45 C46 1.385(9) . ? C45 H45A 0.9500 . ? C46 C47 1.391(8) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 O19 1.281(7) 3_756 ? C48 C49 1.541(8) . ? C49 C50 1.501(9) . ? C49 C56 1.520(9) . ? C49 H49A 1.0000 . ? C50 C55 1.401(9) . ? C50 C51 1.406(9) . ? C51 C52 1.407(10) . ? C51 H51A 0.9500 . ? C52 C53 1.351(13) . ? C52 H52A 0.9500 . ? C53 C54 1.360(13) . ? C53 H53A 0.9500 . ? C54 C55 1.369(11) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? C56 C57 1.369(9) . ? C56 C61 1.374(8) . ? C57 C58 1.389(9) . ? C57 H57A 0.9500 . ? C58 C59 1.385(9) . ? C58 H58A 0.9500 . ? C59 C60 1.357(10) . ? C59 H59A 0.9500 . ? C60 C61 1.424(10) . ? C60 H60A 0.9500 . ? C61 H61A 0.9500 . ? C62 C63 1.534(8) . ? C63 C64 1.511(8) . ? C63 C70 1.511(9) . ? C63 H63A 1.0000 . ? C64 C69 1.389(8) . ? C64 C65 1.398(8) . ? C65 C66 1.365(9) . ? C65 H65A 0.9500 . ? C66 C67 1.380(11) . ? C66 H66A 0.9500 . ? C67 C68 1.366(11) . ? C67 H67A 0.9500 . ? C68 C69 1.384(9) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C70 C74 1.357(10) . ? C70 C71 1.398(9) . ? C71 C75 1.410(11) . ? C71 H71A 0.9500 . ? C72 C73 1.334(11) . ? C72 C75 1.376(12) . ? C72 H72A 0.9500 . ? C73 C74 1.395(10) . ? C73 H73A 0.9500 . ? C74 H74A 0.9500 . ? C75 H75A 0.9500 . ? C80 C81 1.390(11) . ? C80 H80A 0.9500 . ? C81 C82 1.336(14) . ? C81 H81A 0.9500 . ? C82 C83 1.360(14) . ? C82 H82A 0.9500 . ? C83 H83A 0.9500 . ? C84 C85 1.326(12) . ? C84 H84A 0.9500 . ? C85 C86 1.373(13) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? N1 C87 1.109(8) . ? C87 C88 1.457(10) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? N2 C89 1.132(9) . ? C89 C90 1.453(11) . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? N3 C91 1.145(11) . ? C91 C92 1.483(12) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? 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 O6 90.91(15) . 3_756 ? O1 Mn1 O6 174.58(15) . . ? O6 Mn1 O6 83.70(15) 3_756 . ? O1 Mn1 O5 93.22(15) . . ? O6 Mn1 O5 175.86(15) 3_756 . ? O6 Mn1 O5 92.17(15) . . ? O1 Mn1 O4 96.04(13) . . ? O6 Mn1 O4 91.33(14) 3_756 . ? O6 Mn1 O4 83.57(13) . . ? O5 Mn1 O4 87.88(14) . . ? O1 Mn1 O2 87.61(13) . . ? O6 Mn1 O2 83.55(13) 3_756 . ? O6 Mn1 O2 92.31(13) . . ? O5 Mn1 O2 96.97(14) . . ? O4 Mn1 O2 173.77(12) . . ? O1 Mn1 Mn1 132.83(11) . 3_756 ? O6 Mn1 Mn1 41.92(10) 3_756 3_756 ? O6 Mn1 Mn1 41.78(10) . 3_756 ? O5 Mn1 Mn1 133.95(11) . 3_756 ? O4 Mn1 Mn1 86.58(9) . 3_756 ? O2 Mn1 Mn1 87.24(9) . 3_756 ? O1 Mn1 Mn2 134.39(11) . . ? O6 Mn1 Mn2 91.23(11) 3_756 . ? O6 Mn1 Mn2 45.56(10) . . ? O5 Mn1 Mn2 85.62(11) . . ? O4 Mn1 Mn2 38.36(8) . . ? O2 Mn1 Mn2 137.85(9) . . ? Mn1 Mn1 Mn2 62.86(3) 3_756 . ? O1 Mn1 Mn2 85.83(11) . 3_756 ? O6 Mn1 Mn2 45.23(10) 3_756 3_756 ? O6 Mn1 Mn2 90.73(11) . 3_756 ? O5 Mn1 Mn2 135.48(11) . 3_756 ? O4 Mn1 Mn2 136.55(9) . 3_756 ? O2 Mn1 Mn2 38.51(9) . 3_756 ? Mn1 Mn1 Mn2 62.38(3) 3_756 3_756 ? Mn2 Mn1 Mn2 125.24(3) . 3_756 ? O1 Mn1 Mn3 40.11(10) . . ? O6 Mn1 Mn3 51.58(10) 3_756 . ? O6 Mn1 Mn3 134.49(11) . . ? O5 Mn1 Mn3 132.44(10) . . ? O4 Mn1 Mn3 88.88(9) . . ? O2 Mn1 Mn3 90.71(9) . . ? Mn1 Mn1 Mn3 93.13(4) 3_756 . ? Mn2 Mn1 Mn3 118.20(3) . . ? Mn2 Mn1 Mn3 65.14(3) 3_756 . ? O1 Mn1 Mn5 130.76(11) . . ? O6 Mn1 Mn5 137.69(10) 3_756 . ? O6 Mn1 Mn5 54.66(10) . . ? O5 Mn1 Mn5 38.31(10) . . ? O4 Mn1 Mn5 91.08(9) . . ? O2 Mn1 Mn5 90.33(9) . . ? Mn1 Mn1 Mn5 96.13(4) 3_756 . ? Mn2 Mn1 Mn5 66.11(3) . . ? Mn2 Mn1 Mn5 120.08(3) 3_756 . ? Mn3 Mn1 Mn5 170.72(3) . . ? O18 Mn2 O3 86.90(14) . . ? O18 Mn2 O4 173.64(16) . . ? O3 Mn2 O4 94.03(14) . . ? O18 Mn2 O2 93.76(14) . 3_756 ? O3 Mn2 O2 174.58(15) . 3_756 ? O4 Mn2 O2 84.73(14) . 3_756 ? O18 Mn2 O14 89.40(14) . . ? O3 Mn2 O14 89.38(14) . . ? O4 Mn2 O14 96.90(14) . . ? O2 Mn2 O14 96.00(14) 3_756 . ? O18 Mn2 O6 87.66(14) . . ? O3 Mn2 O6 88.80(14) . . ? O4 Mn2 O6 86.07(14) . . ? O2 Mn2 O6 85.86(14) 3_756 . ? O14 Mn2 O6 176.63(14) . . ? O18 Mn2 Mn1 125.43(11) . . ? O3 Mn2 Mn1 87.23(11) . . ? O4 Mn2 Mn1 48.43(11) . . ? O2 Mn2 Mn1 88.02(11) 3_756 . ? O14 Mn2 Mn1 144.70(10) . . ? O6 Mn2 Mn1 38.00(9) . . ? O18 Mn2 Mn1 87.43(10) . 3_756 ? O3 Mn2 Mn1 126.30(11) . 3_756 ? O4 Mn2 Mn1 86.95(10) . 3_756 ? O2 Mn2 Mn1 48.42(10) 3_756 3_756 ? O14 Mn2 Mn1 143.88(10) . 3_756 ? O6 Mn2 Mn1 37.62(9) . 3_756 ? Mn1 Mn2 Mn1 54.76(3) . 3_756 ? O18 Mn2 Mn6 136.42(11) . . ? O3 Mn2 Mn6 134.71(10) . . ? O4 Mn2 Mn6 44.67(11) . . ? O2 Mn2 Mn6 46.25(10) 3_756 . ? O14 Mn2 Mn6 80.44(10) . . ? O6 Mn2 Mn6 102.84(9) . . ? Mn1 Mn2 Mn6 77.27(3) . . ? Mn1 Mn2 Mn6 77.36(3) 3_756 . ? O1 Mn3 O10 156.49(14) . . ? O1 Mn3 O16 94.10(14) . . ? O10 Mn3 O16 94.25(15) . . ? O1 Mn3 O8 110.72(15) . . ? O10 Mn3 O8 87.54(15) . . ? O16 Mn3 O8 107.47(15) . . ? O1 Mn3 O18 82.78(13) . 3_756 ? O10 Mn3 O18 82.73(13) . 3_756 ? O16 Mn3 O18 162.69(13) . 3_756 ? O8 Mn3 O18 89.47(14) . 3_756 ? O1 Mn3 O6 73.22(12) . 3_756 ? O10 Mn3 O6 85.10(13) . 3_756 ? O16 Mn3 O6 88.37(13) . 3_756 ? O8 Mn3 O6 163.00(14) . 3_756 ? O18 Mn3 O6 74.41(12) 3_756 3_756 ? O1 Mn3 Mn1 36.26(9) . . ? O10 Mn3 Mn1 122.63(10) . . ? O16 Mn3 Mn1 86.63(11) . . ? O8 Mn3 Mn1 146.27(11) . . ? O18 Mn3 Mn1 80.81(9) 3_756 . ? O6 Mn3 Mn1 37.54(8) 3_756 . ? O1 Mn3 Mn4 127.28(10) . . ? O10 Mn3 Mn4 41.25(10) . . ? O16 Mn3 Mn4 135.47(11) . . ? O8 Mn3 Mn4 75.51(11) . . ? O18 Mn3 Mn4 44.50(9) 3_756 . ? O6 Mn3 Mn4 88.93(8) 3_756 . ? Mn1 Mn3 Mn4 115.92(3) . . ? O11 Mn4 O7 111.37(16) . . ? O11 Mn4 O10 91.24(15) . . ? O7 Mn4 O10 88.86(15) . . ? O11 Mn4 O12 98.40(17) . . ? O7 Mn4 O12 98.38(16) . . ? O10 Mn4 O12 164.83(16) . . ? O11 Mn4 O18 156.18(15) . 3_756 ? O7 Mn4 O18 91.35(14) . 3_756 ? O10 Mn4 O18 81.82(13) . 3_756 ? O12 Mn4 O18 84.69(15) . 3_756 ? O11 Mn4 O3 85.93(14) . 3_756 ? O7 Mn4 O3 159.92(14) . 3_756 ? O10 Mn4 O3 80.36(13) . 3_756 ? O12 Mn4 O3 88.63(14) . 3_756 ? O18 Mn4 O3 70.48(12) 3_756 3_756 ? O11 Mn4 Mn3 130.82(12) . . ? O7 Mn4 Mn3 77.83(11) . . ? O10 Mn4 Mn3 39.67(10) . . ? O12 Mn4 Mn3 128.95(12) . . ? O18 Mn4 Mn3 45.12(9) 3_756 . ? O3 Mn4 Mn3 83.12(9) 3_756 . ? O10 Mn5 O5 151.72(15) 3_756 . ? O10 Mn5 O20 95.01(15) 3_756 . ? O5 Mn5 O20 91.17(15) . . ? O10 Mn5 O19 90.31(15) 3_756 . ? O5 Mn5 O19 112.57(15) . . ? O20 Mn5 O19 112.88(17) . . ? O10 Mn5 O3 82.47(13) 3_756 . ? O5 Mn5 O3 81.64(13) . . ? O20 Mn5 O3 158.16(15) . . ? O19 Mn5 O3 88.87(14) . . ? O10 Mn5 Mn1 118.47(11) 3_756 . ? O5 Mn5 Mn1 35.04(9) . . ? O20 Mn5 Mn1 83.42(12) . . ? O19 Mn5 Mn1 146.34(11) . . ? O3 Mn5 Mn1 78.87(9) . . ? O13 Mn6 O17 86.55(15) . . ? O13 Mn6 O4 90.18(14) . . ? O17 Mn6 O4 173.54(15) . . ? O13 Mn6 O16 138.88(14) . . ? O17 Mn6 O16 103.71(15) . . ? O4 Mn6 O16 82.38(13) . . ? O13 Mn6 O2 88.07(13) . 3_756 ? O17 Mn6 O2 104.33(14) . 3_756 ? O4 Mn6 O2 69.96(12) . 3_756 ? O16 Mn6 O2 125.86(13) . 3_756 ? O13 Mn6 O15 85.37(14) . . ? O17 Mn6 O15 88.42(15) . . ? O4 Mn6 O15 96.88(13) . . ? O16 Mn6 O15 55.84(13) . . ? O2 Mn6 O15 165.29(14) 3_756 . ? O13 Mn6 O20 133.51(15) . 3_756 ? O17 Mn6 O20 55.25(15) . 3_756 ? O4 Mn6 O20 124.73(14) . 3_756 ? O16 Mn6 O20 80.99(14) . 3_756 ? O2 Mn6 O20 78.49(13) 3_756 3_756 ? O15 Mn6 O20 115.38(14) . 3_756 ? O13 Mn6 Mn2 75.00(10) . . ? O17 Mn6 Mn2 136.50(12) . . ? O4 Mn6 Mn2 37.06(9) . . ? O16 Mn6 Mn2 116.17(10) . . ? O2 Mn6 Mn2 37.59(9) 3_756 . ? O15 Mn6 Mn2 127.74(11) . . ? O20 Mn6 Mn2 113.12(10) 3_756 . ? C8 O1 Mn1 122.9(3) . . ? C8 O1 Mn3 118.1(3) . . ? Mn1 O1 Mn3 103.63(15) . . ? C7 O2 Mn2 121.3(3) . 3_756 ? C7 O2 Mn6 114.1(3) . 3_756 ? Mn2 O2 Mn6 96.16(13) 3_756 3_756 ? C7 O2 Mn1 113.9(3) . . ? Mn2 O2 Mn1 93.07(14) 3_756 . ? Mn6 O2 Mn1 115.81(15) 3_756 . ? C1 O3 Mn2 117.9(3) . . ? C1 O3 Mn5 111.6(3) . . ? Mn2 O3 Mn5 108.69(15) . . ? C1 O3 Mn4 124.9(3) . 3_756 ? Mn2 O3 Mn4 99.93(14) . 3_756 ? Mn5 O3 Mn4 89.81(12) . 3_756 ? C2 O4 Mn2 121.9(3) . . ? C2 O4 Mn6 111.3(3) . . ? Mn2 O4 Mn6 98.27(14) . . ? C2 O4 Mn1 113.1(3) . . ? Mn2 O4 Mn1 93.21(13) . . ? Mn6 O4 Mn1 117.68(15) . . ? C3 O5 Mn1 122.8(3) . . ? C3 O5 Mn5 115.9(3) . . ? Mn1 O5 Mn5 106.65(15) . . ? Mn1 O6 Mn1 96.30(15) 3_756 . ? Mn1 O6 Mn2 97.15(14) 3_756 . ? Mn1 O6 Mn2 96.44(14) . . ? Mn1 O6 Mn3 90.88(13) 3_756 3_756 ? Mn1 O6 Mn3 168.42(18) . 3_756 ? Mn2 O6 Mn3 91.65(12) . 3_756 ? C34 O7 Mn4 127.6(4) . . ? C34 O8 Mn3 130.3(4) . . ? Mn5 O10 Mn3 108.58(16) 3_756 . ? Mn5 O10 Mn4 100.90(15) 3_756 . ? Mn3 O10 Mn4 99.08(15) . . ? C48 O11 Mn4 131.6(4) . . ? Mn4 O12 H12A 109.5 . . ? Mn4 O12 H12B 132(4) . . ? H12A O12 H12B 108.4 . . ? C62 O13 Mn6 132.1(4) . . ? C62 O14 Mn2 126.3(4) . . ? C20 O15 Mn6 90.1(3) . . ? C20 O16 Mn3 138.7(4) . . ? C20 O16 Mn6 94.3(3) . . ? Mn3 O16 Mn6 125.54(17) . . ? C13 O17 Mn6 97.5(4) . . ? C12 O18 Mn2 119.8(3) . . ? C12 O18 Mn4 122.9(3) . 3_756 ? Mn2 O18 Mn4 101.85(14) . 3_756 ? C12 O18 Mn3 111.1(3) . 3_756 ? Mn2 O18 Mn3 106.18(15) . 3_756 ? Mn4 O18 Mn3 90.37(13) 3_756 3_756 ? C48 O19 Mn5 128.9(4) 3_756 . ? C13 O20 Mn5 145.2(4) 3_756 . ? C13 O20 Mn6 88.2(4) 3_756 3_756 ? Mn5 O20 Mn6 126.13(19) . 3_756 ? C10 O21 H21A 109.5 . . ? C5 O22 H22A 109.5 . . ? O3 C1 C4 113.9(4) . . ? O3 C1 H1A 108.8 . . ? C4 C1 H1A 108.8 . . ? O3 C1 H1B 108.8 . . ? C4 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? O4 C2 C4 113.3(4) . . ? O4 C2 H2A 108.9 . . ? C4 C2 H2A 108.9 . . ? O4 C2 H2B 108.9 . . ? C4 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O5 C3 C4 115.7(4) . . ? O5 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? O5 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C1 C4 C2 112.5(4) . . ? C1 C4 C3 113.4(5) . . ? C2 C4 C3 110.8(4) . . ? C1 C4 C5 107.7(4) . . ? C2 C4 C5 106.7(4) . . ? C3 C4 C5 105.2(4) . . ? O22 C5 C4 110.0(4) . . ? O22 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? O22 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O2 C7 C9 114.1(4) . . ? O2 C7 H7A 108.7 . . ? C9 C7 H7A 108.7 . . ? O2 C7 H7B 108.7 . . ? C9 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O1 C8 C9 114.9(4) . . ? O1 C8 H8A 108.5 . . ? C9 C8 H8A 108.5 . . ? O1 C8 H8B 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C8 C9 C7 111.7(4) . . ? C8 C9 C12 113.3(5) . 3_756 ? C7 C9 C12 111.5(4) . 3_756 ? C8 C9 C10 107.6(4) . . ? C7 C9 C10 105.8(4) . . ? C12 C9 C10 106.4(4) 3_756 . ? O21 C10 C9 114.4(4) . . ? O21 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? O21 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? O18 C12 C9 114.2(4) . 3_756 ? O18 C12 H12D 108.7 . . ? C9 C12 H12D 108.7 3_756 . ? O18 C12 H12C 108.7 . . ? C9 C12 H12C 108.7 3_756 . ? H12D C12 H12C 107.6 . . ? O17 C13 O20 119.0(6) . 3_756 ? O17 C13 C14 123.5(6) . . ? O20 C13 C14 117.5(6) 3_756 . ? C16 C14 C13 114.7(5) . . ? C16 C14 C15 112.5(6) . . ? C13 C14 C15 109.6(5) . . ? C16 C14 H14A 106.5 . . ? C13 C14 H14A 106.5 . . ? C15 C14 H14A 106.5 . . ? C80 C15 C19 118.9(8) . . ? C80 C15 C14 118.1(7) . . ? C19 C15 C14 123.1(7) . . ? C17 C16 C18 118.2(7) . . ? C17 C16 C14 123.9(7) . . ? C18 C16 C14 117.8(7) . . ? C84 C17 C16 123.2(9) . . ? C84 C17 H17A 118.4 . . ? C16 C17 H17A 118.4 . . ? C16 C18 C86 118.4(8) . . ? C16 C18 H18A 120.8 . . ? C86 C18 H18A 120.8 . . ? C15 C19 C83 119.9(9) . . ? C15 C19 H19A 120.1 . . ? C83 C19 H19A 120.1 . . ? O15 C20 O16 119.8(5) . . ? O15 C20 C21 123.8(5) . . ? O16 C20 C21 116.3(5) . . ? C22 C21 C20 114.4(5) . . ? C22 C21 C28 111.7(4) . . ? C20 C21 C28 109.4(4) . . ? C22 C21 H21B 107.0 . . ? C20 C21 H21B 107.0 . . ? C28 C21 H21B 107.0 . . ? C23 C22 C27 117.4(6) . . ? C23 C22 C21 123.6(6) . . ? C27 C22 C21 118.9(6) . . ? C24 C23 C22 120.4(8) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 122.6(9) . . ? C25 C24 H24A 118.7 . . ? C23 C24 H24A 118.7 . . ? C24 C25 C26 118.4(8) . . ? C24 C25 H25A 120.8 . . ? C26 C25 H25A 120.8 . . ? C25 C26 C27 120.9(8) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? C26 C27 C22 120.2(8) . . ? C26 C27 H27A 119.9 . . ? C22 C27 H27A 119.9 . . ? C33 C28 C29 119.5(6) . . ? C33 C28 C21 122.6(5) . . ? C29 C28 C21 117.9(5) . . ? C30 C29 C28 119.5(6) . . ? C30 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? C31 C30 C29 120.4(7) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C30 C31 C32 120.4(7) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C33 C32 C31 119.8(7) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C32 C33 C28 120.3(6) . . ? C32 C33 H33A 119.8 . . ? C28 C33 H33A 119.8 . . ? O7 C34 O8 125.8(5) . . ? O7 C34 C35 119.8(6) . . ? O8 C34 C35 114.3(5) . . ? C36 C35 C42 113.7(5) . . ? C36 C35 C34 113.4(5) . . ? C42 C35 C34 113.1(5) . . ? C36 C35 H35A 105.2 . . ? C42 C35 H35A 105.2 . . ? C34 C35 H35A 105.2 . . ? C41 C36 C37 116.9(8) . . ? C41 C36 C35 121.4(7) . . ? C37 C36 C35 121.7(7) . . ? C36 C37 C38 123.2(9) . . ? C36 C37 H37A 118.4 . . ? C38 C37 H37A 118.4 . . ? C39 C38 C37 118.3(9) . . ? C39 C38 H38A 120.8 . . ? C37 C38 H38A 120.8 . . ? C38 C39 C40 121.0(9) . . ? C38 C39 H39A 119.5 . . ? C40 C39 H39A 119.5 . . ? C39 C40 C41 118.1(10) . . ? C39 C40 H40A 121.0 . . ? C41 C40 H40A 121.0 . . ? C36 C41 C40 122.5(9) . . ? C36 C41 H41A 118.8 . . ? C40 C41 H41A 118.8 . . ? C43 C42 C47 118.8(6) . . ? C43 C42 C35 119.0(6) . . ? C47 C42 C35 122.1(6) . . ? C44 C43 C42 120.7(7) . . ? C44 C43 H43A 119.7 . . ? C42 C43 H43A 119.7 . . ? C43 C44 C45 120.7(7) . . ? C43 C44 H44A 119.7 . . ? C45 C44 H44A 119.7 . . ? C46 C45 C44 119.4(6) . . ? C46 C45 H45A 120.3 . . ? C44 C45 H45A 120.3 . . ? C45 C46 C47 119.7(7) . . ? C45 C46 H46A 120.1 . . ? C47 C46 H46A 120.1 . . ? C42 C47 C46 120.6(6) . . ? C42 C47 H47A 119.7 . . ? C46 C47 H47A 119.7 . . ? O11 C48 O19 126.3(6) . 3_756 ? O11 C48 C49 114.9(6) . . ? O19 C48 C49 118.7(6) 3_756 . ? C50 C49 C56 114.6(5) . . ? C50 C49 C48 110.6(5) . . ? C56 C49 C48 112.1(5) . . ? C50 C49 H49A 106.3 . . ? C56 C49 H49A 106.3 . . ? C48 C49 H49A 106.3 . . ? C55 C50 C51 117.8(7) . . ? C55 C50 C49 120.1(7) . . ? C51 C50 C49 122.1(6) . . ? C50 C51 C52 118.8(8) . . ? C50 C51 H51A 120.6 . . ? C52 C51 H51A 120.6 . . ? C53 C52 C51 120.8(9) . . ? C53 C52 H52A 119.6 . . ? C51 C52 H52A 119.6 . . ? C52 C53 C54 121.4(10) . . ? C52 C53 H53A 119.3 . . ? C54 C53 H53A 119.3 . . ? C53 C54 C55 119.4(9) . . ? C53 C54 H54A 120.3 . . ? C55 C54 H54A 120.3 . . ? C54 C55 C50 121.8(9) . . ? C54 C55 H55A 119.1 . . ? C50 C55 H55A 119.1 . . ? C57 C56 C61 119.1(6) . . ? C57 C56 C49 122.1(6) . . ? C61 C56 C49 118.8(6) . . ? C56 C57 C58 121.1(7) . . ? C56 C57 H57A 119.4 . . ? C58 C57 H57A 119.4 . . ? C59 C58 C57 120.3(7) . . ? C59 C58 H58A 119.9 . . ? C57 C58 H58A 119.9 . . ? C60 C59 C58 119.2(7) . . ? C60 C59 H59A 120.4 . . ? C58 C59 H59A 120.4 . . ? C59 C60 C61 120.4(7) . . ? C59 C60 H60A 119.8 . . ? C61 C60 H60A 119.8 . . ? C56 C61 C60 119.8(7) . . ? C56 C61 H61A 120.1 . . ? C60 C61 H61A 120.1 . . ? O13 C62 O14 125.9(5) . . ? O13 C62 C63 118.4(6) . . ? O14 C62 C63 115.6(5) . . ? C64 C63 C70 117.1(5) . . ? C64 C63 C62 112.7(5) . . ? C70 C63 C62 107.0(5) . . ? C64 C63 H63A 106.4 . . ? C70 C63 H63A 106.4 . . ? C62 C63 H63A 106.4 . . ? C69 C64 C65 117.0(6) . . ? C69 C64 C63 122.6(6) . . ? C65 C64 C63 120.1(6) . . ? C66 C65 C64 122.3(7) . . ? C66 C65 H65A 118.9 . . ? C64 C65 H65A 118.9 . . ? C65 C66 C67 118.4(7) . . ? C65 C66 H66A 120.8 . . ? C67 C66 H66A 120.8 . . ? C68 C67 C66 122.0(7) . . ? C68 C67 H67A 119.0 . . ? C66 C67 H67A 119.0 . . ? C67 C68 C69 118.5(8) . . ? C67 C68 H68A 120.7 . . ? C69 C68 H68A 120.7 . . ? C68 C69 C64 121.8(7) . . ? C68 C69 H69A 119.1 . . ? C64 C69 H69A 119.1 . . ? C74 C70 C71 118.2(7) . . ? C74 C70 C63 122.9(6) . . ? C71 C70 C63 118.7(7) . . ? C70 C71 C75 119.8(8) . . ? C70 C71 H71A 120.1 . . ? C75 C71 H71A 120.1 . . ? C73 C72 C75 120.3(8) . . ? C73 C72 H72A 119.9 . . ? C75 C72 H72A 119.9 . . ? C72 C73 C74 120.7(9) . . ? C72 C73 H73A 119.7 . . ? C74 C73 H73A 119.7 . . ? C70 C74 C73 121.4(8) . . ? C70 C74 H74A 119.3 . . ? C73 C74 H74A 119.3 . . ? C72 C75 C71 119.5(8) . . ? C72 C75 H75A 120.2 . . ? C71 C75 H75A 120.2 . . ? C15 C80 C81 119.2(9) . . ? C15 C80 H80A 120.4 . . ? C81 C80 H80A 120.4 . . ? C82 C81 C80 122.7(10) . . ? C82 C81 H81A 118.7 . . ? C80 C81 H81A 118.7 . . ? C81 C82 C83 118.2(10) . . ? C81 C82 H82A 120.9 . . ? C83 C82 H82A 120.9 . . ? C82 C83 C19 121.2(10) . . ? C82 C83 H83A 119.4 . . ? C19 C83 H83A 119.4 . . ? C85 C84 C17 118.5(10) . . ? C85 C84 H84A 120.8 . . ? C17 C84 H84A 120.8 . . ? C84 C85 C86 123.3(9) . . ? C84 C85 H85A 118.4 . . ? C86 C85 H85A 118.4 . . ? C85 C86 C18 118.5(9) . . ? C85 C86 H86A 120.8 . . ? C18 C86 H86A 120.8 . . ? N1 C87 C88 178.8(9) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? N2 C89 C90 179.0(9) . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N3 C91 C92 176.9(10) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.609 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.157 # Attachment 'Mn12 thme Muralee CIF 3 (Dalton).txt' data_xm57 _database_code_depnum_ccdc_archive 'CCDC 290614' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H92 Mn12 N4 Na2 O46' _chemical_formula_weight 2226.57 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' Na Na 0.0362 0.0249 '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 11.5832(6) _cell_length_b 13.4283(8) _cell_length_c 14.0099(8) _cell_angle_alpha 103.462(2) _cell_angle_beta 97.904(2) _cell_angle_gamma 90.706(2) _cell_volume 2096.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 111 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.846 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6234 _exptl_absorpt_correction_T_max 0.8574 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 18537 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9283 _reflns_number_gt 8239 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+4.9407P] 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 9283 _refine_ls_number_parameters 556 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.075 _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 0.60978(4) 0.99155(3) 0.96508(3) 0.01454(11) Uani 1 1 d . . . Mn2 Mn 0.40688(4) 1.07953(3) 0.83935(3) 0.01515(11) Uani 1 1 d . . . Mn3 Mn 0.49973(4) 0.84538(4) 0.76348(4) 0.01871(12) Uani 1 1 d . . . Mn4 Mn 0.29349(4) 0.93203(4) 0.62921(4) 0.02072(12) Uani 1 1 d . . . Mn5 Mn 0.23795(5) 0.86185(4) 0.83878(4) 0.02147(12) Uani 1 1 d . . . Mn6 Mn 0.48555(4) 0.73937(4) 0.98420(4) 0.01839(12) Uani 1 1 d . . . Na Na 0.5000 1.5000 1.0000 0.0253(4) Uani 1 2 d S . . O1 O 0.56365(19) 1.13073(16) 0.90136(16) 0.0158(4) Uani 1 1 d . . . O2 O 0.65455(19) 0.92610(16) 0.83949(16) 0.0177(4) Uani 1 1 d . . . O3 O 0.45000(18) 0.94697(16) 0.91362(16) 0.0154(4) Uani 1 1 d . . . O4 O 0.76497(19) 1.03715(16) 1.02446(16) 0.0177(4) Uani 1 1 d . . . O5 O 0.63664(19) 0.85210(16) 1.03466(16) 0.0158(4) Uani 1 1 d . . . O6 O 0.3694(2) 1.20874(18) 0.77372(18) 0.0237(5) Uani 1 1 d . . . O7 O 0.46004(19) 0.99875(17) 0.72315(16) 0.0175(4) Uani 1 1 d . B . O8 O 0.3184(2) 0.81341(17) 0.71336(17) 0.0206(5) Uani 1 1 d . B . H8C H 0.2964 0.7417 0.6744 0.025 Uiso 0.50 1 calc PR A 11 O9 O 0.5317(2) 0.72187(18) 0.83345(18) 0.0246(5) Uani 1 1 d . B . O10 O 0.5389(2) 0.78832(19) 0.61732(18) 0.0267(5) Uani 1 1 d . B . O11 O 0.2826(11) 1.0796(8) 0.5967(6) 0.044(3) Uani 0.50 1 d P B 3 O11' O 0.2697(7) 1.0564(8) 0.5592(6) 0.036(2) Uani 0.50 1 d P B 4 O12 O 0.3916(2) 0.84085(19) 0.52239(17) 0.0261(5) Uani 1 1 d . B . O13 O 0.1206(3) 0.8794(3) 0.5696(3) 0.0453(8) Uani 1 1 d . B . H13D H 0.072(6) 0.845(5) 0.607(5) 0.08(2) Uiso 1 1 d . . . H13E H 0.070(7) 0.888(6) 0.527(6) 0.10(3) Uiso 1 1 d . . . O14 O 0.3007(2) 0.74196(18) 0.90693(19) 0.0257(5) Uani 1 1 d . B . O15 O 0.0597(3) 0.8217(2) 0.8085(2) 0.0400(7) Uani 1 1 d . B . O16 O 0.3424(2) 0.6100(2) 0.9681(2) 0.0345(6) Uani 1 1 d . . . O17 O 0.74522(19) 0.98609(17) 1.21186(16) 0.0177(4) Uani 1 1 d . . . O18 O 0.7243(2) 1.2025(2) 0.6693(2) 0.0285(6) Uani 1 1 d . B . H18 H 0.697(5) 1.182(4) 0.613(4) 0.054(16) Uiso 1 1 d . . . O19 O 0.0730(8) 1.0479(10) 0.5095(10) 0.238(6) Uani 1 1 d . B 4 O20 O 0.5633(3) 0.5794(2) 0.8804(2) 0.0374(7) Uani 1 1 d . . . O21 O 0.9776(3) 0.7462(2) 1.1167(2) 0.0347(6) Uani 1 1 d . B . H21 H 0.945(4) 0.695(3) 1.083(3) 0.018(10) Uiso 1 1 d . . . O22 O 0.4416(2) 1.33625(18) 0.90134(18) 0.0266(5) Uani 1 1 d . . . O23 O -0.0343(8) 0.8219(11) 0.6635(8) 0.099(4) Uani 0.50 1 d P B . O24 O 0.0306(9) 0.7384(8) 0.6547(6) 0.073(3) Uani 0.50 1 d P B . C1 C 0.6480(3) 1.1571(2) 0.8437(2) 0.0199(6) Uani 1 1 d . . . H1A H 0.7237 1.1760 0.8872 0.024 Uiso 1 1 calc R . . H1B H 0.6224 1.2180 0.8194 0.024 Uiso 1 1 calc R . . C2 C 0.7220(3) 0.9783(3) 0.7873(2) 0.0206(6) Uani 1 1 d . . . H2A H 0.7398 0.9286 0.7275 0.025 Uiso 1 1 calc R . . H2B H 0.7971 1.0026 0.8300 0.025 Uiso 1 1 calc R . . C3 C 0.5522(3) 1.0405(2) 0.6819(2) 0.0196(6) Uani 1 1 d . . . H3A H 0.5243 1.1019 0.6597 0.024 Uiso 1 1 calc R B . H3B H 0.5690 0.9892 0.6228 0.024 Uiso 1 1 calc R . . C4 C 0.6657(3) 1.0703(2) 0.7546(2) 0.0187(6) Uani 1 1 d . B . C5 C 0.7562(3) 1.1114(3) 0.6994(3) 0.0246(7) Uani 1 1 d . . . H5A H 0.8321 1.1249 0.7434 0.030 Uiso 1 1 calc R B . H5B H 0.7670 1.0577 0.6401 0.030 Uiso 1 1 calc R . . C6 C 0.8594(3) 0.9697(2) 1.0232(2) 0.0201(6) Uani 1 1 d . . . H6A H 0.9325 1.0113 1.0517 0.024 Uiso 1 1 calc R . . H6B H 0.8658 0.9369 0.9532 0.024 Uiso 1 1 calc R . . C7 C 0.7491(3) 0.8087(2) 1.0291(2) 0.0188(6) Uani 1 1 d . . . H7A H 0.7579 0.7822 0.9585 0.023 Uiso 1 1 calc R B . H7B H 0.7529 0.7499 1.0608 0.023 Uiso 1 1 calc R . . C8 C 0.8459(3) 0.9267(3) 1.1903(2) 0.0208(6) Uani 1 1 d . . . H8A H 0.8459 0.8682 1.2222 0.025 Uiso 1 1 calc R B . H8B H 0.9173 0.9701 1.2203 0.025 Uiso 1 1 calc R . . C9 C 0.8507(3) 0.8852(2) 1.0791(2) 0.0197(6) Uani 1 1 d . B . C10 C 0.9655(3) 0.8288(3) 1.0692(3) 0.0256(7) Uani 1 1 d . . . H10A H 0.9703 0.8021 0.9978 0.031 Uiso 1 1 calc R B . H10B H 1.0319 0.8789 1.0972 0.031 Uiso 1 1 calc R . . C11 C 0.3840(3) 1.3028(3) 0.8169(2) 0.0225(7) Uani 1 1 d . . . C12 C 0.3275(4) 1.3790(3) 0.7642(3) 0.0387(10) Uani 1 1 d . . . H12A H 0.2589 1.4048 0.7944 0.058 Uiso 1 1 calc R . . H12B H 0.3034 1.3457 0.6941 0.058 Uiso 1 1 calc R . . H12C H 0.3832 1.4363 0.7698 0.058 Uiso 1 1 calc R . . C13 C 0.2839(6) 0.7081(5) 0.6607(5) 0.0208(13) Uiso 0.50 1 d P B 12 H13A H 0.3146 0.6614 0.7014 0.031 Uiso 0.50 1 calc PR B 12 H13B H 0.3154 0.6921 0.5977 0.031 Uiso 0.50 1 calc PR B 12 H13C H 0.1986 0.7001 0.6477 0.031 Uiso 0.50 1 calc PR B 12 C14 C 0.5600(3) 0.6275(3) 0.8153(3) 0.0230(7) Uani 1 1 d . . . C15 C 0.5856(5) 0.5785(3) 0.7134(3) 0.0450(11) Uani 1 1 d . B . H15A H 0.6688 0.5652 0.7162 0.067 Uiso 1 1 calc R . . H15B H 0.5651 0.6245 0.6693 0.067 Uiso 1 1 calc R . . H15C H 0.5395 0.5137 0.6879 0.067 Uiso 1 1 calc R . . C16 C 0.4768(3) 0.7847(3) 0.5352(3) 0.0255(7) Uani 1 1 d . . . C17 C 0.5057(5) 0.7076(4) 0.4463(3) 0.0493(12) Uani 1 1 d . B . H17A H 0.5632 0.6616 0.4679 0.074 Uiso 1 1 calc R . . H17B H 0.5381 0.7434 0.4017 0.074 Uiso 1 1 calc R . . H17C H 0.4347 0.6677 0.4113 0.074 Uiso 1 1 calc R . . C18 C 0.1851(10) 1.0925(8) 0.5225(8) 0.115(3) Uiso 1 1 d . . . C19 C 0.2319(9) 1.1873(7) 0.4566(7) 0.042(2) Uiso 0.50 1 d P B 21 H19A H 0.2319 1.2534 0.5044 0.063 Uiso 0.50 1 d PR B 21 H19B H 0.1757 1.1869 0.3975 0.063 Uiso 0.50 1 d PR B 21 H19C H 0.3101 1.1767 0.4378 0.063 Uiso 0.50 1 d PR B 21 C19' C 0.1904(11) 1.1911(9) 0.4880(10) 0.060(3) Uiso 0.50 1 d P B 22 H20G H 0.1412 1.2405 0.5214 0.090 Uiso 0.50 1 d PR B 22 H20H H 0.2702 1.2166 0.5050 0.090 Uiso 0.50 1 d PR B 22 H20I H 0.1678 1.1792 0.4176 0.090 Uiso 0.50 1 d PR B 22 C20 C 0.2707(3) 0.6554(3) 0.9210(3) 0.0230(7) Uani 1 1 d . . . C21 C 0.1493(4) 0.6114(3) 0.8816(4) 0.0427(11) Uani 1 1 d . B . H21A H 0.1387 0.5466 0.9009 0.064 Uiso 1 1 calc R . . H21B H 0.1370 0.5989 0.8091 0.064 Uiso 1 1 calc R . . H21C H 0.0929 0.6598 0.9090 0.064 Uiso 1 1 calc R . . C22 C -0.0135(5) 0.7803(5) 0.7401(4) 0.0553(14) Uani 1 1 d . . . C23 C -0.1223(4) 0.7289(4) 0.7565(4) 0.0509(12) Uani 1 1 d . B . H22A H -0.1022 0.6866 0.8042 0.076 Uiso 1 1 calc R . . H22B H -0.1602 0.6855 0.6934 0.076 Uiso 1 1 calc R . . H22C H -0.1757 0.7811 0.7826 0.076 Uiso 1 1 calc R . . N1 N 0.264(2) 0.6195(18) 0.6110(17) 0.162(8) Uiso 0.50 1 d PD C 11 C24 C 0.278(4) 0.550(3) 0.547(3) 0.35(3) Uiso 0.50 1 d PD C 11 C25 C 0.210(2) 0.4719(19) 0.4934(19) 0.157(9) Uiso 0.50 1 d PD C 11 H25A H 0.1413 0.4648 0.5258 0.236 Uiso 0.50 1 calc PR C 11 H25B H 0.2529 0.4089 0.4868 0.236 Uiso 0.50 1 calc PR C 11 H25C H 0.1843 0.4838 0.4275 0.236 Uiso 0.50 1 calc PR C 11 N2 N 0.021(3) 0.5458(18) 0.339(3) 0.279(17) Uiso 0.50 1 d PD . . C26 C 0.024(2) 0.6344(16) 0.351(2) 0.156(9) Uiso 0.50 1 d PD . . C27 C 0.0063(10) 0.7251(8) 0.3411(8) 0.052(2) Uiso 0.50 1 d PD . . H27A H 0.0775 0.7685 0.3679 0.078 Uiso 0.50 1 calc PR . . H27B H -0.0573 0.7529 0.3773 0.078 Uiso 0.50 1 calc PR . . H27C H -0.0148 0.7239 0.2707 0.078 Uiso 0.50 1 calc PR . . N3 N 0.8777(4) 0.5773(3) 0.9616(4) 0.0584(12) Uani 1 1 d D . . C28 C 0.8378(4) 0.5042(3) 0.9068(4) 0.0420(10) Uani 1 1 d D . . C29 C 0.7882(5) 0.4120(4) 0.8406(4) 0.0509(12) Uani 1 1 d D . . H29A H 0.8325 0.3539 0.8542 0.076 Uiso 1 1 calc R . . H29B H 0.7911 0.4163 0.7721 0.076 Uiso 1 1 calc R . . H29C H 0.7069 0.4023 0.8500 0.076 Uiso 1 1 calc R . . 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 0.0146(2) 0.0146(2) 0.0136(2) 0.00255(17) 0.00065(17) 0.00069(16) Mn2 0.0161(2) 0.0139(2) 0.0141(2) 0.00156(17) 0.00039(17) 0.00043(17) Mn3 0.0212(3) 0.0159(2) 0.0173(2) 0.00281(18) -0.00135(18) 0.00123(18) Mn4 0.0214(3) 0.0214(2) 0.0173(2) 0.00326(19) -0.00198(19) 0.00212(19) Mn5 0.0268(3) 0.0182(2) 0.0189(2) 0.00383(19) 0.0025(2) 0.00026(19) Mn6 0.0216(2) 0.0150(2) 0.0169(2) 0.00212(18) 0.00001(18) -0.00063(18) Na 0.0330(11) 0.0140(8) 0.0280(10) 0.0056(7) 0.0005(8) 0.0013(7) O1 0.0160(10) 0.0150(10) 0.0157(10) 0.0031(8) 0.0010(8) -0.0017(8) O2 0.0182(11) 0.0174(10) 0.0167(10) 0.0025(8) 0.0027(8) 0.0014(8) O3 0.0152(10) 0.0157(10) 0.0146(10) 0.0029(8) 0.0009(8) 0.0004(8) O4 0.0162(11) 0.0180(10) 0.0179(10) 0.0036(8) -0.0001(8) 0.0008(8) O5 0.0155(10) 0.0146(10) 0.0165(10) 0.0026(8) 0.0011(8) 0.0014(8) O6 0.0307(13) 0.0172(11) 0.0218(11) 0.0048(9) -0.0012(10) 0.0012(9) O7 0.0192(11) 0.0170(10) 0.0160(10) 0.0034(8) 0.0020(8) -0.0001(8) O8 0.0243(12) 0.0168(11) 0.0184(11) 0.0011(9) 0.0003(9) -0.0006(9) O9 0.0354(14) 0.0171(11) 0.0202(11) 0.0031(9) 0.0018(10) 0.0058(10) O10 0.0295(13) 0.0291(13) 0.0200(12) 0.0036(10) 0.0014(10) 0.0058(10) O11 0.071(6) 0.036(4) 0.020(4) 0.012(4) -0.014(4) -0.001(4) O11' 0.022(3) 0.053(6) 0.042(5) 0.033(5) -0.008(4) 0.009(3) O12 0.0312(13) 0.0278(13) 0.0175(11) 0.0034(10) 0.0004(10) 0.0051(10) O13 0.0310(16) 0.053(2) 0.0503(19) 0.0215(16) -0.0150(15) -0.0076(14) O14 0.0281(13) 0.0207(12) 0.0274(12) 0.0081(10) -0.0026(10) -0.0041(10) O15 0.0303(15) 0.0355(15) 0.0484(18) 0.0055(13) -0.0062(13) -0.0065(12) O16 0.0251(13) 0.0283(13) 0.0529(18) 0.0185(12) -0.0006(12) 0.0020(10) O17 0.0171(11) 0.0167(10) 0.0177(10) 0.0025(8) -0.0004(8) 0.0025(8) O18 0.0361(15) 0.0287(13) 0.0213(13) 0.0103(11) -0.0005(11) -0.0073(11) O19 0.090(6) 0.284(14) 0.327(16) 0.083(12) -0.033(8) -0.013(7) O20 0.0518(18) 0.0290(14) 0.0382(16) 0.0175(12) 0.0127(14) 0.0086(13) O21 0.0323(15) 0.0308(15) 0.0408(16) 0.0109(13) -0.0007(12) 0.0107(12) O22 0.0371(14) 0.0164(11) 0.0240(12) 0.0047(9) -0.0036(10) -0.0002(10) O23 0.053(5) 0.172(12) 0.087(7) 0.081(8) -0.017(5) -0.029(6) O24 0.074(6) 0.082(6) 0.054(5) -0.002(4) 0.012(4) -0.035(5) C1 0.0190(15) 0.0214(15) 0.0195(15) 0.0055(12) 0.0027(12) -0.0033(12) C2 0.0185(15) 0.0265(16) 0.0189(15) 0.0084(13) 0.0045(12) 0.0036(12) C3 0.0211(16) 0.0222(15) 0.0160(14) 0.0054(12) 0.0032(12) -0.0007(12) C4 0.0185(15) 0.0215(15) 0.0166(14) 0.0059(12) 0.0015(12) 0.0003(12) C5 0.0248(17) 0.0297(18) 0.0227(16) 0.0117(14) 0.0053(13) 0.0001(13) C6 0.0157(14) 0.0228(15) 0.0212(15) 0.0038(12) 0.0022(12) 0.0029(12) C7 0.0167(15) 0.0184(14) 0.0203(15) 0.0025(12) 0.0028(12) 0.0050(11) C8 0.0158(15) 0.0226(15) 0.0229(16) 0.0053(13) -0.0012(12) 0.0044(12) C9 0.0164(15) 0.0202(15) 0.0215(15) 0.0043(12) 0.0006(12) 0.0039(12) C10 0.0194(16) 0.0285(17) 0.0286(17) 0.0065(14) 0.0026(13) 0.0079(13) C11 0.0271(17) 0.0196(15) 0.0218(16) 0.0074(13) 0.0025(13) 0.0035(13) C12 0.056(3) 0.0252(18) 0.032(2) 0.0086(16) -0.0073(18) 0.0099(18) C14 0.0236(17) 0.0191(15) 0.0265(17) 0.0049(13) 0.0051(13) 0.0026(12) C15 0.071(3) 0.030(2) 0.036(2) 0.0042(17) 0.022(2) 0.016(2) C16 0.0323(19) 0.0226(16) 0.0207(16) 0.0030(13) 0.0047(14) 0.0010(14) C17 0.066(3) 0.050(3) 0.024(2) -0.0044(18) 0.000(2) 0.025(2) C20 0.0239(17) 0.0184(15) 0.0271(17) 0.0058(13) 0.0040(13) 0.0021(12) C21 0.026(2) 0.033(2) 0.070(3) 0.021(2) -0.004(2) -0.0025(16) C22 0.050(3) 0.075(4) 0.039(2) 0.020(2) -0.008(2) -0.029(3) C23 0.036(2) 0.055(3) 0.060(3) 0.017(2) -0.005(2) -0.009(2) N3 0.055(3) 0.036(2) 0.079(3) 0.004(2) 0.007(2) 0.0020(19) C28 0.038(2) 0.032(2) 0.057(3) 0.011(2) 0.006(2) 0.0063(18) C29 0.052(3) 0.035(2) 0.059(3) 0.000(2) 0.003(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 1.903(2) . ? Mn1 O2 1.918(2) . ? Mn1 O3 1.926(2) . ? Mn1 O3 1.932(2) 2_677 ? Mn1 O1 2.290(2) . ? Mn1 O5 2.310(2) . ? Mn1 Mn1 2.8411(9) 2_677 ? Mn1 Mn2 3.1327(7) 2_677 ? Mn2 O7 1.917(2) . ? Mn2 O5 1.927(2) 2_677 ? Mn2 O17 1.927(2) 2_677 ? Mn2 O1 1.945(2) . ? Mn2 O6 2.167(2) . ? Mn2 O3 2.289(2) . ? Mn2 Mn1 3.1327(7) 2_677 ? Mn2 Mn6 3.1395(6) 2_677 ? Mn3 O2 2.101(2) . ? Mn3 O10 2.126(2) . ? Mn3 O9 2.126(2) . ? Mn3 O8 2.127(2) . ? Mn3 O7 2.295(2) . ? Mn3 O3 2.374(2) . ? Mn4 O13 2.107(3) . ? Mn4 O11' 2.128(10) . ? Mn4 O11 2.136(12) . ? Mn4 O12 2.163(3) . ? Mn4 O8 2.191(2) . ? Mn4 O7 2.229(2) . ? Mn4 O17 2.348(2) 2_677 ? Mn5 O8 2.076(2) . ? Mn5 O4 2.079(2) 2_677 ? Mn5 O15 2.088(3) . ? Mn5 O14 2.141(2) . ? Mn5 O17 2.327(2) 2_677 ? Mn6 O22 2.173(2) 2_677 ? Mn6 O9 2.210(2) . ? Mn6 O1 2.216(2) 2_677 ? Mn6 O5 2.225(2) . ? Mn6 O14 2.267(3) . ? Mn6 O16 2.337(3) . ? Mn6 Mn2 3.1395(6) 2_677 ? Mn6 Na 3.2777(5) 1_545 ? Na O22 2.344(2) 2_687 ? Na O22 2.344(2) . ? Na O20 2.373(3) 2_677 ? Na O20 2.373(3) 1_565 ? Na O16 2.421(3) 1_565 ? Na O16 2.421(3) 2_677 ? Na Mn6 3.2777(5) 1_565 ? Na Mn6 3.2777(5) 2_677 ? O1 C1 1.441(4) . ? O1 Mn6 2.216(2) 2_677 ? O2 C2 1.421(4) . ? O3 Mn1 1.932(2) 2_677 ? O4 C6 1.428(4) . ? O4 Mn5 2.079(2) 2_677 ? O5 C7 1.438(4) . ? O5 Mn2 1.927(2) 2_677 ? O6 C11 1.265(4) . ? O7 C3 1.447(4) . ? O8 C13 1.456(7) . ? O8 H8C 1.0000 . ? O9 C14 1.288(4) . ? O10 C16 1.260(4) . ? O11 C18 1.467(14) . ? O11' C18 1.203(14) . ? O12 C16 1.268(4) . ? O13 H13D 0.99(7) . ? O13 H13E 0.81(8) . ? O14 C20 1.276(4) . ? O15 C22 1.210(5) . ? O16 C20 1.243(4) . ? O16 Na 2.421(3) 1_545 ? O17 C8 1.447(4) . ? O17 Mn2 1.927(2) 2_677 ? O17 Mn5 2.327(2) 2_677 ? O17 Mn4 2.348(2) 2_677 ? O18 C5 1.420(4) . ? O18 H18 0.79(6) . ? O19 C18 1.394(13) . ? O20 C14 1.231(4) . ? O20 Na 2.373(3) 1_545 ? O21 C10 1.420(5) . ? O21 H21 0.79(4) . ? O22 C11 1.255(4) . ? O22 Mn6 2.173(2) 2_677 ? O23 C22 1.316(10) . ? O23 O24 1.349(15) . ? O24 C22 1.368(10) . ? C1 C4 1.536(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C4 1.537(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.535(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.552(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C9 1.532(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C9 1.529(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.537(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.546(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.502(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.498(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.502(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19' 1.515(15) . ? C18 C19 1.853(14) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9799 . ? C19 H20G 1.5547 . ? C19 H20H 0.7743 . ? C19 H20I 0.8494 . ? C19' H19A 0.9241 . ? C19' H19B 1.2440 . ? C19' H20G 0.9600 . ? C19' H20H 0.9600 . ? C19' H20I 0.9599 . ? C20 C21 1.498(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.499(7) . ? C23 H22A 0.9800 . ? C23 H22B 0.9800 . ? C23 H22C 0.9800 . ? N1 C24 1.16(2) . ? C24 C25 1.319(19) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? N2 C26 1.162(18) . ? C26 C27 1.274(17) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? N3 C28 1.143(6) . ? C28 C29 1.423(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 O2 94.05(10) . . ? O4 Mn1 O3 176.24(9) . . ? O2 Mn1 O3 89.54(9) . . ? O4 Mn1 O3 91.27(9) . 2_677 ? O2 Mn1 O3 174.69(10) . 2_677 ? O3 Mn1 O3 85.14(10) . 2_677 ? O4 Mn1 O1 97.23(9) . . ? O2 Mn1 O1 88.03(9) . . ? O3 Mn1 O1 84.00(8) . . ? O3 Mn1 O1 91.44(8) 2_677 . ? O4 Mn1 O5 87.26(9) . . ? O2 Mn1 O5 95.89(9) . . ? O3 Mn1 O5 91.26(8) . . ? O3 Mn1 O5 84.21(8) 2_677 . ? O1 Mn1 O5 173.83(8) . . ? O4 Mn1 Mn1 133.74(7) . 2_677 ? O2 Mn1 Mn1 132.21(7) . 2_677 ? O3 Mn1 Mn1 42.66(6) . 2_677 ? O3 Mn1 Mn1 42.48(7) 2_677 2_677 ? O1 Mn1 Mn1 86.91(6) . 2_677 ? O5 Mn1 Mn1 86.92(6) . 2_677 ? O4 Mn1 Mn2 85.09(7) . 2_677 ? O2 Mn1 Mn2 133.69(7) . 2_677 ? O3 Mn1 Mn2 91.62(6) . 2_677 ? O3 Mn1 Mn2 46.68(6) 2_677 2_677 ? O1 Mn1 Mn2 138.11(6) . 2_677 ? O5 Mn1 Mn2 37.80(5) . 2_677 ? Mn1 Mn1 Mn2 63.418(18) 2_677 2_677 ? O7 Mn2 O5 172.35(10) . 2_677 ? O7 Mn2 O17 87.31(10) . 2_677 ? O5 Mn2 O17 94.31(10) 2_677 2_677 ? O7 Mn2 O1 93.23(10) . . ? O5 Mn2 O1 84.12(9) 2_677 . ? O17 Mn2 O1 171.91(9) 2_677 . ? O7 Mn2 O6 93.66(9) . . ? O5 Mn2 O6 93.71(9) 2_677 . ? O17 Mn2 O6 93.25(9) 2_677 . ? O1 Mn2 O6 94.78(9) . . ? O7 Mn2 O3 87.70(9) . . ? O5 Mn2 O3 84.88(8) 2_677 . ? O17 Mn2 O3 88.36(9) 2_677 . ? O1 Mn2 O3 83.60(8) . . ? O6 Mn2 O3 177.94(9) . . ? O7 Mn2 Mn1 125.46(7) . 2_677 ? O5 Mn2 Mn1 47.27(6) 2_677 2_677 ? O17 Mn2 Mn1 87.72(7) 2_677 2_677 ? O1 Mn2 Mn1 85.39(7) . 2_677 ? O6 Mn2 Mn1 140.85(7) . 2_677 ? O3 Mn2 Mn1 37.88(5) . 2_677 ? O7 Mn2 Mn6 135.34(7) . 2_677 ? O5 Mn2 Mn6 44.57(7) 2_677 2_677 ? O17 Mn2 Mn6 136.79(7) 2_677 2_677 ? O1 Mn2 Mn6 44.38(6) . 2_677 ? O6 Mn2 Mn6 79.67(6) . 2_677 ? O3 Mn2 Mn6 98.28(6) . 2_677 ? Mn1 Mn2 Mn6 73.300(16) 2_677 2_677 ? O2 Mn3 O10 103.49(10) . . ? O2 Mn3 O9 92.44(9) . . ? O10 Mn3 O9 104.46(10) . . ? O2 Mn3 O8 159.26(9) . . ? O10 Mn3 O8 91.02(10) . . ? O9 Mn3 O8 98.27(10) . . ? O2 Mn3 O7 82.78(8) . . ? O10 Mn3 O7 88.34(9) . . ? O9 Mn3 O7 167.10(9) . . ? O8 Mn3 O7 82.92(8) . . ? O2 Mn3 O3 74.18(8) . . ? O10 Mn3 O3 165.93(9) . . ? O9 Mn3 O3 89.56(8) . . ? O8 Mn3 O3 88.13(8) . . ? O7 Mn3 O3 77.62(8) . . ? O13 Mn4 O11' 88.8(3) . . ? O13 Mn4 O11 97.0(3) . . ? O11' Mn4 O11 14.7(3) . . ? O13 Mn4 O12 102.00(13) . . ? O11' Mn4 O12 96.5(3) . . ? O11 Mn4 O12 106.5(3) . . ? O13 Mn4 O8 92.87(12) . . ? O11' Mn4 O8 175.2(3) . . ? O11 Mn4 O8 160.6(2) . . ? O12 Mn4 O8 87.63(9) . . ? O13 Mn4 O7 167.42(13) . . ? O11' Mn4 O7 94.4(2) . . ? O11 Mn4 O7 83.7(3) . . ? O12 Mn4 O7 89.75(9) . . ? O8 Mn4 O7 83.03(8) . . ? O13 Mn4 O17 96.65(12) . 2_677 ? O11' Mn4 O17 99.2(3) . 2_677 ? O11 Mn4 O17 86.2(3) . 2_677 ? O12 Mn4 O17 155.78(9) . 2_677 ? O8 Mn4 O17 76.05(8) . 2_677 ? O7 Mn4 O17 70.83(8) . 2_677 ? O8 Mn5 O4 149.14(9) . 2_677 ? O8 Mn5 O15 111.20(11) . . ? O4 Mn5 O15 96.93(11) 2_677 . ? O8 Mn5 O14 95.02(10) . . ? O4 Mn5 O14 92.09(9) 2_677 . ? O15 Mn5 O14 100.30(11) . . ? O8 Mn5 O17 78.73(9) . 2_677 ? O4 Mn5 O17 82.16(8) 2_677 2_677 ? O15 Mn5 O17 104.64(10) . 2_677 ? O14 Mn5 O17 154.89(9) . 2_677 ? O22 Mn6 O9 128.24(10) 2_677 . ? O22 Mn6 O1 90.46(9) 2_677 2_677 ? O9 Mn6 O1 134.81(8) . 2_677 ? O22 Mn6 O5 87.48(9) 2_677 . ? O9 Mn6 O5 86.25(9) . . ? O1 Mn6 O5 71.47(8) 2_677 . ? O22 Mn6 O14 131.68(10) 2_677 . ? O9 Mn6 O14 83.78(10) . . ? O1 Mn6 O14 85.37(9) 2_677 . ? O5 Mn6 O14 135.15(8) . . ? O22 Mn6 O16 78.79(10) 2_677 . ? O9 Mn6 O16 104.87(10) . . ? O1 Mn6 O16 104.96(10) 2_677 . ? O5 Mn6 O16 165.85(9) . . ? O14 Mn6 O16 56.30(9) . . ? O22 Mn6 Mn2 76.00(6) 2_677 2_677 ? O9 Mn6 Mn2 121.52(7) . 2_677 ? O1 Mn6 Mn2 37.87(6) 2_677 2_677 ? O5 Mn6 Mn2 37.44(6) . 2_677 ? O14 Mn6 Mn2 121.23(7) . 2_677 ? O16 Mn6 Mn2 133.42(8) . 2_677 ? O22 Mn6 Na 45.57(6) 2_677 1_545 ? O9 Mn6 Na 99.03(6) . 1_545 ? O1 Mn6 Na 126.13(6) 2_677 1_545 ? O5 Mn6 Na 122.97(6) . 1_545 ? O14 Mn6 Na 101.78(6) . 1_545 ? O16 Mn6 Na 47.54(6) . 1_545 ? Mn2 Mn6 Na 121.569(18) 2_677 1_545 ? O22 Na O22 180.000(1) 2_687 . ? O22 Na O20 100.64(10) 2_687 2_677 ? O22 Na O20 79.36(10) . 2_677 ? O22 Na O20 79.36(10) 2_687 1_565 ? O22 Na O20 100.64(10) . 1_565 ? O20 Na O20 180.000(1) 2_677 1_565 ? O22 Na O16 73.89(9) 2_687 1_565 ? O22 Na O16 106.11(9) . 1_565 ? O20 Na O16 103.16(10) 2_677 1_565 ? O20 Na O16 76.84(10) 1_565 1_565 ? O22 Na O16 106.11(9) 2_687 2_677 ? O22 Na O16 73.89(9) . 2_677 ? O20 Na O16 76.84(10) 2_677 2_677 ? O20 Na O16 103.16(10) 1_565 2_677 ? O16 Na O16 180.000(1) 1_565 2_677 ? O22 Na Mn6 41.45(6) 2_687 1_565 ? O22 Na Mn6 138.55(6) . 1_565 ? O20 Na Mn6 129.44(7) 2_677 1_565 ? O20 Na Mn6 50.56(7) 1_565 1_565 ? O16 Na Mn6 45.40(6) 1_565 1_565 ? O16 Na Mn6 134.60(6) 2_677 1_565 ? O22 Na Mn6 138.55(6) 2_687 2_677 ? O22 Na Mn6 41.45(6) . 2_677 ? O20 Na Mn6 50.56(7) 2_677 2_677 ? O20 Na Mn6 129.44(7) 1_565 2_677 ? O16 Na Mn6 134.60(6) 1_565 2_677 ? O16 Na Mn6 45.40(6) 2_677 2_677 ? Mn6 Na Mn6 180.0 1_565 2_677 ? C1 O1 Mn2 121.00(19) . . ? C1 O1 Mn6 114.71(17) . 2_677 ? Mn2 O1 Mn6 97.75(9) . 2_677 ? C1 O1 Mn1 113.73(18) . . ? Mn2 O1 Mn1 95.75(9) . . ? Mn6 O1 Mn1 111.63(9) 2_677 . ? C2 O2 Mn1 122.34(19) . . ? C2 O2 Mn3 118.69(19) . . ? Mn1 O2 Mn3 102.38(10) . . ? Mn1 O3 Mn1 94.86(9) . 2_677 ? Mn1 O3 Mn2 96.32(9) . . ? Mn1 O3 Mn2 95.44(9) 2_677 . ? Mn1 O3 Mn3 93.01(8) . . ? Mn1 O3 Mn3 169.40(12) 2_677 . ? Mn2 O3 Mn3 90.73(8) . . ? C6 O4 Mn1 122.65(19) . . ? C6 O4 Mn5 113.78(18) . 2_677 ? Mn1 O4 Mn5 109.62(11) . 2_677 ? C7 O5 Mn2 120.67(18) . 2_677 ? C7 O5 Mn6 114.88(17) . . ? Mn2 O5 Mn6 97.99(9) 2_677 . ? C7 O5 Mn1 114.54(18) . . ? Mn2 O5 Mn1 94.93(9) 2_677 . ? Mn6 O5 Mn1 111.30(9) . . ? C11 O6 Mn2 127.0(2) . . ? C3 O7 Mn2 119.22(18) . . ? C3 O7 Mn4 121.50(18) . . ? Mn2 O7 Mn4 102.37(10) . . ? C3 O7 Mn3 114.26(18) . . ? Mn2 O7 Mn3 103.62(10) . . ? Mn4 O7 Mn3 91.22(8) . . ? C13 O8 Mn5 112.7(3) . . ? C13 O8 Mn3 116.2(3) . . ? Mn5 O8 Mn3 105.17(10) . . ? C13 O8 Mn4 117.5(3) . . ? Mn5 O8 Mn4 106.61(10) . . ? Mn3 O8 Mn4 96.94(9) . . ? C13 O8 H8C 2.8 . . ? Mn5 O8 H8C 115.4 . . ? Mn3 O8 H8C 115.4 . . ? Mn4 O8 H8C 115.4 . . ? C14 O9 Mn3 141.6(2) . . ? C14 O9 Mn6 100.0(2) . . ? Mn3 O9 Mn6 117.87(11) . . ? C16 O10 Mn3 129.5(2) . . ? C18 O11 Mn4 116.5(8) . . ? C18 O11' Mn4 133.6(9) . . ? C16 O12 Mn4 130.1(2) . . ? Mn4 O13 H13D 121(4) . . ? Mn4 O13 H13E 138(6) . . ? H13D O13 H13E 99(6) . . ? C20 O14 Mn5 142.6(2) . . ? C20 O14 Mn6 93.4(2) . . ? Mn5 O14 Mn6 123.99(11) . . ? C22 O15 Mn5 140.2(4) . . ? C20 O16 Mn6 91.0(2) . . ? C20 O16 Na 159.2(3) . 1_545 ? Mn6 O16 Na 87.06(9) . 1_545 ? C8 O17 Mn2 117.61(19) . 2_677 ? C8 O17 Mn5 108.74(18) . 2_677 ? Mn2 O17 Mn5 110.15(10) 2_677 2_677 ? C8 O17 Mn4 125.56(18) . 2_677 ? Mn2 O17 Mn4 97.89(9) 2_677 2_677 ? Mn5 O17 Mn4 94.13(8) 2_677 2_677 ? C5 O18 H18 103(4) . . ? C14 O20 Na 159.9(3) . 1_545 ? C10 O21 H21 112(3) . . ? C11 O22 Mn6 132.3(2) . 2_677 ? C11 O22 Na 134.6(2) . . ? Mn6 O22 Na 92.97(9) 2_677 . ? C22 O23 O24 61.8(7) . . ? O23 O24 C22 57.9(6) . . ? O1 C1 C4 113.5(3) . . ? O1 C1 H1A 108.9 . . ? C4 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C4 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O2 C2 C4 115.9(3) . . ? O2 C2 H2A 108.3 . . ? C4 C2 H2A 108.3 . . ? O2 C2 H2B 108.3 . . ? C4 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? O7 C3 C4 113.9(3) . . ? O7 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? O7 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C1 111.4(3) . . ? C3 C4 C2 113.0(3) . . ? C1 C4 C2 111.9(3) . . ? C3 C4 C5 107.9(3) . . ? C1 C4 C5 107.1(3) . . ? C2 C4 C5 105.0(3) . . ? O18 C5 C4 114.0(3) . . ? O18 C5 H5A 108.8 . . ? C4 C5 H5A 108.8 . . ? O18 C5 H5B 108.8 . . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.6 . . ? O4 C6 C9 116.0(3) . . ? O4 C6 H6A 108.3 . . ? C9 C6 H6A 108.3 . . ? O4 C6 H6B 108.3 . . ? C9 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? O5 C7 C9 113.3(2) . . ? O5 C7 H7A 108.9 . . ? C9 C7 H7A 108.9 . . ? O5 C7 H7B 108.9 . . ? C9 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O17 C8 C9 114.2(2) . . ? O17 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? O17 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C7 C9 C6 110.9(3) . . ? C7 C9 C8 112.1(3) . . ? C6 C9 C8 113.3(3) . . ? C7 C9 C10 108.1(3) . . ? C6 C9 C10 104.4(3) . . ? C8 C9 C10 107.5(3) . . ? O21 C10 C9 114.7(3) . . ? O21 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? O21 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? O22 C11 O6 124.1(3) . . ? O22 C11 C12 118.0(3) . . ? O6 C11 C12 117.9(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O8 C13 H13A 109.5 . . ? O8 C13 H13B 109.5 . . ? O8 C13 H13C 109.5 . . ? O20 C14 O9 120.0(3) . . ? O20 C14 C15 121.6(3) . . ? O9 C14 C15 118.3(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O10 C16 O12 124.7(3) . . ? O10 C16 C17 117.5(3) . . ? O12 C16 C17 117.8(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O11' C18 O19 122.8(11) . . ? O11' C18 O11 20.7(7) . . ? O19 C18 O11 125.8(11) . . ? O11' C18 C19' 123.2(11) . . ? O19 C18 C19' 114.0(11) . . ? O11 C18 C19' 115.4(10) . . ? O11' C18 C19 109.5(9) . . ? O19 C18 C19 125.5(10) . . ? O11 C18 C19 108.5(9) . . ? C19' C18 C19 20.7(6) . . ? C18 C19 H19A 104.3 . . ? C18 C19 H19B 110.6 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 113.4 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C19 H20G 73.8 . . ? H19A C19 H20G 46.3 . . ? H19B C19 H20G 88.7 . . ? H19C C19 H20G 154.8 . . ? C18 C19 H20H 89.9 . . ? H19A C19 H20H 42.8 . . ? H19B C19 H20H 150.6 . . ? H19C C19 H20H 79.3 . . ? H20G C19 H20H 76.6 . . ? C18 C19 H20I 92.2 . . ? H19A C19 H20I 107.8 . . ? H19B C19 H20I 20.1 . . ? H19C C19 H20I 126.7 . . ? H20G C19 H20I 75.1 . . ? H20H C19 H20I 149.7 . . ? C18 C19' H19A 139.9 . . ? C18 C19' H19B 119.0 . . ? H19A C19' H19B 94.0 . . ? C18 C19' H20G 110.7 . . ? H19A C19' H20G 73.5 . . ? H19B C19' H20G 110.5 . . ? C18 C19' H20H 106.2 . . ? H19A C19' H20H 41.5 . . ? H19B C19' H20H 100.0 . . ? H20G C19' H20H 109.5 . . ? C18 C19' H20I 111.4 . . ? H19A C19' H20I 103.6 . . ? H19B C19' H20I 10.2 . . ? H20G C19' H20I 109.5 . . ? H20H C19' H20I 109.5 . . ? O16 C20 O14 119.2(3) . . ? O16 C20 C21 121.6(3) . . ? O14 C20 C21 119.2(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O15 C22 O23 118.3(7) . . ? O15 C22 O24 113.9(6) . . ? O23 C22 O24 60.3(7) . . ? O15 C22 C23 121.7(5) . . ? O23 C22 C23 110.8(6) . . ? O24 C22 C23 116.7(5) . . ? C22 C23 H22A 109.5 . . ? C22 C23 H22B 109.5 . . ? H22A C23 H22B 109.5 . . ? C22 C23 H22C 109.5 . . ? H22A C23 H22C 109.5 . . ? H22B C23 H22C 109.5 . . ? N1 C24 C25 134(4) . . ? N2 C26 C27 164(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 178.6(6) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.193 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.113