# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address S.K.Langley ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; N.F.Chilton ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; B.Moubaraki ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; K.S.Murray ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; _publ_contact_author_address ; School of Chemistry, 171 Monash university, Vic 3800, Australia ; _publ_contact_author_email Keith.murray@sci.monash.edu.au _publ_contact_author_fax +61-3-9905-4597 _publ_contact_author_phone +61-3-9905-4512 #========================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Keith. S. Murray' _publ_contact_letter ; ; _publ_requested_category ? _publ_section_title ; Self-assembled decanuclear NaI2MnII4MnIII4 complexes : >From discrete clusters to 1- and 2-D structures, with the MnII4MnIII4 unit displaying a large spin ground state and SMM behaviour. ; data_1 _database_code_depnum_ccdc_archive 'CCDC 822744' #TrackingRef '- 1Mn(sal)(tea)_new.cif' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains the monomer as well as a solvent water molecule. All non H atoms were refined anisotropically. The solvent water molecule was modelled at half occupancy, with a thermal restraint (ISOR) placed on it. All the hydrogen atoms were placed in calculated positions exept for on the water molecule and for H3 and H4 which were found and were refined freely. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H19 Mn N O6.50' _chemical_formula_weight 348.22 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0895(2) _cell_length_b 9.4777(2) _cell_length_c 15.1121(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.4790(10) _cell_angle_gamma 90.00 _cell_volume 1442.44(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8907 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 30.12 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16624 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 30.58 _reflns_number_total 4439 _reflns_number_gt 4167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 structure was solved by direct methods. The asymmetric unit contains the monomer as well as a solvent water molecule. All non H atoms were refined anisotropically. The solvent water molecule was modelled at half occupancy, with a thermal restraint (ISOR) placed on it. All the hydrogen atoms were placed in calculated positions exept for on the water molecule and for H3 and H4 which were found and were refined freely. ; _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^)+(0.0311P)^2^+1.6027P] 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 4439 _refine_ls_number_parameters 207 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.13817(2) 0.97757(3) 0.136024(15) 0.01440(7) Uani 1 1 d . . . O1 O 0.16081(11) 1.07134(13) 0.02923(8) 0.0197(2) Uani 1 1 d . . . O2 O 0.00215(12) 1.10077(13) 0.16317(8) 0.0206(2) Uani 1 1 d . . . O3 O 0.00692(12) 0.80897(13) 0.07825(8) 0.0195(2) Uani 1 1 d . . . O4 O 0.13457(12) 0.88021(13) 0.24534(8) 0.0194(2) Uani 1 1 d . . . O5 O 0.33424(13) 1.06595(14) 0.19203(9) 0.0222(2) Uani 1 1 d . . . O6 O 0.05946(15) 0.80010(15) 0.36834(10) 0.0334(3) Uani 1 1 d . . . O7 O 0.1308(6) 1.3767(5) 0.1116(4) 0.0856(16) Uani 0.50 1 d PU . . N7 N 0.27625(12) 0.83335(14) 0.09076(9) 0.0147(2) Uani 1 1 d . . . C8 C 0.05128(16) 0.88604(17) 0.30669(11) 0.0185(3) Uani 1 1 d . . . C9 C -0.07284(15) 1.09260(17) 0.23295(10) 0.0160(3) Uani 1 1 d . . . C10 C -0.05289(16) 0.99658(16) 0.30327(11) 0.0179(3) Uani 1 1 d . . . C11 C 0.21503(16) 0.69031(17) 0.08960(11) 0.0193(3) Uani 1 1 d . . . H11A H 0.2089 0.6572 0.1499 0.023 Uiso 1 1 calc R . . H11B H 0.2708 0.6251 0.0592 0.023 Uiso 1 1 calc R . . C12 C 0.44574(18) 0.9768(2) 0.17554(14) 0.0269(4) Uani 1 1 d . . . H12A H 0.5071 0.9741 0.2275 0.032 Uiso 1 1 calc R . . H12B H 0.4924 1.0135 0.1262 0.032 Uiso 1 1 calc R . . C13 C -0.17769(16) 1.19054(19) 0.23614(11) 0.0206(3) Uani 1 1 d . . . H13 H -0.1936 1.2536 0.1896 0.025 Uiso 1 1 calc R . . C14 C 0.30569(18) 0.87977(18) -0.00037(11) 0.0216(3) Uani 1 1 d . . . H14A H 0.2502 0.8279 -0.0438 0.026 Uiso 1 1 calc R . . H14B H 0.3978 0.8597 -0.0106 0.026 Uiso 1 1 calc R . . C15 C 0.27971(16) 1.03729(18) -0.01127(11) 0.0196(3) Uani 1 1 d . . . H15A H 0.3532 1.0905 0.0164 0.024 Uiso 1 1 calc R . . H15B H 0.2714 1.0615 -0.0737 0.024 Uiso 1 1 calc R . . C16 C -0.25722(17) 1.1942(2) 0.30742(13) 0.0253(4) Uani 1 1 d . . . H16 H -0.3268 1.2584 0.3078 0.030 Uiso 1 1 calc R . . C17 C 0.07713(18) 0.69360(19) 0.04292(13) 0.0244(3) Uani 1 1 d . . . H17A H 0.0836 0.7056 -0.0204 0.029 Uiso 1 1 calc R . . H17B H 0.0309 0.6058 0.0530 0.029 Uiso 1 1 calc R . . C18 C -0.1336(2) 1.0048(2) 0.37556(14) 0.0283(4) Uani 1 1 d . . . H18 H -0.1188 0.9426 0.4227 0.034 Uiso 1 1 calc R . . C19 C -0.2341(2) 1.1028(2) 0.37839(14) 0.0314(4) Uani 1 1 d . . . H19 H -0.2858 1.1075 0.4272 0.038 Uiso 1 1 calc R . . C21 C 0.39463(16) 0.83068(19) 0.15429(12) 0.0228(3) Uani 1 1 d . . . H21A H 0.4643 0.7758 0.1292 0.027 Uiso 1 1 calc R . . H21B H 0.3715 0.7847 0.2086 0.027 Uiso 1 1 calc R . . H3 H -0.047(3) 0.844(3) 0.0400(19) 0.041(7) Uiso 1 1 d . . . H4 H 0.354(3) 1.142(3) 0.179(2) 0.054(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01491(11) 0.01419(12) 0.01458(12) 0.00225(8) 0.00477(8) 0.00338(8) O1 0.0165(5) 0.0231(6) 0.0201(5) 0.0077(4) 0.0063(4) 0.0037(4) O2 0.0227(6) 0.0221(6) 0.0175(5) 0.0025(4) 0.0064(4) 0.0098(5) O3 0.0164(5) 0.0195(6) 0.0226(6) 0.0038(5) 0.0018(4) 0.0008(4) O4 0.0202(5) 0.0212(6) 0.0176(5) 0.0052(4) 0.0072(4) 0.0064(4) O5 0.0227(6) 0.0163(6) 0.0277(6) -0.0031(5) 0.0022(5) -0.0013(5) O6 0.0461(8) 0.0275(7) 0.0290(7) 0.0127(6) 0.0212(6) 0.0158(6) O7 0.107(4) 0.056(3) 0.089(4) 0.006(3) -0.029(3) -0.001(3) N7 0.0141(5) 0.0149(6) 0.0151(6) 0.0000(5) 0.0028(4) 0.0015(4) C8 0.0202(7) 0.0160(7) 0.0198(7) -0.0008(6) 0.0062(6) 0.0006(6) C9 0.0142(6) 0.0163(7) 0.0178(7) -0.0043(5) 0.0023(5) 0.0007(5) C10 0.0179(7) 0.0143(7) 0.0222(7) -0.0013(6) 0.0074(6) 0.0005(5) C11 0.0220(7) 0.0139(7) 0.0225(8) 0.0007(6) 0.0061(6) 0.0026(6) C12 0.0196(8) 0.0271(9) 0.0334(10) -0.0008(7) -0.0023(7) 0.0002(7) C13 0.0183(7) 0.0223(8) 0.0208(7) -0.0056(6) -0.0008(6) 0.0059(6) C14 0.0261(8) 0.0215(8) 0.0182(7) 0.0016(6) 0.0105(6) 0.0010(6) C15 0.0184(7) 0.0216(8) 0.0197(7) 0.0051(6) 0.0074(6) 0.0006(6) C16 0.0185(7) 0.0267(9) 0.0312(9) -0.0082(7) 0.0053(6) 0.0059(6) C17 0.0234(8) 0.0186(8) 0.0315(9) -0.0041(7) 0.0035(7) -0.0033(6) C18 0.0330(9) 0.0237(9) 0.0302(9) 0.0035(7) 0.0186(8) 0.0055(7) C19 0.0299(9) 0.0307(10) 0.0359(10) 0.0001(8) 0.0207(8) 0.0066(8) C21 0.0177(7) 0.0247(8) 0.0257(8) -0.0014(7) -0.0017(6) 0.0041(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 1.8664(11) . ? Mn1 O1 1.8685(12) . ? Mn1 O4 1.8945(12) . ? Mn1 N7 2.0959(13) . ? Mn1 O3 2.2201(12) . ? Mn1 O5 2.2645(13) . ? O1 C15 1.4166(19) . ? O2 C9 1.3369(19) . ? O3 C17 1.424(2) . ? O3 H3 0.84(3) . ? O4 C8 1.2897(19) . ? O5 C12 1.441(2) . ? O5 H4 0.78(3) . ? O6 C8 1.237(2) . ? N7 C21 1.487(2) . ? N7 C11 1.489(2) . ? N7 C14 1.493(2) . ? C8 C10 1.483(2) . ? C9 C10 1.404(2) . ? C9 C13 1.410(2) . ? C10 C18 1.404(2) . ? C11 C17 1.522(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C21 1.505(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C16 1.382(2) . ? C13 H13 0.9300 . ? C14 C15 1.523(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C19 1.387(3) . ? C16 H16 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.378(3) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O1 91.28(5) . . ? O2 Mn1 O4 93.43(5) . . ? O1 Mn1 O4 174.07(5) . . ? O2 Mn1 N7 172.72(5) . . ? O1 Mn1 N7 84.82(5) . . ? O4 Mn1 N7 90.87(5) . . ? O2 Mn1 O3 96.18(5) . . ? O1 Mn1 O3 95.97(5) . . ? O4 Mn1 O3 87.12(5) . . ? N7 Mn1 O3 78.15(5) . . ? O2 Mn1 O5 108.89(5) . . ? O1 Mn1 O5 89.83(5) . . ? O4 Mn1 O5 85.23(5) . . ? N7 Mn1 O5 77.31(5) . . ? O3 Mn1 O5 154.14(5) . . ? C15 O1 Mn1 114.58(10) . . ? C9 O2 Mn1 126.59(10) . . ? C17 O3 Mn1 113.68(10) . . ? C17 O3 H3 111.3(19) . . ? Mn1 O3 H3 109.2(19) . . ? C8 O4 Mn1 130.83(11) . . ? C12 O5 Mn1 113.07(10) . . ? C12 O5 H4 107(2) . . ? Mn1 O5 H4 118(2) . . ? C21 N7 C11 107.97(13) . . ? C21 N7 C14 113.82(13) . . ? C11 N7 C14 111.28(13) . . ? C21 N7 Mn1 108.91(10) . . ? C11 N7 Mn1 108.30(9) . . ? C14 N7 Mn1 106.40(10) . . ? O6 C8 O4 119.79(15) . . ? O6 C8 C10 120.43(15) . . ? O4 C8 C10 119.78(15) . . ? O2 C9 C10 124.92(14) . . ? O2 C9 C13 116.77(15) . . ? C10 C9 C13 118.29(15) . . ? C18 C10 C9 119.32(15) . . ? C18 C10 C8 117.09(15) . . ? C9 C10 C8 123.58(14) . . ? N7 C11 C17 110.72(13) . . ? N7 C11 H11A 109.5 . . ? C17 C11 H11A 109.5 . . ? N7 C11 H11B 109.5 . . ? C17 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? O5 C12 C21 108.39(14) . . ? O5 C12 H12A 110.0 . . ? C21 C12 H12A 110.0 . . ? O5 C12 H12B 110.0 . . ? C21 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C16 C13 C9 121.01(16) . . ? C16 C13 H13 119.5 . . ? C9 C13 H13 119.5 . . ? N7 C14 C15 110.25(13) . . ? N7 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? N7 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? O1 C15 C14 108.74(13) . . ? O1 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? O1 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C13 C16 C19 120.57(16) . . ? C13 C16 H16 119.7 . . ? C19 C16 H16 119.7 . . ? O3 C17 C11 107.67(14) . . ? O3 C17 H17A 110.2 . . ? C11 C17 H17A 110.2 . . ? O3 C17 H17B 110.2 . . ? C11 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? C19 C18 C10 121.64(18) . . ? C19 C18 H18 119.2 . . ? C10 C18 H18 119.2 . . ? C18 C19 C16 119.10(17) . . ? C18 C19 H19 120.5 . . ? C16 C19 H19 120.5 . . ? N7 C21 C12 111.94(14) . . ? N7 C21 H21A 109.2 . . ? C12 C21 H21A 109.2 . . ? N7 C21 H21B 109.2 . . ? C12 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.943 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.068 # Attachment '- 2_Na2Mn8_new.cif' #========================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 822745' #TrackingRef '- 2_Na2Mn8_new.cif' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains half the cluster as well as solvent MeoH molecules. The free alcohol arm of two of the teaH2- ligands, contains a oxygen atom that is disordered over three positions set at 0.42, 0.3 and 0.28 occupancy. Their bond lengths are restrained using the DFIX command. In the ASU four of the solvent MeOH molecules have been modelled at 0.5 occupancy with bond (DFIX) and thermal (ISOR) restraints placed on them. All non H atoms were refined anisotropically and all H atoms were placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H134 Mn8 N12 Na2 O40' _chemical_formula_weight 2317.43 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.813(4) _cell_length_b 12.949(3) _cell_length_c 23.397(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.75(3) _cell_angle_gamma 90.00 _cell_volume 5302.0(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 34274 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71123 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34274 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9285 _reflns_number_gt 8141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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 structure was solved by direct methods. The asymmetric unit contains half the cluster as well as solvent MeoH molecules. The free alcohol arm of two of the teaH2- ligands, contains a oxygen atom that is disordered over three positions set at 0.42, 0.3 and 0.28 occupancy. Their bond lengths are restrained using the DFIX command. In the ASU four of the solvent MeOH molecules have been modelled at 0.5 occupancy with bond (DFIX) and thermal (ISOR) restraints placed on them. All non H atoms were refined anisotropically and all H atoms were placed in calculated positions. ; _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^)+(0.0784P)^2^+29.8594P] 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 9285 _refine_ls_number_parameters 690 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.096 _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 0.53539(4) 0.28637(6) 0.14385(4) 0.0287(2) Uani 1 1 d . . . Mn2 Mn 0.55973(4) 0.39190(5) 0.02488(4) 0.0254(2) Uani 1 1 d . . . Mn3 Mn 0.56211(4) 0.50150(6) -0.10774(4) 0.0274(2) Uani 1 1 d . . . Mn4 Mn 0.69340(4) 0.33817(6) -0.04663(4) 0.0302(2) Uani 1 1 d . . . Na1 Na 0.66910(12) 0.18104(15) 0.06790(10) 0.0352(5) Uani 1 1 d . . . O1 O 0.5350(2) 0.3202(3) 0.22140(18) 0.0357(9) Uani 1 1 d . . . O2 O 0.6417(2) 0.2389(3) 0.16502(18) 0.0342(9) Uani 1 1 d . . . O3 O 0.7581(2) 0.2290(3) 0.21755(19) 0.0399(10) Uani 1 1 d . . . O4 O 0.43199(19) 0.3362(3) 0.12436(16) 0.0286(8) Uani 1 1 d . . . O5 O 0.5398(2) 0.2424(3) 0.06545(17) 0.0301(9) Uani 1 1 d . . . O6 O 0.5041(3) -0.0869(4) 0.2509(2) 0.0617(15) Uani 1 1 d . . . H6 H 0.5502 -0.0959 0.2489 0.074 Uiso 1 1 calc R . . O7 O 0.56874(19) 0.3487(3) -0.06247(17) 0.0285(8) Uani 1 1 d . . . O8 O 0.68171(19) 0.3556(3) 0.03449(17) 0.0311(9) Uani 1 1 d . . . O9 O 0.44082(19) 0.5615(3) -0.11277(16) 0.0281(8) Uani 1 1 d . . . O10 O 0.6219(2) 0.4721(3) -0.18535(19) 0.0385(10) Uani 1 1 d D . . O11 O 0.6850(2) 0.4804(3) -0.06467(19) 0.0337(9) Uani 1 1 d . . . O12 O 0.7005(2) 0.1916(3) -0.03142(18) 0.0340(9) Uani 1 1 d . . . O13 O 0.7043(2) 0.3152(3) -0.12521(19) 0.0399(10) Uani 1 1 d . . . O14 O 0.7120(3) 0.0246(3) -0.0448(2) 0.0559(13) Uani 1 1 d . . . O15 O 0.9952(11) 0.4261(14) 0.0200(11) 0.099(9) Uani 0.28 1 d PD A 2 H15 H 1.0103 0.4223 0.0561 0.119 Uiso 0.28 1 calc PR A 2 O16 O 0.6388(3) 0.0071(3) 0.0450(2) 0.0422(11) Uani 1 1 d . . . O17 O 0.7873(3) 0.1403(4) 0.1197(2) 0.0505(12) Uani 1 1 d . . . N1 N 0.4675(3) 0.1331(3) 0.1439(2) 0.0338(11) Uani 1 1 d . . . N2 N 0.5637(2) 0.5587(3) -0.0070(2) 0.0273(10) Uani 1 1 d . . . N3 N 0.6183(2) 0.6148(3) 0.0072(2) 0.0311(11) Uani 1 1 d . . . N4 N 0.6707(3) 0.6676(4) 0.0199(3) 0.0416(13) Uani 1 1 d . . . N5 N 0.8166(3) 0.3885(4) -0.0069(3) 0.0410(13) Uani 1 1 d . . . N6 N 0.4796(3) 0.3879(3) -0.1722(2) 0.0298(10) Uani 1 1 d . . . C1 C 0.5826(3) 0.2912(4) 0.2691(3) 0.0385(14) Uani 1 1 d . . . C2 C 0.5591(4) 0.3002(6) 0.3221(3) 0.057(2) Uani 1 1 d . . . H2 H 0.5093 0.3254 0.3229 0.068 Uiso 1 1 calc R . . C3 C 0.6063(5) 0.2734(9) 0.3739(4) 0.078(3) Uani 1 1 d . . . H3 H 0.5887 0.2799 0.4096 0.094 Uiso 1 1 calc R . . C4 C 0.6799(4) 0.2369(7) 0.3734(4) 0.068(3) Uani 1 1 d . . . H4 H 0.7124 0.2179 0.4088 0.082 Uiso 1 1 calc R . . C5 C 0.7049(4) 0.2286(5) 0.3222(3) 0.0472(17) Uani 1 1 d . . . H5 H 0.7554 0.2049 0.3224 0.057 Uiso 1 1 calc R . . C6 C 0.6580(3) 0.2544(4) 0.2688(3) 0.0369(14) Uani 1 1 d . . . C7 C 0.6876(3) 0.2413(4) 0.2157(3) 0.0357(14) Uani 1 1 d . . . C8 C 0.3863(3) 0.1666(4) 0.1377(3) 0.0383(14) Uani 1 1 d . . . H8A H 0.3603 0.1245 0.1635 0.046 Uiso 1 1 calc R . . H8B H 0.3596 0.1557 0.0971 0.046 Uiso 1 1 calc R . . C9 C 0.3825(3) 0.2796(4) 0.1535(3) 0.0346(13) Uani 1 1 d . . . H9A H 0.3295 0.3052 0.1418 0.041 Uiso 1 1 calc R . . H9B H 0.3982 0.2884 0.1961 0.041 Uiso 1 1 calc R . . C10 C 0.4846(3) 0.0825(4) 0.0909(3) 0.0367(14) Uani 1 1 d . . . H10A H 0.4452 0.0296 0.0771 0.044 Uiso 1 1 calc R . . H10B H 0.5348 0.0476 0.1002 0.044 Uiso 1 1 calc R . . C11 C 0.4857(3) 0.1618(4) 0.0440(3) 0.0337(13) Uani 1 1 d . . . H11A H 0.5004 0.1285 0.0096 0.040 Uiso 1 1 calc R . . H11B H 0.4341 0.1919 0.0319 0.040 Uiso 1 1 calc R . . C12 C 0.4953(3) 0.0751(4) 0.1980(3) 0.0406(15) Uani 1 1 d . . . H12A H 0.4806 0.1136 0.2308 0.049 Uiso 1 1 calc R . . H12B H 0.5518 0.0733 0.2046 0.049 Uiso 1 1 calc R . . C13 C 0.4661(4) -0.0359(4) 0.1996(3) 0.0477(17) Uani 1 1 d . . . H13A H 0.4104 -0.0353 0.1988 0.057 Uiso 1 1 calc R . . H13B H 0.4754 -0.0738 0.1648 0.057 Uiso 1 1 calc R . . C14 C 0.8191(3) 0.3683(5) 0.0552(3) 0.0421(15) Uani 1 1 d . . . H14A H 0.8622 0.4069 0.0785 0.050 Uiso 1 1 calc R . . H14B H 0.8278 0.2938 0.0631 0.050 Uiso 1 1 calc R . . C15 C 0.7450(3) 0.4007(4) 0.0731(3) 0.0357(14) Uani 1 1 d . . . H15A H 0.7449 0.3778 0.1134 0.043 Uiso 1 1 calc R . . H15B H 0.7405 0.4769 0.0718 0.043 Uiso 1 1 calc R . . C16 C 0.8174(3) 0.5009(4) -0.0212(3) 0.0431(16) Uani 1 1 d . . . H16A H 0.8678 0.5201 -0.0299 0.052 Uiso 1 1 calc R . . H16B H 0.8086 0.5422 0.0125 0.052 Uiso 1 1 calc R . . C17 C 0.7551(3) 0.5237(5) -0.0737(3) 0.0441(16) Uani 1 1 d . . . H17A H 0.7494 0.5993 -0.0793 0.053 Uiso 1 1 calc R . . H17B H 0.7692 0.4937 -0.1092 0.053 Uiso 1 1 calc R . . C18 C 0.8733(4) 0.3278(6) -0.0317(4) 0.0549(19) Uani 1 1 d . A . H18A H 0.8712 0.3502 -0.0724 0.066 Uiso 1 1 calc R . . H18B H 0.8580 0.2543 -0.0327 0.066 Uiso 1 1 calc R . . C19 C 0.9552(4) 0.3357(11) 0.0000(5) 0.098(4) Uani 1 1 d D . . H19A H 0.9617 0.4028 0.0206 0.117 Uiso 1 1 calc R A 1 H19B H 0.9642 0.2807 0.0300 0.117 Uiso 1 1 calc R A 1 C20 C 0.7237(3) 0.2276(5) -0.1498(3) 0.0408(14) Uani 1 1 d . . . C21 C 0.7358(5) 0.2337(6) -0.2070(4) 0.065(2) Uani 1 1 d . . . H21 H 0.7294 0.2981 -0.2267 0.078 Uiso 1 1 calc R . . C22 C 0.7571(6) 0.1476(6) -0.2355(4) 0.076(3) Uani 1 1 d . . . H22 H 0.7671 0.1543 -0.2738 0.091 Uiso 1 1 calc R . . C23 C 0.7636(5) 0.0521(6) -0.2086(4) 0.063(2) Uani 1 1 d . . . H23 H 0.7763 -0.0074 -0.2285 0.076 Uiso 1 1 calc R . . C24 C 0.7515(3) 0.0451(5) -0.1524(3) 0.0445(16) Uani 1 1 d . . . H24 H 0.7576 -0.0200 -0.1333 0.053 Uiso 1 1 calc R . . C25 C 0.7303(3) 0.1314(4) -0.1220(3) 0.0365(14) Uani 1 1 d . . . C26 C 0.7132(3) 0.1141(4) -0.0637(3) 0.0375(14) Uani 1 1 d . . . C27 C 0.5326(3) 0.2640(4) -0.0951(2) 0.0293(12) Uani 1 1 d . . . H27A H 0.5183 0.2114 -0.0684 0.035 Uiso 1 1 calc R . . H27B H 0.5684 0.2319 -0.1175 0.035 Uiso 1 1 calc R . . C28 C 0.4615(3) 0.3003(4) -0.1366(2) 0.0298(12) Uani 1 1 d . . . H28A H 0.4402 0.2426 -0.1624 0.036 Uiso 1 1 calc R . . H28B H 0.4223 0.3218 -0.1141 0.036 Uiso 1 1 calc R . . C29 C 0.4091(3) 0.4471(4) -0.1958(2) 0.0323(13) Uani 1 1 d . . . H29A H 0.3688 0.3990 -0.2147 0.039 Uiso 1 1 calc R . . H29B H 0.4197 0.4965 -0.2255 0.039 Uiso 1 1 calc R . . C30 C 0.3810(3) 0.5052(4) -0.1477(2) 0.0301(12) Uani 1 1 d . . . H30A H 0.3399 0.5535 -0.1651 0.036 Uiso 1 1 calc R . . H30B H 0.3591 0.4557 -0.1231 0.036 Uiso 1 1 calc R . . C31 C 0.5684(4) 0.4388(5) -0.2362(3) 0.0412(14) Uani 1 1 d . . . H31A H 0.5966 0.4130 -0.2660 0.049 Uiso 1 1 calc R . . H31B H 0.5364 0.4979 -0.2530 0.049 Uiso 1 1 calc R . . C32 C 0.5179(3) 0.3538(4) -0.2199(3) 0.0358(13) Uani 1 1 d . . . H32A H 0.4789 0.3349 -0.2542 0.043 Uiso 1 1 calc R . . H32B H 0.5492 0.2919 -0.2074 0.043 Uiso 1 1 calc R . . C33 C 0.6653(4) -0.0794(5) 0.0812(3) 0.054(2) Uani 1 1 d . . . H33A H 0.7204 -0.0729 0.0954 0.081 Uiso 1 1 calc R . . H33B H 0.6549 -0.1433 0.0586 0.081 Uiso 1 1 calc R . . H33C H 0.6388 -0.0814 0.1143 0.081 Uiso 1 1 calc R . . C34 C 0.8537(4) 0.0817(7) 0.1188(4) 0.072(3) Uani 1 1 d . . . H34A H 0.8527 0.0555 0.0793 0.108 Uiso 1 1 calc R . . H34B H 0.8556 0.0236 0.1458 0.108 Uiso 1 1 calc R . . H34C H 0.8989 0.1253 0.1305 0.108 Uiso 1 1 calc R . . H10 H 0.644(5) 0.417(4) -0.167(3) 0.086 Uiso 1 1 d D . . H16 H 0.664(5) 0.024(8) 0.016(4) 0.086 Uiso 1 1 d . . . H17 H 0.782(5) 0.164(8) 0.155(4) 0.086 Uiso 1 1 d . . . O15A O 1.0111(7) 0.3277(15) -0.0341(7) 0.091(5) Uani 0.42 1 d PD A 1 H15X H 0.9953 0.2896 -0.0629 0.110 Uiso 0.42 1 calc PR A 1 O15B O 0.9790(10) 0.2844(16) 0.0535(8) 0.100(9) Uani 0.30 1 d PD A 3 H15Y H 1.0227 0.3053 0.0690 0.120 Uiso 0.30 1 calc PR A 3 O1S O 0.6501(3) -0.1135(3) 0.2317(2) 0.0559(14) Uani 1 1 d . . . O2S O 0.4837(10) -0.0615(16) 0.3639(7) 0.124(6) Uani 0.50 1 d PDU B 1 H2S H 0.4468 -0.0902 0.3459 0.149 Uiso 0.50 1 d P C 1 O3S O 0.9374(9) 0.0597(11) -0.0627(12) 0.192(13) Uani 0.50 1 d PD . . H3S H 0.9655 0.1087 -0.0636 0.231 Uiso 0.50 1 d P . . O4S O 0.3646(19) -0.308(3) 0.3530(15) 0.229(13) Uani 0.50 1 d PDU D 2 H4S H 0.3918 -0.3534 0.3720 0.275 Uiso 0.50 1 d P E 2 O5S O 0.8222(8) -0.1968(11) -0.0354(8) 0.112(6) Uani 0.50 1 d PD F 4 H5S H 0.7890 -0.1815 -0.0646 0.135 Uiso 0.50 1 calc PR F 4 C1S C 0.7021(4) -0.0285(5) 0.2370(3) 0.057(2) Uani 1 1 d . . . H1S1 H 0.6815 0.0252 0.2089 0.085 Uiso 1 1 calc R . . H1S2 H 0.7515 -0.0521 0.2293 0.085 Uiso 1 1 calc R . . H1S3 H 0.7088 -0.0002 0.2765 0.085 Uiso 1 1 calc R . . C2S C 0.4705(19) 0.0466(17) 0.3704(14) 0.139(10) Uani 0.50 1 d PDU B 1 H2S1 H 0.4761 0.0655 0.4099 0.208 Uiso 0.50 1 d P G 1 H2S2 H 0.4139 0.0580 0.3511 0.208 Uiso 0.50 1 d P H 1 H2S3 H 0.5005 0.0875 0.3486 0.208 Uiso 0.50 1 d P I 1 C3S C 0.9661(15) -0.0324(19) -0.0844(13) 0.144(12) Uani 0.50 1 d PD . . H3S1 H 0.9896 -0.0155 -0.1180 0.216 Uiso 0.50 1 calc PR . . H3S2 H 0.9241 -0.0811 -0.0964 0.216 Uiso 0.50 1 calc PR . . H3S3 H 1.0045 -0.0637 -0.0539 0.216 Uiso 0.50 1 calc PR . . C4S C 0.411(2) -0.217(3) 0.3468(17) 0.171(14) Uani 0.50 1 d PDU D 2 H4S1 H 0.4085 -0.1632 0.3784 0.257 Uiso 0.50 1 d P J 2 H4S2 H 0.3963 -0.1823 0.3097 0.257 Uiso 0.50 1 d P K 2 H4S3 H 0.4685 -0.2316 0.3519 0.257 Uiso 0.50 1 d P L 2 C5S C 0.8919(14) -0.141(3) -0.0376(16) 0.170(14) Uani 0.50 1 d PDU . . H5S1 H 0.9266 -0.1469 0.0000 0.255 Uiso 0.50 1 calc PR F 4 H5S2 H 0.8800 -0.0686 -0.0464 0.255 Uiso 0.50 1 calc PR F 4 H5S3 H 0.9164 -0.1711 -0.0681 0.255 Uiso 0.50 1 calc PR F 4 H1S H 0.669(9) -0.167(13) 0.249(7) 0.204 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0224(4) 0.0118(4) 0.0429(5) -0.0017(3) -0.0174(3) 0.0008(3) Mn2 0.0178(4) 0.0106(4) 0.0400(5) -0.0049(3) -0.0150(3) 0.0033(3) Mn3 0.0206(4) 0.0110(4) 0.0439(5) -0.0046(3) -0.0112(3) 0.0008(3) Mn4 0.0190(4) 0.0136(4) 0.0525(5) -0.0055(3) -0.0078(3) 0.0035(3) Na1 0.0294(11) 0.0149(10) 0.0521(14) -0.0028(9) -0.0160(10) 0.0066(8) O1 0.032(2) 0.0198(19) 0.046(2) 0.0014(17) -0.0186(17) 0.0011(15) O2 0.0260(19) 0.0154(17) 0.050(2) -0.0020(16) -0.0217(17) 0.0016(14) O3 0.024(2) 0.023(2) 0.061(3) -0.0096(18) -0.0224(18) 0.0043(15) O4 0.0229(18) 0.0137(17) 0.042(2) 0.0001(15) -0.0122(15) 0.0014(14) O5 0.0223(17) 0.0106(16) 0.049(2) -0.0024(15) -0.0158(16) -0.0003(14) O6 0.060(3) 0.027(2) 0.085(4) 0.019(2) -0.021(3) -0.003(2) O7 0.0187(17) 0.0123(16) 0.047(2) -0.0086(15) -0.0116(15) 0.0024(13) O8 0.0195(17) 0.0153(17) 0.050(2) -0.0076(16) -0.0160(16) 0.0011(14) O9 0.0197(17) 0.0120(16) 0.044(2) -0.0033(15) -0.0150(15) -0.0011(13) O10 0.033(2) 0.024(2) 0.054(3) -0.0020(18) -0.0031(19) -0.0026(17) O11 0.0202(18) 0.0143(17) 0.061(3) -0.0030(17) -0.0072(17) 0.0017(14) O12 0.0251(19) 0.0124(17) 0.058(3) -0.0064(17) -0.0088(17) 0.0069(14) O13 0.040(2) 0.0202(19) 0.058(3) -0.0044(18) 0.005(2) 0.0068(17) O14 0.078(3) 0.014(2) 0.074(3) -0.007(2) 0.010(3) 0.007(2) O15 0.038(11) 0.16(3) 0.094(18) 0.015(18) 0.007(12) 0.046(15) O16 0.047(3) 0.0153(19) 0.055(3) 0.0009(18) -0.013(2) 0.0066(17) O17 0.040(2) 0.037(2) 0.063(3) -0.009(2) -0.023(2) 0.018(2) N1 0.028(2) 0.014(2) 0.052(3) 0.001(2) -0.012(2) 0.0013(18) N2 0.019(2) 0.0103(19) 0.044(3) -0.0049(18) -0.0165(18) 0.0021(17) N3 0.027(2) 0.011(2) 0.047(3) -0.0054(19) -0.013(2) 0.0075(19) N4 0.022(2) 0.021(2) 0.072(4) -0.011(2) -0.018(2) -0.006(2) N5 0.019(2) 0.027(3) 0.071(4) -0.003(2) -0.010(2) 0.0019(19) N6 0.027(2) 0.017(2) 0.039(3) -0.0037(19) -0.0089(19) 0.0007(18) C1 0.038(3) 0.025(3) 0.043(3) 0.005(2) -0.018(3) -0.010(2) C2 0.036(3) 0.073(5) 0.053(4) 0.019(4) -0.016(3) -0.006(3) C3 0.048(4) 0.126(9) 0.052(5) 0.031(5) -0.012(4) -0.013(5) C4 0.041(4) 0.090(6) 0.059(5) 0.036(4) -0.027(4) -0.013(4) C5 0.039(3) 0.036(3) 0.054(4) 0.015(3) -0.025(3) -0.007(3) C6 0.030(3) 0.014(2) 0.055(4) 0.008(2) -0.021(3) -0.007(2) C7 0.037(3) 0.005(2) 0.055(4) 0.000(2) -0.018(3) -0.002(2) C8 0.028(3) 0.025(3) 0.053(4) 0.001(3) -0.014(3) -0.003(2) C9 0.023(3) 0.025(3) 0.051(3) 0.002(2) -0.006(2) -0.002(2) C10 0.035(3) 0.013(2) 0.053(4) -0.006(2) -0.017(3) -0.002(2) C11 0.030(3) 0.014(2) 0.046(3) -0.004(2) -0.018(2) -0.004(2) C12 0.040(3) 0.013(3) 0.057(4) 0.004(2) -0.020(3) -0.005(2) C13 0.044(4) 0.015(3) 0.072(5) 0.008(3) -0.020(3) -0.005(2) C14 0.025(3) 0.028(3) 0.061(4) -0.002(3) -0.022(3) 0.001(2) C15 0.023(3) 0.020(3) 0.054(4) -0.011(2) -0.020(2) -0.001(2) C16 0.024(3) 0.025(3) 0.074(5) -0.005(3) -0.006(3) -0.004(2) C17 0.024(3) 0.030(3) 0.074(5) -0.002(3) -0.002(3) -0.008(2) C18 0.026(3) 0.054(4) 0.083(5) -0.006(4) 0.004(3) 0.009(3) C19 0.027(4) 0.144(11) 0.119(9) -0.029(8) 0.005(5) 0.017(5) C20 0.033(3) 0.026(3) 0.063(4) -0.009(3) 0.009(3) 0.002(2) C21 0.085(6) 0.040(4) 0.078(6) 0.003(4) 0.038(5) 0.012(4) C22 0.102(7) 0.048(5) 0.093(7) -0.011(4) 0.054(6) -0.002(5) C23 0.060(5) 0.040(4) 0.096(6) -0.015(4) 0.030(4) 0.007(3) C24 0.029(3) 0.027(3) 0.079(5) -0.014(3) 0.013(3) 0.001(2) C25 0.021(3) 0.019(3) 0.066(4) -0.013(3) 0.000(3) 0.002(2) C26 0.027(3) 0.019(3) 0.062(4) -0.010(3) -0.005(3) 0.003(2) C27 0.024(3) 0.017(2) 0.041(3) -0.008(2) -0.009(2) 0.001(2) C28 0.027(3) 0.015(2) 0.040(3) -0.006(2) -0.011(2) -0.003(2) C29 0.029(3) 0.019(3) 0.040(3) -0.003(2) -0.017(2) -0.002(2) C30 0.025(3) 0.014(2) 0.042(3) -0.006(2) -0.019(2) 0.000(2) C31 0.045(3) 0.026(3) 0.049(4) -0.004(3) 0.000(3) -0.004(3) C32 0.036(3) 0.022(3) 0.045(3) -0.006(2) -0.003(3) -0.003(2) C33 0.067(5) 0.017(3) 0.063(4) 0.001(3) -0.026(4) 0.004(3) C34 0.046(4) 0.063(5) 0.094(6) -0.013(5) -0.017(4) 0.035(4) O15A 0.047(8) 0.108(14) 0.113(14) -0.012(11) 0.001(8) 0.012(8) O15B 0.035(10) 0.078(15) 0.17(2) -0.027(15) -0.022(13) 0.035(10) O1S 0.043(3) 0.017(2) 0.090(4) 0.004(2) -0.032(2) -0.0004(18) O2S 0.120(9) 0.150(10) 0.100(8) 0.039(8) 0.012(7) 0.029(8) O3S 0.076(10) 0.049(8) 0.40(3) -0.057(14) -0.095(15) 0.038(8) O4S 0.236(16) 0.220(16) 0.232(16) 0.015(10) 0.049(10) -0.016(10) O5S 0.065(8) 0.071(9) 0.180(17) 0.040(10) -0.029(9) -0.037(7) C1S 0.050(4) 0.021(3) 0.081(5) 0.001(3) -0.038(4) -0.002(3) C2S 0.152(13) 0.135(13) 0.130(13) -0.018(9) 0.029(9) 0.000(9) C3S 0.089(18) 0.21(4) 0.14(3) 0.00(2) 0.058(18) 0.01(2) C4S 0.176(16) 0.172(17) 0.162(16) 0.007(10) 0.024(10) 0.012(10) C5S 0.163(16) 0.178(16) 0.165(16) -0.012(10) 0.021(10) 0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.868(4) . ? Mn1 O4 1.925(3) . ? Mn1 O5 1.936(4) . ? Mn1 O2 1.964(4) . ? Mn1 O9 2.169(4) 3_665 ? Mn1 N1 2.324(4) . ? Mn2 O9 2.145(4) 3_665 ? Mn2 O7 2.153(4) . ? Mn2 O8 2.193(4) . ? Mn2 O5 2.214(4) . ? Mn2 N2 2.252(4) 3_665 ? Mn2 N2 2.291(4) . ? Mn3 O4 2.143(3) 3_665 ? Mn3 O7 2.236(4) . ? Mn3 O11 2.249(4) . ? Mn3 O9 2.278(3) . ? Mn3 O10 2.302(5) . ? Mn3 N6 2.402(4) . ? Mn3 N2 2.465(5) . ? Mn4 O11 1.890(4) . ? Mn4 O13 1.908(5) . ? Mn4 O12 1.931(4) . ? Mn4 O8 1.961(4) . ? Mn4 O7 2.186(3) . ? Mn4 N5 2.311(5) . ? Na1 O17 2.287(4) . ? Na1 O16 2.355(4) . ? Na1 O8 2.416(4) . ? Na1 O5 2.427(4) . ? Na1 O12 2.494(5) . ? Na1 O2 2.525(5) . ? Na1 H16 2.36(10) . ? Na1 H17 2.58(10) . ? O1 C1 1.323(7) . ? O2 C7 1.309(7) . ? O3 C7 1.258(7) . ? O4 C9 1.415(7) . ? O4 Mn3 2.143(3) 3_665 ? O5 C11 1.445(6) . ? O6 C13 1.425(8) . ? O6 H6 0.8400 . ? O7 C27 1.421(6) . ? O8 C15 1.431(6) . ? O9 C30 1.418(6) . ? O9 Mn2 2.145(4) 3_665 ? O9 Mn1 2.169(4) 3_665 ? O10 C31 1.446(7) . ? O10 H10 0.891(10) . ? O11 C17 1.420(7) . ? O12 C26 1.301(7) . ? O13 C20 1.346(7) . ? O14 C26 1.242(8) . ? O15 C19 1.404(10) . ? O15 H15 0.8400 . ? O16 C33 1.430(7) . ? O16 H16 0.91(9) . ? O17 C34 1.408(8) . ? O17 H17 0.90(9) . ? N1 C12 1.477(7) . ? N1 C10 1.482(8) . ? N1 C8 1.490(7) . ? N2 N3 1.211(6) . ? N2 Mn2 2.252(4) 3_665 ? N3 N4 1.150(6) . ? N5 C14 1.469(9) . ? N5 C18 1.482(8) . ? N5 C16 1.493(8) . ? N6 C32 1.478(8) . ? N6 C28 1.479(7) . ? N6 C29 1.487(6) . ? C1 C2 1.386(10) . ? C1 C6 1.426(9) . ? C2 C3 1.384(10) . ? C2 H2 0.9500 . ? C3 C4 1.394(12) . ? C3 H3 0.9500 . ? C4 C5 1.359(11) . ? C4 H4 0.9500 . ? C5 C6 1.406(8) . ? C5 H5 0.9500 . ? C6 C7 1.449(9) . ? C8 C9 1.514(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.507(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.531(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.517(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.523(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.510(10) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O15A 1.393(9) . ? C19 O15B 1.410(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.397(10) . ? C20 C25 1.400(9) . ? C21 C22 1.388(11) . ? C21 H21 0.9500 . ? C22 C23 1.382(12) . ? C22 H22 0.9500 . ? C23 C24 1.375(11) . ? C23 H23 0.9500 . ? C24 C25 1.413(8) . ? C24 H24 0.9500 . ? C25 C26 1.469(10) . ? C27 C28 1.519(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.513(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.515(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O15A H15X 0.8400 . ? O15B H15Y 0.8400 . ? O1S C1S 1.429(8) . ? O1S H1S 0.84(17) . ? O2S C2S 1.432(10) . ? O2S H2S 0.8019 . ? O3S C3S 1.428(10) . ? O3S H3S 0.8102 . ? O4S C4S 1.456(10) . ? O4S H4S 0.8369 . ? O5S C5S 1.443(10) . ? O5S H5S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S H2S1 0.9451 . ? C2S H2S2 1.0343 . ? C2S H2S3 0.9627 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4S H4S1 1.0281 . ? C4S H4S2 0.9707 . ? C4S H4S3 1.0234 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 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 O4 88.55(17) . . ? O1 Mn1 O5 175.88(15) . . ? O4 Mn1 O5 94.60(16) . . ? O1 Mn1 O2 90.38(17) . . ? O4 Mn1 O2 178.45(16) . . ? O5 Mn1 O2 86.52(16) . . ? O1 Mn1 O9 98.58(16) . 3_665 ? O4 Mn1 O9 81.61(14) . 3_665 ? O5 Mn1 O9 84.53(15) . 3_665 ? O2 Mn1 O9 97.44(14) . 3_665 ? O1 Mn1 N1 95.95(18) . . ? O4 Mn1 N1 79.12(15) . . ? O5 Mn1 N1 82.07(17) . . ? O2 Mn1 N1 102.12(15) . . ? O9 Mn1 N1 155.48(14) 3_665 . ? O9 Mn2 O7 175.86(13) 3_665 . ? O9 Mn2 O8 98.26(14) 3_665 . ? O7 Mn2 O8 78.11(14) . . ? O9 Mn2 O5 78.77(14) 3_665 . ? O7 Mn2 O5 103.08(14) . . ? O8 Mn2 O5 90.22(14) . . ? O9 Mn2 N2 85.34(15) 3_665 3_665 ? O7 Mn2 N2 98.10(15) . 3_665 ? O8 Mn2 N2 173.62(16) . 3_665 ? O5 Mn2 N2 95.66(15) . 3_665 ? O9 Mn2 N2 93.05(15) 3_665 . ? O7 Mn2 N2 85.58(15) . . ? O8 Mn2 N2 98.36(14) . . ? O5 Mn2 N2 168.95(16) . . ? N2 Mn2 N2 76.11(17) 3_665 . ? O4 Mn3 O7 162.37(14) 3_665 . ? O4 Mn3 O11 97.10(13) 3_665 . ? O7 Mn3 O11 73.72(13) . . ? O4 Mn3 O9 74.60(13) 3_665 . ? O7 Mn3 O9 106.96(13) . . ? O11 Mn3 O9 154.00(14) . . ? O4 Mn3 O10 88.47(15) 3_665 . ? O7 Mn3 O10 103.66(14) . . ? O11 Mn3 O10 77.20(15) . . ? O9 Mn3 O10 126.13(14) . . ? O4 Mn3 N6 122.09(14) 3_665 . ? O7 Mn3 N6 74.22(14) . . ? O11 Mn3 N6 129.60(14) . . ? O9 Mn3 N6 73.33(14) . . ? O10 Mn3 N6 73.88(16) . . ? O4 Mn3 N2 83.48(14) 3_665 . ? O7 Mn3 N2 79.80(14) . . ? O11 Mn3 N2 76.80(15) . . ? O9 Mn3 N2 77.78(14) . . ? O10 Mn3 N2 151.56(14) . . ? N6 Mn3 N2 132.89(16) . . ? O11 Mn4 O13 87.40(18) . . ? O11 Mn4 O12 177.73(18) . . ? O13 Mn4 O12 90.55(18) . . ? O11 Mn4 O8 94.91(17) . . ? O13 Mn4 O8 177.65(16) . . ? O12 Mn4 O8 87.14(17) . . ? O11 Mn4 O7 82.26(14) . . ? O13 Mn4 O7 97.44(17) . . ? O12 Mn4 O7 97.06(14) . . ? O8 Mn4 O7 82.47(15) . . ? O11 Mn4 N5 81.05(16) . . ? O13 Mn4 N5 99.9(2) . . ? O12 Mn4 N5 100.27(16) . . ? O8 Mn4 N5 80.96(18) . . ? O7 Mn4 N5 155.29(16) . . ? O17 Na1 O16 92.83(17) . . ? O17 Na1 O8 104.77(17) . . ? O16 Na1 O8 148.50(18) . . ? O17 Na1 O5 149.8(2) . . ? O16 Na1 O5 97.55(16) . . ? O8 Na1 O5 80.28(13) . . ? O17 Na1 O12 99.28(19) . . ? O16 Na1 O12 85.55(17) . . ? O8 Na1 O12 66.20(14) . . ? O5 Na1 O12 109.70(15) . . ? O17 Na1 O2 84.58(17) . . ? O16 Na1 O2 114.44(18) . . ? O8 Na1 O2 93.38(14) . . ? O5 Na1 O2 65.30(13) . . ? O12 Na1 O2 159.56(15) . . ? O17 Na1 H16 91(2) . . ? O16 Na1 H16 22(2) . . ? O8 Na1 H16 129(2) . . ? O5 Na1 H16 109(2) . . ? O12 Na1 H16 64(2) . . ? O2 Na1 H16 136(2) . . ? O17 Na1 H17 20(2) . . ? O16 Na1 H17 102(2) . . ? O8 Na1 H17 103(2) . . ? O5 Na1 H17 130(2) . . ? O12 Na1 H17 117(2) . . ? O2 Na1 H17 64(2) . . ? H16 Na1 H17 106(3) . . ? C1 O1 Mn1 129.4(4) . . ? C7 O2 Mn1 129.1(4) . . ? C7 O2 Na1 129.0(4) . . ? Mn1 O2 Na1 101.84(16) . . ? C9 O4 Mn1 111.5(3) . . ? C9 O4 Mn3 130.7(3) . 3_665 ? Mn1 O4 Mn3 107.15(16) . 3_665 ? C11 O5 Mn1 113.6(4) . . ? C11 O5 Mn2 129.2(3) . . ? Mn1 O5 Mn2 100.78(15) . . ? C11 O5 Na1 109.9(3) . . ? Mn1 O5 Na1 106.25(15) . . ? Mn2 O5 Na1 93.94(15) . . ? C13 O6 H6 109.5 . . ? C27 O7 Mn2 127.2(3) . . ? C27 O7 Mn4 112.8(3) . . ? Mn2 O7 Mn4 96.23(14) . . ? C27 O7 Mn3 116.7(3) . . ? Mn2 O7 Mn3 102.31(14) . . ? Mn4 O7 Mn3 95.62(14) . . ? C15 O8 Mn4 116.4(4) . . ? C15 O8 Mn2 128.7(3) . . ? Mn4 O8 Mn2 101.98(15) . . ? C15 O8 Na1 106.7(3) . . ? Mn4 O8 Na1 103.80(16) . . ? Mn2 O8 Na1 94.79(15) . . ? C30 O9 Mn2 124.1(3) . 3_665 ? C30 O9 Mn1 116.5(3) . 3_665 ? Mn2 O9 Mn1 95.85(13) 3_665 3_665 ? C30 O9 Mn3 117.3(3) . . ? Mn2 O9 Mn3 102.73(14) 3_665 . ? Mn1 O9 Mn3 94.83(14) 3_665 . ? C31 O10 Mn3 111.6(4) . . ? C31 O10 H10 109(6) . . ? Mn3 O10 H10 89(6) . . ? C17 O11 Mn4 112.5(3) . . ? C17 O11 Mn3 134.0(4) . . ? Mn4 O11 Mn3 104.38(16) . . ? C26 O12 Mn4 131.6(4) . . ? C26 O12 Na1 126.3(4) . . ? Mn4 O12 Na1 101.96(17) . . ? C20 O13 Mn4 128.5(4) . . ? C19 O15 H15 109.5 . . ? C33 O16 Na1 125.3(4) . . ? C33 O16 H16 118(6) . . ? Na1 O16 H16 79(6) . . ? C34 O17 Na1 144.0(5) . . ? C34 O17 H17 116(6) . . ? Na1 O17 H17 99(6) . . ? C12 N1 C10 113.8(4) . . ? C12 N1 C8 113.3(5) . . ? C10 N1 C8 113.2(4) . . ? C12 N1 Mn1 110.1(3) . . ? C10 N1 Mn1 100.9(3) . . ? C8 N1 Mn1 104.3(3) . . ? N3 N2 Mn2 126.0(3) . 3_665 ? N3 N2 Mn2 123.3(3) . . ? Mn2 N2 Mn2 103.89(17) 3_665 . ? N3 N2 Mn3 107.9(4) . . ? Mn2 N2 Mn3 94.12(15) 3_665 . ? Mn2 N2 Mn3 91.88(14) . . ? N4 N3 N2 178.9(6) . . ? C14 N5 C18 113.3(5) . . ? C14 N5 C16 113.3(5) . . ? C18 N5 C16 113.2(6) . . ? C14 N5 Mn4 101.5(3) . . ? C18 N5 Mn4 111.1(4) . . ? C16 N5 Mn4 103.5(3) . . ? C32 N6 C28 112.1(4) . . ? C32 N6 C29 110.6(4) . . ? C28 N6 C29 110.2(4) . . ? C32 N6 Mn3 110.0(3) . . ? C28 N6 Mn3 106.7(3) . . ? C29 N6 Mn3 107.0(3) . . ? O1 C1 C2 118.6(6) . . ? O1 C1 C6 123.2(6) . . ? C2 C1 C6 118.2(5) . . ? C3 C2 C1 121.8(8) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 119.8(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.7(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.8(7) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 118.7(7) . . ? C5 C6 C7 118.9(6) . . ? C1 C6 C7 122.5(5) . . ? O3 C7 O2 118.7(6) . . ? O3 C7 C6 120.4(5) . . ? O2 C7 C6 120.9(5) . . ? N1 C8 C9 110.1(4) . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? O4 C9 C8 108.9(5) . . ? O4 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? O4 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N1 C10 C11 109.9(4) . . ? N1 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N1 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? O5 C11 C10 109.7(4) . . ? O5 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? O5 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N1 C12 C13 115.9(5) . . ? N1 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? N1 C12 H12B 108.3 . . ? C13 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? O6 C13 C12 110.2(5) . . ? O6 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? O6 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N5 C14 C15 110.9(4) . . ? N5 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.0 . . ? O8 C15 C14 109.6(5) . . ? O8 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? O8 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N5 C16 C17 109.5(5) . . ? N5 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? N5 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? O11 C17 C16 109.4(5) . . ? O11 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? O11 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? N5 C18 C19 116.0(7) . . ? N5 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? N5 C18 H18B 108.3 . . ? C19 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? O15A C19 O15 83.0(14) . . ? O15A C19 O15B 110.1(13) . . ? O15 C19 O15B 92.7(15) . . ? O15A C19 C18 116.2(10) . . ? O15 C19 C18 127.1(13) . . ? O15B C19 C18 120.5(12) . . ? O15A C19 H19A 108.2 . . ? O15B C19 H19A 89.6 . . ? C18 C19 H19A 108.2 . . ? O15A C19 H19B 108.2 . . ? O15 C19 H19B 111.0 . . ? C18 C19 H19B 108.2 . . ? H19A C19 H19B 107.4 . . ? O13 C20 C21 117.3(6) . . ? O13 C20 C25 123.9(6) . . ? C21 C20 C25 118.7(6) . . ? C22 C21 C20 121.3(8) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 120.5(8) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 118.7(7) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 122.2(7) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C20 C25 C24 118.5(6) . . ? C20 C25 C26 123.6(5) . . ? C24 C25 C26 117.9(6) . . ? O14 C26 O12 119.8(6) . . ? O14 C26 C25 119.5(5) . . ? O12 C26 C25 120.7(5) . . ? O7 C27 C28 110.2(4) . . ? O7 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? O7 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? N6 C28 C27 110.7(4) . . ? N6 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? N6 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? N6 C29 C30 110.8(4) . . ? N6 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? O9 C30 C29 111.5(4) . . ? O9 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? O9 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? O10 C31 C32 109.9(5) . . ? O10 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O10 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? N6 C32 C31 110.7(5) . . ? N6 C32 H32A 109.5 . . ? C31 C32 H32A 109.5 . . ? N6 C32 H32B 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? O16 C33 H33A 109.5 . . ? O16 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O16 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O17 C34 H34A 109.5 . . ? O17 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O17 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C19 O15A H15X 109.5 . . ? C19 O15B H15Y 109.5 . . ? C1S O1S H1S 114(10) . . ? C2S O2S H2S 112.0 . . ? C3S O3S H3S 112.4 . . ? C4S O4S H4S 109.6 . . ? C5S O5S H5S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2S C2S H2S1 111.6 . . ? O2S C2S H2S2 105.0 . . ? H2S1 C2S H2S2 107.8 . . ? O2S C2S H2S3 111.3 . . ? H2S1 C2S H2S3 114.0 . . ? H2S2 C2S H2S3 106.5 . . ? O3S C3S H3S1 109.5 . . ? O3S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? O3S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? O4S C4S H4S1 111.9 . . ? O4S C4S H4S2 113.6 . . ? H4S1 C4S H4S2 106.3 . . ? O4S C4S H4S3 114.8 . . ? H4S1 C4S H4S3 102.5 . . ? H4S2 C4S H4S3 106.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.374 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.116 # Attachment '- 3 Na2Mn8 1-D final.CIF' #========================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 822746' #TrackingRef '- 3 Na2Mn8 1-D final.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains half the cluster as well as solvent MeoH molecules. In the ASU several of the solvent MeOH molecules have been modelled at 0.5 occupancy with bond (DFIX) and thermal (ISOR) restraints placed on them. All non H atoms were refined anisotropically and all H atoms were placed in calculated positions except for on one of the disordered MeOH solvent molecules. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H130 Mn8 N12 Na2 O39' _chemical_formula_weight 2285.33 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' Na Na 0.0362 0.0249 '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 12.8576(3) _cell_length_b 14.5491(3) _cell_length_c 14.8713(3) _cell_angle_alpha 76.2500(10) _cell_angle_beta 68.6450(10) _cell_angle_gamma 84.7590(10) _cell_volume 2516.64(9) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8967 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.12 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1178 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.606 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28474 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11452 _reflns_number_gt 9616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 structure was solved by direct methods. The asymmetric unit contains half the cluster as well as solvent MeoH molecules. In the ASU several of the solvent MeOH molecules have been modelled at 0.5 occupancy with bond (DFIX) and thermal (ISOR) restraints placed on them. All non H atoms were refined anisotropically and all H atoms were placed in calculated positions except for on one of the disordered MeOH solvent molecules. ; _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^)+(0.0876P)^2^+6.8103P] 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 11452 _refine_ls_number_parameters 640 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1630 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.22462(4) 0.24070(4) 0.40450(4) 0.01999(14) Uani 1 1 d . . . Mn2 Mn 0.13909(4) 0.03377(4) 0.41924(4) 0.01764(13) Uani 1 1 d . . . Mn3 Mn 0.04178(4) -0.19184(4) 0.46179(4) 0.01846(13) Uani 1 1 d . . . Mn4 Mn 0.27174(4) -0.11087(4) 0.28052(4) 0.01895(14) Uani 1 1 d . . . Na1 Na 0.40451(12) 0.08505(11) 0.27753(11) 0.0239(3) Uani 1 1 d . . . O1 O 0.1916(2) 0.36980(19) 0.3667(2) 0.0265(6) Uani 1 1 d . . . O2 O 0.3426(2) 0.2464(2) 0.27689(19) 0.0279(6) Uani 1 1 d . . . O3 O 0.4786(3) 0.3113(3) 0.1399(3) 0.0599(11) Uani 1 1 d . . . O4 O 0.1141(2) 0.23541(18) 0.53372(18) 0.0212(5) Uani 1 1 d . . . O5 O 0.2701(2) 0.10835(18) 0.43483(18) 0.0204(5) Uani 1 1 d . . . O6 O 0.5570(3) 0.4320(3) 0.4467(3) 0.0594(11) Uani 1 1 d . . . H6 H 0.5879 0.4359 0.3870 0.071 Uiso 1 1 calc R . . O7 O 0.1955(2) -0.11121(17) 0.43707(17) 0.0189(5) Uani 1 1 d . . . O8 O 0.2423(2) 0.02442(18) 0.26720(17) 0.0196(5) Uani 1 1 d . . . O9 O -0.0867(2) -0.17813(18) 0.61224(18) 0.0200(5) Uani 1 1 d . . . O10 O 0.1119(2) -0.32988(19) 0.4110(2) 0.0254(6) Uani 1 1 d . . . O11 O 0.1247(2) -0.14232(18) 0.29902(18) 0.0215(5) Uani 1 1 d . . . O12 O 0.4229(2) -0.08296(19) 0.26476(19) 0.0233(5) Uani 1 1 d . . . O13 O 0.3085(2) -0.24149(18) 0.2919(2) 0.0245(5) Uani 1 1 d . . . O14 O 0.6002(2) -0.1027(2) 0.2483(2) 0.0356(7) Uani 1 1 d . . . O15 O 0.4935(3) -0.1361(2) -0.1109(2) 0.0370(7) Uani 1 1 d . . . O16 O 0.5633(3) 0.0549(2) 0.3217(3) 0.0372(7) Uani 1 1 d . . . N1 N 0.3344(3) 0.2584(2) 0.4946(2) 0.0261(7) Uani 1 1 d . . . N2 N -0.0235(2) -0.0263(2) 0.4244(2) 0.0209(6) Uani 1 1 d . . . N3 N -0.0505(2) -0.0115(2) 0.3522(2) 0.0232(6) Uani 1 1 d . . . N4 N -0.0751(3) 0.0018(3) 0.2830(3) 0.0344(8) Uani 1 1 d . . . N5 N 0.2806(3) -0.0746(2) 0.1172(2) 0.0239(6) Uani 1 1 d . . . N6 N 0.1166(2) -0.2783(2) 0.5809(2) 0.0213(6) Uani 1 1 d . . . C1 C 0.2272(4) 0.4265(3) 0.2768(3) 0.0322(9) Uani 1 1 d . . . C2 C 0.1683(4) 0.5109(3) 0.2596(3) 0.0386(10) Uani 1 1 d . . . H2 H 0.1051 0.5249 0.3102 0.046 Uiso 1 1 calc R . . C3 C 0.2030(6) 0.5737(4) 0.1685(4) 0.0566(15) Uani 1 1 d . . . H3 H 0.1620 0.6288 0.1586 0.068 Uiso 1 1 calc R . . C4 C 0.2972(7) 0.5560(4) 0.0921(4) 0.070(2) Uani 1 1 d . . . H4 H 0.3207 0.5993 0.0316 0.084 Uiso 1 1 calc R . . C5 C 0.3553(6) 0.4742(4) 0.1067(4) 0.0648(18) Uani 1 1 d . . . H5 H 0.4187 0.4622 0.0553 0.078 Uiso 1 1 calc R . . C6 C 0.3221(4) 0.4072(3) 0.1974(3) 0.0430(12) Uani 1 1 d . . . C7 C 0.3859(4) 0.3181(3) 0.2045(3) 0.0398(11) Uani 1 1 d . . . C8 C 0.2531(3) 0.2656(3) 0.5936(3) 0.0322(9) Uani 1 1 d . . . H8A H 0.2785 0.3119 0.6184 0.039 Uiso 1 1 calc R . . H8B H 0.2466 0.2050 0.6398 0.039 Uiso 1 1 calc R . . C9 C 0.1404(3) 0.2956(3) 0.5842(3) 0.0274(8) Uani 1 1 d . . . H9A H 0.0834 0.2910 0.6493 0.033 Uiso 1 1 calc R . . H9B H 0.1435 0.3607 0.5477 0.033 Uiso 1 1 calc R . . C10 C 0.3962(3) 0.1682(3) 0.4955(3) 0.0269(8) Uani 1 1 d . . . H10A H 0.4250 0.1553 0.5491 0.032 Uiso 1 1 calc R . . H10B H 0.4591 0.1728 0.4338 0.032 Uiso 1 1 calc R . . C11 C 0.3207(3) 0.0870(3) 0.5086(3) 0.0261(8) Uani 1 1 d . . . H11A H 0.3645 0.0292 0.5032 0.031 Uiso 1 1 calc R . . H11B H 0.2632 0.0770 0.5739 0.031 Uiso 1 1 calc R . . C12 C 0.4081(3) 0.3416(3) 0.4466(3) 0.0327(9) Uani 1 1 d . . . H12A H 0.3622 0.3983 0.4510 0.039 Uiso 1 1 calc R . . H12B H 0.4446 0.3413 0.3770 0.039 Uiso 1 1 calc R . . C13 C 0.4973(4) 0.3476(4) 0.4895(4) 0.0453(12) Uani 1 1 d . . . H13A H 0.4623 0.3426 0.5603 0.054 Uiso 1 1 calc R . . H13B H 0.5487 0.2948 0.4791 0.054 Uiso 1 1 calc R . . C14 C 0.2966(3) 0.0283(3) 0.0921(3) 0.0268(8) Uani 1 1 d . . . H14A H 0.2765 0.0562 0.0346 0.032 Uiso 1 1 calc R . . H14B H 0.3747 0.0419 0.0757 0.032 Uiso 1 1 calc R . . C15 C 0.2252(3) 0.0722(3) 0.1787(3) 0.0260(8) Uani 1 1 d . . . H15A H 0.2443 0.1384 0.1641 0.031 Uiso 1 1 calc R . . H15B H 0.1470 0.0686 0.1875 0.031 Uiso 1 1 calc R . . C16 C 0.1683(3) -0.1003(3) 0.1238(3) 0.0276(8) Uani 1 1 d . . . H16A H 0.1750 -0.1255 0.0671 0.033 Uiso 1 1 calc R . . H16B H 0.1209 -0.0445 0.1235 0.033 Uiso 1 1 calc R . . C17 C 0.1166(3) -0.1740(3) 0.2187(3) 0.0269(8) Uani 1 1 d . . . H17A H 0.0388 -0.1832 0.2295 0.032 Uiso 1 1 calc R . . H17B H 0.1554 -0.2340 0.2137 0.032 Uiso 1 1 calc R . . C18 C 0.3717(3) -0.1254(3) 0.0551(3) 0.0274(8) Uani 1 1 d . . . H18A H 0.3556 -0.1925 0.0773 0.033 Uiso 1 1 calc R . . H18B H 0.4399 -0.1155 0.0652 0.033 Uiso 1 1 calc R . . C19 C 0.3921(4) -0.0964(4) -0.0552(3) 0.0370(10) Uani 1 1 d . . . H19A H 0.3304 -0.1176 -0.0679 0.044 Uiso 1 1 calc R . . H19B H 0.3954 -0.0280 -0.0761 0.044 Uiso 1 1 calc R . . C20 C 0.4096(3) -0.2817(3) 0.2661(3) 0.0282(8) Uani 1 1 d . . . C21 C 0.4139(4) -0.3761(4) 0.2604(5) 0.0516(14) Uani 1 1 d . . . H21 H 0.3483 -0.4080 0.2751 0.062 Uiso 1 1 calc R . . C22 C 0.5154(5) -0.4228(5) 0.2331(7) 0.092(3) Uani 1 1 d . . . H22 H 0.5179 -0.4859 0.2292 0.111 Uiso 1 1 calc R . . C23 C 0.6130(5) -0.3760(5) 0.2114(8) 0.109(4) Uani 1 1 d . . . H23 H 0.6812 -0.4074 0.1926 0.131 Uiso 1 1 calc R . . C24 C 0.6098(4) -0.2825(4) 0.2177(5) 0.0598(17) Uani 1 1 d . . . H24 H 0.6760 -0.2517 0.2038 0.072 Uiso 1 1 calc R . . C25 C 0.5091(3) -0.2340(3) 0.2445(3) 0.0310(9) Uani 1 1 d . . . C26 C 0.5123(3) -0.1356(3) 0.2526(3) 0.0251(8) Uani 1 1 d . . . C27 C 0.2630(3) -0.1573(3) 0.4922(3) 0.0229(7) Uani 1 1 d . . . H27A H 0.3049 -0.1104 0.5014 0.027 Uiso 1 1 calc R . . H27B H 0.3159 -0.1990 0.4554 0.027 Uiso 1 1 calc R . . C28 C 0.1921(3) -0.2142(3) 0.5922(3) 0.0231(7) Uani 1 1 d . . . H28A H 0.2401 -0.2511 0.6249 0.028 Uiso 1 1 calc R . . H28B H 0.1481 -0.1716 0.6333 0.028 Uiso 1 1 calc R . . C29 C 0.0215(3) -0.3063(3) 0.6741(3) 0.0250(8) Uani 1 1 d . . . H29A H 0.0490 -0.3291 0.7281 0.030 Uiso 1 1 calc R . . H29B H -0.0183 -0.3576 0.6697 0.030 Uiso 1 1 calc R . . C30 C -0.0584(3) -0.2240(3) 0.6957(3) 0.0229(7) Uani 1 1 d . . . H30A H -0.1258 -0.2471 0.7508 0.027 Uiso 1 1 calc R . . H30B H -0.0240 -0.1788 0.7148 0.027 Uiso 1 1 calc R . . C31 C 0.1216(3) -0.4021(3) 0.4918(3) 0.0284(8) Uani 1 1 d . . . H31A H 0.1652 -0.4545 0.4668 0.034 Uiso 1 1 calc R . . H31B H 0.0480 -0.4254 0.5357 0.034 Uiso 1 1 calc R . . C32 C 0.1773(3) -0.3632(3) 0.5485(3) 0.0269(8) Uani 1 1 d . . . H32A H 0.1783 -0.4113 0.6060 0.032 Uiso 1 1 calc R . . H32B H 0.2540 -0.3467 0.5068 0.032 Uiso 1 1 calc R . . C33 C 0.6577(4) 0.1134(3) 0.2834(4) 0.0386(10) Uani 1 1 d . . . H33A H 0.6759 0.1360 0.2133 0.058 Uiso 1 1 calc R . . H33B H 0.7196 0.0780 0.2959 0.058 Uiso 1 1 calc R . . H33C H 0.6419 0.1662 0.3147 0.058 Uiso 1 1 calc R . . H15 H 0.480(5) -0.190(4) -0.099(4) 0.046 Uiso 1 1 d . . . H18 H 0.578(5) 0.017(4) 0.297(4) 0.046 Uiso 1 1 d . . . O7' O 1.030(3) 0.178(3) -0.007(2) 0.36(2) Uani 0.50 1 d PDU A 1 O2S O 0.7098(6) 0.4032(6) 0.2607(5) 0.114(2) Uani 1 1 d . . . H2S H 0.7754 0.4125 0.2509 0.137 Uiso 1 1 calc R . . O3S O 0.8931(6) 0.5147(6) 0.1784(6) 0.058(2) Uani 0.50 1 d P . . H3S H 0.9330 0.5176 0.1205 0.070 Uiso 0.50 1 calc PR . . O5S O -0.059(3) -0.427(2) 0.976(3) 0.335(18) Uiso 0.50 1 d PD . . H5S H -0.0445 -0.4678 0.9217 0.402 Uiso 0.50 1 d P . . O6S O 0.7993(18) -0.1409(14) 0.1084(16) 0.200 Uiso 0.50 1 d PD . . H6S H 0.7315 -0.1317 0.1196 0.240 Uiso 0.50 1 d P . . O7S O 0.8924(12) 0.2367(10) 0.0281(10) 0.113(4) Uani 0.50 1 d PU A 2 C2S C 0.7014(8) 0.3812(6) 0.1748(7) 0.091(2) Uani 1 1 d . . . H2S1 H 0.6401 0.3389 0.1945 0.137 Uiso 1 1 calc R . . H2S2 H 0.7694 0.3516 0.1405 0.137 Uiso 1 1 calc R . . H2S3 H 0.6892 0.4384 0.1319 0.137 Uiso 1 1 calc R . . C3S C 0.9057(12) 0.5914(10) 0.2049(13) 0.077(4) Uani 0.50 1 d P . . H3S1 H 0.8228 0.6196 0.2380 0.116 Uiso 0.50 1 d P . . H3S2 H 0.9394 0.5906 0.2477 0.116 Uiso 0.50 1 d P . . H3S3 H 0.9325 0.6475 0.1463 0.116 Uiso 0.50 1 d P . . C5S C -0.149(2) -0.3656(18) 0.9604(19) 0.140(8) Uiso 0.50 1 d PD . . H5S1 H -0.2196 -0.3962 0.9995 0.210 Uiso 0.50 1 calc PR . . H5S2 H -0.1409 -0.3521 0.8917 0.210 Uiso 0.50 1 calc PR . . H5S3 H -0.1472 -0.3076 0.9798 0.210 Uiso 0.50 1 calc PR . . C6S C 0.8525(9) -0.0839(9) 0.1373(10) 0.057(3) Uani 0.50 1 d PDU . . H6S1 H 0.8121 -0.0254 0.1421 0.085 Uiso 0.50 1 calc PR . . H6S2 H 0.9266 -0.0715 0.0897 0.085 Uiso 0.50 1 calc PR . . H6S3 H 0.8567 -0.1145 0.2007 0.085 Uiso 0.50 1 calc PR . . C7S C 0.9507(15) 0.1840(13) 0.0909(13) 0.188(6) Uani 1 1 d DU . . H14X H 0.172(4) -0.316(3) 0.372(4) 0.033(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0147(3) 0.0221(3) 0.0235(3) -0.0111(2) -0.0030(2) -0.0012(2) Mn2 0.0126(2) 0.0206(3) 0.0207(3) -0.0100(2) -0.00382(19) 0.0008(2) Mn3 0.0127(2) 0.0222(3) 0.0216(3) -0.0101(2) -0.0044(2) 0.0009(2) Mn4 0.0131(2) 0.0226(3) 0.0224(3) -0.0112(2) -0.0042(2) 0.0016(2) Na1 0.0157(7) 0.0312(8) 0.0258(7) -0.0137(6) -0.0039(6) 0.0005(6) O1 0.0253(13) 0.0238(14) 0.0301(14) -0.0112(11) -0.0058(11) -0.0025(11) O2 0.0238(13) 0.0286(14) 0.0256(13) -0.0105(11) 0.0020(11) -0.0054(11) O3 0.046(2) 0.047(2) 0.056(2) -0.0158(17) 0.0235(17) -0.0128(17) O4 0.0148(11) 0.0271(13) 0.0241(12) -0.0135(10) -0.0044(9) -0.0014(10) O5 0.0151(11) 0.0249(13) 0.0240(12) -0.0113(10) -0.0064(10) -0.0005(10) O6 0.0313(18) 0.056(2) 0.101(3) -0.041(2) -0.0176(19) -0.0087(16) O7 0.0151(11) 0.0215(12) 0.0228(12) -0.0091(10) -0.0078(9) 0.0030(9) O8 0.0158(11) 0.0242(13) 0.0193(11) -0.0091(9) -0.0046(9) 0.0014(10) O9 0.0165(12) 0.0215(12) 0.0235(12) -0.0081(10) -0.0066(10) -0.0005(10) O10 0.0202(13) 0.0252(14) 0.0309(14) -0.0128(11) -0.0053(11) 0.0003(11) O11 0.0156(11) 0.0284(14) 0.0230(12) -0.0125(10) -0.0054(10) 0.0003(10) O12 0.0152(12) 0.0264(14) 0.0297(13) -0.0126(11) -0.0063(10) 0.0034(10) O13 0.0148(12) 0.0236(13) 0.0351(14) -0.0136(11) -0.0050(10) 0.0020(10) O14 0.0196(14) 0.0381(17) 0.0564(19) -0.0215(14) -0.0158(13) 0.0035(12) O15 0.0349(17) 0.0403(18) 0.0285(15) -0.0177(13) 0.0038(12) -0.0012(14) O16 0.0234(15) 0.0437(19) 0.0520(19) -0.0236(15) -0.0147(14) 0.0024(13) N1 0.0163(14) 0.0318(18) 0.0344(17) -0.0197(14) -0.0058(13) -0.0012(13) N2 0.0169(14) 0.0254(16) 0.0209(14) -0.0103(12) -0.0042(11) -0.0002(12) N3 0.0150(14) 0.0233(16) 0.0281(16) -0.0107(12) -0.0015(12) 0.0036(12) N4 0.0273(18) 0.050(2) 0.0287(17) -0.0127(16) -0.0127(14) 0.0084(16) N5 0.0163(14) 0.0322(17) 0.0242(15) -0.0133(13) -0.0035(12) -0.0012(13) N6 0.0180(14) 0.0213(15) 0.0269(15) -0.0110(12) -0.0075(12) 0.0023(12) C1 0.039(2) 0.024(2) 0.034(2) -0.0079(16) -0.0098(18) -0.0113(17) C2 0.053(3) 0.024(2) 0.042(2) -0.0123(18) -0.015(2) -0.0069(19) C3 0.101(5) 0.025(2) 0.047(3) -0.008(2) -0.028(3) -0.007(3) C4 0.122(6) 0.033(3) 0.039(3) 0.000(2) -0.013(3) -0.016(3) C5 0.094(5) 0.032(3) 0.043(3) -0.008(2) 0.010(3) -0.020(3) C6 0.055(3) 0.029(2) 0.035(2) -0.0076(18) 0.000(2) -0.017(2) C7 0.039(2) 0.033(2) 0.038(2) -0.0150(19) 0.0030(19) -0.0074(19) C8 0.0195(18) 0.051(3) 0.034(2) -0.0277(19) -0.0071(16) -0.0012(17) C9 0.0177(17) 0.039(2) 0.0303(19) -0.0221(17) -0.0043(15) -0.0031(16) C10 0.0198(17) 0.034(2) 0.0325(19) -0.0154(16) -0.0100(15) -0.0012(16) C11 0.0245(18) 0.030(2) 0.0295(19) -0.0089(15) -0.0140(15) -0.0029(15) C12 0.0202(18) 0.031(2) 0.052(2) -0.0229(19) -0.0106(17) 0.0009(16) C13 0.024(2) 0.047(3) 0.078(4) -0.035(3) -0.020(2) -0.002(2) C14 0.0241(18) 0.034(2) 0.0215(17) -0.0098(15) -0.0051(14) 0.0023(16) C15 0.0268(19) 0.028(2) 0.0237(17) -0.0099(15) -0.0077(15) 0.0024(15) C16 0.0202(18) 0.044(2) 0.0241(18) -0.0156(16) -0.0088(14) -0.0003(16) C17 0.0195(17) 0.038(2) 0.0273(18) -0.0194(16) -0.0046(14) -0.0033(16) C18 0.0229(18) 0.031(2) 0.0261(18) -0.0122(15) -0.0030(15) 0.0008(16) C19 0.036(2) 0.050(3) 0.0233(19) -0.0169(18) -0.0043(17) 0.008(2) C20 0.0194(18) 0.027(2) 0.038(2) -0.0143(16) -0.0066(16) 0.0059(15) C21 0.022(2) 0.035(3) 0.100(4) -0.032(3) -0.014(2) 0.0038(19) C22 0.031(3) 0.045(3) 0.206(9) -0.062(5) -0.031(4) 0.018(3) C23 0.029(3) 0.059(4) 0.254(12) -0.090(6) -0.036(5) 0.022(3) C24 0.019(2) 0.046(3) 0.120(5) -0.043(3) -0.017(3) 0.010(2) C25 0.0208(19) 0.030(2) 0.044(2) -0.0176(17) -0.0081(17) 0.0047(16) C26 0.0169(17) 0.032(2) 0.0273(18) -0.0124(15) -0.0066(14) 0.0037(15) C27 0.0173(16) 0.0243(18) 0.0308(18) -0.0089(15) -0.0118(14) 0.0019(14) C28 0.0220(17) 0.0246(18) 0.0257(17) -0.0097(14) -0.0099(14) 0.0017(14) C29 0.0226(18) 0.0259(19) 0.0259(18) -0.0047(14) -0.0083(15) -0.0015(15) C30 0.0213(17) 0.0257(19) 0.0223(17) -0.0077(14) -0.0068(14) -0.0010(14) C31 0.030(2) 0.0212(18) 0.034(2) -0.0112(15) -0.0088(16) 0.0012(16) C32 0.0240(19) 0.0228(19) 0.036(2) -0.0106(15) -0.0116(16) 0.0048(15) C33 0.029(2) 0.046(3) 0.047(3) -0.017(2) -0.0146(19) -0.0037(19) O7' 0.35(2) 0.36(2) 0.36(2) -0.088(11) -0.121(12) 0.001(10) O2S 0.099(5) 0.119(5) 0.109(5) -0.009(4) -0.034(4) 0.016(4) O3S 0.039(4) 0.063(5) 0.070(5) -0.020(4) -0.012(4) -0.005(4) O7S 0.118(8) 0.130(8) 0.105(7) -0.028(6) -0.058(6) 0.016(6) C2S 0.122(7) 0.070(5) 0.100(6) -0.032(4) -0.058(5) 0.018(5) C3S 0.062(8) 0.067(8) 0.133(13) -0.050(9) -0.056(9) 0.009(7) C6S 0.043(5) 0.071(6) 0.096(7) -0.049(5) -0.054(5) 0.015(4) C7S 0.191(10) 0.206(10) 0.158(9) 0.021(7) -0.091(8) 0.007(8) _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 1.884(3) . ? Mn1 O4 1.918(2) . ? Mn1 O2 1.940(3) . ? Mn1 O5 1.956(3) . ? Mn1 O9 2.181(2) 2_556 ? Mn1 N1 2.337(3) . ? Mn1 Mn2 3.2305(7) . ? Mn2 O9 2.142(3) 2_556 ? Mn2 O7 2.154(3) . ? Mn2 O5 2.193(2) . ? Mn2 O8 2.195(2) . ? Mn2 N2 2.240(3) 2_556 ? Mn2 N2 2.307(3) . ? Mn2 Mn4 3.2310(7) . ? Mn3 O4 2.130(2) 2_556 ? Mn3 O11 2.224(2) . ? Mn3 O7 2.260(2) . ? Mn3 O9 2.288(2) . ? Mn3 O10 2.305(3) . ? Mn3 N6 2.368(3) . ? Mn3 N2 2.480(3) . ? Mn4 O11 1.892(2) . ? Mn4 O13 1.899(3) . ? Mn4 O12 1.940(2) . ? Mn4 O8 1.947(3) . ? Mn4 O7 2.171(2) . ? Mn4 N5 2.322(3) . ? Na1 O15 2.313(3) 2_655 ? Na1 O16 2.339(3) . ? Na1 O8 2.405(3) . ? Na1 O2 2.408(3) . ? Na1 O5 2.429(3) . ? Na1 O12 2.480(3) . ? O1 C1 1.333(5) . ? O2 C7 1.301(5) . ? O3 C7 1.242(5) . ? O4 C9 1.413(4) . ? O4 Mn3 2.130(2) 2_556 ? O5 C11 1.430(4) . ? O6 C13 1.395(6) . ? O6 H6 0.8200 . ? O7 C27 1.423(4) . ? O8 C15 1.419(4) . ? O9 C30 1.418(4) . ? O9 Mn2 2.142(3) 2_556 ? O9 Mn1 2.181(2) 2_556 ? O10 C31 1.432(5) . ? O10 H14X 0.79(5) . ? O11 C17 1.418(4) . ? O12 C26 1.301(4) . ? O13 C20 1.336(4) . ? O14 C26 1.242(5) . ? O15 C19 1.423(5) . ? O15 Na1 2.313(3) 2_655 ? O15 H15 0.78(6) . ? O16 C33 1.406(5) . ? O16 H18 0.71(6) . ? N1 C10 1.470(5) . ? N1 C12 1.477(5) . ? N1 C8 1.485(5) . ? N2 N3 1.211(4) . ? N2 Mn2 2.240(3) 2_556 ? N3 N4 1.153(5) . ? N5 C18 1.466(5) . ? N5 C14 1.469(5) . ? N5 C16 1.487(5) . ? N6 C29 1.473(5) . ? N6 C32 1.483(5) . ? N6 C28 1.483(5) . ? C1 C2 1.403(6) . ? C1 C6 1.417(6) . ? C2 C3 1.384(7) . ? C2 H2 0.9300 . ? C3 C4 1.380(9) . ? C3 H3 0.9300 . ? C4 C5 1.362(9) . ? C4 H4 0.9300 . ? C5 C6 1.408(7) . ? C5 H5 0.9300 . ? C6 C7 1.472(7) . ? C8 C9 1.521(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.529(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.519(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.527(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.521(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.523(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.391(6) . ? C20 C25 1.407(6) . ? C21 C22 1.383(7) . ? C21 H21 0.9300 . ? C22 C23 1.378(8) . ? C22 H22 0.9300 . ? C23 C24 1.381(8) . ? C23 H23 0.9300 . ? C24 C25 1.388(6) . ? C24 H24 0.9300 . ? C25 C26 1.471(6) . ? C27 C28 1.515(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.519(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.511(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? O7' C7S 1.464(10) . ? O2S C2S 1.430(10) . ? O2S H2S 0.8200 . ? O3S C3S 1.309(15) . ? O3S H3S 0.8200 . ? O5S C5S 1.451(10) . ? O5S H5S 1.0598 . ? O6S C6S 1.352(10) . ? O6S H6S 0.8295 . ? O7S C7S 1.444(18) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3S H3S1 1.0864 . ? C3S H3S2 0.8885 . ? C3S H3S3 1.0197 . ? C5S H5S1 0.9600 . ? C5S H5S2 0.9600 . ? C5S H5S3 0.9600 . ? C6S H6S1 0.9600 . ? C6S H6S2 0.9600 . ? C6S H6S3 0.9600 . ? 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 O4 90.01(11) . . ? O1 Mn1 O2 90.61(12) . . ? O4 Mn1 O2 176.83(11) . . ? O1 Mn1 O5 175.44(11) . . ? O4 Mn1 O5 94.32(11) . . ? O2 Mn1 O5 84.99(11) . . ? O1 Mn1 O9 99.42(11) . 2_556 ? O4 Mn1 O9 80.12(10) . 2_556 ? O2 Mn1 O9 102.84(10) . 2_556 ? O5 Mn1 O9 82.75(10) . 2_556 ? O1 Mn1 N1 97.45(12) . . ? O4 Mn1 N1 78.51(11) . . ? O2 Mn1 N1 98.33(12) . . ? O5 Mn1 N1 82.05(11) . . ? O9 Mn1 N1 152.65(11) 2_556 . ? O1 Mn1 Mn2 140.40(8) . . ? O4 Mn1 Mn2 86.75(8) . . ? O2 Mn1 Mn2 94.74(8) . . ? O5 Mn1 Mn2 41.58(7) . . ? O9 Mn1 Mn2 41.18(7) 2_556 . ? N1 Mn1 Mn2 120.36(9) . . ? O9 Mn2 O7 174.87(9) 2_556 . ? O9 Mn2 O5 78.41(9) 2_556 . ? O7 Mn2 O5 103.25(9) . . ? O9 Mn2 O8 97.86(9) 2_556 . ? O7 Mn2 O8 77.28(9) . . ? O5 Mn2 O8 92.27(9) . . ? O9 Mn2 N2 86.89(10) 2_556 2_556 ? O7 Mn2 N2 97.79(10) . 2_556 ? O5 Mn2 N2 94.13(10) . 2_556 ? O8 Mn2 N2 172.69(10) . 2_556 ? O9 Mn2 N2 93.93(10) 2_556 . ? O7 Mn2 N2 85.18(10) . . ? O5 Mn2 N2 168.15(10) . . ? O8 Mn2 N2 97.76(10) . . ? N2 Mn2 N2 76.29(12) 2_556 . ? O9 Mn2 Mn1 42.11(6) 2_556 . ? O7 Mn2 Mn1 139.30(7) . . ? O5 Mn2 Mn1 36.30(7) . . ? O8 Mn2 Mn1 95.87(7) . . ? N2 Mn2 Mn1 91.38(8) 2_556 . ? N2 Mn2 Mn1 135.43(8) . . ? O9 Mn2 Mn4 133.08(7) 2_556 . ? O7 Mn2 Mn4 41.87(6) . . ? O5 Mn2 Mn4 104.82(7) . . ? O8 Mn2 Mn4 36.06(7) . . ? N2 Mn2 Mn4 138.03(8) 2_556 . ? N2 Mn2 Mn4 87.02(8) . . ? Mn1 Mn2 Mn4 125.62(2) . . ? O4 Mn3 O11 99.48(9) 2_556 . ? O4 Mn3 O7 165.86(10) 2_556 . ? O11 Mn3 O7 73.06(9) . . ? O4 Mn3 O9 73.47(9) 2_556 . ? O11 Mn3 O9 152.88(10) . . ? O7 Mn3 O9 107.53(9) . . ? O4 Mn3 O10 85.47(10) 2_556 . ? O11 Mn3 O10 77.09(10) . . ? O7 Mn3 O10 104.04(10) . . ? O9 Mn3 O10 127.03(10) . . ? O4 Mn3 N6 118.34(10) 2_556 . ? O11 Mn3 N6 129.63(10) . . ? O7 Mn3 N6 74.83(10) . . ? O9 Mn3 N6 74.35(10) . . ? O10 Mn3 N6 74.34(10) . . ? O4 Mn3 N2 87.48(10) 2_556 . ? O11 Mn3 N2 75.21(10) . . ? O7 Mn3 N2 79.05(9) . . ? O9 Mn3 N2 78.31(9) . . ? O10 Mn3 N2 149.82(10) . . ? N6 Mn3 N2 133.88(10) . . ? O11 Mn4 O13 88.08(11) . . ? O11 Mn4 O12 177.92(12) . . ? O13 Mn4 O12 90.19(11) . . ? O11 Mn4 O8 94.91(11) . . ? O13 Mn4 O8 177.00(10) . . ? O12 Mn4 O8 86.83(11) . . ? O11 Mn4 O7 81.82(10) . . ? O13 Mn4 O7 98.40(11) . . ? O12 Mn4 O7 97.29(10) . . ? O8 Mn4 O7 82.34(10) . . ? O11 Mn4 N5 80.02(11) . . ? O13 Mn4 N5 98.48(12) . . ? O12 Mn4 N5 101.39(11) . . ? O8 Mn4 N5 81.79(11) . . ? O7 Mn4 N5 154.68(10) . . ? O11 Mn4 Mn2 81.92(8) . . ? O13 Mn4 Mn2 139.53(8) . . ? O12 Mn4 Mn2 98.68(8) . . ? O8 Mn4 Mn2 41.59(7) . . ? O7 Mn4 Mn2 41.47(7) . . ? N5 Mn4 Mn2 117.94(8) . . ? O15 Na1 O16 93.65(13) 2_655 . ? O15 Na1 O8 99.90(11) 2_655 . ? O16 Na1 O8 148.34(13) . . ? O15 Na1 O2 87.10(11) 2_655 . ? O16 Na1 O2 111.03(12) . . ? O8 Na1 O2 98.20(10) . . ? O15 Na1 O5 152.84(13) 2_655 . ? O16 Na1 O5 98.84(11) . . ? O8 Na1 O5 81.76(9) . . ? O2 Na1 O5 65.93(9) . . ? O15 Na1 O12 92.10(11) 2_655 . ? O16 Na1 O12 84.86(11) . . ? O8 Na1 O12 66.29(9) . . ? O2 Na1 O12 164.11(11) . . ? O5 Na1 O12 112.88(10) . . ? O15 Na1 H18 87.3(14) 2_655 . ? O16 Na1 H18 16.9(14) . . ? O8 Na1 H18 135.3(14) . . ? O2 Na1 H18 126.3(14) . . ? O5 Na1 H18 110.7(14) . . ? O12 Na1 H18 69.4(14) . . ? C1 O1 Mn1 128.4(3) . . ? C7 O2 Mn1 130.9(3) . . ? C7 O2 Na1 124.3(3) . . ? Mn1 O2 Na1 104.75(12) . . ? C9 O4 Mn1 112.0(2) . . ? C9 O4 Mn3 131.7(2) . 2_556 ? Mn1 O4 Mn3 109.94(11) . 2_556 ? C11 O5 Mn1 114.2(2) . . ? C11 O5 Mn2 130.2(2) . . ? Mn1 O5 Mn2 102.12(11) . . ? C11 O5 Na1 110.0(2) . . ? Mn1 O5 Na1 103.46(11) . . ? Mn2 O5 Na1 92.25(9) . . ? C13 O6 H6 109.5 . . ? C27 O7 Mn2 128.2(2) . . ? C27 O7 Mn4 112.7(2) . . ? Mn2 O7 Mn4 96.66(10) . . ? C27 O7 Mn3 115.0(2) . . ? Mn2 O7 Mn3 102.95(10) . . ? Mn4 O7 Mn3 95.26(9) . . ? C15 O8 Mn4 115.7(2) . . ? C15 O8 Mn2 127.4(2) . . ? Mn4 O8 Mn2 102.35(11) . . ? C15 O8 Na1 110.5(2) . . ? Mn4 O8 Na1 103.84(11) . . ? Mn2 O8 Na1 92.82(9) . . ? C30 O9 Mn2 126.1(2) . 2_556 ? C30 O9 Mn1 115.5(2) . 2_556 ? Mn2 O9 Mn1 96.71(10) 2_556 2_556 ? C30 O9 Mn3 115.6(2) . . ? Mn2 O9 Mn3 101.57(10) 2_556 . ? Mn1 O9 Mn3 95.81(9) 2_556 . ? C31 O10 Mn3 110.9(2) . . ? C31 O10 H14X 110(4) . . ? Mn3 O10 H14X 104(4) . . ? C17 O11 Mn4 113.6(2) . . ? C17 O11 Mn3 131.4(2) . . ? Mn4 O11 Mn3 105.12(11) . . ? C26 O12 Mn4 131.5(2) . . ? C26 O12 Na1 127.1(2) . . ? Mn4 O12 Na1 101.39(11) . . ? C20 O13 Mn4 128.4(2) . . ? C19 O15 Na1 126.9(3) . 2_655 ? C19 O15 H15 103(4) . . ? Na1 O15 H15 110(4) 2_655 . ? C33 O16 Na1 125.2(3) . . ? C33 O16 H18 107(5) . . ? Na1 O16 H18 90(5) . . ? C10 N1 C12 113.0(3) . . ? C10 N1 C8 113.1(3) . . ? C12 N1 C8 112.4(3) . . ? C10 N1 Mn1 100.5(2) . . ? C12 N1 Mn1 112.3(3) . . ? C8 N1 Mn1 104.7(2) . . ? N3 N2 Mn2 126.0(2) . 2_556 ? N3 N2 Mn2 121.9(2) . . ? Mn2 N2 Mn2 103.71(12) 2_556 . ? N3 N2 Mn3 110.8(2) . . ? Mn2 N2 Mn3 93.19(11) 2_556 . ? Mn2 N2 Mn3 92.28(11) . . ? N4 N3 N2 179.1(4) . . ? C18 N5 C14 113.7(3) . . ? C18 N5 C16 113.1(3) . . ? C14 N5 C16 112.3(3) . . ? C18 N5 Mn4 111.9(2) . . ? C14 N5 Mn4 100.8(2) . . ? C16 N5 Mn4 104.0(2) . . ? C29 N6 C32 110.4(3) . . ? C29 N6 C28 110.6(3) . . ? C32 N6 C28 111.3(3) . . ? C29 N6 Mn3 106.7(2) . . ? C32 N6 Mn3 110.2(2) . . ? C28 N6 Mn3 107.5(2) . . ? O1 C1 C2 118.3(4) . . ? O1 C1 C6 123.8(4) . . ? C2 C1 C6 117.8(4) . . ? C3 C2 C1 121.0(5) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 121.1(6) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.0(5) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 122.0(6) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.1(5) . . ? C5 C6 C7 118.2(5) . . ? C1 C6 C7 122.7(4) . . ? O3 C7 O2 120.8(5) . . ? O3 C7 C6 119.8(4) . . ? O2 C7 C6 119.4(4) . . ? N1 C8 C9 108.7(3) . . ? N1 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? N1 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? O4 C9 C8 108.5(3) . . ? O4 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? O4 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N1 C10 C11 110.9(3) . . ? N1 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? O5 C11 C10 110.2(3) . . ? O5 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? O5 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N1 C12 C13 115.4(4) . . ? N1 C12 H12A 108.4 . . ? C13 C12 H12A 108.4 . . ? N1 C12 H12B 108.4 . . ? C13 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? O6 C13 C12 112.2(5) . . ? O6 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? O6 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N5 C14 C15 110.8(3) . . ? N5 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O8 C15 C14 110.8(3) . . ? O8 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? O8 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N5 C16 C17 109.3(3) . . ? N5 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? N5 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O11 C17 C16 108.9(3) . . ? O11 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? O11 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N5 C18 C19 115.0(3) . . ? N5 C18 H18A 108.5 . . ? C19 C18 H18A 108.5 . . ? N5 C18 H18B 108.5 . . ? C19 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? O15 C19 C18 111.0(4) . . ? O15 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? O15 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? O13 C20 C21 116.6(4) . . ? O13 C20 C25 123.8(4) . . ? C21 C20 C25 119.6(4) . . ? C22 C21 C20 120.3(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 120.2(5) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.2(5) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C25 120.8(5) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C20 119.0(4) . . ? C24 C25 C26 117.5(4) . . ? C20 C25 C26 123.5(4) . . ? O14 C26 O12 119.9(4) . . ? O14 C26 C25 120.1(4) . . ? O12 C26 C25 120.0(3) . . ? O7 C27 C28 111.0(3) . . ? O7 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? O7 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? N6 C28 C27 110.6(3) . . ? N6 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? N6 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? N6 C29 C30 111.6(3) . . ? N6 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N6 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? O9 C30 C29 111.5(3) . . ? O9 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? O9 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? O10 C31 C32 110.3(3) . . ? O10 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? O10 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? N6 C32 C31 110.4(3) . . ? N6 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? N6 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? O16 C33 H33A 109.5 . . ? O16 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O16 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C2S O2S H2S 109.5 . . ? C3S O3S H3S 109.5 . . ? C5S O5S H5S 101.4 . . ? C6S O6S H6S 117.6 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O3S C3S H3S1 107.3 . . ? O3S C3S H3S2 122.1 . . ? H3S1 C3S H3S2 104.6 . . ? O3S C3S H3S3 112.7 . . ? H3S1 C3S H3S3 96.2 . . ? H3S2 C3S H3S3 110.3 . . ? O5S C5S H5S1 109.5 . . ? O5S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? O5S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? O6S C6S H6S1 109.5 . . ? O6S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? O6S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? O7S C7S O7' 79(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.464 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.115 # Attachment '- 4_Na2Mn8_2-D_final+sq.CIF' data_747sq _database_code_depnum_ccdc_archive 'CCDC 822747' #TrackingRef '- 4_Na2Mn8_2-D_final+sq.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains half the cluster as well as some solvent MeOH and Et2O molecules. After a preliminary model with 2 MeOH each at half occupancy and half an Et2O molecule at full occupancy was refined with restained bond (DFIX) and thermal (ISOR) parameters, all solvent molecules were removed and the associated electron density accounted for using PLATON/SQUEEZE. The free alcohol arm of two of the teaH2- ligands was modelled with the oxygen atom disordered over two positions set at 0.83 and 0.17 occupancy. The phenyl rings of two of the salycylate ligands are disordered over two positions and each set at 0.5 occupancy. The terminal MeOH coordinated to the Na ion has the carbon atom disorderd over two positions, with refined occupancies of 0.75 and 0.25 and with restrained bond(DFIX) also parameters. All H atoms were placed in calculated positions, except for H15 and H27 which located and refined but then fixed for the final refinement. ; _publ_section_references ; Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H111 Mn8 N12 Na2 O35' _chemical_formula_weight 2190.23 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 monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.8728(6) _cell_length_b 24.3303(5) _cell_length_c 16.0384(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.2860(10) _cell_angle_gamma 90.00 _cell_volume 9933.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9657 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 26.32 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4544 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35026 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10121 _reflns_number_gt 8059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 structure was solved by direct methods. The asymmetric unit contains half the cluster as well as some solvent MeOH and Et2O molecules. After a preliminary model with 2 MeOH each at half occupancy and half an Et2O molecule at full occupancy was refined with restained bond (DFIX) and thermal (ISOR) parameters, all solvent molecules were removed and the associated electron density accounted for using PLATON/SQUEEZE. The free alcohol arm of two of the teaH2- ligands was modelled with the oxygen atom disordered over two positions set at 0.83 and 0.17 occupancy. The phenyl rings of two of the salycylate ligands are disordered over two positions and each set at 0.5 occupancy. The terminal MeOH coordinated to the Na ion has the carbon atom disorderd over two positions, with refined occupancies of 0.75 and 0.25 and with restrained bond(DFIX) also parameters. All H atoms were placed in calculated positions, except for H15 and H27 which located and refined but then fixed for the final refinement. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.002 -0.009 -0.008 2353.0 753 _platon_squeeze_details ; PLATON/SQUEEZE Spek, A.L. (1990), Acta Cryst. A46, C-34 ; _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^)+(0.0612P)^2^+51.2899P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10121 _refine_ls_number_parameters 644 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1549 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.073 _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 0.11314(3) 0.30221(3) 0.60292(4) 0.03007(17) Uani 1 1 d . . . Na1 Na 0.12404(8) 0.41757(7) 0.48046(11) 0.0361(4) Uani 1 1 d . . . O1 O 0.05646(13) 0.25872(15) 0.6223(2) 0.0427(8) Uani 1 1 d . . . N1 N 0.12304(16) 0.35068(18) 0.7308(3) 0.0392(10) Uani 1 1 d . . . C1 C 0.00566(19) 0.2617(2) 0.5862(3) 0.0373(11) Uani 1 1 d . . . Mn2 Mn 0.20581(2) 0.30743(2) 0.49284(4) 0.02308(16) Uani 1 1 d . . . O2 O 0.06579(12) 0.34844(13) 0.5248(2) 0.0353(7) Uani 1 1 d . . . N2 N 0.24232(13) 0.24537(13) 0.4120(2) 0.0229(7) Uani 1 1 d . . . C2 C -0.0276(2) 0.2224(2) 0.6121(3) 0.0437(12) Uani 1 1 d . . . H2 H -0.0137 0.1964 0.6545 0.052 Uiso 1 1 calc R . . Mn3 Mn 0.31462(3) 0.30878(3) 0.39826(4) 0.02756(17) Uani 1 1 d . . . O3 O -0.0002(5) 0.3672(6) 0.4235(9) 0.038(3) Uani 0.50 1 d P A 2 N3 N 0.21980(15) 0.23227(14) 0.3419(2) 0.0291(8) Uani 1 1 d . . . C3 C -0.0803(2) 0.2209(3) 0.5769(4) 0.0526(15) Uani 1 1 d . . . H3 H -0.1023 0.1938 0.5949 0.063 Uiso 1 1 calc R . . Mn4 Mn 0.22071(3) 0.39933(3) 0.35437(4) 0.02986(18) Uani 1 1 d . . . O4 O 0.15961(12) 0.25466(13) 0.67581(19) 0.0330(7) Uani 1 1 d . . . N4 N 0.19847(17) 0.22011(17) 0.2754(3) 0.0409(10) Uani 1 1 d . . . C4 C -0.1013(2) 0.2592(3) 0.5148(5) 0.0651(18) Uani 1 1 d . . . H4 H -0.1375 0.2581 0.4897 0.078 Uiso 1 1 calc R . . O5 O 0.16825(12) 0.35279(12) 0.58354(18) 0.0293(7) Uani 1 1 d . . . N5 N 0.16342(16) 0.39833(15) 0.2278(2) 0.0336(9) Uani 1 1 d . . . C5 C -0.0689(2) 0.2981(3) 0.4909(4) 0.0580(16) Uani 1 1 d . . . H5 H -0.0832 0.3248 0.4499 0.070 Uiso 1 1 calc R . . O6 O 0.0735(4) 0.4570(3) 0.7928(6) 0.124(4) Uani 0.805(11) 1 d PU B 1 H6 H 0.0528 0.4770 0.8141 0.149 Uiso 0.805(11) 1 calc PR B 1 N6 N 0.37598(14) 0.36062(15) 0.4980(2) 0.0322(9) Uani 1 1 d . . . C6 C -0.01535(19) 0.2997(2) 0.5250(4) 0.0415(12) Uani 1 1 d . A . O7 O 0.26630(11) 0.36305(11) 0.46740(18) 0.0272(7) Uani 1 1 d . . . C7 C 0.0164(2) 0.3427(2) 0.4927(4) 0.0463(13) Uani 1 1 d . . . O8 O 0.16338(11) 0.35834(11) 0.38991(18) 0.0250(6) Uani 1 1 d . . . C8 C 0.1551(2) 0.3131(2) 0.7931(3) 0.0417(12) Uani 1 1 d . . . H8A H 0.1436 0.3158 0.8486 0.050 Uiso 1 1 calc R . . H8B H 0.1927 0.3237 0.8009 0.050 Uiso 1 1 calc R . . O9 O 0.35717(11) 0.24709(11) 0.49147(18) 0.0258(6) Uani 1 1 d . . . C9 C 0.1481(2) 0.2546(2) 0.7599(3) 0.0401(12) Uani 1 1 d . . . H9A H 0.1722 0.2295 0.7966 0.048 Uiso 1 1 calc R . . H9B H 0.1116 0.2422 0.7590 0.048 Uiso 1 1 calc R . . O10 O 0.35427(14) 0.36993(16) 0.3186(2) 0.0492(9) Uani 1 1 d . . . C10 C 0.1525(2) 0.3984(2) 0.7113(3) 0.0392(12) Uani 1 1 d . . . H10A H 0.1705 0.4156 0.7647 0.047 Uiso 1 1 calc R . . H10B H 0.1281 0.4258 0.6801 0.047 Uiso 1 1 calc R . . O11 O 0.24744(12) 0.33888(13) 0.30217(18) 0.0304(7) Uani 1 1 d . . . C11 C 0.19286(18) 0.38162(19) 0.6579(3) 0.0325(10) Uani 1 1 d . . . H11A H 0.2107 0.4148 0.6412 0.039 Uiso 1 1 calc R . . H11B H 0.2197 0.3578 0.6918 0.039 Uiso 1 1 calc R . . O12 O 0.19634(13) 0.46210(12) 0.4100(2) 0.0379(8) Uani 1 1 d . . . C12 C 0.0724(2) 0.3643(3) 0.7560(4) 0.0575(16) Uani 1 1 d . B . H12A H 0.0566 0.3300 0.7730 0.069 Uiso 1 1 calc R . . H12B H 0.0484 0.3791 0.7059 0.069 Uiso 1 1 calc R . . O13 O 0.27450(14) 0.44253(14) 0.3201(2) 0.0452(9) Uani 1 1 d . . . C13 C 0.0753(3) 0.4059(3) 0.8284(5) 0.071(2) Uani 1 1 d . . . H13A H 0.0454 0.4007 0.8584 0.086 Uiso 1 1 calc R B 1 H13B H 0.1084 0.4010 0.8696 0.086 Uiso 1 1 calc R B 1 O14 O 0.1974(9) 0.5436(8) 0.4810(8) 0.052(4) Uani 0.50 1 d P C 8 C14 C 0.11368(18) 0.38704(18) 0.2548(3) 0.0317(10) Uani 1 1 d . . . H14A H 0.0875 0.3743 0.2059 0.038 Uiso 1 1 calc R . . H14B H 0.1001 0.4210 0.2772 0.038 Uiso 1 1 calc R . . O15 O 0.13265(18) 0.50349(16) 0.0570(3) 0.0601(11) Uani 1 1 d . . . C15 C 0.12193(17) 0.34302(17) 0.3234(3) 0.0270(9) Uani 1 1 d . . . H15A H 0.0891 0.3380 0.3463 0.032 Uiso 1 1 calc R C . H15B H 0.1305 0.3076 0.2987 0.032 Uiso 1 1 calc R . . O16 O 0.04792(17) 0.45738(18) 0.3956(3) 0.0629(12) Uani 1 1 d D . . C16 C 0.1821(2) 0.3524(2) 0.1789(3) 0.0374(11) Uani 1 1 d . . . H16A H 0.1771 0.3622 0.1181 0.045 Uiso 1 1 calc R . . H16B H 0.1615 0.3187 0.1848 0.045 Uiso 1 1 calc R . . C17 C 0.2393(2) 0.3423(2) 0.2127(3) 0.0386(11) Uani 1 1 d . . . H17A H 0.2505 0.3076 0.1890 0.046 Uiso 1 1 calc R . . H17B H 0.2606 0.3726 0.1954 0.046 Uiso 1 1 calc R . . C18 C 0.1643(2) 0.4519(2) 0.1838(4) 0.0491(14) Uani 1 1 d . . . H18A H 0.1979 0.4550 0.1627 0.059 Uiso 1 1 calc R . . H18B H 0.1636 0.4817 0.2256 0.059 Uiso 1 1 calc R . . C19 C 0.1195(2) 0.4609(2) 0.1100(4) 0.0567(17) Uani 1 1 d . . . H19A H 0.1126 0.4265 0.0770 0.068 Uiso 1 1 calc R . . H19B H 0.0873 0.4709 0.1317 0.068 Uiso 1 1 calc R . . C26 C 0.2076(9) 0.5123(16) 0.4253(19) 0.040(7) Uani 0.50 1 d PD C 8 C27 C 0.29388(19) 0.40246(18) 0.5243(3) 0.0337(10) Uani 1 1 d . . . H27A H 0.2737 0.4104 0.5699 0.040 Uiso 1 1 calc R . . H27B H 0.2974 0.4371 0.4935 0.040 Uiso 1 1 calc R . . C28 C 0.34795(19) 0.38116(18) 0.5628(3) 0.0346(11) Uani 1 1 d . . . H28A H 0.3685 0.4111 0.5947 0.042 Uiso 1 1 calc R . . H28B H 0.3444 0.3512 0.6032 0.042 Uiso 1 1 calc R . . C29 C 0.41787(18) 0.3218(2) 0.5353(3) 0.0347(11) Uani 1 1 d . . . H29A H 0.4391 0.3385 0.5865 0.042 Uiso 1 1 calc R . . H29B H 0.4413 0.3147 0.4940 0.042 Uiso 1 1 calc R . . C30 C 0.39471(17) 0.26838(18) 0.5586(3) 0.0314(10) Uani 1 1 d . . . H30A H 0.4233 0.2412 0.5743 0.038 Uiso 1 1 calc R . . H30B H 0.3779 0.2743 0.6086 0.038 Uiso 1 1 calc R . . C31 C 0.4036(2) 0.3891(3) 0.3655(4) 0.0556(16) Uani 1 1 d . . . H31A H 0.4159 0.4209 0.3359 0.067 Uiso 1 1 calc R . . H31B H 0.4302 0.3595 0.3685 0.067 Uiso 1 1 calc R . . C32 C 0.3981(2) 0.4057(2) 0.4531(4) 0.0480(14) Uani 1 1 d . . . H32A H 0.4330 0.4162 0.4854 0.058 Uiso 1 1 calc R . . H32B H 0.3749 0.4383 0.4502 0.058 Uiso 1 1 calc R . . C33 C 0.0234(5) 0.4949(5) 0.4491(8) 0.107(4) Uani 0.75 1 d PDU C 3 H33A H 0.0445 0.5285 0.4597 0.161 Uiso 0.75 1 calc PR C 3 H33B H 0.0214 0.4769 0.5031 0.161 Uiso 0.75 1 calc PR C 3 H33C H -0.0121 0.5044 0.4200 0.161 Uiso 0.75 1 calc PR C 3 C34 C 0.0159(13) 0.4554(16) 0.3147(12) 0.111(12) Uani 0.25 1 d PDU C 4 H34A H -0.0175 0.4376 0.3188 0.166 Uiso 0.25 1 calc PR C 4 H34B H 0.0338 0.4344 0.2761 0.166 Uiso 0.25 1 calc PR C 4 H34C H 0.0092 0.4928 0.2929 0.166 Uiso 0.25 1 calc PR C 4 O3' O -0.0093(6) 0.3802(7) 0.4493(12) 0.064(5) Uani 0.50 1 d P A 1 O6' O 0.0297(9) 0.4360(9) 0.8469(15) 0.066(8) Uani 0.195(11) 1 d PU B 2 H6' H 0.0167 0.4549 0.8045 0.079 Uiso 0.195(11) 1 calc PR B 2 C20' C 0.2887(7) 0.4936(9) 0.3194(12) 0.030(4) Uani 0.50 1 d PU C 7 C21' C 0.3262(8) 0.5122(8) 0.2788(13) 0.048(5) Uani 0.50 1 d PU C 7 H21' H 0.3431 0.4872 0.2470 0.058 Uiso 0.50 1 calc PR C 7 C22' C 0.3408(9) 0.5671(8) 0.2823(13) 0.060(5) Uani 0.50 1 d P C 7 H22' H 0.3676 0.5805 0.2542 0.072 Uiso 0.50 1 calc PR C 7 C23' C 0.3145(7) 0.6009(9) 0.3284(13) 0.055(6) Uani 0.50 1 d PU C 7 H23' H 0.3241 0.6386 0.3325 0.066 Uiso 0.50 1 calc PR C 7 C24' C 0.2755(8) 0.5841(9) 0.3686(13) 0.046(5) Uani 0.50 1 d P C 7 H24' H 0.2575 0.6093 0.3986 0.056 Uiso 0.50 1 calc PR C 7 C25' C 0.2621(6) 0.5258(7) 0.3639(10) 0.032(4) Uani 0.50 1 d PU C 7 H27 H 0.3336 0.3990 0.3046 0.050 Uiso 1 1 d . . . H15 H 0.1668 0.4936 0.0532 0.050 Uiso 1 1 d . . . C20 C 0.2772(7) 0.4994(10) 0.3348(12) 0.026(4) Uani 0.50 1 d PU C 8 C21 C 0.3173(8) 0.5262(7) 0.2953(11) 0.039(4) Uani 0.50 1 d PU C 8 H21 H 0.3373 0.5042 0.2639 0.047 Uiso 0.50 1 calc PR C 8 C22 C 0.3274(7) 0.5817(7) 0.3012(11) 0.038(4) Uani 0.50 1 d P C 8 H22 H 0.3520 0.5981 0.2712 0.046 Uiso 0.50 1 calc PR C 8 C23 C 0.3008(6) 0.6132(5) 0.3525(9) 0.036(3) Uani 0.50 1 d PU C 8 H23 H 0.3077 0.6515 0.3579 0.043 Uiso 0.50 1 calc PR C 8 C24 C 0.2648(9) 0.5902(9) 0.3955(11) 0.032(4) Uani 0.50 1 d P C 8 H24 H 0.2484 0.6126 0.4317 0.039 Uiso 0.50 1 calc PR C 8 C25 C 0.2520(6) 0.5346(6) 0.3867(9) 0.022(3) Uani 0.50 1 d PDU C 8 C26' C 0.2203(10) 0.5130(12) 0.416(2) 0.044(5) Uani 0.50 1 d P C 7 O14' O 0.1939(10) 0.5463(9) 0.4496(10) 0.070(6) Uani 0.50 1 d P C 7 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 0.0225(4) 0.0364(4) 0.0286(4) 0.0014(3) -0.0027(3) 0.0028(3) Na1 0.0431(11) 0.0299(9) 0.0303(10) -0.0053(7) -0.0072(8) 0.0092(8) O1 0.0240(18) 0.053(2) 0.048(2) 0.0061(17) -0.0010(15) -0.0024(15) N1 0.033(2) 0.049(2) 0.034(2) -0.0050(19) 0.0014(18) 0.0093(19) C1 0.025(2) 0.048(3) 0.040(3) -0.008(2) 0.006(2) 0.000(2) Mn2 0.0222(3) 0.0218(3) 0.0220(3) 0.0021(2) -0.0051(2) 0.0002(2) O2 0.0223(17) 0.0405(18) 0.0380(18) -0.0016(15) -0.0087(14) 0.0050(13) N2 0.0218(18) 0.0248(17) 0.0185(17) 0.0024(14) -0.0061(14) -0.0003(14) C2 0.031(3) 0.058(3) 0.043(3) -0.005(2) 0.011(2) 0.004(2) Mn3 0.0241(4) 0.0300(3) 0.0260(3) 0.0057(3) -0.0025(3) -0.0014(3) O3 0.018(6) 0.040(6) 0.048(6) 0.001(4) -0.017(4) 0.006(4) N3 0.030(2) 0.0225(17) 0.033(2) 0.0036(16) -0.0008(17) 0.0052(15) C3 0.029(3) 0.070(4) 0.063(4) -0.014(3) 0.018(3) -0.011(3) Mn4 0.0309(4) 0.0240(3) 0.0300(4) 0.0066(3) -0.0073(3) -0.0028(3) O4 0.0284(17) 0.0446(18) 0.0241(16) 0.0026(14) -0.0006(13) 0.0066(14) N4 0.049(3) 0.037(2) 0.029(2) -0.0059(18) -0.0138(19) 0.0060(19) C4 0.028(3) 0.084(5) 0.080(5) -0.003(4) 0.001(3) -0.001(3) O5 0.0295(17) 0.0292(15) 0.0255(16) -0.0035(12) -0.0050(13) 0.0027(13) N5 0.034(2) 0.0288(19) 0.034(2) 0.0113(16) -0.0042(17) 0.0029(16) C5 0.031(3) 0.057(4) 0.077(4) -0.002(3) -0.013(3) -0.001(3) O6 0.196(8) 0.076(5) 0.112(6) -0.023(4) 0.056(5) 0.037(5) N6 0.0197(19) 0.0325(19) 0.040(2) 0.0081(17) -0.0082(16) -0.0069(15) C6 0.021(2) 0.044(3) 0.057(3) -0.003(2) 0.001(2) 0.004(2) O7 0.0264(16) 0.0228(14) 0.0267(15) 0.0030(12) -0.0105(12) -0.0067(12) C7 0.033(3) 0.042(3) 0.055(3) 0.005(3) -0.014(2) 0.005(2) O8 0.0254(16) 0.0218(13) 0.0236(15) 0.0027(11) -0.0072(12) 0.0003(11) C8 0.037(3) 0.065(3) 0.023(2) 0.001(2) 0.004(2) 0.010(2) O9 0.0205(15) 0.0288(15) 0.0236(15) 0.0043(12) -0.0086(12) -0.0004(12) C9 0.037(3) 0.057(3) 0.025(2) 0.006(2) 0.003(2) 0.006(2) O10 0.036(2) 0.060(2) 0.048(2) 0.0193(18) -0.0015(17) -0.0103(17) C10 0.037(3) 0.045(3) 0.030(3) -0.012(2) -0.008(2) 0.010(2) O11 0.0309(17) 0.0360(16) 0.0215(15) 0.0064(13) -0.0029(13) 0.0001(13) C11 0.026(2) 0.038(2) 0.029(2) -0.0077(19) -0.0062(19) -0.0020(19) O12 0.040(2) 0.0194(15) 0.046(2) 0.0000(14) -0.0150(15) -0.0017(14) C12 0.035(3) 0.086(5) 0.051(4) -0.011(3) 0.008(3) 0.012(3) O13 0.046(2) 0.0347(18) 0.050(2) 0.0147(16) -0.0048(17) -0.0114(16) C13 0.069(5) 0.079(5) 0.075(5) -0.017(4) 0.035(4) 0.020(4) O14 0.083(10) 0.036(6) 0.037(8) -0.018(6) 0.013(8) -0.026(6) C14 0.035(3) 0.027(2) 0.029(2) 0.0015(18) -0.0062(19) 0.0058(18) O15 0.086(3) 0.042(2) 0.048(2) 0.0214(18) -0.002(2) 0.001(2) C15 0.024(2) 0.030(2) 0.024(2) 0.0024(17) -0.0040(17) -0.0002(17) O16 0.052(3) 0.064(3) 0.066(3) 0.023(2) -0.008(2) 0.010(2) C16 0.044(3) 0.051(3) 0.015(2) 0.005(2) -0.002(2) 0.001(2) C17 0.038(3) 0.043(3) 0.032(3) 0.006(2) -0.001(2) 0.001(2) C18 0.052(3) 0.038(3) 0.050(3) 0.021(2) -0.013(3) -0.005(2) C19 0.062(4) 0.051(3) 0.046(3) 0.027(3) -0.018(3) -0.012(3) C26 0.020(12) 0.046(11) 0.049(10) 0.016(7) -0.010(8) -0.012(9) C27 0.037(3) 0.026(2) 0.034(2) 0.0033(19) -0.004(2) -0.0060(19) C28 0.038(3) 0.028(2) 0.032(2) 0.0008(19) -0.009(2) -0.0014(19) C29 0.021(2) 0.045(3) 0.034(3) 0.002(2) -0.0088(19) -0.0037(19) C30 0.021(2) 0.032(2) 0.036(3) -0.0013(19) -0.0077(19) -0.0034(18) C31 0.033(3) 0.071(4) 0.061(4) 0.025(3) 0.003(3) -0.019(3) C32 0.037(3) 0.043(3) 0.059(4) 0.016(3) -0.006(3) -0.015(2) C33 0.102(7) 0.108(7) 0.109(7) -0.004(6) 0.009(6) -0.012(6) C34 0.106(15) 0.114(15) 0.117(15) -0.001(10) 0.032(10) 0.007(9) O3' 0.025(6) 0.055(9) 0.107(14) 0.020(8) 0.001(7) 0.018(5) O6' 0.061(11) 0.062(11) 0.075(11) 0.001(8) 0.015(8) -0.003(8) C20' 0.020(7) 0.031(6) 0.036(8) 0.006(6) -0.006(6) -0.002(5) C21' 0.048(8) 0.039(8) 0.056(8) 0.012(6) 0.006(6) -0.017(6) C22' 0.085(15) 0.047(10) 0.046(11) 0.007(8) 0.009(9) 0.000(9) C23' 0.050(8) 0.053(9) 0.061(10) 0.010(7) 0.006(7) -0.014(7) C24' 0.035(9) 0.025(7) 0.070(15) -0.005(10) -0.017(10) 0.003(6) C25' 0.031(7) 0.027(6) 0.035(7) -0.001(5) -0.005(5) -0.005(5) C20 0.023(7) 0.037(7) 0.021(6) 0.000(5) 0.010(5) 0.001(6) C21 0.051(7) 0.032(7) 0.036(6) 0.005(5) 0.012(5) -0.005(6) C22 0.048(10) 0.036(10) 0.038(8) -0.017(6) 0.028(6) -0.024(7) C23 0.043(7) 0.023(5) 0.037(6) 0.000(5) -0.004(5) -0.012(5) C24 0.053(11) 0.023(7) 0.020(7) -0.001(5) 0.004(5) -0.002(6) C25 0.025(6) 0.019(5) 0.025(6) -0.002(4) 0.008(4) 0.005(4) C26' 0.015(10) 0.014(7) 0.100(15) 0.001(7) 0.000(8) 0.002(7) O14' 0.097(10) 0.033(6) 0.069(13) -0.025(9) -0.019(10) 0.013(6) _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 1.879(3) . ? Mn1 O4 1.910(3) . ? Mn1 O2 1.946(3) . ? Mn1 O5 1.950(3) . ? Mn1 O9 2.176(3) 7_556 ? Mn1 N1 2.339(4) . ? Mn1 Mn2 3.2236(9) . ? Mn1 Na1 3.466(2) . ? Na1 O15 2.269(4) 6_566 ? Na1 O16 2.390(4) . ? Na1 O8 2.398(3) . ? Na1 O5 2.419(3) . ? Na1 O2 2.447(4) . ? Na1 O12 2.589(4) . ? Na1 C15 3.097(5) . ? Na1 Mn2 3.3980(18) . ? Na1 Mn4 3.514(2) . ? O1 C1 1.340(6) . ? N1 C10 1.453(7) . ? N1 C12 1.478(7) . ? N1 C8 1.493(6) . ? C1 C6 1.388(7) . ? C1 C2 1.397(7) . ? Mn2 O9 2.150(3) 7_556 ? Mn2 O7 2.162(3) . ? Mn2 O5 2.187(3) . ? Mn2 O8 2.195(3) . ? Mn2 N2 2.247(3) 7_556 ? Mn2 N2 2.300(3) . ? Mn2 Mn4 3.2229(9) . ? O2 C7 1.297(6) . ? N2 N3 1.212(5) . ? N2 Mn2 2.247(3) 7_556 ? N2 Mn3 2.465(3) . ? C2 C3 1.380(7) . ? C2 H2 0.9500 . ? Mn3 O4 2.126(3) 7_556 ? Mn3 O11 2.231(3) . ? Mn3 O7 2.243(3) . ? Mn3 O9 2.261(3) . ? Mn3 O10 2.317(4) . ? Mn3 N6 2.400(4) . ? O3 C7 1.264(17) . ? N3 N4 1.150(5) . ? C3 C4 1.402(9) . ? C3 H3 0.9500 . ? Mn4 O11 1.884(3) . ? Mn4 O13 1.902(4) . ? Mn4 O12 1.931(3) . ? Mn4 O8 1.955(3) . ? Mn4 O7 2.166(3) . ? Mn4 N5 2.290(4) . ? O4 C9 1.432(5) . ? O4 Mn3 2.126(3) 7_556 ? C4 C5 1.365(9) . ? C4 H4 0.9500 . ? O5 C11 1.431(5) . ? N5 C14 1.456(6) . ? N5 C18 1.484(6) . ? N5 C16 1.493(6) . ? C5 C6 1.397(7) . ? C5 H5 0.9500 . ? O6 C13 1.367(10) . ? O6 H6 0.8400 . ? N6 C28 1.458(6) . ? N6 C29 1.480(6) . ? N6 C32 1.482(6) . ? C6 C7 1.480(7) . ? O7 C27 1.424(5) . ? C7 O3' 1.262(18) . ? O8 C15 1.421(5) . ? C8 C9 1.519(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O9 C30 1.413(5) . ? O9 Mn2 2.150(3) 7_556 ? O9 Mn1 2.176(3) 7_556 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O10 C31 1.438(6) . ? O10 H27 0.8909 . ? C10 C11 1.521(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O11 C17 1.415(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O12 C26 1.27(4) . ? O12 C26' 1.38(3) . ? C12 C13 1.531(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O13 C20' 1.30(2) . ? O13 C20 1.40(2) . ? C13 O6' 1.46(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O14 C26 1.24(4) . ? C14 C15 1.523(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C19 1.420(6) . ? O15 Na1 2.269(4) 6_565 ? O15 H15 0.9282 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C34 1.410(10) . ? O16 C33 1.472(8) . ? C16 C17 1.503(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.517(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C26 C25 1.500(5) . ? C27 C28 1.516(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.507(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.494(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O6' H6' 0.8400 . ? C20' C25' 1.33(2) . ? C20' C21' 1.34(3) . ? C21' C22' 1.39(3) . ? C21' H21' 0.9500 . ? C22' C23' 1.37(2) . ? C22' H22' 0.9500 . ? C23' C24' 1.35(3) . ? C23' H23' 0.9500 . ? C24' C25' 1.46(3) . ? C24' H24' 0.9500 . ? C25' C26' 1.52(3) . ? C20 C25 1.432(18) . ? C20 C21 1.46(3) . ? C21 C22 1.37(2) . ? C21 H21 0.9500 . ? C22 C23 1.395(18) . ? C22 H22 0.9500 . ? C23 C24 1.37(3) . ? C23 H23 0.9500 . ? C24 C25 1.39(3) . ? C24 H24 0.9500 . ? C26' O14' 1.24(4) . ? 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 O4 88.97(15) . . ? O1 Mn1 O2 90.69(15) . . ? O4 Mn1 O2 177.57(14) . . ? O1 Mn1 O5 175.14(14) . . ? O4 Mn1 O5 94.68(13) . . ? O2 Mn1 O5 85.80(13) . . ? O1 Mn1 O9 100.82(14) . 7_556 ? O4 Mn1 O9 80.22(12) . 7_556 ? O2 Mn1 O9 97.49(12) . 7_556 ? O5 Mn1 O9 83.00(12) . 7_556 ? O1 Mn1 N1 96.03(16) . . ? O4 Mn1 N1 79.08(14) . . ? O2 Mn1 N1 103.35(14) . . ? O5 Mn1 N1 81.54(14) . . ? O9 Mn1 N1 152.95(13) 7_556 . ? O1 Mn1 Mn2 142.35(12) . . ? O4 Mn1 Mn2 84.87(10) . . ? O2 Mn1 Mn2 93.94(10) . . ? O5 Mn1 Mn2 41.54(9) . . ? O9 Mn1 Mn2 41.53(8) 7_556 . ? N1 Mn1 Mn2 118.98(11) . . ? O1 Mn1 Na1 134.02(11) . . ? O4 Mn1 Na1 137.00(11) . . ? O2 Mn1 Na1 43.34(10) . . ? O5 Mn1 Na1 42.51(9) . . ? O9 Mn1 Na1 88.72(8) 7_556 . ? N1 Mn1 Na1 94.66(11) . . ? Mn2 Mn1 Na1 60.93(4) . . ? O15 Na1 O16 87.50(17) 6_566 . ? O15 Na1 O8 145.61(17) 6_566 . ? O16 Na1 O8 107.13(15) . . ? O15 Na1 O5 101.11(14) 6_566 . ? O16 Na1 O5 153.42(16) . . ? O8 Na1 O5 79.77(11) . . ? O15 Na1 O2 115.51(16) 6_566 . ? O16 Na1 O2 87.50(14) . . ? O8 Na1 O2 96.48(12) . . ? O5 Na1 O2 66.06(11) . . ? O15 Na1 O12 82.71(15) 6_566 . ? O16 Na1 O12 99.68(14) . . ? O8 Na1 O12 64.49(11) . . ? O5 Na1 O12 106.29(12) . . ? O2 Na1 O12 160.86(13) . . ? O15 Na1 C15 157.19(16) 6_566 . ? O16 Na1 C15 83.18(15) . . ? O8 Na1 C15 26.24(10) . . ? O5 Na1 C15 96.43(11) . . ? O2 Na1 C15 84.92(12) . . ? O12 Na1 C15 78.42(12) . . ? O15 Na1 Mn2 129.49(13) 6_566 . ? O16 Na1 Mn2 142.57(13) . . ? O8 Na1 Mn2 40.03(7) . . ? O5 Na1 Mn2 39.89(8) . . ? O2 Na1 Mn2 81.39(9) . . ? O12 Na1 Mn2 82.23(8) . . ? C15 Na1 Mn2 60.40(8) . . ? O15 Na1 Mn1 112.88(13) 6_566 . ? O16 Na1 Mn1 120.58(13) . . ? O8 Na1 Mn1 86.72(8) . . ? O5 Na1 Mn1 33.00(8) . . ? O2 Na1 Mn1 33.09(7) . . ? O12 Na1 Mn1 136.41(9) . . ? C15 Na1 Mn1 89.73(9) . . ? Mn2 Na1 Mn1 56.02(3) . . ? O15 Na1 Mn4 114.02(14) 6_566 . ? O16 Na1 Mn4 108.81(13) . . ? O8 Na1 Mn4 32.10(7) . . ? O5 Na1 Mn4 90.73(9) . . ? O2 Na1 Mn4 128.24(10) . . ? O12 Na1 Mn4 32.63(7) . . ? C15 Na1 Mn4 50.87(9) . . ? Mn2 Na1 Mn4 55.55(3) . . ? Mn1 Na1 Mn4 111.23(5) . . ? C1 O1 Mn1 129.2(3) . . ? C10 N1 C12 113.8(4) . . ? C10 N1 C8 112.5(4) . . ? C12 N1 C8 111.6(4) . . ? C10 N1 Mn1 101.2(3) . . ? C12 N1 Mn1 113.0(3) . . ? C8 N1 Mn1 103.9(3) . . ? O1 C1 C6 124.8(5) . . ? O1 C1 C2 116.3(5) . . ? C6 C1 C2 118.9(5) . . ? O9 Mn2 O7 175.75(11) 7_556 . ? O9 Mn2 O5 78.32(11) 7_556 . ? O7 Mn2 O5 103.42(12) . . ? O9 Mn2 O8 98.54(11) 7_556 . ? O7 Mn2 O8 77.67(11) . . ? O5 Mn2 O8 89.63(11) . . ? O9 Mn2 N2 86.62(11) 7_556 7_556 ? O7 Mn2 N2 96.97(12) . 7_556 ? O5 Mn2 N2 96.84(12) . 7_556 ? O8 Mn2 N2 172.45(12) . 7_556 ? O9 Mn2 N2 93.28(12) 7_556 . ? O7 Mn2 N2 85.44(12) . . ? O5 Mn2 N2 169.17(12) . . ? O8 Mn2 N2 98.45(11) . . ? N2 Mn2 N2 75.65(13) 7_556 . ? O9 Mn2 Mn4 134.03(8) 7_556 . ? O7 Mn2 Mn4 41.93(7) . . ? O5 Mn2 Mn4 103.31(8) . . ? O8 Mn2 Mn4 36.43(8) . . ? N2 Mn2 Mn4 137.24(9) 7_556 . ? N2 Mn2 Mn4 87.43(8) . . ? O9 Mn2 Mn1 42.14(8) 7_556 . ? O7 Mn2 Mn1 139.65(8) . . ? O5 Mn2 Mn1 36.24(8) . . ? O8 Mn2 Mn1 96.50(8) . . ? N2 Mn2 Mn1 91.03(9) 7_556 . ? N2 Mn2 Mn1 134.70(9) . . ? Mn4 Mn2 Mn1 126.65(3) . . ? O9 Mn2 Na1 90.94(8) 7_556 . ? O7 Mn2 Na1 87.68(9) . . ? O5 Mn2 Na1 45.16(8) . . ? O8 Mn2 Na1 44.64(8) . . ? N2 Mn2 Na1 141.32(10) 7_556 . ? N2 Mn2 Na1 143.01(9) . . ? Mn4 Mn2 Na1 64.05(4) . . ? Mn1 Mn2 Na1 63.06(4) . . ? C7 O2 Mn1 131.0(3) . . ? C7 O2 Na1 124.9(3) . . ? Mn1 O2 Na1 103.57(13) . . ? N3 N2 Mn2 127.5(3) . 7_556 ? N3 N2 Mn2 121.1(3) . . ? Mn2 N2 Mn2 104.35(13) 7_556 . ? N3 N2 Mn3 109.2(3) . . ? Mn2 N2 Mn3 92.73(12) 7_556 . ? Mn2 N2 Mn3 91.96(12) . . ? C3 C2 C1 120.8(5) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? O4 Mn3 O11 97.80(12) 7_556 . ? O4 Mn3 O7 164.07(11) 7_556 . ? O11 Mn3 O7 73.38(11) . . ? O4 Mn3 O9 73.94(11) 7_556 . ? O11 Mn3 O9 154.43(11) . . ? O7 Mn3 O9 108.21(11) . . ? O4 Mn3 O10 86.80(14) 7_556 . ? O11 Mn3 O10 77.01(12) . . ? O7 Mn3 O10 103.61(13) . . ? O9 Mn3 O10 125.44(12) . . ? O4 Mn3 N6 121.18(13) 7_556 . ? O11 Mn3 N6 128.96(12) . . ? O7 Mn3 N6 73.85(12) . . ? O9 Mn3 N6 73.88(11) . . ? O10 Mn3 N6 74.03(13) . . ? O4 Mn3 N2 85.08(12) 7_556 . ? O11 Mn3 N2 75.94(11) . . ? O7 Mn3 N2 79.94(11) . . ? O9 Mn3 N2 79.23(11) . . ? O10 Mn3 N2 150.35(12) . . ? N6 Mn3 N2 133.75(12) . . ? N4 N3 N2 179.7(5) . . ? C2 C3 C4 120.2(6) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? O11 Mn4 O13 87.55(15) . . ? O11 Mn4 O12 177.57(14) . . ? O13 Mn4 O12 90.74(16) . . ? O11 Mn4 O8 95.11(13) . . ? O13 Mn4 O8 177.10(14) . . ? O12 Mn4 O8 86.63(13) . . ? O11 Mn4 O7 82.27(12) . . ? O13 Mn4 O7 98.63(13) . . ? O12 Mn4 O7 96.28(12) . . ? O8 Mn4 O7 82.89(11) . . ? O11 Mn4 N5 80.13(13) . . ? O13 Mn4 N5 98.09(15) . . ? O12 Mn4 N5 101.84(14) . . ? O8 Mn4 N5 81.28(13) . . ? O7 Mn4 N5 155.09(12) . . ? O11 Mn4 Mn2 82.13(9) . . ? O13 Mn4 Mn2 140.04(11) . . ? O12 Mn4 Mn2 98.11(10) . . ? O8 Mn4 Mn2 41.82(8) . . ? O7 Mn4 Mn2 41.83(8) . . ? N5 Mn4 Mn2 117.73(10) . . ? O11 Mn4 Na1 135.21(10) . . ? O13 Mn4 Na1 136.84(12) . . ? O12 Mn4 Na1 46.31(11) . . ? O8 Mn4 Na1 40.67(9) . . ? O7 Mn4 Na1 84.66(9) . . ? N5 Mn4 Na1 95.57(11) . . ? Mn2 Mn4 Na1 60.39(3) . . ? C9 O4 Mn1 111.3(3) . . ? C9 O4 Mn3 131.7(3) . 7_556 ? Mn1 O4 Mn3 108.88(14) . 7_556 ? C5 C4 C3 118.7(6) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C11 O5 Mn1 113.9(3) . . ? C11 O5 Mn2 128.1(3) . . ? Mn1 O5 Mn2 102.23(13) . . ? C11 O5 Na1 109.6(2) . . ? Mn1 O5 Na1 104.49(13) . . ? Mn2 O5 Na1 94.95(12) . . ? C14 N5 C18 113.4(4) . . ? C14 N5 C16 113.6(4) . . ? C18 N5 C16 112.0(4) . . ? C14 N5 Mn4 101.8(3) . . ? C18 N5 Mn4 110.4(3) . . ? C16 N5 Mn4 104.7(3) . . ? C4 C5 C6 121.7(6) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C13 O6 H6 109.5 . . ? C28 N6 C29 110.6(4) . . ? C28 N6 C32 112.1(4) . . ? C29 N6 C32 110.5(4) . . ? C28 N6 Mn3 107.5(3) . . ? C29 N6 Mn3 106.5(3) . . ? C32 N6 Mn3 109.4(3) . . ? C1 C6 C5 119.6(5) . . ? C1 C6 C7 123.2(4) . . ? C5 C6 C7 117.2(5) . . ? C27 O7 Mn2 126.7(3) . . ? C27 O7 Mn4 113.4(2) . . ? Mn2 O7 Mn4 96.24(11) . . ? C27 O7 Mn3 116.9(3) . . ? Mn2 O7 Mn3 102.18(11) . . ? Mn4 O7 Mn3 95.42(12) . . ? O3' C7 O3 27.5(8) . . ? O3' C7 O2 121.8(10) . . ? O3 C7 O2 117.0(8) . . ? O3' C7 C6 115.6(10) . . ? O3 C7 C6 121.2(8) . . ? O2 C7 C6 120.4(4) . . ? C15 O8 Mn4 115.2(2) . . ? C15 O8 Mn2 128.7(2) . . ? Mn4 O8 Mn2 101.75(12) . . ? C15 O8 Na1 105.5(2) . . ? Mn4 O8 Na1 107.23(13) . . ? Mn2 O8 Na1 95.34(11) . . ? N1 C8 C9 108.7(4) . . ? N1 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? N1 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? C30 O9 Mn2 124.7(3) . 7_556 ? C30 O9 Mn1 116.9(3) . 7_556 ? Mn2 O9 Mn1 96.34(11) 7_556 7_556 ? C30 O9 Mn3 116.6(2) . . ? Mn2 O9 Mn3 101.37(11) 7_556 . ? Mn1 O9 Mn3 95.54(11) 7_556 . ? O4 C9 C8 107.4(4) . . ? O4 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? O4 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C31 O10 Mn3 111.0(3) . . ? C31 O10 H27 108.1 . . ? Mn3 O10 H27 110.1 . . ? N1 C10 C11 110.2(4) . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C17 O11 Mn4 113.9(3) . . ? C17 O11 Mn3 132.6(3) . . ? Mn4 O11 Mn3 104.59(13) . . ? O5 C11 C10 110.7(4) . . ? O5 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? O5 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C26 O12 C26' 16(2) . . ? C26 O12 Mn4 140.2(11) . . ? C26' O12 Mn4 124.4(13) . . ? C26 O12 Na1 118.5(11) . . ? C26' O12 Na1 133.9(13) . . ? Mn4 O12 Na1 101.06(13) . . ? N1 C12 C13 115.5(5) . . ? N1 C12 H12A 108.4 . . ? C13 C12 H12A 108.4 . . ? N1 C12 H12B 108.4 . . ? C13 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C20' O13 C20 18.4(11) . . ? C20' O13 Mn4 139.1(8) . . ? C20 O13 Mn4 120.9(7) . . ? O6 C13 O6' 70.1(10) . . ? O6 C13 C12 106.9(6) . . ? O6' C13 C12 123.5(11) . . ? O6 C13 H13A 110.4 . . ? O6' C13 H13A 40.2 . . ? C12 C13 H13A 110.4 . . ? O6 C13 H13B 110.4 . . ? O6' C13 H13B 123.8 . . ? C12 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? N5 C14 C15 109.3(4) . . ? N5 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N5 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C19 O15 Na1 158.6(4) . 6_565 ? C19 O15 H15 100.5 . . ? Na1 O15 H15 100.7 6_565 . ? O8 C15 C14 110.3(3) . . ? O8 C15 Na1 48.25(19) . . ? C14 C15 Na1 98.9(3) . . ? O8 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? Na1 C15 H15A 70.2 . . ? O8 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? Na1 C15 H15B 149.6 . . ? H15A C15 H15B 108.1 . . ? C34 O16 C33 108.3(17) . . ? C34 O16 Na1 143.0(16) . . ? C33 O16 Na1 108.5(6) . . ? N5 C16 C17 108.9(4) . . ? N5 C16 H16A 109.9 . . ? C17 C16 H16A 109.9 . . ? N5 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O11 C17 C16 109.5(4) . . ? O11 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? O11 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? N5 C18 C19 115.0(4) . . ? N5 C18 H18A 108.5 . . ? C19 C18 H18A 108.5 . . ? N5 C18 H18B 108.5 . . ? C19 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? O15 C19 C18 109.9(5) . . ? O15 C19 H19A 109.7 . . ? C18 C19 H19A 109.7 . . ? O15 C19 H19B 109.7 . . ? C18 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? O14 C26 O12 131.3(17) . . ? O14 C26 C25 111(3) . . ? O12 C26 C25 116(3) . . ? O7 C27 C28 110.6(4) . . ? O7 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? O7 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? N6 C28 C27 111.5(4) . . ? N6 C28 H28A 109.3 . . ? C27 C28 H28A 109.3 . . ? N6 C28 H28B 109.3 . . ? C27 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? N6 C29 C30 110.8(4) . . ? N6 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? O9 C30 C29 112.1(4) . . ? O9 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? O9 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? O10 C31 C32 110.8(4) . . ? O10 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? O10 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N6 C32 C31 111.5(4) . . ? N6 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? N6 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? O16 C33 H33A 109.5 . . ? O16 C33 H33B 109.5 . . ? O16 C33 H33C 109.5 . . ? O16 C34 H34A 109.5 . . ? O16 C34 H34B 109.5 . . ? O16 C34 H34C 109.5 . . ? C13 O6' H6' 109.5 . . ? O13 C20' C25' 112.6(16) . . ? O13 C20' C21' 124.0(17) . . ? C25' C20' C21' 123(2) . . ? C20' C21' C22' 121.4(19) . . ? C20' C21' H21' 119.3 . . ? C22' C21' H21' 119.3 . . ? C23' C22' C21' 116(2) . . ? C23' C22' H22' 121.8 . . ? C21' C22' H22' 121.8 . . ? C24' C23' C22' 124(2) . . ? C24' C23' H23' 117.9 . . ? C22' C23' H23' 117.9 . . ? C23' C24' C25' 117.3(17) . . ? C23' C24' H24' 121.3 . . ? C25' C24' H24' 121.3 . . ? C20' C25' C24' 117.3(17) . . ? C20' C25' C26' 131.7(19) . . ? C24' C25' C26' 111.0(18) . . ? O13 C20 C25 132.4(16) . . ? O13 C20 C21 112.7(13) . . ? C25 C20 C21 114.6(18) . . ? C22 C21 C20 123.4(15) . . ? C22 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? C21 C22 C23 118.1(14) . . ? C21 C22 H22 121.0 . . ? C23 C22 H22 121.0 . . ? C24 C23 C22 121.6(14) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 121.1(13) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C20 120.9(16) . . ? C24 C25 C26 120(2) . . ? C20 C25 C26 119(2) . . ? O14' C26' O12 110(2) . . ? O14' C26' C25' 127(2) . . ? O12 C26' C25' 120(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.659 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.093 # Attachment '- 5_K2Mn8_1-D_new.cif' #========================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 822748' #TrackingRef '- 5_K2Mn8_1-D_new.cif' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains two halves the cluster as well as solvent MeoH molecules. There is a disorderd water molecule found coordinated to the K ion set each at 0.5 occupancy. There are several solvent MeOH molecules that have been modelled at 0.5 occupancy with bond (DFIX) and thermal (ISOR) restraints placed on them. All non H atoms were refined anisotropically. All H atoms were placed in calculated positions, except for on the water molecule. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H118 K2 Mn8 N12 O37' _chemical_formula_weight 2225.44 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' K K 0.2009 0.2494 '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 14.798(3) _cell_length_b 18.608(4) _cell_length_c 18.879(4) _cell_angle_alpha 77.060(3) _cell_angle_beta 75.811(5) _cell_angle_gamma 82.295(5) _cell_volume 4894.3(17) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8767 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 23.45 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 1.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details SADABS _exptl_special_details ; The Theta(max) value is low due to the poor diffacting nature of the crystals. Numerous samples where looked at with this particular sample providing the best data. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22307 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.1076 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.26 _reflns_number_total 13515 _reflns_number_gt 8958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 structure was solved by direct methods. The asymmetric unit contains two halves the cluster as well as solvent MeoH molecules. There is a disorderd water molecule found coordinated to the K ion set each at 0.5 occupancy. There are several solvent MeOH molecules that have been modelled at 0.5 occupancy with bond (DFIX) and thermal (ISOR) restraints placed on them. All non H atoms were refined anisotropically. All H atoms were placed in calculated positions, except for on the water molecule. ; _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^)+(0.1287P)^2^+45.7230P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13515 _refine_ls_number_parameters 1238 _refine_ls_number_restraints 112 _refine_ls_R_factor_all 0.1367 _refine_ls_R_factor_gt 0.0975 _refine_ls_wR_factor_ref 0.2720 _refine_ls_wR_factor_gt 0.2446 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.055 _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 0.85371(10) -0.04598(9) -0.15417(8) 0.0200(4) Uani 1 1 d . . . Mn2 Mn 0.88357(10) 0.02066(9) -0.01990(8) 0.0181(4) Uani 1 1 d . . . Mn3 Mn 0.92912(10) 0.05460(9) 0.14058(8) 0.0177(4) Uani 1 1 d . . . Mn4 Mn 0.73137(10) 0.10922(9) 0.08954(8) 0.0216(4) Uani 1 1 d . . . Mn5 Mn 0.16860(12) 0.58724(8) 0.61630(10) 0.0251(4) Uani 1 1 d . . . Mn6 Mn -0.02463(12) 0.63840(8) 0.55568(10) 0.0244(4) Uani 1 1 d . . . Mn7 Mn 0.11502(12) 0.47847(8) 0.52489(10) 0.0256(4) Uani 1 1 d . . . Mn8 Mn 0.24388(12) 0.34507(9) 0.45647(10) 0.0282(4) Uani 1 1 d . . . K1 K 0.62387(18) 0.06042(18) -0.06320(14) 0.0431(8) Uani 1 1 d . . . K2 K 0.3765(2) 0.43270(16) 0.5674(2) 0.0512(8) Uani 1 1 d . . . O1 O 0.9073(5) -0.0422(4) -0.2576(4) 0.0220(16) Uani 1 1 d . . . O2 O 0.7586(5) 0.0295(5) -0.1802(4) 0.034(2) Uani 1 1 d . B . O3 O 0.6950(7) 0.1310(6) -0.2434(6) 0.065(3) Uani 1 1 d . B . O4 O 0.9511(5) -0.1186(4) -0.1319(4) 0.0221(16) Uani 1 1 d . . . O5 O 0.7934(5) -0.0455(4) -0.0513(4) 0.0277(18) Uani 1 1 d . B . O6 O 0.6882(6) -0.2808(5) -0.1441(5) 0.047(2) Uani 1 1 d . . . H6 H 0.6448 -0.3070 -0.1356 0.056 Uiso 1 1 calc R . . O7 O 0.8233(5) 0.0083(4) 0.0971(3) 0.0195(16) Uani 1 1 d . . . O8 O 0.7827(5) 0.1164(4) -0.0162(4) 0.0257(18) Uani 1 1 d . B . O9 O 1.0548(4) -0.0286(4) 0.1375(3) 0.0182(15) Uani 1 1 d . . . O10 O 0.9090(4) 0.0829(4) 0.2595(4) 0.0297(18) Uani 1 1 d D . . O11 O 0.8350(5) 0.1479(4) 0.1086(4) 0.0256(17) Uani 1 1 d . . . O12 O 0.6261(5) 0.0675(4) 0.0745(4) 0.0250(17) Uani 1 1 d . B . O13 O 0.6708(5) 0.1072(4) 0.1896(4) 0.0258(17) Uani 1 1 d . . . O14 O 0.4999(6) 0.0118(5) 0.0949(4) 0.041(2) Uani 1 1 d . . . O15 O 0.4735(6) 0.3533(5) 0.1035(5) 0.045(2) Uani 1 1 d . . . H15 H 0.4822 0.3597 0.1429 0.054 Uiso 1 1 calc R . . O17 O 0.3673(7) 0.2453(5) 0.6278(5) 0.050(2) Uani 1 1 d . A . O18 O 0.3146(5) 0.3142(4) 0.5328(5) 0.036(2) Uani 1 1 d . A . O19 O 0.476(4) 0.370(2) 0.6876(17) 0.20(3) Uani 0.50 1 d P A 14 O20 O 0.1612(6) 0.4825(4) 0.6244(4) 0.033(2) Uani 1 1 d . A . O21 O 0.2345(5) 0.2439(4) 0.4557(4) 0.0272(18) Uani 1 1 d . A . O22 O -0.1062(5) 0.6378(4) 0.4692(4) 0.0260(17) Uani 1 1 d U . . O23 O -0.0734(5) 0.7544(4) 0.5860(5) 0.035(2) Uani 1 1 d D . . O24 O 0.1248(5) 0.5949(4) 0.5126(4) 0.0252(17) Uani 1 1 d . . . O25 O 0.1725(5) 0.3710(4) 0.3833(4) 0.0286(18) Uani 1 1 d . . . O26 O 0.5290(6) 0.3763(4) 0.2224(5) 0.049(2) Uani 1 1 d D . . H26 H 0.5821 0.3858 0.1992 0.059 Uiso 1 1 calc R . . O27 O 0.2540(5) 0.4462(4) 0.4622(5) 0.033(2) Uani 1 1 d . A . O28 O 0.0367(5) 0.6095(4) 0.6508(4) 0.0273(18) Uani 1 1 d . . . O29 O 0.1864(5) 0.6852(4) 0.6164(4) 0.0279(18) Uani 1 1 d . . . O30 O 0.3014(5) 0.5694(4) 0.5746(5) 0.0317(19) Uani 1 1 d . A . O31 O 0.4427(6) 0.5901(5) 0.5100(5) 0.042(2) Uani 1 1 d . . . O32 O 0.3094(11) 0.5707(9) 0.8665(10) 0.130(6) Uani 1 1 d . . . H32 H 0.3142 0.5531 0.9094 0.157 Uiso 1 1 calc R . . N1 N 0.7753(6) -0.1517(5) -0.1291(5) 0.027(2) Uani 1 1 d . B . N2 N 1.0005(6) 0.0746(5) 0.0044(5) 0.0195(19) Uani 1 1 d . . . N3 N 1.0167(6) 0.1381(6) -0.0175(5) 0.024(2) Uani 1 1 d . . . N4 N 1.0357(8) 0.1997(6) -0.0405(5) 0.039(3) Uani 1 1 d . . . N5 N 0.6961(6) 0.2341(5) 0.0507(5) 0.029(2) Uani 1 1 d . . . N6 N 0.8776(6) -0.0549(5) 0.2312(4) 0.0173(19) Uani 1 1 d . . . N7 N 0.3643(7) 0.3738(5) 0.3509(6) 0.034(2) Uani 1 1 d . . . N8 N 0.0400(6) 0.7287(4) 0.4465(5) 0.024(2) Uani 1 1 d . . . N9 N 0.1531(7) 0.5499(5) 0.7465(6) 0.036(3) Uani 1 1 d . . . N10 N -0.0412(7) 0.5041(5) 0.5745(6) 0.030(2) Uani 1 1 d . . . N11 N -0.0840(7) 0.4824(5) 0.6383(7) 0.027(2) Uani 1 1 d . . . N12 N -0.1255(8) 0.4607(6) 0.6983(7) 0.043(3) Uani 1 1 d . . . C1 C 0.8744(8) -0.0031(6) -0.3158(6) 0.026(3) Uani 1 1 d U B . C2 C 0.9196(10) -0.0196(7) -0.3854(6) 0.037(3) Uani 1 1 d . . . H2 H 0.9702 -0.0552 -0.3890 0.045 Uiso 1 1 calc R . . C3 C 0.8884(11) 0.0181(8) -0.4509(6) 0.047(4) Uani 1 1 d . . . H3 H 0.9159 0.0053 -0.4968 0.056 Uiso 1 1 calc R . . C4 C 0.8168(9) 0.0737(7) -0.4452(7) 0.037(3) Uani 1 1 d . . . H4 H 0.7976 0.0998 -0.4879 0.044 Uiso 1 1 calc R . . C5 C 0.7747(9) 0.0904(7) -0.3788(6) 0.035(3) Uani 1 1 d . B . H5 H 0.7258 0.1275 -0.3758 0.042 Uiso 1 1 calc R . . C6 C 0.8034(8) 0.0525(6) -0.3135(6) 0.025(3) Uani 1 1 d . . . C7 C 0.7492(8) 0.0738(6) -0.2427(6) 0.028(3) Uani 1 1 d . B . C8 C 0.8463(8) -0.2131(7) -0.1095(7) 0.034(3) Uani 1 1 d . . . H8A H 0.8378 -0.2564 -0.1270 0.041 Uiso 1 1 calc R . . H8B H 0.8391 -0.2261 -0.0559 0.041 Uiso 1 1 calc R . . C9 C 0.9436(8) -0.1874(6) -0.1463(6) 0.030(3) Uani 1 1 d . . . H9A H 0.9903 -0.2232 -0.1273 0.036 Uiso 1 1 calc R . . H9B H 0.9552 -0.1843 -0.1997 0.036 Uiso 1 1 calc R . . C10 C 0.7018(8) -0.1362(7) -0.0662(6) 0.032(3) Uani 1 1 d . . . H10A H 0.6720 -0.1811 -0.0408 0.038 Uiso 1 1 calc R B . H10B H 0.6549 -0.1000 -0.0843 0.038 Uiso 1 1 calc R . . C11 C 0.7401(8) -0.1066(7) -0.0111(6) 0.033(3) Uani 1 1 d . B . H11A H 0.6889 -0.0907 0.0267 0.040 Uiso 1 1 calc R . . H11B H 0.7795 -0.1453 0.0134 0.040 Uiso 1 1 calc R . . C12 C 0.7404(8) -0.1603(7) -0.1932(6) 0.034(3) Uani 1 1 d . . . H12A H 0.7923 -0.1804 -0.2277 0.041 Uiso 1 1 calc R B . H12B H 0.7211 -0.1114 -0.2185 0.041 Uiso 1 1 calc R . . C13 C 0.6605(8) -0.2081(7) -0.1777(7) 0.041(3) Uani 1 1 d . B . H13A H 0.6065 -0.1882 -0.1448 0.049 Uiso 1 1 calc R . . H13B H 0.6432 -0.2086 -0.2240 0.049 Uiso 1 1 calc R . . C14 C 0.7059(9) 0.2392(7) -0.0295(6) 0.043(3) Uani 1 1 d . B . H14A H 0.7134 0.2900 -0.0556 0.051 Uiso 1 1 calc R . . H14B H 0.6502 0.2240 -0.0384 0.051 Uiso 1 1 calc R . . C15 C 0.7892(9) 0.1905(7) -0.0581(7) 0.044(4) Uani 1 1 d . . . H15A H 0.7931 0.1909 -0.1103 0.052 Uiso 1 1 calc R B . H15B H 0.8456 0.2092 -0.0544 0.052 Uiso 1 1 calc R . . C16 C 0.7681(8) 0.2697(7) 0.0694(8) 0.042(3) Uani 1 1 d . . . H16A H 0.7405 0.3148 0.0865 0.050 Uiso 1 1 calc R . . H16B H 0.8173 0.2825 0.0253 0.050 Uiso 1 1 calc R . . C17 C 0.8089(8) 0.2170(6) 0.1301(7) 0.036(3) Uani 1 1 d . . . H17A H 0.8632 0.2366 0.1367 0.043 Uiso 1 1 calc R . . H17B H 0.7629 0.2114 0.1770 0.043 Uiso 1 1 calc R . . C18 C 0.5998(8) 0.2582(7) 0.0891(6) 0.033(3) Uani 1 1 d . . . H18A H 0.5998 0.2566 0.1408 0.039 Uiso 1 1 calc R . . H18B H 0.5580 0.2225 0.0886 0.039 Uiso 1 1 calc R . . C19 C 0.5609(8) 0.3335(8) 0.0571(7) 0.042(3) Uani 1 1 d . . . H19A H 0.6049 0.3695 0.0526 0.051 Uiso 1 1 calc R . . H19B H 0.5523 0.3342 0.0077 0.051 Uiso 1 1 calc R . . C20 C 0.5859(7) 0.0865(6) 0.2259(6) 0.021(2) Uani 1 1 d . B . C21 C 0.5538(7) 0.1034(6) 0.2970(5) 0.024(2) Uani 1 1 d . . . H21 H 0.5896 0.1296 0.3150 0.029 Uiso 1 1 calc R . . C22 C 0.4703(8) 0.0813(7) 0.3397(6) 0.036(3) Uani 1 1 d . . . H22 H 0.4499 0.0931 0.3867 0.043 Uiso 1 1 calc R . . C23 C 0.4134(8) 0.0412(8) 0.3154(6) 0.041(3) Uani 1 1 d . . . H23 H 0.3575 0.0246 0.3457 0.049 Uiso 1 1 calc R . . C24 C 0.4460(9) 0.0280(7) 0.2430(7) 0.038(3) Uani 1 1 d . B . H24 H 0.4098 0.0021 0.2250 0.045 Uiso 1 1 calc R . . C25 C 0.5297(7) 0.0514(6) 0.1964(6) 0.022(2) Uani 1 1 d U . . C26 C 0.5516(7) 0.0418(6) 0.1188(5) 0.019(2) Uani 1 1 d U B . C27 C 0.7837(7) -0.0558(6) 0.1400(5) 0.021(2) Uani 1 1 d . . . H27A H 0.8190 -0.0985 0.1221 0.026 Uiso 1 1 calc R . . H27B H 0.7201 -0.0545 0.1344 0.026 Uiso 1 1 calc R . . C28 C 0.7833(7) -0.0634(7) 0.2226(6) 0.027(3) Uani 1 1 d . . . H28A H 0.7390 -0.0259 0.2431 0.033 Uiso 1 1 calc R . . H28B H 0.7640 -0.1116 0.2499 0.033 Uiso 1 1 calc R . . C29 C 0.9447(7) -0.1156(6) 0.2104(5) 0.019(2) Uani 1 1 d U . . H29A H 0.9318 -0.1297 0.1676 0.023 Uiso 1 1 calc R . . H29B H 0.9375 -0.1581 0.2513 0.023 Uiso 1 1 calc R . . C30 C 1.0450(7) -0.0943(6) 0.1915(5) 0.019(2) Uani 1 1 d . . . H30A H 1.0613 -0.0875 0.2362 0.023 Uiso 1 1 calc R . . H30B H 1.0873 -0.1337 0.1728 0.023 Uiso 1 1 calc R . . C31 C 0.8745(7) -0.0449(6) 0.3081(5) 0.021(2) Uani 1 1 d . . . H31A H 0.9359 -0.0583 0.3191 0.026 Uiso 1 1 calc R . . H31B H 0.8310 -0.0771 0.3440 0.026 Uiso 1 1 calc R . . C32 C 0.8442(8) 0.0341(6) 0.3148(6) 0.023(2) Uani 1 1 d . . . H32A H 0.7814 0.0469 0.3064 0.027 Uiso 1 1 calc R . . H32B H 0.8436 0.0403 0.3645 0.027 Uiso 1 1 calc R . . C33 C 0.3369(8) 0.2502(7) 0.5714(7) 0.033(3) Uani 1 1 d . . . C34 C 0.3224(7) 0.1815(6) 0.5479(6) 0.020(2) Uani 1 1 d . A . C35 C 0.3633(7) 0.1152(6) 0.5819(6) 0.027(3) Uani 1 1 d . . . H35 H 0.3953 0.1153 0.6185 0.032 Uiso 1 1 calc R A . C36 C 0.3571(7) 0.0495(6) 0.5622(6) 0.025(3) Uani 1 1 d . A . H36 H 0.3871 0.0058 0.5834 0.030 Uiso 1 1 calc R . . C37 C 0.3053(7) 0.0495(6) 0.5103(6) 0.025(3) Uani 1 1 d . . . H37 H 0.2987 0.0051 0.4981 0.030 Uiso 1 1 calc R A . C38 C 0.2633(7) 0.1146(6) 0.4762(5) 0.020(2) Uani 1 1 d . A . H38 H 0.2274 0.1134 0.4425 0.024 Uiso 1 1 calc R . . C39 C 0.2746(7) 0.1830(6) 0.4923(6) 0.025(3) Uani 1 1 d . . . C40 C 0.2220(8) 0.3595(6) 0.3111(7) 0.032(3) Uani 1 1 d . . . H40A H 0.1844 0.3807 0.2748 0.039 Uiso 1 1 calc R . . H40B H 0.2347 0.3069 0.3115 0.039 Uiso 1 1 calc R . . C41 C 0.3136(8) 0.3962(6) 0.2899(7) 0.034(3) Uani 1 1 d . . . H41A H 0.3523 0.3820 0.2449 0.041 Uiso 1 1 calc R . . H41B H 0.3007 0.4496 0.2798 0.041 Uiso 1 1 calc R . . C42 C 0.4372(8) 0.3138(7) 0.3389(8) 0.040(3) Uani 1 1 d . . . H42A H 0.4147 0.2812 0.3146 0.048 Uiso 1 1 calc R . . H42B H 0.4438 0.2856 0.3875 0.048 Uiso 1 1 calc R . . C43 C 0.5327(9) 0.3323(7) 0.2946(8) 0.046(4) Uani 1 1 d . . . H43A H 0.5605 0.3591 0.3213 0.055 Uiso 1 1 calc R . . H43B H 0.5720 0.2869 0.2890 0.055 Uiso 1 1 calc R . . C44 C 0.3989(9) 0.4353(7) 0.3710(8) 0.041(3) Uani 1 1 d . A . H44A H 0.4383 0.4627 0.3271 0.049 Uiso 1 1 calc R . . H44B H 0.4368 0.4156 0.4074 0.049 Uiso 1 1 calc R . . C45 C 0.3192(9) 0.4877(6) 0.4032(7) 0.038(3) Uani 1 1 d . . . H45A H 0.3438 0.5235 0.4223 0.046 Uiso 1 1 calc R A . H45B H 0.2878 0.5145 0.3645 0.046 Uiso 1 1 calc R . . C46 C -0.0895(8) 0.6923(6) 0.4034(6) 0.025(3) Uani 1 1 d . . . H46A H -0.1298 0.7368 0.4107 0.030 Uiso 1 1 calc R . . H46B H -0.1041 0.6747 0.3631 0.030 Uiso 1 1 calc R . . C47 C 0.0124(8) 0.7100(6) 0.3824(6) 0.029(3) Uani 1 1 d . . . H47A H 0.0521 0.6676 0.3674 0.034 Uiso 1 1 calc R . . H47B H 0.0212 0.7514 0.3404 0.034 Uiso 1 1 calc R . . C48 C 0.0024(8) 0.8034(5) 0.4568(6) 0.026(3) Uani 1 1 d U . . H48A H -0.0567 0.8152 0.4414 0.031 Uiso 1 1 calc R . . H48B H 0.0454 0.8388 0.4257 0.031 Uiso 1 1 calc R . . C49 C -0.0125(8) 0.8095(6) 0.5383(7) 0.032(3) Uani 1 1 d . . . H49A H 0.0473 0.8021 0.5525 0.039 Uiso 1 1 calc R . . H49B H -0.0403 0.8586 0.5445 0.039 Uiso 1 1 calc R . . C50 C 0.1426(7) 0.7187(5) 0.4377(6) 0.024(2) Uani 1 1 d . . . H50A H 0.1598 0.7396 0.4747 0.028 Uiso 1 1 calc R . . H50B H 0.1723 0.7448 0.3888 0.028 Uiso 1 1 calc R . . C51 C 0.1771(8) 0.6377(6) 0.4466(6) 0.026(3) Uani 1 1 d . . . H51A H 0.1721 0.6195 0.4035 0.031 Uiso 1 1 calc R . . H51B H 0.2426 0.6321 0.4487 0.031 Uiso 1 1 calc R . . C52 C 0.3672(8) 0.6139(6) 0.5445(6) 0.030(3) Uani 1 1 d . A . C53 C 0.3500(8) 0.6925(6) 0.5509(6) 0.024(2) Uani 1 1 d . . . C54 C 0.4206(10) 0.7381(7) 0.5218(7) 0.042(3) Uani 1 1 d . A . H54 H 0.4761 0.7202 0.4932 0.050 Uiso 1 1 calc R . . C55 C 0.4131(10) 0.8109(6) 0.5332(7) 0.039(3) Uani 1 1 d . . . H55 H 0.4625 0.8407 0.5130 0.047 Uiso 1 1 calc R A . C56 C 0.3310(8) 0.8369(6) 0.5748(6) 0.029(3) Uani 1 1 d U A . H56 H 0.3247 0.8848 0.5834 0.035 Uiso 1 1 calc R . . C57 C 0.2579(7) 0.7930(5) 0.6039(6) 0.021(2) Uani 1 1 d . . . H57 H 0.2034 0.8113 0.6332 0.026 Uiso 1 1 calc R A . C58 C 0.2635(7) 0.7215(6) 0.5906(6) 0.022(2) Uani 1 1 d U A . C59 C 0.0165(8) 0.6345(7) 0.7193(6) 0.033(3) Uani 1 1 d . . . H59A H -0.0506 0.6426 0.7370 0.039 Uiso 1 1 calc R . . H59B H 0.0437 0.6810 0.7121 0.039 Uiso 1 1 calc R . . C60 C 0.0562(9) 0.5778(7) 0.7747(7) 0.044(3) Uani 1 1 d . . . H60A H 0.0539 0.5988 0.8179 0.053 Uiso 1 1 calc R . . H60B H 0.0174 0.5365 0.7911 0.053 Uiso 1 1 calc R . . C61 C 0.2258(10) 0.5807(7) 0.7729(8) 0.046(3) Uani 1 1 d . . . H61A H 0.2113 0.6337 0.7686 0.055 Uiso 1 1 calc R . . H61B H 0.2864 0.5727 0.7403 0.055 Uiso 1 1 calc R . . C62 C 0.2321(13) 0.5461(10) 0.8537(10) 0.076(5) Uani 1 1 d U . . H62A H 0.1760 0.5610 0.8881 0.091 Uiso 1 1 calc R . . H62B H 0.2384 0.4926 0.8610 0.091 Uiso 1 1 calc R . . C63 C 0.1695(12) 0.4696(6) 0.7536(8) 0.054(4) Uani 1 1 d . A . H63A H 0.1421 0.4454 0.8041 0.065 Uiso 1 1 calc R . . H63B H 0.2362 0.4554 0.7437 0.065 Uiso 1 1 calc R . . C64 C 0.1259(12) 0.4448(7) 0.6986(8) 0.056(4) Uani 1 1 d . . . H64A H 0.1398 0.3919 0.7017 0.067 Uiso 1 1 calc R A . H64B H 0.0585 0.4549 0.7116 0.067 Uiso 1 1 calc R . . O16' O 0.474(2) 0.1765(17) -0.1470(18) 0.123(10) Uani 0.50 1 d PU B 16 O1S O 0.2614(18) 0.5374(11) 1.0280(12) 0.076(7) Uani 0.50 1 d PD . . H1S H 0.2061 0.5530 1.0338 0.091 Uiso 0.50 1 calc PR . . O2S O -0.0305(19) 0.5573(13) 0.0370(13) 0.092(8) Uani 0.50 1 d PD . . H2S H 0.0274 0.5588 0.0301 0.111 Uiso 0.50 1 d P . . O3S O 0.073(2) 0.6420(18) 0.1482(16) 0.111(10) Uani 0.50 1 d PD . . H3S H 0.0245 0.6687 0.1445 0.133 Uiso 0.50 1 calc PR . . O6S O 0.2919(14) 0.3104(11) 0.7495(12) 0.154(7) Uani 1 1 d . . . H6S H 0.3283 0.3263 0.7676 0.184 Uiso 1 1 calc R . . O7S O 0.333(2) 0.7315(19) 0.1976(18) 0.124(11) Uani 0.50 1 d PU C 4 H7S H 0.3829 0.7111 0.1790 0.148 Uiso 0.50 1 d P D 4 O8S O 0.353(3) 0.7321(17) 0.288(2) 0.120(10) Uani 0.50 1 d P E 6 H8S H 0.3131 0.7674 0.2895 0.144 Uiso 0.50 1 calc PR E 6 O9S O 0.541(4) 0.5263(9) 0.1971(19) 0.19(2) Uani 0.50 1 d PD F 1 H9S H 0.5596 0.4834 0.2021 0.223 Uiso 0.50 1 d PD G 1 O16S O 0.432(3) 0.631(2) 0.204(2) 0.168(15) Uani 0.50 1 d PDU H 2 H16S H 0.4002 0.6219 0.2483 0.201 Uiso 0.50 1 d P I 2 O20S O 0.428(3) 0.311(2) 0.927(3) 0.190(18) Uani 0.50 1 d PDU . . H20S H 0.4252 0.2717 0.9135 0.228 Uiso 0.50 1 d P . . C1S C 0.272(2) 0.6822(17) 0.2373(17) 0.063(8) Uani 0.50 1 d PU C 4 H1S1 H 0.2751 0.6725 0.2888 0.095 Uiso 0.50 1 calc PR C 4 H1S2 H 0.2874 0.6370 0.2188 0.095 Uiso 0.50 1 calc PR C 4 H1S3 H 0.2099 0.7018 0.2325 0.095 Uiso 0.50 1 calc PR C 4 C4S C 0.2270(18) 0.2677(13) 0.8080(13) 0.124(9) Uani 1 1 d . . . H4S1 H 0.2126 0.2895 0.8513 0.186 Uiso 1 1 calc R . . H4S2 H 0.2544 0.2180 0.8201 0.186 Uiso 1 1 calc R . . H4S3 H 0.1706 0.2669 0.7917 0.186 Uiso 1 1 calc R . . C7S C 0.410(4) 0.730(2) 0.3409(19) 0.110(17) Uani 0.50 1 d P E 6 H7S1 H 0.4369 0.7726 0.3362 0.165 Uiso 0.50 1 d P J 6 H7S2 H 0.4578 0.6879 0.3353 0.165 Uiso 0.50 1 d P K 6 H7S3 H 0.3704 0.7158 0.3914 0.165 Uiso 0.50 1 d P L 6 O16 O 0.5105(4) 0.2112(4) -0.0835(17) 0.050(2) Uani 0.50 1 d P B 15 O19' O 0.4175(5) 0.4246(5) 0.7134(16) 0.050(2) Uani 0.50 1 d P A 13 H10 H 0.9779 0.0731 0.2634 0.060 Uiso 1 1 d D . . H23' H -0.1397 0.7670 0.5853 0.060 Uiso 1 1 d D . . C12S C 0.273(4) 0.4769(18) 1.088(2) 0.13(2) Uani 0.50 1 d PD . . H12C H 0.3382 0.4597 1.0824 0.191 Uiso 0.50 1 calc PR . . H12D H 0.2379 0.4373 1.0879 0.191 Uiso 0.50 1 calc PR . . H12E H 0.2514 0.4932 1.1348 0.191 Uiso 0.50 1 calc PR . . C13S C -0.067(2) 0.6179(16) -0.0124(15) 0.068(10) Uani 0.50 1 d PD . . H13C H -0.1062 0.6518 0.0160 0.102 Uiso 0.50 1 calc PR . . H13D H -0.1036 0.5996 -0.0392 0.102 Uiso 0.50 1 calc PR . . H13E H -0.0166 0.6428 -0.0470 0.102 Uiso 0.50 1 calc PR . . C14S C 0.091(4) 0.593(3) 0.095(3) 0.130(18) Uani 0.50 1 d PDU . . H14C H 0.1293 0.6167 0.0490 0.194 Uiso 0.50 1 calc PR . . H14D H 0.0330 0.5836 0.0866 0.194 Uiso 0.50 1 calc PR . . H14E H 0.1231 0.5477 0.1147 0.194 Uiso 0.50 1 calc PR . . C17S C 0.389(5) 0.586(4) 0.170(4) 0.20(3) Uani 0.50 1 d PDU H 2 H17C H 0.4336 0.5922 0.1127 0.303 Uiso 0.50 1 d P M 2 H17D H 0.3332 0.5983 0.1640 0.303 Uiso 0.50 1 d P N 2 H17E H 0.4057 0.5325 0.1855 0.303 Uiso 0.50 1 d P O 2 C18S C 0.494(4) 0.548(4) 0.135(3) 0.16(2) Uani 0.50 1 d PDU F 1 H18C H 0.5412 0.5323 0.0889 0.244 Uiso 0.50 1 d P P 1 H18D H 0.4998 0.6059 0.1163 0.244 Uiso 0.50 1 d P Q 1 H18E H 0.4397 0.5377 0.1385 0.244 Uiso 0.50 1 d P R 1 C19S C 0.337(2) 0.351(2) 0.941(3) 0.106(15) Uani 0.50 1 d PD . . H19C H 0.3403 0.4014 0.9147 0.158 Uiso 0.50 1 calc PR . . H19D H 0.3158 0.3502 0.9938 0.158 Uiso 0.50 1 calc PR . . H19E H 0.2935 0.3279 0.9249 0.158 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0136(8) 0.0344(10) 0.0117(8) -0.0055(7) -0.0017(6) -0.0017(7) Mn2 0.0099(8) 0.0328(10) 0.0093(8) -0.0039(7) 0.0008(6) 0.0003(7) Mn3 0.0099(8) 0.0296(9) 0.0109(8) -0.0023(7) 0.0005(6) -0.0005(7) Mn4 0.0103(8) 0.0384(10) 0.0144(8) -0.0082(7) 0.0009(6) 0.0018(7) Mn5 0.0275(10) 0.0114(8) 0.0442(11) -0.0100(7) -0.0194(8) 0.0003(7) Mn6 0.0274(10) 0.0107(8) 0.0419(10) -0.0068(7) -0.0196(8) -0.0005(7) Mn7 0.0320(10) 0.0086(8) 0.0440(11) -0.0073(7) -0.0231(8) 0.0015(7) Mn8 0.0299(10) 0.0128(8) 0.0508(11) -0.0114(8) -0.0224(9) 0.0014(7) K1 0.0247(14) 0.083(2) 0.0271(14) -0.0244(15) -0.0001(11) -0.0103(14) K2 0.0399(18) 0.0369(17) 0.087(2) -0.0303(16) -0.0195(16) 0.0033(14) O1 0.019(4) 0.034(4) 0.011(4) -0.003(3) -0.004(3) 0.000(3) O2 0.013(4) 0.054(5) 0.034(5) -0.015(4) 0.001(3) 0.000(4) O3 0.039(6) 0.064(7) 0.079(8) -0.008(6) -0.008(5) 0.019(5) O4 0.014(4) 0.030(4) 0.019(4) 0.000(3) -0.002(3) -0.003(3) O5 0.016(4) 0.050(5) 0.016(4) -0.003(4) 0.004(3) -0.014(4) O6 0.037(5) 0.045(6) 0.066(6) -0.008(5) -0.025(5) -0.005(4) O7 0.014(4) 0.028(4) 0.012(3) -0.001(3) 0.004(3) -0.004(3) O8 0.017(4) 0.038(5) 0.014(4) -0.001(3) 0.002(3) 0.010(3) O9 0.014(4) 0.027(4) 0.011(3) -0.003(3) 0.001(3) 0.000(3) O10 0.028(4) 0.033(5) 0.025(4) -0.004(4) -0.001(3) -0.004(4) O11 0.009(4) 0.033(4) 0.032(4) -0.005(3) -0.002(3) 0.001(3) O12 0.017(4) 0.046(5) 0.017(4) -0.013(3) -0.007(3) -0.002(3) O13 0.010(4) 0.048(5) 0.021(4) -0.017(4) 0.004(3) -0.006(3) O14 0.027(5) 0.074(6) 0.031(5) -0.021(4) -0.005(4) -0.016(4) O15 0.028(5) 0.056(6) 0.054(6) -0.025(5) -0.010(4) 0.008(4) O17 0.058(6) 0.044(6) 0.063(6) -0.016(5) -0.037(5) -0.002(5) O18 0.033(5) 0.023(4) 0.066(6) -0.018(4) -0.030(4) 0.002(4) O19 0.39(7) 0.18(4) 0.07(2) 0.03(2) -0.07(3) -0.22(4) O20 0.050(5) 0.017(4) 0.044(5) -0.006(4) -0.036(4) 0.000(4) O21 0.040(5) 0.011(4) 0.042(5) -0.012(3) -0.031(4) 0.009(3) O22 0.033(4) 0.009(3) 0.041(4) -0.007(3) -0.016(3) -0.005(3) O23 0.037(5) 0.025(4) 0.050(5) -0.013(4) -0.020(4) 0.000(4) O24 0.030(4) 0.008(4) 0.041(5) -0.004(3) -0.016(4) 0.002(3) O25 0.025(4) 0.018(4) 0.050(5) -0.012(4) -0.018(4) 0.000(3) O26 0.032(5) 0.076(7) 0.041(5) -0.014(5) -0.007(4) -0.004(5) O27 0.030(5) 0.015(4) 0.062(6) -0.013(4) -0.021(4) 0.000(3) O28 0.023(4) 0.026(4) 0.038(5) -0.007(4) -0.014(3) -0.004(3) O29 0.017(4) 0.018(4) 0.052(5) -0.017(4) -0.006(4) 0.001(3) O30 0.026(4) 0.025(4) 0.053(5) -0.021(4) -0.022(4) 0.013(4) O31 0.023(5) 0.047(5) 0.062(6) -0.030(5) -0.010(4) 0.010(4) O32 0.103(12) 0.148(15) 0.171(16) -0.046(12) -0.060(11) -0.040(10) N1 0.023(5) 0.035(6) 0.023(5) -0.002(4) -0.007(4) -0.007(4) N2 0.015(5) 0.029(6) 0.017(5) -0.007(4) -0.005(4) -0.003(4) N3 0.010(5) 0.040(7) 0.019(5) -0.010(5) 0.002(4) 0.003(4) N4 0.046(7) 0.046(7) 0.022(5) -0.001(5) 0.000(5) -0.012(5) N5 0.014(5) 0.040(6) 0.026(5) -0.004(4) -0.001(4) 0.009(4) N6 0.015(5) 0.026(5) 0.007(4) -0.001(4) 0.004(3) -0.002(4) N7 0.030(6) 0.015(5) 0.062(7) -0.008(5) -0.018(5) -0.003(4) N8 0.023(5) 0.012(5) 0.039(6) -0.008(4) -0.012(4) -0.001(4) N9 0.051(7) 0.025(5) 0.043(6) -0.001(5) -0.029(5) -0.016(5) N10 0.039(6) 0.013(5) 0.050(7) -0.015(5) -0.035(6) 0.009(4) N11 0.036(6) 0.011(5) 0.045(7) -0.007(5) -0.029(6) 0.004(4) N12 0.059(8) 0.029(6) 0.041(7) 0.003(5) -0.020(6) -0.001(5) C1 0.034(6) 0.033(6) 0.019(5) -0.007(4) -0.013(4) -0.017(5) C2 0.064(9) 0.032(7) 0.021(6) -0.011(5) -0.011(6) -0.007(6) C3 0.073(10) 0.060(9) 0.011(6) -0.007(6) -0.004(6) -0.025(8) C4 0.042(8) 0.032(7) 0.040(8) 0.010(6) -0.023(6) -0.018(6) C5 0.042(8) 0.034(7) 0.032(7) 0.011(6) -0.019(6) -0.023(6) C6 0.025(6) 0.024(6) 0.031(6) 0.001(5) -0.018(5) -0.005(5) C7 0.025(6) 0.031(7) 0.036(7) -0.005(6) -0.022(5) 0.000(5) C8 0.021(6) 0.048(8) 0.032(7) -0.005(6) -0.006(5) 0.000(6) C9 0.030(7) 0.028(7) 0.033(7) -0.002(5) -0.014(5) 0.000(5) C10 0.015(6) 0.051(8) 0.031(7) -0.013(6) 0.000(5) -0.011(5) C11 0.030(7) 0.053(8) 0.018(6) -0.011(6) 0.004(5) -0.016(6) C12 0.031(7) 0.045(8) 0.031(7) -0.021(6) -0.009(5) 0.004(6) C13 0.024(7) 0.054(9) 0.053(8) -0.028(7) -0.016(6) 0.006(6) C14 0.044(8) 0.043(8) 0.025(7) -0.001(6) 0.005(6) 0.013(6) C15 0.038(8) 0.033(7) 0.038(7) 0.006(6) 0.008(6) 0.020(6) C16 0.021(7) 0.034(7) 0.069(9) -0.010(7) -0.006(6) 0.001(5) C17 0.018(6) 0.039(7) 0.049(8) -0.022(6) 0.003(5) 0.004(5) C18 0.024(6) 0.051(8) 0.023(6) -0.016(6) 0.001(5) -0.001(6) C19 0.022(7) 0.069(9) 0.035(7) -0.022(7) -0.008(5) 0.021(6) C20 0.012(6) 0.025(6) 0.027(6) -0.006(5) -0.008(5) 0.002(4) C21 0.019(6) 0.041(7) 0.015(5) -0.012(5) -0.005(5) -0.002(5) C22 0.025(7) 0.062(9) 0.016(6) -0.011(6) 0.002(5) 0.001(6) C23 0.022(7) 0.070(10) 0.026(7) -0.006(6) 0.006(5) -0.015(6) C24 0.035(7) 0.046(8) 0.040(7) -0.011(6) -0.015(6) -0.012(6) C25 0.010(5) 0.035(6) 0.020(5) -0.001(4) -0.007(4) 0.003(4) C26 0.011(5) 0.036(6) 0.013(5) -0.008(4) -0.006(4) 0.002(4) C27 0.014(5) 0.034(6) 0.017(5) -0.005(5) -0.003(4) -0.004(5) C28 0.014(6) 0.045(7) 0.023(6) -0.011(5) 0.000(5) -0.006(5) C29 0.016(5) 0.025(5) 0.010(5) -0.003(4) 0.006(4) -0.003(4) C30 0.016(6) 0.029(6) 0.011(5) -0.006(5) 0.004(4) -0.006(5) C31 0.022(6) 0.031(6) 0.014(5) -0.006(5) -0.005(4) -0.008(5) C32 0.027(6) 0.024(6) 0.016(5) -0.005(5) 0.002(5) -0.007(5) C33 0.032(7) 0.037(7) 0.032(7) -0.014(6) -0.016(6) 0.017(6) C34 0.011(5) 0.020(6) 0.028(6) 0.003(5) -0.002(4) -0.009(4) C35 0.013(6) 0.034(7) 0.026(6) -0.003(5) 0.006(5) -0.001(5) C36 0.015(6) 0.024(6) 0.026(6) 0.006(5) 0.004(5) -0.001(5) C37 0.025(6) 0.015(6) 0.030(6) -0.006(5) 0.002(5) 0.008(5) C38 0.018(6) 0.026(6) 0.012(5) -0.005(4) 0.007(4) -0.001(5) C39 0.013(6) 0.028(6) 0.034(6) -0.010(5) -0.005(5) 0.003(5) C40 0.031(7) 0.027(6) 0.044(7) -0.009(6) -0.018(6) 0.003(5) C41 0.035(7) 0.021(6) 0.051(8) -0.010(6) -0.016(6) -0.005(5) C42 0.033(7) 0.037(7) 0.055(8) -0.017(6) -0.017(6) 0.006(6) C43 0.041(8) 0.040(8) 0.068(10) -0.024(7) -0.020(7) -0.007(6) C44 0.038(8) 0.038(7) 0.062(9) -0.021(7) -0.039(7) 0.012(6) C45 0.039(8) 0.019(6) 0.063(9) -0.018(6) -0.014(7) -0.005(6) C46 0.028(6) 0.021(6) 0.035(7) -0.007(5) -0.020(5) -0.002(5) C47 0.049(8) 0.009(5) 0.031(6) -0.008(5) -0.015(6) 0.006(5) C48 0.027(6) 0.013(5) 0.043(6) -0.003(4) -0.020(5) -0.005(4) C49 0.034(7) 0.014(6) 0.055(8) -0.009(5) -0.017(6) -0.004(5) C50 0.022(6) 0.016(6) 0.042(7) -0.018(5) -0.013(5) 0.000(5) C51 0.026(6) 0.027(6) 0.024(6) -0.005(5) -0.007(5) -0.001(5) C52 0.023(7) 0.033(7) 0.038(7) -0.009(6) -0.012(6) -0.005(6) C53 0.031(7) 0.015(6) 0.031(6) -0.006(5) -0.015(5) -0.003(5) C54 0.051(9) 0.044(8) 0.035(7) -0.017(6) -0.018(6) 0.008(7) C55 0.057(9) 0.017(6) 0.048(8) -0.003(6) -0.024(7) -0.008(6) C56 0.035(6) 0.014(5) 0.043(6) -0.001(5) -0.020(5) -0.004(5) C57 0.025(6) 0.018(6) 0.026(6) -0.008(5) -0.013(5) 0.000(5) C58 0.021(5) 0.024(5) 0.030(5) -0.010(4) -0.019(4) -0.002(4) C59 0.027(7) 0.042(7) 0.028(7) -0.007(6) 0.003(5) -0.016(6) C60 0.044(8) 0.047(8) 0.040(8) 0.004(6) -0.012(6) -0.019(7) C61 0.054(9) 0.033(7) 0.060(9) -0.022(7) -0.019(7) -0.005(6) C62 0.077(9) 0.087(9) 0.087(9) -0.033(7) -0.036(7) -0.029(7) C63 0.097(12) 0.019(7) 0.071(10) -0.006(6) -0.069(9) -0.001(7) C64 0.103(13) 0.029(7) 0.049(9) -0.003(7) -0.046(9) -0.010(8) O16' 0.118(13) 0.106(13) 0.128(13) -0.021(9) -0.002(9) 0.000(9) O1S 0.12(2) 0.049(13) 0.076(15) -0.012(12) -0.059(15) 0.017(13) O2S 0.12(2) 0.10(2) 0.078(17) -0.011(15) -0.033(16) -0.044(17) O3S 0.11(3) 0.12(3) 0.09(2) 0.019(19) -0.024(18) -0.058(19) O6S 0.111(16) 0.108(14) 0.24(2) -0.044(14) -0.021(14) -0.033(11) O7S 0.119(13) 0.139(14) 0.114(13) -0.020(9) -0.032(9) -0.013(9) O8S 0.14(3) 0.10(2) 0.12(3) 0.00(2) -0.03(2) -0.02(2) O9S 0.28(6) 0.17(4) 0.08(2) -0.03(2) -0.04(3) 0.03(4) O16S 0.174(18) 0.166(17) 0.170(17) -0.043(10) -0.039(10) -0.022(10) O20S 0.20(2) 0.19(2) 0.19(2) -0.040(10) -0.045(11) -0.024(10) C1S 0.068(12) 0.059(12) 0.057(11) 0.000(9) -0.011(9) -0.011(9) C4S 0.13(2) 0.097(17) 0.116(19) -0.024(15) 0.030(16) -0.009(16) C7S 0.20(5) 0.10(3) 0.034(19) 0.00(2) -0.04(3) -0.04(3) O16 0.050(4) 0.050(4) 0.050(4) -0.010 -0.011 -0.004 O19' 0.050(5) 0.050(4) 0.050(6) -0.010 -0.011 -0.004 C12S 0.20(6) 0.07(3) 0.13(4) -0.03(3) -0.10(4) 0.03(3) C13S 0.08(2) 0.06(2) 0.044(18) -0.013(16) 0.008(16) 0.016(18) C14S 0.12(2) 0.13(2) 0.13(2) -0.020(10) -0.027(11) -0.012(10) C17S 0.20(3) 0.20(3) 0.20(3) -0.035(12) -0.050(12) -0.022(11) C18S 0.16(2) 0.16(2) 0.16(2) -0.028(11) -0.034(11) -0.004(10) C19S 0.05(2) 0.09(3) 0.17(4) 0.00(3) -0.03(3) 0.00(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 1.897(7) . ? Mn1 O1 1.909(7) . ? Mn1 O2 1.922(8) . ? Mn1 O5 1.930(7) . ? Mn1 O9 2.182(7) 2_755 ? Mn1 N1 2.316(9) . ? Mn2 O7 2.143(6) . ? Mn2 O9 2.163(6) 2_755 ? Mn2 O8 2.167(7) . ? Mn2 O5 2.190(7) . ? Mn2 N2 2.296(9) . ? Mn2 N2 2.317(9) 2_755 ? Mn3 O11 2.148(7) . ? Mn3 O4 2.218(7) 2_755 ? Mn3 O9 2.252(7) . ? Mn3 O7 2.275(7) . ? Mn3 O10 2.360(7) . ? Mn3 N6 2.424(8) . ? Mn3 N2 2.491(8) . ? Mn4 O13 1.877(7) . ? Mn4 O11 1.918(7) . ? Mn4 O8 1.936(7) . ? Mn4 O12 1.935(7) . ? Mn4 O7 2.165(7) . ? Mn4 N5 2.305(9) . ? Mn5 O29 1.877(7) . ? Mn5 O28 1.920(7) . ? Mn5 O20 1.936(7) . ? Mn5 O30 1.943(8) . ? Mn5 O24 2.179(7) . ? Mn5 N9 2.362(10) . ? Mn6 O28 2.139(7) . ? Mn6 O25 2.219(8) 2_566 ? Mn6 O22 2.258(7) . ? Mn6 O24 2.267(7) . ? Mn6 O23 2.333(7) . ? Mn6 N8 2.429(9) . ? Mn6 N10 2.481(9) . ? Mn7 O24 2.147(7) . ? Mn7 O22 2.161(7) 2_566 ? Mn7 O20 2.170(7) . ? Mn7 O27 2.188(8) . ? Mn7 N10 2.300(11) . ? Mn7 N10 2.336(9) 2_566 ? Mn8 O25 1.880(7) . ? Mn8 O21 1.909(7) . ? Mn8 O18 1.925(8) . ? Mn8 O27 1.937(7) . ? Mn8 O22 2.201(8) 2_566 ? Mn8 N7 2.339(11) . ? K1 O12 2.641(7) . ? K1 O14 2.661(8) 2_655 ? K1 O2 2.700(8) . ? K1 O5 2.997(8) . ? K1 O16 3.067(3) . ? K1 O8 3.080(8) . ? K1 O14 3.106(8) . ? K1 C26 3.292(10) . ? K1 O16' 3.32(3) . ? K1 O3 3.319(11) . ? K1 C11 3.408(14) . ? K1 C7 3.413(12) . ? K2 O30 2.654(7) . ? K2 O31 2.745(9) 2_666 ? K2 O18 2.758(8) . ? K2 O19' 2.932(3) . ? K2 O19 2.95(4) . ? K2 O27 2.951(8) . ? K2 O31 3.089(9) . ? K2 O20 3.184(9) . ? K2 C52 3.291(12) . ? K2 O17 3.428(9) . ? O1 C1 1.334(12) . ? O2 C7 1.306(13) . ? O3 C7 1.243(14) . ? O4 C9 1.392(13) . ? O4 Mn3 2.218(7) 2_755 ? O5 C11 1.433(13) . ? O6 C13 1.412(15) . ? O6 H6 0.8200 . ? O7 C27 1.393(12) . ? O8 C15 1.431(14) . ? O9 C30 1.404(12) . ? O9 Mn2 2.163(6) 2_755 ? O9 Mn1 2.182(7) 2_755 ? O10 C32 1.467(12) . ? O10 H10 1.0284 . ? O11 C17 1.411(13) . ? O12 C26 1.286(12) . ? O13 C20 1.337(12) . ? O14 C26 1.223(12) . ? O14 K1 2.661(8) 2_655 ? O15 C19 1.428(14) . ? O15 H15 0.8200 . ? O17 C33 1.234(14) . ? O18 C33 1.297(13) . ? O20 C64 1.422(16) . ? O21 C39 1.336(12) . ? O22 C46 1.410(13) . ? O22 Mn7 2.161(7) 2_566 ? O22 Mn8 2.201(8) 2_566 ? O23 C49 1.453(14) . ? O23 H23' 0.9805 . ? O24 C51 1.427(13) . ? O25 C40 1.428(14) . ? O25 Mn6 2.219(8) 2_566 ? O26 C43 1.436(16) . ? O26 H26 0.8200 . ? O27 C45 1.433(15) . ? O28 C59 1.421(13) . ? O29 C58 1.335(13) . ? O30 C52 1.301(14) . ? O31 C52 1.229(14) . ? O31 K2 2.745(8) 2_666 ? O32 C62 1.379(19) . ? O32 H32 0.8200 . ? N1 C10 1.453(14) . ? N1 C12 1.475(14) . ? N1 C8 1.491(14) . ? N2 N3 1.197(13) . ? N2 Mn2 2.317(9) 2_755 ? N3 N4 1.177(14) . ? N5 C14 1.468(14) . ? N5 C16 1.474(15) . ? N5 C18 1.491(13) . ? N6 C29 1.457(12) . ? N6 C28 1.476(13) . ? N6 C31 1.495(12) . ? N7 C42 1.460(15) . ? N7 C44 1.472(15) . ? N7 C41 1.479(15) . ? N8 C48 1.463(13) . ? N8 C50 1.477(13) . ? N8 C47 1.491(14) . ? N9 C63 1.463(15) . ? N9 C60 1.469(17) . ? N9 C61 1.513(15) . ? N10 N11 1.222(15) . ? N10 Mn7 2.335(9) 2_566 ? N11 N12 1.159(15) . ? C1 C6 1.373(16) . ? C1 C2 1.402(16) . ? C2 C3 1.428(17) . ? C2 H2 0.9300 . ? C3 C4 1.380(19) . ? C3 H3 0.9300 . ? C4 C5 1.340(17) . ? C4 H4 0.9300 . ? C5 C6 1.409(15) . ? C5 H5 0.9300 . ? C6 C7 1.487(16) . ? C8 C9 1.526(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.527(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.507(17) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.492(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.522(17) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.495(17) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.401(14) . ? C20 C25 1.402(15) . ? C21 C22 1.357(16) . ? C21 H21 0.9300 . ? C22 C23 1.410(17) . ? C22 H22 0.9300 . ? C23 C24 1.399(17) . ? C23 H23 0.9300 . ? C24 C25 1.391(16) . ? C24 H24 0.9300 . ? C25 C26 1.467(14) . ? C27 C28 1.533(14) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.524(14) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.501(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.500(16) . ? C34 C35 1.390(15) . ? C34 C39 1.397(15) . ? C35 C36 1.374(16) . ? C35 H35 0.9300 . ? C36 C37 1.384(16) . ? C36 H36 0.9300 . ? C37 C38 1.383(14) . ? C37 H37 0.9300 . ? C38 C39 1.412(15) . ? C38 H38 0.9300 . ? C40 C41 1.525(16) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.496(18) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.522(17) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.523(16) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.528(16) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.510(14) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.477(15) . ? C53 C54 1.364(17) . ? C53 C58 1.420(15) . ? C54 C55 1.405(16) . ? C54 H54 0.9300 . ? C55 C56 1.367(17) . ? C55 H55 0.9300 . ? C56 C57 1.373(15) . ? C56 H56 0.9300 . ? C57 C58 1.396(14) . ? C57 H57 0.9300 . ? C59 C60 1.482(17) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.54(2) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.526(17) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? O1S C12S 1.437(10) . ? O1S H1S 0.8200 . ? O2S C13S 1.431(10) . ? O2S H2S 0.8377 . ? O3S C14S 1.449(10) . ? O3S H3S 0.8200 . ? O6S C4S 1.44(3) . ? O6S H6S 0.8200 . ? O7S C1S 1.34(4) . ? O7S H7S 0.8160 . ? O8S C7S 1.46(5) . ? O8S H8S 0.8200 . ? O9S C18S 1.453(10) . ? O9S H9S 0.8009 . ? O16S C17S 1.455(11) . ? O16S H16S 0.8389 . ? O20S C19S 1.449(10) . ? O20S H20S 0.8452 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? C7S H7S1 0.9096 . ? C7S H7S2 0.9901 . ? C7S H7S3 0.9890 . ? C12S H12C 0.9600 . ? C12S H12D 0.9600 . ? C12S H12E 0.9600 . ? C13S H13C 0.9600 . ? C13S H13D 0.9600 . ? C13S H13E 0.9600 . ? C14S H14C 0.9600 . ? C14S H14D 0.9600 . ? C14S H14E 0.9600 . ? C17S H17C 1.1183 . ? C17S H17D 0.8526 . ? C17S H17E 0.9865 . ? C18S H18C 1.0487 . ? C18S H18D 1.0630 . ? C18S H18E 0.8407 . ? C19S H19C 0.9600 . ? C19S H19D 0.9600 . ? C19S H19E 0.9600 . ? 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 O1 88.7(3) . . ? O4 Mn1 O2 177.6(3) . . ? O1 Mn1 O2 89.4(3) . . ? O4 Mn1 O5 94.8(3) . . ? O1 Mn1 O5 176.5(3) . . ? O2 Mn1 O5 87.1(3) . . ? O4 Mn1 O9 82.8(3) . 2_755 ? O1 Mn1 O9 96.5(3) . 2_755 ? O2 Mn1 O9 96.1(3) . 2_755 ? O5 Mn1 O9 84.1(3) . 2_755 ? O4 Mn1 N1 80.4(3) . . ? O1 Mn1 N1 98.9(3) . . ? O2 Mn1 N1 101.3(3) . . ? O5 Mn1 N1 81.5(3) . . ? O9 Mn1 N1 156.8(3) 2_755 . ? O7 Mn2 O9 177.8(3) . 2_755 ? O7 Mn2 O8 78.0(3) . . ? O9 Mn2 O8 103.8(3) 2_755 . ? O7 Mn2 O5 100.1(3) . . ? O9 Mn2 O5 78.7(3) 2_755 . ? O8 Mn2 O5 94.5(3) . . ? O7 Mn2 N2 85.6(3) . . ? O9 Mn2 N2 95.3(3) 2_755 . ? O8 Mn2 N2 95.7(3) . . ? O5 Mn2 N2 169.2(3) . . ? O7 Mn2 N2 94.0(3) . 2_755 ? O9 Mn2 N2 84.3(3) 2_755 2_755 ? O8 Mn2 N2 168.6(3) . 2_755 ? O5 Mn2 N2 94.9(3) . 2_755 ? N2 Mn2 N2 75.4(4) . 2_755 ? O11 Mn3 O4 96.6(3) . 2_755 ? O11 Mn3 O9 161.6(3) . . ? O4 Mn3 O9 74.5(3) 2_755 . ? O11 Mn3 O7 74.7(3) . . ? O4 Mn3 O7 155.7(2) 2_755 . ? O9 Mn3 O7 106.8(2) . . ? O11 Mn3 O10 91.3(3) . . ? O4 Mn3 O10 74.8(2) 2_755 . ? O9 Mn3 O10 101.5(2) . . ? O7 Mn3 O10 127.1(2) . . ? O11 Mn3 N6 123.0(3) . . ? O4 Mn3 N6 128.7(3) 2_755 . ? O9 Mn3 N6 73.9(3) . . ? O7 Mn3 N6 73.1(3) . . ? O10 Mn3 N6 73.2(3) . . ? O11 Mn3 N2 83.8(3) . . ? O4 Mn3 N2 78.1(3) 2_755 . ? O9 Mn3 N2 78.6(3) . . ? O7 Mn3 N2 78.4(3) . . ? O10 Mn3 N2 151.7(3) . . ? N6 Mn3 N2 132.1(3) . . ? O13 Mn4 O11 88.1(3) . . ? O13 Mn4 O8 174.4(3) . . ? O11 Mn4 O8 95.4(3) . . ? O13 Mn4 O12 89.9(3) . . ? O11 Mn4 O12 177.5(3) . . ? O8 Mn4 O12 86.6(3) . . ? O13 Mn4 O7 102.2(3) . . ? O11 Mn4 O7 82.0(3) . . ? O8 Mn4 O7 82.7(3) . . ? O12 Mn4 O7 96.9(3) . . ? O13 Mn4 N5 94.9(3) . . ? O11 Mn4 N5 79.8(3) . . ? O8 Mn4 N5 81.5(3) . . ? O12 Mn4 N5 101.9(3) . . ? O7 Mn4 N5 154.5(3) . . ? O29 Mn5 O28 88.6(3) . . ? O29 Mn5 O20 172.8(3) . . ? O28 Mn5 O20 95.4(3) . . ? O29 Mn5 O30 89.9(3) . . ? O28 Mn5 O30 175.8(3) . . ? O20 Mn5 O30 86.5(3) . . ? O29 Mn5 O24 104.0(3) . . ? O28 Mn5 O24 81.1(3) . . ? O20 Mn5 O24 82.5(3) . . ? O30 Mn5 O24 95.5(3) . . ? O29 Mn5 N9 93.1(3) . . ? O28 Mn5 N9 79.3(3) . . ? O20 Mn5 N9 81.8(3) . . ? O30 Mn5 N9 104.7(4) . . ? O24 Mn5 N9 153.5(3) . . ? O28 Mn6 O25 97.3(3) . 2_566 ? O28 Mn6 O22 163.8(3) . . ? O25 Mn6 O22 73.9(3) 2_566 . ? O28 Mn6 O24 74.6(3) . . ? O25 Mn6 O24 155.2(3) 2_566 . ? O22 Mn6 O24 107.6(3) . . ? O28 Mn6 O23 88.4(3) . . ? O25 Mn6 O23 75.8(3) 2_566 . ? O22 Mn6 O23 102.1(2) . . ? O24 Mn6 O23 126.3(2) . . ? O28 Mn6 N8 121.5(3) . . ? O25 Mn6 N8 128.9(3) 2_566 . ? O22 Mn6 N8 73.8(3) . . ? O24 Mn6 N8 73.3(3) . . ? O23 Mn6 N8 73.7(3) . . ? O28 Mn6 N10 85.7(3) . . ? O25 Mn6 N10 77.4(3) 2_566 . ? O22 Mn6 N10 79.1(3) . . ? O24 Mn6 N10 78.6(3) . . ? O23 Mn6 N10 151.6(3) . . ? N8 Mn6 N10 132.2(3) . . ? O24 Mn7 O22 176.9(3) . 2_566 ? O24 Mn7 O20 78.1(3) . . ? O22 Mn7 O20 104.7(3) 2_566 . ? O24 Mn7 O27 100.4(3) . . ? O22 Mn7 O27 78.2(3) 2_566 . ? O20 Mn7 O27 95.1(3) . . ? O24 Mn7 N10 85.2(3) . . ? O22 Mn7 N10 95.8(3) 2_566 . ? O20 Mn7 N10 95.2(3) . . ? O27 Mn7 N10 169.1(3) . . ? O24 Mn7 N10 93.0(3) . 2_566 ? O22 Mn7 N10 84.4(3) 2_566 2_566 ? O20 Mn7 N10 167.1(3) . 2_566 ? O27 Mn7 N10 95.7(3) . 2_566 ? N10 Mn7 N10 74.5(4) . 2_566 ? O25 Mn8 O21 87.7(3) . . ? O25 Mn8 O18 177.4(3) . . ? O21 Mn8 O18 89.9(3) . . ? O25 Mn8 O27 94.8(3) . . ? O21 Mn8 O27 177.2(3) . . ? O18 Mn8 O27 87.6(3) . . ? O25 Mn8 O22 82.1(3) . 2_566 ? O21 Mn8 O22 96.3(3) . 2_566 ? O18 Mn8 O22 97.2(3) . 2_566 ? O27 Mn8 O22 82.8(3) . 2_566 ? O25 Mn8 N7 80.8(3) . . ? O21 Mn8 N7 100.1(3) . . ? O18 Mn8 N7 100.6(4) . . ? O27 Mn8 N7 81.6(3) . . ? O22 Mn8 N7 155.7(3) 2_566 . ? O12 K1 O14 122.8(3) . 2_655 ? O12 K1 O2 133.0(2) . . ? O14 K1 O2 92.7(3) 2_655 . ? O12 K1 O5 83.4(2) . . ? O14 K1 O5 106.9(3) 2_655 . ? O2 K1 O5 55.2(2) . . ? O12 K1 O16 91.06(18) . . ? O14 K1 O16 94.9(2) 2_655 . ? O2 K1 O16 117.7(2) . . ? O5 K1 O16 156.91(18) . . ? O12 K1 O8 54.7(2) . . ? O14 K1 O8 169.8(3) 2_655 . ? O2 K1 O8 84.8(2) . . ? O5 K1 O8 63.6(2) . . ? O16 K1 O8 95.04(15) . . ? O12 K1 O14 43.4(2) . . ? O14 K1 O14 79.6(2) 2_655 . ? O2 K1 O14 150.8(3) . . ? O5 K1 O14 99.9(2) . . ? O16 K1 O14 91.15(18) . . ? O8 K1 O14 97.9(2) . . ? O12 K1 C26 21.7(2) . . ? O14 K1 C26 101.4(3) 2_655 . ? O2 K1 C26 148.1(3) . . ? O5 K1 C26 93.1(2) . . ? O16 K1 C26 89.68(19) . . ? O8 K1 C26 76.3(2) . . ? O14 K1 C26 21.8(2) . . ? O12 K1 O16' 118.3(6) . . ? O14 K1 O16' 68.7(6) 2_655 . ? O2 K1 O16' 102.0(6) . . ? O5 K1 O16' 157.1(6) . . ? O16 K1 O16' 30.7(6) . . ? O8 K1 O16' 121.5(6) . . ? O14 K1 O16' 101.3(6) . . ? C26 K1 O16' 109.7(6) . . ? O12 K1 O3 146.4(3) . . ? O14 K1 O3 89.6(3) 2_655 . ? O2 K1 O3 41.8(2) . . ? O5 K1 O3 95.9(2) . . ? O16 K1 O3 76.51(18) . . ? O8 K1 O3 94.9(2) . . ? O14 K1 O3 163.0(2) . . ? C26 K1 O3 163.1(3) . . ? O16' K1 O3 62.2(6) . . ? O12 K1 C11 80.1(3) . . ? O14 K1 C11 88.0(3) 2_655 . ? O2 K1 C11 70.7(3) . . ? O5 K1 C11 24.8(2) . . ? O16 K1 C11 170.9(2) . . ? O8 K1 C11 81.8(2) . . ? O14 K1 C11 80.8(3) . . ? C26 K1 C11 81.2(3) . . ? O16' K1 C11 155.5(6) . . ? O3 K1 C11 112.2(2) . . ? O12 K1 C7 146.1(2) . . ? O14 K1 C7 89.1(3) 2_655 . ? O2 K1 C7 20.8(2) . . ? O5 K1 C7 75.7(2) . . ? O16 K1 C7 97.7(2) . . ? O8 K1 C7 91.8(2) . . ? O14 K1 C7 166.2(3) . . ? C26 K1 C7 166.6(3) . . ? O16' K1 C7 81.6(6) . . ? O3 K1 C7 21.2(2) . . ? C11 K1 C7 91.0(3) . . ? O30 K2 O31 119.9(3) . 2_666 ? O30 K2 O18 132.6(2) . . ? O31 K2 O18 94.6(3) 2_666 . ? O30 K2 O19' 87.23(18) . . ? O31 K2 O19' 97.5(2) 2_666 . ? O18 K2 O19' 121.6(2) . . ? O30 K2 O19 112.1(9) . . ? O31 K2 O19 77.5(10) 2_666 . ? O18 K2 O19 106.1(6) . . ? O19' K2 O19 26.4(10) . . ? O30 K2 O27 82.0(2) . . ? O31 K2 O27 107.2(3) 2_666 . ? O18 K2 O27 55.7(2) . . ? O19' K2 O27 155.2(2) . . ? O19 K2 O27 161.0(6) . . ? O30 K2 O31 43.9(2) . . ? O31 K2 O31 76.1(3) 2_666 . ? O18 K2 O31 146.5(3) . . ? O19' K2 O31 91.70(18) . . ? O19 K2 O31 103.2(6) . . ? O27 K2 O31 95.8(2) . . ? O30 K2 O20 53.2(2) . . ? O31 K2 O20 167.6(3) 2_666 . ? O18 K2 O20 86.1(2) . . ? O19' K2 O20 92.61(16) . . ? O19 K2 O20 114.3(10) . . ? O27 K2 O20 63.1(2) . . ? O31 K2 O20 96.5(2) . . ? O30 K2 C52 22.1(3) . . ? O31 K2 C52 97.9(3) 2_666 . ? O18 K2 C52 146.4(3) . . ? O19' K2 C52 87.4(2) . . ? O19 K2 C52 107.0(7) . . ? O27 K2 C52 90.8(2) . . ? O31 K2 C52 21.9(2) . . ? O20 K2 C52 75.3(2) . . ? O30 K2 O17 149.8(3) . . ? O31 K2 O17 89.8(3) 2_666 . ? O18 K2 O17 39.9(2) . . ? O19' K2 O17 83.21(17) . . ? O19 K2 O17 66.4(6) . . ? O27 K2 O17 95.0(2) . . ? O31 K2 O17 164.2(2) . . ? O20 K2 O17 98.6(2) . . ? C52 K2 O17 168.6(3) . . ? O30 K2 K2 79.2(2) . 2_666 ? O31 K2 K2 40.67(19) 2_666 2_666 ? O18 K2 K2 127.5(2) . 2_666 ? O19' K2 K2 95.62(10) . 2_666 ? O19 K2 K2 91.4(7) . 2_666 ? O27 K2 K2 104.2(2) . 2_666 ? O31 K2 K2 35.38(15) . 2_666 ? O20 K2 K2 131.23(17) . 2_666 ? C52 K2 K2 57.3(2) . 2_666 ? O17 K2 K2 130.1(2) . 2_666 ? C1 O1 Mn1 128.0(7) . . ? C7 O2 Mn1 133.1(7) . . ? C7 O2 K1 112.1(7) . . ? Mn1 O2 K1 114.5(3) . . ? C7 O3 K1 83.7(7) . . ? C9 O4 Mn1 114.2(6) . . ? C9 O4 Mn3 133.8(6) . 2_755 ? Mn1 O4 Mn3 104.8(3) . 2_755 ? C11 O5 Mn1 117.3(6) . . ? C11 O5 Mn2 133.1(6) . . ? Mn1 O5 Mn2 101.9(3) . . ? C11 O5 K1 93.9(6) . . ? Mn1 O5 K1 102.9(3) . . ? Mn2 O5 K1 101.9(3) . . ? C13 O6 H6 109.5 . . ? C27 O7 Mn2 122.8(6) . . ? C27 O7 Mn4 116.8(6) . . ? Mn2 O7 Mn4 96.4(3) . . ? C27 O7 Mn3 117.6(6) . . ? Mn2 O7 Mn3 103.3(3) . . ? Mn4 O7 Mn3 94.7(3) . . ? C15 O8 Mn4 114.4(7) . . ? C15 O8 Mn2 130.2(6) . . ? Mn4 O8 Mn2 102.8(3) . . ? C15 O8 K1 104.0(7) . . ? Mn4 O8 K1 100.9(3) . . ? Mn2 O8 K1 100.0(3) . . ? C30 O9 Mn2 125.8(6) . 2_755 ? C30 O9 Mn1 114.4(6) . 2_755 ? Mn2 O9 Mn1 95.0(3) 2_755 2_755 ? C30 O9 Mn3 116.6(5) . . ? Mn2 O9 Mn3 104.1(3) 2_755 . ? Mn1 O9 Mn3 94.8(3) 2_755 . ? C32 O10 Mn3 109.9(6) . . ? C32 O10 H10 115.5 . . ? Mn3 O10 H10 97.5 . . ? C17 O11 Mn4 111.6(6) . . ? C17 O11 Mn3 133.7(7) . . ? Mn4 O11 Mn3 106.8(3) . . ? C26 O12 Mn4 133.3(6) . . ? C26 O12 K1 108.9(6) . . ? Mn4 O12 K1 117.7(3) . . ? C20 O13 Mn4 129.2(6) . . ? C26 O14 K1 171.9(7) . 2_655 ? C26 O14 K1 87.7(6) . . ? K1 O14 K1 100.4(2) 2_655 . ? C19 O15 H15 109.5 . . ? C33 O17 K2 83.2(7) . . ? C33 O18 Mn8 133.3(7) . . ? C33 O18 K2 114.6(7) . . ? Mn8 O18 K2 112.0(3) . . ? C64 O20 Mn5 113.4(7) . . ? C64 O20 Mn7 127.4(7) . . ? Mn5 O20 Mn7 103.1(3) . . ? C64 O20 K2 111.3(8) . . ? Mn5 O20 K2 99.9(3) . . ? Mn7 O20 K2 97.6(3) . . ? C39 O21 Mn8 128.9(6) . . ? C46 O22 Mn7 125.7(6) . 2_566 ? C46 O22 Mn8 113.9(6) . 2_566 ? Mn7 O22 Mn8 95.5(3) 2_566 2_566 ? C46 O22 Mn6 117.2(6) . . ? Mn7 O22 Mn6 103.8(3) 2_566 . ? Mn8 O22 Mn6 94.6(3) 2_566 . ? C49 O23 Mn6 110.5(6) . . ? C49 O23 H23' 113.8 . . ? Mn6 O23 H23' 110.1 . . ? C51 O24 Mn7 122.2(6) . . ? C51 O24 Mn5 117.4(6) . . ? Mn7 O24 Mn5 96.2(3) . . ? C51 O24 Mn6 117.4(6) . . ? Mn7 O24 Mn6 103.4(3) . . ? Mn5 O24 Mn6 95.2(3) . . ? C40 O25 Mn8 114.4(6) . . ? C40 O25 Mn6 132.8(6) . 2_566 ? Mn8 O25 Mn6 105.8(4) . 2_566 ? C43 O26 H26 109.5 . . ? C45 O27 Mn8 117.2(7) . . ? C45 O27 Mn7 131.5(6) . . ? Mn8 O27 Mn7 102.9(3) . . ? C45 O27 K2 91.7(6) . . ? Mn8 O27 K2 104.4(3) . . ? Mn7 O27 K2 104.2(3) . . ? C59 O28 Mn5 111.5(6) . . ? C59 O28 Mn6 132.9(7) . . ? Mn5 O28 Mn6 107.9(4) . . ? C58 O29 Mn5 129.8(6) . . ? C52 O30 Mn5 132.1(7) . . ? C52 O30 K2 107.7(6) . . ? Mn5 O30 K2 120.2(4) . . ? C52 O31 K2 167.2(8) . 2_666 ? C52 O31 K2 88.3(7) . . ? K2 O31 K2 103.9(3) 2_666 . ? C62 O32 H32 109.5 . . ? C10 N1 C12 113.8(9) . . ? C10 N1 C8 114.5(9) . . ? C12 N1 C8 111.7(9) . . ? C10 N1 Mn1 99.3(7) . . ? C12 N1 Mn1 112.4(7) . . ? C8 N1 Mn1 104.0(7) . . ? N3 N2 Mn2 125.5(7) . . ? N3 N2 Mn2 122.9(7) . 2_755 ? Mn2 N2 Mn2 104.6(4) . 2_755 ? N3 N2 Mn3 108.9(6) . . ? Mn2 N2 Mn3 92.6(3) . . ? Mn2 N2 Mn3 92.7(3) 2_755 . ? N4 N3 N2 177.6(11) . . ? C14 N5 C16 114.2(10) . . ? C14 N5 C18 112.9(9) . . ? C16 N5 C18 111.9(9) . . ? C14 N5 Mn4 101.2(7) . . ? C16 N5 Mn4 104.4(6) . . ? C18 N5 Mn4 111.2(7) . . ? C29 N6 C28 111.9(8) . . ? C29 N6 C31 112.2(8) . . ? C28 N6 C31 110.9(7) . . ? C29 N6 Mn3 105.7(6) . . ? C28 N6 Mn3 105.7(6) . . ? C31 N6 Mn3 110.2(6) . . ? C42 N7 C44 112.0(9) . . ? C42 N7 C41 112.8(10) . . ? C44 N7 C41 114.6(9) . . ? C42 N7 Mn8 114.8(8) . . ? C44 N7 Mn8 98.8(8) . . ? C41 N7 Mn8 102.8(7) . . ? C48 N8 C50 111.9(8) . . ? C48 N8 C47 111.2(8) . . ? C50 N8 C47 110.9(8) . . ? C48 N8 Mn6 110.0(6) . . ? C50 N8 Mn6 106.5(6) . . ? C47 N8 Mn6 106.2(6) . . ? C63 N9 C60 115.5(11) . . ? C63 N9 C61 111.4(9) . . ? C60 N9 C61 114.5(10) . . ? C63 N9 Mn5 100.5(7) . . ? C60 N9 Mn5 101.7(7) . . ? C61 N9 Mn5 111.7(8) . . ? N11 N10 Mn7 127.2(7) . . ? N11 N10 Mn7 120.4(8) . 2_566 ? Mn7 N10 Mn7 105.5(4) . 2_566 ? N11 N10 Mn6 108.9(7) . . ? Mn7 N10 Mn6 92.8(4) . . ? Mn7 N10 Mn6 92.4(3) 2_566 . ? N12 N11 N10 178.4(11) . . ? O1 C1 C6 126.0(10) . . ? O1 C1 C2 115.9(10) . . ? C6 C1 C2 118.0(10) . . ? C1 C2 C3 120.2(12) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 119.1(11) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C5 C4 C3 120.6(11) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.9(12) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 121.0(11) . . ? C1 C6 C7 122.8(9) . . ? C5 C6 C7 116.1(10) . . ? O3 C7 O2 121.4(11) . . ? O3 C7 C6 120.9(11) . . ? O2 C7 C6 117.8(10) . . ? O3 C7 K1 75.1(7) . . ? O2 C7 K1 47.1(5) . . ? C6 C7 K1 160.9(8) . . ? N1 C8 C9 108.6(9) . . ? N1 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? N1 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? O4 C9 C8 110.5(9) . . ? O4 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? O4 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N1 C10 C11 111.7(9) . . ? N1 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N1 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? O5 C11 C10 108.5(9) . . ? O5 C11 K1 61.3(6) . . ? C10 C11 K1 88.3(7) . . ? O5 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? K1 C11 H11A 63.9 . . ? O5 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? K1 C11 H11B 161.7 . . ? H11A C11 H11B 108.4 . . ? N1 C12 C13 117.7(10) . . ? N1 C12 H12A 107.9 . . ? C13 C12 H12A 107.9 . . ? N1 C12 H12B 107.9 . . ? C13 C12 H12B 107.9 . . ? H12A C12 H12B 107.2 . . ? O6 C13 C12 109.2(9) . . ? O6 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? O6 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N5 C14 C15 109.4(10) . . ? N5 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N5 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? O8 C15 C14 110.5(10) . . ? O8 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? O8 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N5 C16 C17 109.8(10) . . ? N5 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? N5 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? O11 C17 C16 108.4(10) . . ? O11 C17 H17A 110.0 . . ? C16 C17 H17A 110.0 . . ? O11 C17 H17B 110.0 . . ? C16 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? N5 C18 C19 116.2(9) . . ? N5 C18 H18A 108.2 . . ? C19 C18 H18A 108.2 . . ? N5 C18 H18B 108.2 . . ? C19 C18 H18B 108.2 . . ? H18A C18 H18B 107.4 . . ? O15 C19 C18 110.7(10) . . ? O15 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? O15 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? O13 C20 C21 115.5(9) . . ? O13 C20 C25 124.1(9) . . ? C21 C20 C25 120.5(10) . . ? C22 C21 C20 119.8(10) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 122.5(10) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C24 C23 C22 116.1(11) . . ? C24 C23 H23 122.0 . . ? C22 C23 H23 122.0 . . ? C25 C24 C23 123.5(11) . . ? C25 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? C24 C25 C20 117.5(10) . . ? C24 C25 C26 118.6(10) . . ? C20 C25 C26 123.8(9) . . ? O14 C26 O12 119.5(9) . . ? O14 C26 C25 121.8(9) . . ? O12 C26 C25 118.7(9) . . ? O14 C26 K1 70.5(6) . . ? O12 C26 K1 49.4(4) . . ? C25 C26 K1 165.5(8) . . ? O7 C27 C28 111.4(8) . . ? O7 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? O7 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? N6 C28 C27 110.1(8) . . ? N6 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? N6 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.2 . . ? N6 C29 C30 111.6(8) . . ? N6 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N6 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? O9 C30 C29 110.4(8) . . ? O9 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? O9 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? N6 C31 C32 110.3(8) . . ? N6 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? N6 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? O10 C32 C31 109.5(8) . . ? O10 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? O10 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? O17 C33 O18 121.1(11) . . ? O17 C33 C34 119.9(10) . . ? O18 C33 C34 119.0(10) . . ? C35 C34 C39 120.6(10) . . ? C35 C34 C33 116.7(10) . . ? C39 C34 C33 122.7(9) . . ? C36 C35 C34 121.1(11) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 118.9(10) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C38 C37 C36 121.0(10) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 120.5(10) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? O21 C39 C34 124.9(9) . . ? O21 C39 C38 117.4(9) . . ? C34 C39 C38 117.6(10) . . ? O25 C40 C41 108.9(9) . . ? O25 C40 H40A 109.9 . . ? C41 C40 H40A 109.9 . . ? O25 C40 H40B 109.9 . . ? C41 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? N7 C41 C40 110.4(10) . . ? N7 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? N7 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? N7 C42 C43 119.0(11) . . ? N7 C42 H42A 107.6 . . ? C43 C42 H42A 107.6 . . ? N7 C42 H42B 107.6 . . ? C43 C42 H42B 107.6 . . ? H42A C42 H42B 107.0 . . ? O26 C43 C42 111.2(10) . . ? O26 C43 H43A 109.4 . . ? C42 C43 H43A 109.4 . . ? O26 C43 H43B 109.4 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? N7 C44 C45 111.9(10) . . ? N7 C44 H44A 109.2 . . ? C45 C44 H44A 109.2 . . ? N7 C44 H44B 109.2 . . ? C45 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? O27 C45 C44 109.6(10) . . ? O27 C45 H45A 109.8 . . ? C44 C45 H45A 109.8 . . ? O27 C45 H45B 109.8 . . ? C44 C45 H45B 109.8 . . ? H45A C45 H45B 108.2 . . ? O22 C46 C47 110.5(8) . . ? O22 C46 H46A 109.6 . . ? C47 C46 H46A 109.6 . . ? O22 C46 H46B 109.6 . . ? C47 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? N8 C47 C46 110.8(9) . . ? N8 C47 H47A 109.5 . . ? C46 C47 H47A 109.5 . . ? N8 C47 H47B 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 108.1 . . ? N8 C48 C49 110.7(9) . . ? N8 C48 H48A 109.5 . . ? C49 C48 H48A 109.5 . . ? N8 C48 H48B 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 108.1 . . ? O23 C49 C48 110.2(8) . . ? O23 C49 H49A 109.6 . . ? C48 C49 H49A 109.6 . . ? O23 C49 H49B 109.6 . . ? C48 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? N8 C50 C51 111.0(8) . . ? N8 C50 H50A 109.4 . . ? C51 C50 H50A 109.4 . . ? N8 C50 H50B 109.4 . . ? C51 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? O24 C51 C50 111.5(8) . . ? O24 C51 H51A 109.3 . . ? C50 C51 H51A 109.3 . . ? O24 C51 H51B 109.3 . . ? C50 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? O31 C52 O30 119.3(10) . . ? O31 C52 C53 120.8(11) . . ? O30 C52 C53 120.0(10) . . ? O31 C52 K2 69.8(7) . . ? O30 C52 K2 50.2(5) . . ? C53 C52 K2 167.4(8) . . ? C54 C53 C58 118.4(10) . . ? C54 C53 C52 119.5(10) . . ? C58 C53 C52 122.0(10) . . ? C53 C54 C55 122.7(12) . . ? C53 C54 H54 118.7 . . ? C55 C54 H54 118.7 . . ? C56 C55 C54 118.2(12) . . ? C56 C55 H55 120.9 . . ? C54 C55 H55 120.9 . . ? C55 C56 C57 120.6(10) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C56 C57 C58 121.6(10) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? O29 C58 C57 117.2(9) . . ? O29 C58 C53 124.6(9) . . ? C57 C58 C53 118.2(10) . . ? O28 C59 C60 108.8(10) . . ? O28 C59 H59A 109.9 . . ? C60 C59 H59A 109.9 . . ? O28 C59 H59B 109.9 . . ? C60 C59 H59B 109.9 . . ? H59A C59 H59B 108.3 . . ? N9 C60 C59 113.9(10) . . ? N9 C60 H60A 108.8 . . ? C59 C60 H60A 108.8 . . ? N9 C60 H60B 108.8 . . ? C59 C60 H60B 108.8 . . ? H60A C60 H60B 107.7 . . ? N9 C61 C62 114.0(11) . . ? N9 C61 H61A 108.8 . . ? C62 C61 H61A 108.8 . . ? N9 C61 H61B 108.8 . . ? C62 C61 H61B 108.8 . . ? H61A C61 H61B 107.6 . . ? O32 C62 C61 107.7(15) . . ? O32 C62 H62A 110.2 . . ? C61 C62 H62A 110.2 . . ? O32 C62 H62B 110.2 . . ? C61 C62 H62B 110.2 . . ? H62A C62 H62B 108.5 . . ? N9 C63 C64 109.8(10) . . ? N9 C63 H63A 109.7 . . ? C64 C63 H63A 109.7 . . ? N9 C63 H63B 109.7 . . ? C64 C63 H63B 109.7 . . ? H63A C63 H63B 108.2 . . ? O20 C64 C63 110.8(12) . . ? O20 C64 H64A 109.5 . . ? C63 C64 H64A 109.5 . . ? O20 C64 H64B 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? C12S O1S H1S 109.5 . . ? C13S O2S H2S 109.6 . . ? C14S O3S H3S 109.5 . . ? C4S O6S H6S 109.5 . . ? C1S O7S H7S 111.4 . . ? C18S O9S H9S 110.6 . . ? C17S O16S H16S 99.9 . . ? C19S O20S H20S 110.3 . . ? O6S C4S H4S1 109.5 . . ? O6S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? O6S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? O8S C7S H7S1 115.3 . . ? O8S C7S H7S2 106.4 . . ? H7S1 C7S H7S2 111.2 . . ? O8S C7S H7S3 107.4 . . ? H7S1 C7S H7S3 111.2 . . ? H7S2 C7S H7S3 104.8 . . ? O1S C12S H12C 109.5 . . ? O1S C12S H12D 109.5 . . ? H12C C12S H12D 109.5 . . ? O1S C12S H12E 109.5 . . ? H12C C12S H12E 109.5 . . ? H12D C12S H12E 109.5 . . ? O2S C13S H13C 109.5 . . ? O2S C13S H13D 109.5 . . ? H13C C13S H13D 109.5 . . ? O2S C13S H13E 109.5 . . ? H13C C13S H13E 109.5 . . ? H13D C13S H13E 109.5 . . ? O3S C14S H14C 109.5 . . ? O3S C14S H14D 109.5 . . ? H14C C14S H14D 109.5 . . ? O3S C14S H14E 109.5 . . ? H14C C14S H14E 109.5 . . ? H14D C14S H14E 109.5 . . ? O16S C17S H17C 102.2 . . ? O16S C17S H17D 119.9 . . ? H17C C17S H17D 104.6 . . ? O16S C17S H17E 112.5 . . ? H17C C17S H17E 96.1 . . ? H17D C17S H17E 116.8 . . ? O16S C17S H18E 118.3 . . ? H17C C17S H18E 50.8 . . ? H17D C17S H18E 120.4 . . ? H17E C17S H18E 45.3 . . ? O9S C18S H17C 142.1 . . ? O9S C18S H17E 90.4 . . ? H17C C18S H17E 71.6 . . ? O9S C18S H18C 106.6 . . ? H17C C18S H18C 107.8 . . ? H17E C18S H18C 142.3 . . ? O9S C18S H18D 106.0 . . ? H17C C18S H18D 55.0 . . ? H17E C18S H18D 111.7 . . ? H18C C18S H18D 95.9 . . ? O9S C18S H18E 122.9 . . ? H17C C18S H18E 55.8 . . ? H17E C18S H18E 35.5 . . ? H18C C18S H18E 111.7 . . ? H18D C18S H18E 110.3 . . ? O20S C19S H19C 109.5 . . ? O20S C19S H19D 109.5 . . ? H19C C19S H19D 109.5 . . ? O20S C19S H19E 109.5 . . ? H19C C19S H19E 109.5 . . ? H19D C19S H19E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.818 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.165 # Attachment '- 2_Na2Mn8_final+sq.CIF' #========================================================================== data_745sq _database_code_depnum_ccdc_archive 'CCDC 834649' #TrackingRef '- 2_Na2Mn8_final+sq.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains half the cluster as well as solvent MeOH molecules. The free alcohol arm of two of the teaH2- ligands, contains a oxygen atom that is disordered over three positions set at 0.42, 0.3 and 0.28 occupancy. After preliminary modelleing of the lattice MeOH, as one fully occupied and four partial occupancy, the latter with restrained bond (DFIX) and thermal (ISOR) parameters, the four partial MeOH molecules were removed and the associated electron density was accounted for using PLATON/SQUEEZE. All hydrogen atoms were placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H134 Mn8 N12 Na2 O40' _chemical_formula_weight 2317.43 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.813(4) _cell_length_b 12.949(3) _cell_length_c 23.397(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.75(3) _cell_angle_gamma 90.00 _cell_volume 5302.0(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9285 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71123 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34270 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9284 _reflns_number_gt 8108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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 structure was solved by direct methods. The asymmetric unit contains half the cluster as well as solvent MeOH molecules. The free alcohol arm of two of the teaH2- ligands, contains a oxygen atom that is disordered over three positions set at 0.42, 0.3 and 0.28 occupancy. After preliminary modelleing of the lattice MeOH, as one fully occupied and four partial occupancy, the latter with restrained bond (DFIX) and thermal (ISOR) parameters, the four partial MeOH molecules were removed and the associated electron density was accounted for using PLATON/SQUEEZE. All hydrogen atoms were placed in calculated positions. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 548.0 58 2 0.500 -0.496 0.500 548.0 58 _platon_squeeze_details ; PLATON/SQUEEZE Spek, A.L. (1990), Acta Cryst. A46, C-34 ; _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^)+(0.0658P)^2^+17.9586P] 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 9284 _refine_ls_number_parameters 614 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.093 _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 0.53538(3) 0.28634(5) 0.14385(3) 0.02856(18) Uani 1 1 d . . . Mn2 Mn 0.55973(3) 0.39188(4) 0.02488(3) 0.02536(17) Uani 1 1 d . . . Mn3 Mn 0.56212(3) 0.50149(4) -0.10773(3) 0.02727(18) Uani 1 1 d . . . Mn4 Mn 0.69341(3) 0.33819(5) -0.04665(3) 0.03014(18) Uani 1 1 d . . . Na1 Na 0.66908(10) 0.18102(12) 0.06788(8) 0.0352(4) Uani 1 1 d . . . O1 O 0.53500(17) 0.3202(2) 0.22142(14) 0.0355(8) Uani 1 1 d . . . O2 O 0.64174(16) 0.2387(2) 0.16504(14) 0.0341(7) Uani 1 1 d . . . O3 O 0.75823(17) 0.2290(2) 0.21761(15) 0.0399(8) Uani 1 1 d . . . O4 O 0.43208(16) 0.3362(2) 0.12453(13) 0.0283(7) Uani 1 1 d . . . O5 O 0.53986(16) 0.2425(2) 0.06552(14) 0.0303(7) Uani 1 1 d . . . O6 O 0.5042(2) -0.0870(3) 0.2505(2) 0.0617(12) Uani 1 1 d . . . H6 H 0.5501 -0.0971 0.2481 0.074 Uiso 1 1 calc R . . O7 O 0.56874(15) 0.3486(2) -0.06238(13) 0.0282(7) Uani 1 1 d . . . O8 O 0.68187(16) 0.3557(2) 0.03438(14) 0.0306(7) Uani 1 1 d . . . O9 O 0.44082(15) 0.5618(2) -0.11288(13) 0.0283(7) Uani 1 1 d . . . O10 O 0.62192(18) 0.4722(2) -0.18543(16) 0.0379(8) Uani 1 1 d D . . O11 O 0.68507(16) 0.4804(2) -0.06460(15) 0.0334(7) Uani 1 1 d . . . O12 O 0.70061(16) 0.1917(2) -0.03133(15) 0.0339(7) Uani 1 1 d . . . O13 O 0.70436(19) 0.3150(2) -0.12519(16) 0.0394(8) Uani 1 1 d . . . O14 O 0.7122(3) 0.0247(3) -0.04470(18) 0.0555(10) Uani 1 1 d . . . O15 O 0.9948(9) 0.4214(11) 0.0256(9) 0.104(8) Uani 0.28 1 d PD A 2 H15 H 0.9826 0.4330 0.0580 0.125 Uiso 0.28 1 calc PR A 2 O16 O 0.6388(2) 0.0070(2) 0.04520(17) 0.0421(9) Uani 1 1 d . . . O17 O 0.7873(2) 0.1400(3) 0.11968(18) 0.0502(10) Uani 1 1 d . . . N1 N 0.4675(2) 0.1332(3) 0.14390(18) 0.0341(9) Uani 1 1 d . . . N2 N 0.56374(19) 0.5587(2) -0.00695(16) 0.0279(8) Uani 1 1 d . . . N3 N 0.6184(2) 0.6147(3) 0.00714(17) 0.0308(9) Uani 1 1 d . . . N4 N 0.6708(2) 0.6673(3) 0.0198(2) 0.0412(10) Uani 1 1 d . . . N5 N 0.8168(2) 0.3885(3) -0.0070(2) 0.0415(10) Uani 1 1 d . . . N6 N 0.4796(2) 0.3881(3) -0.17233(16) 0.0295(8) Uani 1 1 d . . . C1 C 0.5826(3) 0.2913(4) 0.2690(2) 0.0383(12) Uani 1 1 d . . . C2 C 0.5592(3) 0.3002(5) 0.3223(3) 0.0560(16) Uani 1 1 d . . . H2 H 0.5095 0.3260 0.3233 0.067 Uiso 1 1 calc R . . C3 C 0.6060(4) 0.2726(7) 0.3736(3) 0.077(2) Uani 1 1 d . . . H3 H 0.5880 0.2780 0.4092 0.093 Uiso 1 1 calc R . . C4 C 0.6796(3) 0.2368(6) 0.3735(3) 0.068(2) Uani 1 1 d . . . H4 H 0.7120 0.2184 0.4090 0.082 Uiso 1 1 calc R . . C5 C 0.7049(3) 0.2282(4) 0.3223(2) 0.0483(14) Uani 1 1 d . . . H5 H 0.7553 0.2041 0.3226 0.058 Uiso 1 1 calc R . . C6 C 0.6579(3) 0.2542(3) 0.2689(2) 0.0367(12) Uani 1 1 d . . . C7 C 0.6877(3) 0.2413(3) 0.2156(2) 0.0354(11) Uani 1 1 d . . . C8 C 0.3861(3) 0.1664(3) 0.1380(2) 0.0376(11) Uani 1 1 d . . . H8A H 0.3605 0.1246 0.1642 0.045 Uiso 1 1 calc R . . H8B H 0.3590 0.1550 0.0976 0.045 Uiso 1 1 calc R . . C9 C 0.3826(2) 0.2795(3) 0.1534(2) 0.0340(10) Uani 1 1 d . . . H9A H 0.3296 0.3052 0.1416 0.041 Uiso 1 1 calc R . . H9B H 0.3981 0.2886 0.1960 0.041 Uiso 1 1 calc R . . C10 C 0.4847(3) 0.0824(3) 0.0911(2) 0.0366(11) Uani 1 1 d . . . H10A H 0.4454 0.0295 0.0772 0.044 Uiso 1 1 calc R . . H10B H 0.5350 0.0474 0.1006 0.044 Uiso 1 1 calc R . . C11 C 0.4861(3) 0.1619(3) 0.0436(2) 0.0335(11) Uani 1 1 d . . . H11A H 0.5014 0.1286 0.0094 0.040 Uiso 1 1 calc R . . H11B H 0.4345 0.1919 0.0311 0.040 Uiso 1 1 calc R . . C12 C 0.4951(3) 0.0747(3) 0.1978(2) 0.0398(12) Uani 1 1 d . . . H12A H 0.4807 0.1131 0.2307 0.048 Uiso 1 1 calc R . . H12B H 0.5517 0.0728 0.2042 0.048 Uiso 1 1 calc R . . C13 C 0.4662(3) -0.0359(4) 0.1995(3) 0.0476(14) Uani 1 1 d . . . H13A H 0.4104 -0.0352 0.1989 0.057 Uiso 1 1 calc R . . H13B H 0.4753 -0.0738 0.1646 0.057 Uiso 1 1 calc R . . C14 C 0.8191(3) 0.3684(4) 0.0554(2) 0.0414(12) Uani 1 1 d . . . H14A H 0.8620 0.4070 0.0788 0.050 Uiso 1 1 calc R . . H14B H 0.8278 0.2938 0.0634 0.050 Uiso 1 1 calc R . . C15 C 0.7452(2) 0.4006(3) 0.0729(2) 0.0361(11) Uani 1 1 d . . . H15A H 0.7449 0.3779 0.1133 0.043 Uiso 1 1 calc R . . H15B H 0.7407 0.4768 0.0716 0.043 Uiso 1 1 calc R . . C16 C 0.8174(3) 0.5010(4) -0.0214(3) 0.0432(13) Uani 1 1 d . . . H16A H 0.8678 0.5203 -0.0303 0.052 Uiso 1 1 calc R . . H16B H 0.8088 0.5424 0.0123 0.052 Uiso 1 1 calc R . . C17 C 0.7551(3) 0.5238(4) -0.0736(3) 0.0435(12) Uani 1 1 d . . . H17A H 0.7494 0.5994 -0.0790 0.052 Uiso 1 1 calc R . . H17B H 0.7692 0.4940 -0.1091 0.052 Uiso 1 1 calc R . . C18 C 0.8736(3) 0.3276(5) -0.0319(3) 0.0551(15) Uani 1 1 d . A . H18A H 0.8715 0.3502 -0.0726 0.066 Uiso 1 1 calc R . . H18B H 0.8582 0.2541 -0.0329 0.066 Uiso 1 1 calc R . . C19 C 0.9549(4) 0.3356(9) 0.0000(4) 0.098(3) Uani 1 1 d D . . H19A H 0.9612 0.4029 0.0203 0.118 Uiso 1 1 calc R A 1 H19B H 0.9635 0.2810 0.0301 0.118 Uiso 1 1 calc R A 1 C20 C 0.7239(3) 0.2272(4) -0.1498(2) 0.0409(12) Uani 1 1 d . . . C21 C 0.7364(4) 0.2337(5) -0.2067(3) 0.0638(17) Uani 1 1 d . . . H21 H 0.7305 0.2982 -0.2264 0.077 Uiso 1 1 calc R . . C22 C 0.7574(5) 0.1472(5) -0.2351(4) 0.077(2) Uani 1 1 d . . . H22 H 0.7674 0.1538 -0.2734 0.092 Uiso 1 1 calc R . . C23 C 0.7637(4) 0.0523(5) -0.2083(3) 0.0628(17) Uani 1 1 d . . . H23 H 0.7764 -0.0072 -0.2283 0.075 Uiso 1 1 calc R . . C24 C 0.7515(3) 0.0450(4) -0.1526(3) 0.0450(13) Uani 1 1 d . . . H24 H 0.7574 -0.0202 -0.1336 0.054 Uiso 1 1 calc R . . C25 C 0.7303(2) 0.1315(3) -0.1221(2) 0.0366(11) Uani 1 1 d . . . C26 C 0.7135(3) 0.1140(3) -0.0636(2) 0.0373(11) Uani 1 1 d . . . C27 C 0.5322(2) 0.2641(3) -0.0954(2) 0.0293(10) Uani 1 1 d . . . H27A H 0.5179 0.2113 -0.0688 0.035 Uiso 1 1 calc R . . H27B H 0.5681 0.2321 -0.1178 0.035 Uiso 1 1 calc R . . C28 C 0.4617(2) 0.3000(3) -0.1367(2) 0.0302(10) Uani 1 1 d . . . H28A H 0.4407 0.2423 -0.1625 0.036 Uiso 1 1 calc R . . H28B H 0.4223 0.3212 -0.1142 0.036 Uiso 1 1 calc R . . C29 C 0.4093(2) 0.4471(3) -0.1956(2) 0.0322(10) Uani 1 1 d . . . H29A H 0.3690 0.3990 -0.2146 0.039 Uiso 1 1 calc R . . H29B H 0.4199 0.4965 -0.2253 0.039 Uiso 1 1 calc R . . C30 C 0.3809(2) 0.5053(3) -0.14798(19) 0.0297(10) Uani 1 1 d . . . H30A H 0.3399 0.5535 -0.1656 0.036 Uiso 1 1 calc R . . H30B H 0.3589 0.4558 -0.1233 0.036 Uiso 1 1 calc R . . C31 C 0.5685(3) 0.4386(4) -0.2361(2) 0.0410(11) Uani 1 1 d . . . H31A H 0.5967 0.4127 -0.2658 0.049 Uiso 1 1 calc R . . H31B H 0.5367 0.4978 -0.2529 0.049 Uiso 1 1 calc R . . C32 C 0.5176(3) 0.3537(3) -0.2198(2) 0.0360(11) Uani 1 1 d . . . H32A H 0.4787 0.3349 -0.2542 0.043 Uiso 1 1 calc R . . H32B H 0.5488 0.2916 -0.2073 0.043 Uiso 1 1 calc R . . C33 C 0.6654(3) -0.0792(4) 0.0810(3) 0.0542(16) Uani 1 1 d . . . H33A H 0.7196 -0.0698 0.0978 0.081 Uiso 1 1 calc R . . H33B H 0.6589 -0.1424 0.0575 0.081 Uiso 1 1 calc R . . H33C H 0.6360 -0.0849 0.1124 0.081 Uiso 1 1 calc R . . C34 C 0.8538(4) 0.0816(5) 0.1186(3) 0.073(2) Uani 1 1 d . . . H34A H 0.8532 0.0565 0.0790 0.109 Uiso 1 1 calc R . . H34B H 0.8554 0.0226 0.1451 0.109 Uiso 1 1 calc R . . H34C H 0.8990 0.1250 0.1310 0.109 Uiso 1 1 calc R . . H10 H 0.649(4) 0.418(4) -0.170(3) 0.088 Uiso 1 1 d D . . H16 H 0.668(5) 0.019(6) 0.020(3) 0.088 Uiso 1 1 d . . . H17 H 0.778(5) 0.162(6) 0.151(3) 0.088 Uiso 1 1 d . . . O15A O 1.0115(6) 0.3271(14) -0.0329(6) 0.102(5) Uani 0.42 1 d PD A 1 H15X H 0.9914 0.3221 -0.0683 0.123 Uiso 0.42 1 calc PR A 1 O15B O 0.9793(9) 0.2851(15) 0.0532(8) 0.122(9) Uani 0.30 1 d PD A 3 H15Y H 1.0265 0.2940 0.0642 0.147 Uiso 0.30 1 calc PR A 3 O1S O 0.6497(2) -0.1133(3) 0.2318(2) 0.0580(13) Uani 1 1 d . . . H1S H 0.668(4) -0.154(6) 0.247(3) 0.070 Uiso 1 1 d . . . C1S C 0.7022(3) -0.0284(4) 0.2372(3) 0.0567(17) Uani 1 1 d . . . H1S1 H 0.6818 0.0256 0.2093 0.085 Uiso 1 1 calc R . . H1S2 H 0.7514 -0.0523 0.2293 0.085 Uiso 1 1 calc R . . H1S3 H 0.7093 -0.0005 0.2768 0.085 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 0.0223(3) 0.0117(3) 0.0426(4) -0.0017(3) -0.0174(3) 0.0008(2) Mn2 0.0178(3) 0.0106(3) 0.0399(4) -0.0049(2) -0.0151(3) 0.0034(2) Mn3 0.0205(3) 0.0108(3) 0.0439(4) -0.0046(3) -0.0112(3) 0.0008(2) Mn4 0.0189(3) 0.0137(3) 0.0523(4) -0.0053(3) -0.0078(3) 0.0035(2) Na1 0.0288(9) 0.0146(8) 0.0530(11) -0.0027(7) -0.0158(8) 0.0068(7) O1 0.0315(16) 0.0196(15) 0.0453(19) 0.0017(13) -0.0189(14) 0.0013(12) O2 0.0258(15) 0.0161(14) 0.0492(19) -0.0014(13) -0.0215(14) 0.0017(12) O3 0.0242(16) 0.0225(16) 0.062(2) -0.0093(15) -0.0216(15) 0.0043(12) O4 0.0231(14) 0.0139(14) 0.0408(17) -0.0004(12) -0.0123(12) 0.0011(11) O5 0.0225(14) 0.0104(13) 0.0492(18) -0.0028(12) -0.0159(13) -0.0001(11) O6 0.059(2) 0.0278(19) 0.085(3) 0.0189(19) -0.020(2) -0.0031(18) O7 0.0191(13) 0.0120(13) 0.0468(18) -0.0086(12) -0.0116(12) 0.0023(11) O8 0.0194(14) 0.0148(14) 0.0490(18) -0.0078(13) -0.0158(13) 0.0007(11) O9 0.0205(14) 0.0116(13) 0.0447(17) -0.0037(12) -0.0152(12) -0.0015(11) O10 0.0324(17) 0.0239(16) 0.053(2) -0.0019(15) -0.0038(15) -0.0023(13) O11 0.0196(14) 0.0144(14) 0.061(2) -0.0036(14) -0.0067(14) 0.0014(11) O12 0.0248(15) 0.0128(14) 0.058(2) -0.0067(13) -0.0085(14) 0.0066(11) O13 0.0391(18) 0.0196(16) 0.058(2) -0.0045(15) 0.0046(16) 0.0063(13) O14 0.078(3) 0.0139(17) 0.073(3) -0.0074(17) 0.010(2) 0.0071(17) O15 0.038(9) 0.113(17) 0.17(2) 0.077(16) 0.043(12) 0.033(10) O16 0.047(2) 0.0149(15) 0.056(2) -0.0005(15) -0.0142(16) 0.0064(14) O17 0.0387(19) 0.037(2) 0.063(2) -0.0093(18) -0.0217(18) 0.0179(16) N1 0.0283(19) 0.0145(17) 0.052(2) 0.0007(16) -0.0129(17) 0.0016(14) N2 0.0196(17) 0.0109(16) 0.045(2) -0.0049(15) -0.0159(15) 0.0029(14) N3 0.0262(19) 0.0106(16) 0.048(2) -0.0069(15) -0.0139(16) 0.0058(15) N4 0.0217(19) 0.0221(19) 0.070(3) -0.0099(19) -0.0162(18) -0.0050(16) N5 0.0187(18) 0.027(2) 0.072(3) -0.004(2) -0.0092(18) 0.0021(15) N6 0.0275(18) 0.0176(17) 0.038(2) -0.0038(15) -0.0082(15) 0.0006(14) C1 0.037(3) 0.024(2) 0.044(3) 0.004(2) -0.016(2) -0.0112(19) C2 0.034(3) 0.074(4) 0.052(3) 0.017(3) -0.015(2) -0.006(3) C3 0.049(4) 0.127(7) 0.049(4) 0.029(4) -0.012(3) -0.013(4) C4 0.042(3) 0.092(5) 0.056(4) 0.034(4) -0.026(3) -0.014(3) C5 0.039(3) 0.037(3) 0.055(3) 0.016(2) -0.025(2) -0.006(2) C6 0.030(2) 0.014(2) 0.054(3) 0.0080(19) -0.022(2) -0.0056(17) C7 0.037(3) 0.0054(18) 0.054(3) -0.0009(18) -0.017(2) -0.0017(17) C8 0.028(2) 0.025(2) 0.052(3) 0.001(2) -0.014(2) -0.0037(18) C9 0.022(2) 0.025(2) 0.049(3) 0.002(2) -0.0066(19) -0.0036(17) C10 0.036(2) 0.0106(19) 0.054(3) -0.0049(19) -0.018(2) -0.0017(17) C11 0.030(2) 0.014(2) 0.047(3) -0.0053(18) -0.016(2) -0.0051(17) C12 0.040(3) 0.014(2) 0.055(3) 0.004(2) -0.019(2) -0.0042(18) C13 0.046(3) 0.017(2) 0.068(4) 0.008(2) -0.019(3) -0.005(2) C14 0.026(2) 0.029(2) 0.059(3) -0.003(2) -0.021(2) 0.0012(19) C15 0.022(2) 0.020(2) 0.056(3) -0.010(2) -0.021(2) -0.0013(17) C16 0.024(2) 0.025(2) 0.075(4) -0.004(2) -0.006(2) -0.0044(18) C17 0.024(2) 0.031(3) 0.070(4) -0.001(2) -0.004(2) -0.0072(19) C18 0.025(3) 0.054(3) 0.084(4) -0.008(3) 0.005(3) 0.009(2) C19 0.030(3) 0.145(9) 0.117(7) -0.022(7) 0.008(4) 0.021(5) C20 0.035(3) 0.026(2) 0.062(3) -0.008(2) 0.008(2) 0.002(2) C21 0.083(5) 0.040(3) 0.077(4) 0.003(3) 0.038(4) 0.011(3) C22 0.102(6) 0.047(4) 0.098(6) -0.007(4) 0.060(5) 0.002(4) C23 0.059(4) 0.040(3) 0.096(5) -0.016(3) 0.032(4) 0.007(3) C24 0.029(2) 0.025(2) 0.082(4) -0.014(2) 0.013(3) 0.0012(19) C25 0.022(2) 0.019(2) 0.066(3) -0.013(2) 0.000(2) 0.0010(17) C26 0.026(2) 0.019(2) 0.062(3) -0.011(2) -0.005(2) 0.0029(17) C27 0.023(2) 0.017(2) 0.042(2) -0.0083(18) -0.0081(18) 0.0020(16) C28 0.028(2) 0.0146(19) 0.042(3) -0.0066(18) -0.0111(19) -0.0035(16) C29 0.028(2) 0.019(2) 0.041(3) -0.0027(18) -0.0169(19) -0.0016(17) C30 0.025(2) 0.0139(19) 0.040(2) -0.0061(17) -0.0215(18) 0.0001(16) C31 0.046(3) 0.025(2) 0.048(3) -0.002(2) 0.000(2) -0.004(2) C32 0.036(2) 0.021(2) 0.046(3) -0.005(2) -0.004(2) -0.0019(19) C33 0.066(4) 0.017(2) 0.064(4) 0.001(2) -0.027(3) 0.003(2) C34 0.052(4) 0.063(4) 0.091(5) -0.014(4) -0.020(3) 0.037(3) O15A 0.049(7) 0.142(14) 0.108(11) -0.025(11) -0.006(7) 0.019(8) O15B 0.033(8) 0.079(13) 0.24(3) -0.014(15) -0.018(12) 0.035(9) O1S 0.046(2) 0.0159(17) 0.093(3) 0.0067(18) -0.036(2) 0.0003(15) C1S 0.049(3) 0.022(2) 0.080(4) 0.002(3) -0.036(3) -0.001(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 O1 1.868(3) . ? Mn1 O4 1.922(3) . ? Mn1 O5 1.935(3) . ? Mn1 O2 1.966(3) . ? Mn1 O9 2.165(3) 3_665 ? Mn1 N1 2.323(4) . ? Mn1 Mn2 3.2023(11) . ? Mn1 Na1 3.503(2) . ? Mn2 O9 2.146(3) 3_665 ? Mn2 O7 2.152(3) . ? Mn2 O8 2.196(3) . ? Mn2 O5 2.213(3) . ? Mn2 N2 2.254(3) 3_665 ? Mn2 N2 2.291(3) . ? Mn2 Mn4 3.2314(12) . ? Mn2 Na1 3.3956(17) . ? Mn3 O4 2.145(3) 3_665 ? Mn3 O7 2.239(3) . ? Mn3 O11 2.250(3) . ? Mn3 O9 2.279(3) . ? Mn3 O10 2.304(4) . ? Mn3 N6 2.403(3) . ? Mn3 N2 2.467(4) . ? Mn4 O11 1.889(3) . ? Mn4 O13 1.908(4) . ? Mn4 O12 1.931(3) . ? Mn4 O8 1.958(3) . ? Mn4 O7 2.187(3) . ? Mn4 N5 2.314(4) . ? Mn4 Na1 3.456(2) . ? Na1 O17 2.287(4) . ? Na1 O16 2.354(4) . ? Na1 O8 2.418(3) . ? Na1 O5 2.426(3) . ? Na1 O12 2.492(4) . ? Na1 O2 2.525(4) . ? Na1 H16 2.38(8) . ? Na1 H17 2.49(8) . ? O1 C1 1.321(5) . ? O2 C7 1.307(5) . ? O3 C7 1.259(6) . ? O4 C9 1.412(5) . ? O4 Mn3 2.145(3) 3_665 ? O5 C11 1.444(5) . ? O6 C13 1.421(6) . ? O6 H6 0.8400 . ? O7 C27 1.425(5) . ? O8 C15 1.430(5) . ? O9 C30 1.422(4) . ? O9 Mn2 2.146(3) 3_665 ? O9 Mn1 2.165(3) 3_665 ? O10 C31 1.441(6) . ? O10 H10 0.888(10) . ? O11 C17 1.420(6) . ? O12 C26 1.304(5) . ? O13 C20 1.349(6) . ? O14 C26 1.240(6) . ? O15 C19 1.394(10) . ? O15 H15 0.8400 . ? O16 C33 1.424(6) . ? O16 H16 0.86(8) . ? O17 C34 1.410(6) . ? O17 H17 0.84(8) . ? N1 C12 1.474(6) . ? N1 C10 1.482(6) . ? N1 C8 1.493(6) . ? N2 N3 1.209(5) . ? N2 Mn2 2.254(3) 3_665 ? N3 N4 1.150(5) . ? N5 C14 1.476(7) . ? N5 C18 1.485(7) . ? N5 C16 1.496(6) . ? N6 C32 1.474(6) . ? N6 C29 1.481(5) . ? N6 C28 1.483(6) . ? C1 C2 1.393(8) . ? C1 C6 1.424(7) . ? C2 C3 1.374(8) . ? C2 H2 0.9500 . ? C3 C4 1.391(10) . ? C3 H3 0.9500 . ? C4 C5 1.361(9) . ? C4 H4 0.9500 . ? C5 C6 1.409(6) . ? C5 H5 0.9500 . ? C6 C7 1.454(8) . ? C8 C9 1.513(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.520(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.525(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.509(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.517(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.505(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O15A 1.382(9) . ? C19 O15B 1.403(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.393(7) . ? C20 C21 1.393(8) . ? C21 C22 1.387(9) . ? C21 H21 0.9500 . ? C22 C23 1.374(10) . ? C22 H22 0.9500 . ? C23 C24 1.365(9) . ? C23 H23 0.9500 . ? C24 C25 1.416(6) . ? C24 H24 0.9500 . ? C25 C26 1.473(8) . ? C27 C28 1.508(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.507(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.518(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O15A H15X 0.8400 . ? O15B H15Y 0.8400 . ? O1S C1S 1.433(6) . ? O1S H1S 0.68(7) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 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 O4 88.44(13) . . ? O1 Mn1 O5 175.91(12) . . ? O4 Mn1 O5 94.74(13) . . ? O1 Mn1 O2 90.39(14) . . ? O4 Mn1 O2 178.41(13) . . ? O5 Mn1 O2 86.48(13) . . ? O1 Mn1 O9 98.52(13) . 3_665 ? O4 Mn1 O9 81.67(11) . 3_665 ? O5 Mn1 O9 84.51(12) . 3_665 ? O2 Mn1 O9 97.44(12) . 3_665 ? O1 Mn1 N1 95.96(14) . . ? O4 Mn1 N1 79.10(12) . . ? O5 Mn1 N1 82.15(14) . . ? O2 Mn1 N1 102.10(12) . . ? O9 Mn1 N1 155.52(12) 3_665 . ? O1 Mn1 Mn2 140.33(10) . . ? O4 Mn1 Mn2 86.07(10) . . ? O5 Mn1 Mn2 42.74(8) . . ? O2 Mn1 Mn2 94.16(11) . . ? O9 Mn1 Mn2 41.81(8) 3_665 . ? N1 Mn1 Mn2 121.32(11) . . ? O1 Mn1 Na1 135.26(10) . . ? O4 Mn1 Na1 136.29(10) . . ? O5 Mn1 Na1 41.65(9) . . ? O2 Mn1 Na1 44.88(10) . . ? O9 Mn1 Na1 89.41(9) 3_665 . ? N1 Mn1 Na1 94.09(11) . . ? Mn2 Mn1 Na1 60.65(4) . . ? O9 Mn2 O7 175.90(11) 3_665 . ? O9 Mn2 O8 98.30(11) 3_665 . ? O7 Mn2 O8 78.03(11) . . ? O9 Mn2 O5 78.62(11) 3_665 . ? O7 Mn2 O5 103.08(11) . . ? O8 Mn2 O5 90.27(11) . . ? O9 Mn2 N2 85.42(12) 3_665 3_665 ? O7 Mn2 N2 98.06(12) . 3_665 ? O8 Mn2 N2 173.50(13) . 3_665 ? O5 Mn2 N2 95.70(12) . 3_665 ? O9 Mn2 N2 93.10(12) 3_665 . ? O7 Mn2 N2 85.68(12) . . ? O8 Mn2 N2 98.27(12) . . ? O5 Mn2 N2 168.92(13) . . ? N2 Mn2 N2 76.13(14) 3_665 . ? O9 Mn2 Mn1 42.27(8) 3_665 . ? O7 Mn2 Mn1 139.45(8) . . ? O8 Mn2 Mn1 96.50(9) . . ? O5 Mn2 Mn1 36.39(8) . . ? N2 Mn2 Mn1 89.84(11) 3_665 . ? N2 Mn2 Mn1 134.64(10) . . ? O9 Mn2 Mn4 133.84(8) 3_665 . ? O7 Mn2 Mn4 42.27(7) . . ? O8 Mn2 Mn4 36.35(9) . . ? O5 Mn2 Mn4 103.11(9) . . ? N2 Mn2 Mn4 138.82(10) 3_665 . ? N2 Mn2 Mn4 87.93(10) . . ? Mn1 Mn2 Mn4 126.21(3) . . ? O9 Mn2 Na1 92.62(8) 3_665 . ? O7 Mn2 Na1 86.08(8) . . ? O8 Mn2 Na1 45.22(8) . . ? O5 Mn2 Na1 45.47(8) . . ? N2 Mn2 Na1 140.30(10) 3_665 . ? N2 Mn2 Na1 143.49(9) . . ? Mn1 Mn2 Na1 64.06(4) . . ? Mn4 Mn2 Na1 62.81(4) . . ? O4 Mn3 O7 162.46(11) 3_665 . ? O4 Mn3 O11 97.18(10) 3_665 . ? O7 Mn3 O11 73.70(10) . . ? O4 Mn3 O9 74.48(10) 3_665 . ? O7 Mn3 O9 107.06(11) . . ? O11 Mn3 O9 154.00(12) . . ? O4 Mn3 O10 88.38(12) 3_665 . ? O7 Mn3 O10 103.72(11) . . ? O11 Mn3 O10 77.25(12) . . ? O9 Mn3 O10 126.03(12) . . ? O4 Mn3 N6 121.91(11) 3_665 . ? O7 Mn3 N6 74.31(11) . . ? O11 Mn3 N6 129.65(12) . . ? O9 Mn3 N6 73.33(11) . . ? O10 Mn3 N6 73.84(12) . . ? O4 Mn3 N2 83.59(12) 3_665 . ? O7 Mn3 N2 79.77(11) . . ? O11 Mn3 N2 76.76(12) . . ? O9 Mn3 N2 77.85(11) . . ? O10 Mn3 N2 151.55(11) . . ? N6 Mn3 N2 132.96(13) . . ? O11 Mn4 O13 87.54(14) . . ? O11 Mn4 O12 177.86(15) . . ? O13 Mn4 O12 90.52(14) . . ? O11 Mn4 O8 94.84(14) . . ? O13 Mn4 O8 177.59(13) . . ? O12 Mn4 O8 87.10(13) . . ? O11 Mn4 O7 82.35(11) . . ? O13 Mn4 O7 97.51(13) . . ? O12 Mn4 O7 97.02(11) . . ? O8 Mn4 O7 82.47(12) . . ? O11 Mn4 N5 81.01(13) . . ? O13 Mn4 N5 99.81(16) . . ? O12 Mn4 N5 100.22(13) . . ? O8 Mn4 N5 80.94(15) . . ? O7 Mn4 N5 155.35(13) . . ? O11 Mn4 Mn2 82.55(10) . . ? O13 Mn4 Mn2 138.63(10) . . ? O12 Mn4 Mn2 98.35(10) . . ? O8 Mn4 Mn2 41.66(8) . . ? O7 Mn4 Mn2 41.44(8) . . ? N5 Mn4 Mn2 117.92(12) . . ? O11 Mn4 Na1 136.94(11) . . ? O13 Mn4 Na1 134.79(10) . . ? O12 Mn4 Na1 44.84(11) . . ? O8 Mn4 Na1 42.81(9) . . ? O7 Mn4 Na1 84.06(9) . . ? N5 Mn4 Na1 95.87(12) . . ? Mn2 Mn4 Na1 60.92(4) . . ? O17 Na1 O16 92.68(14) . . ? O17 Na1 O8 104.82(14) . . ? O16 Na1 O8 148.60(14) . . ? O17 Na1 O5 149.74(16) . . ? O16 Na1 O5 97.60(13) . . ? O8 Na1 O5 80.34(11) . . ? O17 Na1 O12 99.28(15) . . ? O16 Na1 O12 85.69(13) . . ? O8 Na1 O12 66.12(11) . . ? O5 Na1 O12 109.78(12) . . ? O17 Na1 O2 84.53(14) . . ? O16 Na1 O2 114.30(15) . . ? O8 Na1 O2 93.48(11) . . ? O5 Na1 O2 65.29(11) . . ? O12 Na1 O2 159.58(12) . . ? O17 Na1 Mn2 139.83(11) . . ? O16 Na1 Mn2 127.45(10) . . ? O8 Na1 Mn2 40.13(7) . . ? O5 Na1 Mn2 40.55(7) . . ? O12 Na1 Mn2 84.04(8) . . ? O2 Na1 Mn2 80.35(8) . . ? O17 Na1 Mn4 108.14(14) . . ? O16 Na1 Mn4 116.45(12) . . ? O8 Na1 Mn4 33.38(8) . . ? O5 Na1 Mn4 92.57(9) . . ? O12 Na1 Mn4 33.12(7) . . ? O2 Na1 Mn4 126.65(9) . . ? Mn2 Na1 Mn4 56.27(3) . . ? O17 Na1 Mn1 117.85(13) . . ? O16 Na1 Mn1 109.76(12) . . ? O8 Na1 Mn1 85.09(9) . . ? O5 Na1 Mn1 32.00(8) . . ? O12 Na1 Mn1 138.07(9) . . ? O2 Na1 Mn1 33.32(7) . . ? Mn2 Na1 Mn1 55.29(3) . . ? Mn4 Na1 Mn1 111.08(5) . . ? O17 Na1 H16 88(2) . . ? O16 Na1 H16 20.9(18) . . ? O8 Na1 H16 132.0(19) . . ? O5 Na1 H16 110.6(19) . . ? O12 Na1 H16 66.2(19) . . ? O2 Na1 H16 134.2(19) . . ? Mn2 Na1 H16 128.1(19) . . ? Mn4 Na1 H16 98.6(19) . . ? Mn1 Na1 H16 129.3(19) . . ? O17 Na1 H17 19.6(17) . . ? O16 Na1 H17 101.2(19) . . ? O8 Na1 H17 103.8(19) . . ? O5 Na1 H17 130.2(18) . . ? O12 Na1 H17 117.3(18) . . ? O2 Na1 H17 64.9(18) . . ? Mn2 Na1 H17 129.1(19) . . ? Mn4 Na1 H17 118.3(18) . . ? Mn1 Na1 H17 98.2(18) . . ? H16 Na1 H17 103(3) . . ? C1 O1 Mn1 129.3(3) . . ? C7 O2 Mn1 129.1(3) . . ? C7 O2 Na1 129.0(3) . . ? Mn1 O2 Na1 101.80(13) . . ? C9 O4 Mn1 111.6(2) . . ? C9 O4 Mn3 130.7(3) . 3_665 ? Mn1 O4 Mn3 107.17(13) . 3_665 ? C11 O5 Mn1 114.0(3) . . ? C11 O5 Mn2 128.8(3) . . ? Mn1 O5 Mn2 100.87(12) . . ? C11 O5 Na1 109.5(2) . . ? Mn1 O5 Na1 106.35(13) . . ? Mn2 O5 Na1 93.98(12) . . ? C13 O6 H6 109.5 . . ? C27 O7 Mn2 127.4(3) . . ? C27 O7 Mn4 113.0(2) . . ? Mn2 O7 Mn4 96.29(11) . . ? C27 O7 Mn3 116.3(2) . . ? Mn2 O7 Mn3 102.29(11) . . ? Mn4 O7 Mn3 95.54(12) . . ? C15 O8 Mn4 116.4(3) . . ? C15 O8 Mn2 128.8(3) . . ? Mn4 O8 Mn2 101.99(12) . . ? C15 O8 Na1 106.7(2) . . ? Mn4 O8 Na1 103.82(13) . . ? Mn2 O8 Na1 94.65(12) . . ? C30 O9 Mn2 124.1(3) . 3_665 ? C30 O9 Mn1 116.5(2) . 3_665 ? Mn2 O9 Mn1 95.92(11) 3_665 3_665 ? C30 O9 Mn3 117.2(2) . . ? Mn2 O9 Mn3 102.65(11) 3_665 . ? Mn1 O9 Mn3 94.92(11) 3_665 . ? C31 O10 Mn3 111.5(3) . . ? C31 O10 H10 108(5) . . ? Mn3 O10 H10 96(5) . . ? C17 O11 Mn4 112.6(3) . . ? C17 O11 Mn3 134.0(3) . . ? Mn4 O11 Mn3 104.34(13) . . ? C26 O12 Mn4 131.6(3) . . ? C26 O12 Na1 126.3(3) . . ? Mn4 O12 Na1 102.03(13) . . ? C20 O13 Mn4 128.6(3) . . ? C19 O15 H15 109.5 . . ? C33 O16 Na1 125.5(3) . . ? C33 O16 H16 111(6) . . ? Na1 O16 H16 81(6) . . ? C34 O17 Na1 144.0(4) . . ? C34 O17 H17 120(6) . . ? Na1 O17 H17 94(5) . . ? C12 N1 C10 113.3(4) . . ? C12 N1 C8 113.0(4) . . ? C10 N1 C8 113.6(4) . . ? C12 N1 Mn1 110.4(2) . . ? C10 N1 Mn1 100.9(3) . . ? C8 N1 Mn1 104.5(2) . . ? N3 N2 Mn2 126.1(3) . 3_665 ? N3 N2 Mn2 123.3(3) . . ? Mn2 N2 Mn2 103.87(14) 3_665 . ? N3 N2 Mn3 107.8(3) . . ? Mn2 N2 Mn3 94.04(12) 3_665 . ? Mn2 N2 Mn3 91.83(12) . . ? N4 N3 N2 178.9(5) . . ? C14 N5 C18 113.5(4) . . ? C14 N5 C16 113.3(4) . . ? C18 N5 C16 113.2(4) . . ? C14 N5 Mn4 101.3(3) . . ? C18 N5 Mn4 111.0(3) . . ? C16 N5 Mn4 103.3(3) . . ? C32 N6 C29 110.9(4) . . ? C32 N6 C28 111.6(3) . . ? C29 N6 C28 110.3(3) . . ? C32 N6 Mn3 110.2(3) . . ? C29 N6 Mn3 107.0(2) . . ? C28 N6 Mn3 106.7(2) . . ? O1 C1 C2 118.6(5) . . ? O1 C1 C6 123.4(5) . . ? C2 C1 C6 117.9(4) . . ? C3 C2 C1 121.7(6) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 120.3(7) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.4(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.9(5) . . ? C5 C6 C7 118.8(5) . . ? C1 C6 C7 122.3(4) . . ? O3 C7 O2 118.9(5) . . ? O3 C7 C6 120.3(4) . . ? O2 C7 C6 120.8(4) . . ? N1 C8 C9 109.8(3) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O4 C9 C8 109.4(4) . . ? O4 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? O4 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? N1 C10 C11 110.1(3) . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? O5 C11 C10 109.2(3) . . ? O5 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? O5 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? N1 C12 C13 116.4(4) . . ? N1 C12 H12A 108.2 . . ? C13 C12 H12A 108.2 . . ? N1 C12 H12B 108.2 . . ? C13 C12 H12B 108.2 . . ? H12A C12 H12B 107.3 . . ? O6 C13 C12 110.4(4) . . ? O6 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? O6 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N5 C14 C15 110.8(4) . . ? N5 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O8 C15 C14 109.9(4) . . ? O8 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? O8 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N5 C16 C17 109.6(4) . . ? N5 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? N5 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? O11 C17 C16 109.6(4) . . ? O11 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? O11 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? N5 C18 C19 115.7(5) . . ? N5 C18 H18A 108.4 . . ? C19 C18 H18A 108.4 . . ? N5 C18 H18B 108.4 . . ? C19 C18 H18B 108.4 . . ? H18A C18 H18B 107.4 . . ? O15A C19 O15 86.4(11) . . ? O15A C19 O15B 108.7(11) . . ? O15 C19 O15B 86.6(13) . . ? O15A C19 C18 117.0(8) . . ? O15 C19 C18 129.4(11) . . ? O15B C19 C18 121.2(11) . . ? O15A C19 H19A 108.0 . . ? O15 C19 H19A 24.2 . . ? O15B C19 H19A 89.7 . . ? C18 C19 H19A 108.0 . . ? O15A C19 H19B 108.0 . . ? O15 C19 H19B 105.3 . . ? O15B C19 H19B 18.8 . . ? C18 C19 H19B 108.0 . . ? H19A C19 H19B 107.3 . . ? O13 C20 C25 123.9(5) . . ? O13 C20 C21 117.2(5) . . ? C25 C20 C21 118.9(5) . . ? C22 C21 C20 120.9(6) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C21 120.7(7) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 118.8(6) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 122.1(5) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C20 C25 C24 118.5(5) . . ? C20 C25 C26 123.7(4) . . ? C24 C25 C26 117.8(5) . . ? O14 C26 O12 119.7(5) . . ? O14 C26 C25 119.7(4) . . ? O12 C26 C25 120.6(4) . . ? O7 C27 C28 110.7(3) . . ? O7 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? O7 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? N6 C28 C27 110.9(3) . . ? N6 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? N6 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? N6 C29 C30 111.3(3) . . ? N6 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? N6 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O9 C30 C29 111.4(4) . . ? O9 C30 H30A 109.4 . . ? C29 C30 H30A 109.4 . . ? O9 C30 H30B 109.4 . . ? C29 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? O10 C31 C32 110.2(4) . . ? O10 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? O10 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? N6 C32 C31 110.5(4) . . ? N6 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? N6 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? O16 C33 H33A 109.5 . . ? O16 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O16 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O17 C34 H34A 109.5 . . ? O17 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O17 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C19 O15A H15X 109.5 . . ? C19 O15B H15Y 109.5 . . ? C1S O1S H1S 108(6) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.766 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.094 # Attachment '- 3_Na2Mn8_1-D_final+sq.CIF' #========================================================================== data_746sq _database_code_depnum_ccdc_archive 'CCDC 834650' #TrackingRef '- 3_Na2Mn8_1-D_final+sq.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains half the cluster as well as solvent MeOH molecules. After preliminary modelling as one fully occupied and four partially occupied MeOH molecules with restrained bond (DFIX) and thermal (ISOR) parameters, the MeOH molecules were removed from the model and the associated electron density was accounted for by PLATON/SQUEEZE. All H atoms were placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H122 Mn8 N12 Na2 O39' _chemical_formula_weight 2277.33 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' Na Na 0.0362 0.0249 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8576(3) _cell_length_b 14.5491(3) _cell_length_c 14.8713(3) _cell_angle_alpha 76.2500(10) _cell_angle_beta 68.6450(10) _cell_angle_gamma 84.7590(10) _cell_volume 2516.64(9) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8967 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.12 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1178 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.606 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_process_details ; SADABS (Sheldrick, G. M. (1996), University of Gottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEXII CCD' _diffrn_measurement_method 'scans in \f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28474 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11452 _reflns_number_gt 9379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 structure was solved by direct methods. The asymmetric unit contains half the cluster as well as solvent MeOH molecules. After preliminary modelling as one fully occupied and four partially occupied MeOH molecules with restrained bond (DFIX) and thermal (ISOR) parameters, the MeOH molecules were removed from the model and the associated electron density was accounted for by PLATON/SQUEEZE. All H atoms were placed in calculated positions. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.009 0.000 616.0 211 _platon_squeeze_details ; PLATON/SQUEEZE Spek, A.L. (1990), Acta Cryst. A46, C-34 ; _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^)+(0.0916P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11452 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.22466(3) 0.24067(3) 0.40448(3) 0.02017(11) Uani 1 1 d . . . Mn2 Mn 0.13909(3) 0.03377(3) 0.41928(2) 0.01769(10) Uani 1 1 d . . . Mn3 Mn 0.04177(3) -0.19182(3) 0.46184(3) 0.01859(11) Uani 1 1 d . . . Mn4 Mn 0.27176(3) -0.11086(3) 0.28049(3) 0.01906(11) Uani 1 1 d . . . Na1 Na 0.40435(8) 0.08494(8) 0.27764(7) 0.0241(2) Uani 1 1 d . . . O1 O 0.19149(15) 0.36991(13) 0.36688(13) 0.0264(4) Uani 1 1 d . . . O2 O 0.34286(15) 0.24635(14) 0.27707(13) 0.0282(4) Uani 1 1 d . . . O3 O 0.4787(2) 0.31139(18) 0.13937(18) 0.0594(8) Uani 1 1 d . . . O4 O 0.11399(14) 0.23542(13) 0.53363(12) 0.0217(4) Uani 1 1 d . . . O5 O 0.27006(13) 0.10844(12) 0.43456(12) 0.0200(4) Uani 1 1 d . . . O6 O 0.5570(2) 0.43199(18) 0.4466(2) 0.0598(7) Uani 1 1 d . . . H6 H 0.5887 0.4361 0.3854 0.072 Uiso 1 1 calc R . . O7 O 0.19535(14) -0.11127(12) 0.43735(12) 0.0188(4) Uani 1 1 d . . . O8 O 0.24241(14) 0.02436(13) 0.26711(12) 0.0199(4) Uani 1 1 d . . . O9 O -0.08685(14) -0.17825(12) 0.61226(12) 0.0202(4) Uani 1 1 d . . . O10 O 0.11179(17) -0.32995(14) 0.41111(14) 0.0253(4) Uani 1 1 d . . . O11 O 0.12461(14) -0.14250(13) 0.29904(12) 0.0219(4) Uani 1 1 d . . . O12 O 0.42277(14) -0.08297(13) 0.26490(13) 0.0234(4) Uani 1 1 d . . . O13 O 0.30847(14) -0.24173(13) 0.29201(13) 0.0241(4) Uani 1 1 d . . . O14 O 0.60044(16) -0.10286(15) 0.24833(16) 0.0363(5) Uani 1 1 d . . . O15 O 0.49359(18) -0.13649(17) -0.11080(14) 0.0370(5) Uani 1 1 d . . . O16 O 0.56355(18) 0.05488(17) 0.32163(17) 0.0379(5) Uani 1 1 d . . . N1 N 0.33478(18) 0.25820(17) 0.49467(16) 0.0262(5) Uani 1 1 d . . . N2 N -0.02348(17) -0.02654(16) 0.42446(14) 0.0209(4) Uani 1 1 d . . . N3 N -0.05044(17) -0.01163(16) 0.35240(16) 0.0236(5) Uani 1 1 d . . . N4 N -0.0752(2) 0.0023(2) 0.28289(17) 0.0352(6) Uani 1 1 d . . . N5 N 0.28039(17) -0.07482(16) 0.11704(15) 0.0241(5) Uani 1 1 d . . . N6 N 0.11659(17) -0.27867(15) 0.58101(15) 0.0214(4) Uani 1 1 d . . . C1 C 0.2276(3) 0.4267(2) 0.2764(2) 0.0317(6) Uani 1 1 d . . . C2 C 0.1686(3) 0.5109(2) 0.2594(2) 0.0398(7) Uani 1 1 d . . . H2 H 0.1039 0.5250 0.3110 0.048 Uiso 1 1 calc R . . C3 C 0.2035(4) 0.5737(2) 0.1685(3) 0.0583(11) Uani 1 1 d . . . H3 H 0.1621 0.6303 0.1583 0.070 Uiso 1 1 calc R . . C4 C 0.2976(4) 0.5554(3) 0.0923(3) 0.0701(14) Uani 1 1 d . . . H4 H 0.3218 0.5999 0.0307 0.084 Uiso 1 1 calc R . . C5 C 0.3549(4) 0.4741(3) 0.1055(3) 0.0627(12) Uani 1 1 d . . . H5 H 0.4185 0.4613 0.0522 0.075 Uiso 1 1 calc R . . C6 C 0.3225(3) 0.4074(2) 0.1974(2) 0.0427(8) Uani 1 1 d . . . C7 C 0.3863(3) 0.3182(2) 0.2044(2) 0.0401(8) Uani 1 1 d . . . C8 C 0.2527(2) 0.2657(2) 0.5934(2) 0.0325(7) Uani 1 1 d . . . H8A H 0.2785 0.3129 0.6188 0.039 Uiso 1 1 calc R . . H8B H 0.2460 0.2038 0.6407 0.039 Uiso 1 1 calc R . . C9 C 0.1405(2) 0.2954(2) 0.58437(19) 0.0268(6) Uani 1 1 d . . . H9A H 0.0825 0.2904 0.6510 0.032 Uiso 1 1 calc R . . H9B H 0.1434 0.3620 0.5474 0.032 Uiso 1 1 calc R . . C10 C 0.3965(2) 0.1681(2) 0.4956(2) 0.0269(6) Uani 1 1 d . . . H10A H 0.4259 0.1549 0.5504 0.032 Uiso 1 1 calc R . . H10B H 0.4608 0.1728 0.4326 0.032 Uiso 1 1 calc R . . C11 C 0.3210(2) 0.0870(2) 0.50867(19) 0.0260(6) Uani 1 1 d . . . H11A H 0.3655 0.0280 0.5032 0.031 Uiso 1 1 calc R . . H11B H 0.2622 0.0768 0.5753 0.031 Uiso 1 1 calc R . . C12 C 0.4080(2) 0.3418(2) 0.4463(2) 0.0323(6) Uani 1 1 d . . . H12A H 0.3610 0.3996 0.4512 0.039 Uiso 1 1 calc R . . H12B H 0.4449 0.3417 0.3751 0.039 Uiso 1 1 calc R . . C13 C 0.4978(3) 0.3471(2) 0.4895(3) 0.0444(8) Uani 1 1 d . . . H13A H 0.4623 0.3417 0.5618 0.053 Uiso 1 1 calc R . . H13B H 0.5503 0.2933 0.4783 0.053 Uiso 1 1 calc R . . C14 C 0.2966(2) 0.0287(2) 0.09219(18) 0.0265(6) Uani 1 1 d . . . H14A H 0.2765 0.0573 0.0333 0.032 Uiso 1 1 calc R . . H14B H 0.3762 0.0424 0.0758 0.032 Uiso 1 1 calc R . . C15 C 0.2250(2) 0.0726(2) 0.17831(18) 0.0263(6) Uani 1 1 d . . . H15A H 0.2444 0.1402 0.1635 0.032 Uiso 1 1 calc R . . H15B H 0.1452 0.0689 0.1873 0.032 Uiso 1 1 calc R . . C16 C 0.1684(2) -0.1007(2) 0.12357(18) 0.0281(6) Uani 1 1 d . . . H16A H 0.1754 -0.1268 0.0659 0.034 Uiso 1 1 calc R . . H16B H 0.1200 -0.0438 0.1229 0.034 Uiso 1 1 calc R . . C17 C 0.1165(2) -0.1742(2) 0.21889(18) 0.0272(6) Uani 1 1 d . . . H17A H 0.0371 -0.1835 0.2299 0.033 Uiso 1 1 calc R . . H17B H 0.1561 -0.2354 0.2139 0.033 Uiso 1 1 calc R . . C18 C 0.3720(2) -0.1255(2) 0.05496(19) 0.0275(6) Uani 1 1 d . . . H18A H 0.3556 -0.1941 0.0772 0.033 Uiso 1 1 calc R . . H18B H 0.4414 -0.1154 0.0655 0.033 Uiso 1 1 calc R . . C19 C 0.3925(3) -0.0959(2) -0.0553(2) 0.0374(7) Uani 1 1 d . . . H19A H 0.3292 -0.1166 -0.0685 0.045 Uiso 1 1 calc R . . H19B H 0.3969 -0.0260 -0.0765 0.045 Uiso 1 1 calc R . . C20 C 0.4091(2) -0.2823(2) 0.2665(2) 0.0281(6) Uani 1 1 d . . . C21 C 0.4142(3) -0.3762(2) 0.2594(3) 0.0511(9) Uani 1 1 d . . . H21 H 0.3472 -0.4084 0.2731 0.061 Uiso 1 1 calc R . . C22 C 0.5140(3) -0.4231(3) 0.2331(5) 0.0898(19) Uani 1 1 d . . . H22 H 0.5163 -0.4876 0.2297 0.108 Uiso 1 1 calc R . . C23 C 0.6131(4) -0.3755(4) 0.2113(6) 0.111(2) Uani 1 1 d . . . H23 H 0.6826 -0.4079 0.1929 0.133 Uiso 1 1 calc R . . C24 C 0.6104(3) -0.2827(3) 0.2163(3) 0.0584(11) Uani 1 1 d . . . H24 H 0.6782 -0.2510 0.2008 0.070 Uiso 1 1 calc R . . C25 C 0.5093(2) -0.2341(2) 0.2440(2) 0.0307(6) Uani 1 1 d . . . C26 C 0.5125(2) -0.1357(2) 0.25271(18) 0.0255(6) Uani 1 1 d . . . C27 C 0.2629(2) -0.15740(19) 0.49232(18) 0.0225(5) Uani 1 1 d . . . H27A H 0.3056 -0.1096 0.5019 0.027 Uiso 1 1 calc R . . H27B H 0.3170 -0.1999 0.4548 0.027 Uiso 1 1 calc R . . C28 C 0.1918(2) -0.21428(19) 0.59201(18) 0.0238(5) Uani 1 1 d . . . H28A H 0.2408 -0.2518 0.6256 0.029 Uiso 1 1 calc R . . H28B H 0.1468 -0.1707 0.6337 0.029 Uiso 1 1 calc R . . C29 C 0.0216(2) -0.30608(19) 0.67432(18) 0.0252(5) Uani 1 1 d . . . H29A H 0.0499 -0.3287 0.7294 0.030 Uiso 1 1 calc R . . H29B H -0.0189 -0.3589 0.6704 0.030 Uiso 1 1 calc R . . C30 C -0.0584(2) -0.22438(19) 0.69561(18) 0.0234(5) Uani 1 1 d . . . H30A H -0.1272 -0.2482 0.7517 0.028 Uiso 1 1 calc R . . H30B H -0.0237 -0.1782 0.7153 0.028 Uiso 1 1 calc R . . C31 C 0.1215(2) -0.4022(2) 0.4922(2) 0.0285(6) Uani 1 1 d . . . H31A H 0.1663 -0.4558 0.4668 0.034 Uiso 1 1 calc R . . H31B H 0.0464 -0.4262 0.5370 0.034 Uiso 1 1 calc R . . C32 C 0.1767(2) -0.36293(19) 0.5484(2) 0.0263(6) Uani 1 1 d . . . H32A H 0.1783 -0.4119 0.6069 0.032 Uiso 1 1 calc R . . H32B H 0.2548 -0.3458 0.5056 0.032 Uiso 1 1 calc R . . C33 C 0.6578(3) 0.1133(2) 0.2829(2) 0.0385(7) Uani 1 1 d . . . H33A H 0.6707 0.1424 0.2132 0.058 Uiso 1 1 calc R . . H33B H 0.7232 0.0754 0.2882 0.058 Uiso 1 1 calc R . . H33C H 0.6452 0.1630 0.3202 0.058 Uiso 1 1 calc R . . H15 H 0.485(3) -0.195(3) -0.102(3) 0.046 Uiso 1 1 d . . . H18 H 0.581(3) 0.017(3) 0.299(3) 0.046 Uiso 1 1 d . . . H14X H 0.165(3) -0.313(2) 0.373(2) 0.031(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01485(19) 0.0224(2) 0.02351(19) -0.01121(15) -0.00289(15) -0.00131(16) Mn2 0.01265(19) 0.0205(2) 0.02078(19) -0.01001(14) -0.00375(14) 0.00085(15) Mn3 0.01284(19) 0.0226(2) 0.02165(19) -0.01023(15) -0.00442(14) 0.00078(15) Mn4 0.01312(19) 0.0227(2) 0.02260(19) -0.01124(15) -0.00422(14) 0.00156(15) Na1 0.0165(5) 0.0306(6) 0.0258(5) -0.0133(4) -0.0041(4) 0.0006(4) O1 0.0260(10) 0.0238(10) 0.0293(9) -0.0112(7) -0.0058(7) -0.0019(8) O2 0.0236(10) 0.0285(11) 0.0260(9) -0.0105(8) 0.0026(7) -0.0053(8) O3 0.0472(15) 0.0453(15) 0.0549(14) -0.0153(11) 0.0232(12) -0.0126(12) O4 0.0153(8) 0.0270(10) 0.0252(8) -0.0137(7) -0.0047(7) -0.0016(7) O5 0.0149(8) 0.0250(10) 0.0229(8) -0.0106(7) -0.0064(7) -0.0008(7) O6 0.0329(13) 0.0543(17) 0.101(2) -0.0387(15) -0.0174(13) -0.0101(12) O7 0.0145(8) 0.0224(9) 0.0219(8) -0.0091(7) -0.0075(6) 0.0029(7) O8 0.0169(8) 0.0252(10) 0.0189(8) -0.0093(7) -0.0053(7) 0.0010(7) O9 0.0170(8) 0.0215(9) 0.0236(8) -0.0082(7) -0.0070(7) 0.0002(7) O10 0.0197(10) 0.0266(11) 0.0298(10) -0.0132(8) -0.0047(8) 0.0009(8) O11 0.0160(8) 0.0289(10) 0.0230(8) -0.0127(7) -0.0054(7) 0.0012(7) O12 0.0155(8) 0.0264(10) 0.0293(9) -0.0121(7) -0.0061(7) 0.0031(7) O13 0.0154(8) 0.0223(10) 0.0341(9) -0.0127(7) -0.0046(7) 0.0017(7) O14 0.0204(10) 0.0385(12) 0.0570(13) -0.0216(10) -0.0157(9) 0.0034(9) O15 0.0341(11) 0.0404(13) 0.0295(10) -0.0181(9) 0.0038(8) -0.0020(10) O16 0.0231(10) 0.0462(15) 0.0517(13) -0.0249(10) -0.0135(9) 0.0022(10) N1 0.0158(10) 0.0330(13) 0.0343(12) -0.0204(10) -0.0061(9) -0.0002(9) N2 0.0164(10) 0.0259(12) 0.0213(10) -0.0109(8) -0.0044(8) 0.0010(9) N3 0.0155(10) 0.0245(12) 0.0281(11) -0.0112(9) -0.0022(9) 0.0040(9) N4 0.0287(13) 0.0509(17) 0.0290(12) -0.0125(11) -0.0128(10) 0.0064(12) N5 0.0166(10) 0.0319(13) 0.0244(10) -0.0127(9) -0.0040(8) 0.0002(9) N6 0.0180(10) 0.0208(11) 0.0273(10) -0.0111(8) -0.0070(8) 0.0020(9) C1 0.0378(16) 0.0225(14) 0.0355(14) -0.0089(11) -0.0104(12) -0.0085(13) C2 0.054(2) 0.0249(16) 0.0409(16) -0.0110(12) -0.0135(15) -0.0087(15) C3 0.104(3) 0.0248(17) 0.048(2) -0.0073(14) -0.027(2) -0.007(2) C4 0.119(4) 0.033(2) 0.042(2) -0.0016(16) -0.010(2) -0.017(2) C5 0.088(3) 0.032(2) 0.0448(19) -0.0058(15) 0.0057(19) -0.019(2) C6 0.054(2) 0.0279(17) 0.0360(16) -0.0063(12) -0.0004(14) -0.0166(15) C7 0.0402(18) 0.0321(17) 0.0385(16) -0.0145(13) 0.0029(13) -0.0073(14) C8 0.0197(13) 0.0525(19) 0.0335(14) -0.0286(13) -0.0066(11) -0.0019(13) C9 0.0174(12) 0.0371(16) 0.0299(13) -0.0219(11) -0.0029(10) -0.0042(11) C10 0.0197(13) 0.0343(16) 0.0320(13) -0.0152(11) -0.0101(11) -0.0015(11) C11 0.0256(14) 0.0286(15) 0.0289(13) -0.0078(11) -0.0143(11) -0.0018(11) C12 0.0204(13) 0.0314(16) 0.0510(17) -0.0239(13) -0.0106(12) 0.0013(12) C13 0.0249(15) 0.044(2) 0.077(2) -0.0324(17) -0.0202(15) -0.0021(14) C14 0.0238(13) 0.0330(15) 0.0211(12) -0.0093(10) -0.0044(10) 0.0013(11) C15 0.0267(14) 0.0286(15) 0.0236(12) -0.0094(10) -0.0073(10) 0.0020(11) C16 0.0211(13) 0.0438(17) 0.0236(12) -0.0142(11) -0.0084(10) -0.0011(12) C17 0.0186(12) 0.0384(16) 0.0288(13) -0.0193(11) -0.0052(10) -0.0032(11) C18 0.0236(13) 0.0312(15) 0.0268(13) -0.0138(11) -0.0034(10) 0.0020(12) C19 0.0360(16) 0.049(2) 0.0236(13) -0.0160(12) -0.0027(12) 0.0071(14) C20 0.0196(13) 0.0270(15) 0.0364(14) -0.0125(11) -0.0068(11) 0.0072(11) C21 0.0232(16) 0.0344(19) 0.096(3) -0.0279(18) -0.0140(17) 0.0012(14) C22 0.033(2) 0.044(2) 0.197(6) -0.058(3) -0.031(3) 0.0162(18) C23 0.029(2) 0.061(3) 0.250(8) -0.088(4) -0.028(3) 0.018(2) C24 0.0196(16) 0.044(2) 0.116(3) -0.041(2) -0.0164(18) 0.0086(15) C25 0.0200(13) 0.0298(16) 0.0432(15) -0.0176(12) -0.0079(11) 0.0059(12) C26 0.0174(12) 0.0325(15) 0.0272(12) -0.0121(11) -0.0058(10) 0.0025(11) C27 0.0186(12) 0.0237(13) 0.0295(12) -0.0095(10) -0.0120(10) 0.0026(10) C28 0.0223(13) 0.0257(14) 0.0263(12) -0.0115(10) -0.0090(10) 0.0025(11) C29 0.0244(13) 0.0253(14) 0.0266(12) -0.0054(10) -0.0095(10) -0.0017(11) C30 0.0216(13) 0.0262(14) 0.0228(12) -0.0079(10) -0.0064(10) -0.0014(11) C31 0.0275(14) 0.0222(14) 0.0349(14) -0.0106(11) -0.0078(11) 0.0015(11) C32 0.0225(13) 0.0233(14) 0.0354(14) -0.0109(11) -0.0116(11) 0.0057(11) C33 0.0285(15) 0.0448(19) 0.0475(17) -0.0153(14) -0.0154(13) -0.0046(14) _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 1.8862(19) . ? Mn1 O4 1.9181(17) . ? Mn1 O2 1.9385(17) . ? Mn1 O5 1.9540(18) . ? Mn1 O9 2.1794(17) 2_556 ? Mn1 N1 2.341(2) . ? Mn1 Mn2 3.2302(5) . ? Mn1 Na1 3.4541(11) . ? Mn2 O9 2.1430(18) 2_556 ? Mn2 O7 2.1544(18) . ? Mn2 O5 2.1904(16) . ? Mn2 O8 2.1975(16) . ? Mn2 N2 2.240(2) 2_556 ? Mn2 N2 2.309(2) . ? Mn2 Mn4 3.2315(5) . ? Mn2 Na1 3.3331(10) . ? Mn3 O4 2.1286(16) 2_556 ? Mn3 O11 2.2241(17) . ? Mn3 O7 2.2587(17) . ? Mn3 O9 2.2878(17) . ? Mn3 O10 2.3052(19) . ? Mn3 N6 2.370(2) . ? Mn3 N2 2.476(2) . ? Mn4 O11 1.8937(17) . ? Mn4 O13 1.9019(19) . ? Mn4 O12 1.9390(17) . ? Mn4 O8 1.9456(18) . ? Mn4 O7 2.1754(16) . ? Mn4 N5 2.325(2) . ? Mn4 Na1 3.4352(11) . ? Na1 O15 2.316(2) 2_655 ? Na1 O16 2.342(2) . ? Na1 O8 2.4032(19) . ? Na1 O2 2.408(2) . ? Na1 O5 2.4250(18) . ? Na1 O12 2.478(2) . ? Na1 H18 2.50(4) . ? O1 C1 1.340(3) . ? O2 C7 1.305(3) . ? O3 C7 1.243(4) . ? O4 C9 1.415(3) . ? O4 Mn3 2.1286(16) 2_556 ? O5 C11 1.437(3) . ? O6 C13 1.398(4) . ? O6 H6 0.8400 . ? O7 C27 1.422(3) . ? O8 C15 1.426(3) . ? O9 C30 1.418(3) . ? O9 Mn2 2.1430(18) 2_556 ? O9 Mn1 2.1794(17) 2_556 ? O10 C31 1.435(3) . ? O10 H14X 0.73(3) . ? O11 C17 1.416(3) . ? O12 C26 1.305(3) . ? O13 C20 1.333(3) . ? O14 C26 1.242(3) . ? O15 C19 1.425(4) . ? O15 Na1 2.316(2) 2_655 ? O15 H15 0.84(4) . ? O16 C33 1.403(4) . ? O16 H18 0.69(4) . ? N1 C10 1.469(4) . ? N1 C12 1.478(4) . ? N1 C8 1.486(3) . ? N2 N3 1.209(3) . ? N2 Mn2 2.240(2) 2_556 ? N3 N4 1.157(3) . ? N5 C18 1.468(3) . ? N5 C14 1.478(4) . ? N5 C16 1.485(3) . ? N6 C29 1.473(3) . ? N6 C32 1.474(3) . ? N6 C28 1.481(3) . ? C1 C2 1.401(5) . ? C1 C6 1.413(4) . ? C2 C3 1.382(4) . ? C2 H2 0.9500 . ? C3 C4 1.380(6) . ? C3 H3 0.9500 . ? C4 C5 1.347(6) . ? C4 H4 0.9500 . ? C5 C6 1.418(4) . ? C5 H5 0.9500 . ? C6 C7 1.473(5) . ? C8 C9 1.512(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.528(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.528(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.523(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.523(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.522(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.389(4) . ? C20 C25 1.415(4) . ? C21 C22 1.366(5) . ? C21 H21 0.9500 . ? C22 C23 1.400(6) . ? C22 H22 0.9500 . ? C23 C24 1.366(5) . ? C23 H23 0.9500 . ? C24 C25 1.392(4) . ? C24 H24 0.9500 . ? C25 C26 1.474(4) . ? C27 C28 1.512(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.513(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.505(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 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 O4 89.88(8) . . ? O1 Mn1 O2 90.76(8) . . ? O4 Mn1 O2 176.79(8) . . ? O1 Mn1 O5 175.49(7) . . ? O4 Mn1 O5 94.41(7) . . ? O2 Mn1 O5 84.88(8) . . ? O1 Mn1 O9 99.42(7) . 2_556 ? O4 Mn1 O9 80.04(7) . 2_556 ? O2 Mn1 O9 102.95(7) . 2_556 ? O5 Mn1 O9 82.71(7) . 2_556 ? O1 Mn1 N1 97.45(8) . . ? O4 Mn1 N1 78.62(7) . . ? O2 Mn1 N1 98.18(8) . . ? O5 Mn1 N1 82.08(8) . . ? O9 Mn1 N1 152.65(7) 2_556 . ? O1 Mn1 Mn2 140.44(6) . . ? O4 Mn1 Mn2 86.71(5) . . ? O2 Mn1 Mn2 94.79(6) . . ? O5 Mn1 Mn2 41.50(5) . . ? O9 Mn1 Mn2 41.21(5) 2_556 . ? N1 Mn1 Mn2 120.30(6) . . ? O1 Mn1 Na1 132.78(6) . . ? O4 Mn1 Na1 137.26(6) . . ? O2 Mn1 Na1 42.38(6) . . ? O5 Mn1 Na1 43.03(5) . . ? O9 Mn1 Na1 88.80(5) 2_556 . ? N1 Mn1 Na1 95.37(6) . . ? Mn2 Mn1 Na1 59.710(18) . . ? O9 Mn2 O7 174.95(6) 2_556 . ? O9 Mn2 O5 78.31(7) 2_556 . ? O7 Mn2 O5 103.30(7) . . ? O9 Mn2 O8 97.86(7) 2_556 . ? O7 Mn2 O8 77.35(6) . . ? O5 Mn2 O8 92.20(6) . . ? O9 Mn2 N2 86.82(7) 2_556 2_556 ? O7 Mn2 N2 97.80(7) . 2_556 ? O5 Mn2 N2 94.17(7) . 2_556 ? O8 Mn2 N2 172.76(7) . 2_556 ? O9 Mn2 N2 94.05(7) 2_556 . ? O7 Mn2 N2 85.08(7) . . ? O5 Mn2 N2 168.25(7) . . ? O8 Mn2 N2 97.73(7) . . ? N2 Mn2 N2 76.35(8) 2_556 . ? O9 Mn2 Mn1 42.07(4) 2_556 . ? O7 Mn2 Mn1 139.30(4) . . ? O5 Mn2 Mn1 36.24(5) . . ? O8 Mn2 Mn1 95.87(5) . . ? N2 Mn2 Mn1 91.30(6) 2_556 . ? N2 Mn2 Mn1 135.53(6) . . ? O9 Mn2 Mn4 133.05(5) 2_556 . ? O7 Mn2 Mn4 41.98(4) . . ? O5 Mn2 Mn4 104.80(5) . . ? O8 Mn2 Mn4 36.03(5) . . ? N2 Mn2 Mn4 138.14(6) 2_556 . ? N2 Mn2 Mn4 86.94(5) . . ? Mn1 Mn2 Mn4 125.598(14) . . ? O9 Mn2 Na1 92.66(5) 2_556 . ? O7 Mn2 Na1 85.17(5) . . ? O5 Mn2 Na1 46.63(5) . . ? O8 Mn2 Na1 46.07(5) . . ? N2 Mn2 Na1 139.61(6) 2_556 . ? N2 Mn2 Na1 143.78(5) . . ? Mn1 Mn2 Na1 63.49(2) . . ? Mn4 Mn2 Na1 63.08(2) . . ? O4 Mn3 O11 99.44(6) 2_556 . ? O4 Mn3 O7 165.93(7) 2_556 . ? O11 Mn3 O7 73.22(6) . . ? O4 Mn3 O9 73.40(6) 2_556 . ? O11 Mn3 O9 152.94(7) . . ? O7 Mn3 O9 107.53(6) . . ? O4 Mn3 O10 85.44(7) 2_556 . ? O11 Mn3 O10 77.06(7) . . ? O7 Mn3 O10 104.08(7) . . ? O9 Mn3 O10 126.94(7) . . ? O4 Mn3 N6 118.23(7) 2_556 . ? O11 Mn3 N6 129.65(7) . . ? O7 Mn3 N6 74.86(6) . . ? O9 Mn3 N6 74.38(7) . . ? O10 Mn3 N6 74.23(7) . . ? O4 Mn3 N2 87.47(7) 2_556 . ? O11 Mn3 N2 75.25(7) . . ? O7 Mn3 N2 79.11(7) . . ? O9 Mn3 N2 78.35(6) . . ? O10 Mn3 N2 149.82(7) . . ? N6 Mn3 N2 134.03(7) . . ? O11 Mn4 O13 87.99(8) . . ? O11 Mn4 O12 177.82(8) . . ? O13 Mn4 O12 90.21(8) . . ? O11 Mn4 O8 95.00(8) . . ? O13 Mn4 O8 177.00(7) . . ? O12 Mn4 O8 86.81(7) . . ? O11 Mn4 O7 81.82(7) . . ? O13 Mn4 O7 98.32(7) . . ? O12 Mn4 O7 97.23(7) . . ? O8 Mn4 O7 82.39(7) . . ? O11 Mn4 N5 79.94(7) . . ? O13 Mn4 N5 98.43(8) . . ? O12 Mn4 N5 101.55(7) . . ? O8 Mn4 N5 81.87(7) . . ? O7 Mn4 N5 154.69(7) . . ? O11 Mn4 Mn2 81.97(5) . . ? O13 Mn4 Mn2 139.46(5) . . ? O12 Mn4 Mn2 98.63(5) . . ? O8 Mn4 Mn2 41.63(5) . . ? O7 Mn4 Mn2 41.48(5) . . ? N5 Mn4 Mn2 118.02(6) . . ? O11 Mn4 Na1 136.53(6) . . ? O13 Mn4 Na1 134.34(6) . . ? O12 Mn4 Na1 45.01(6) . . ? O8 Mn4 Na1 42.78(5) . . ? O7 Mn4 Na1 82.34(5) . . ? N5 Mn4 Na1 99.12(6) . . ? Mn2 Mn4 Na1 59.903(18) . . ? O15 Na1 O16 93.59(9) 2_655 . ? O15 Na1 O8 99.88(7) 2_655 . ? O16 Na1 O8 148.41(9) . . ? O15 Na1 O2 86.96(8) 2_655 . ? O16 Na1 O2 110.88(8) . . ? O8 Na1 O2 98.34(7) . . ? O15 Na1 O5 152.62(9) 2_655 . ? O16 Na1 O5 98.97(8) . . ? O8 Na1 O5 81.81(6) . . ? O2 Na1 O5 65.85(6) . . ? O15 Na1 O12 92.25(8) 2_655 . ? O16 Na1 O12 84.88(8) . . ? O8 Na1 O12 66.28(6) . . ? O2 Na1 O12 164.25(7) . . ? O5 Na1 O12 112.95(7) . . ? O15 Na1 Mn2 137.38(7) 2_655 . ? O16 Na1 Mn2 128.49(7) . . ? O8 Na1 Mn2 41.19(4) . . ? O2 Na1 Mn2 84.04(5) . . ? O5 Na1 Mn2 41.04(4) . . ? O12 Na1 Mn2 85.94(5) . . ? O15 Na1 Mn4 102.26(6) 2_655 . ? O16 Na1 Mn4 115.80(7) . . ? O8 Na1 Mn4 33.36(5) . . ? O2 Na1 Mn4 131.50(6) . . ? O5 Na1 Mn4 94.04(5) . . ? O12 Na1 Mn4 33.59(4) . . ? Mn2 Na1 Mn4 57.012(18) . . ? O15 Na1 Mn1 119.26(7) 2_655 . ? O16 Na1 Mn1 111.45(6) . . ? O8 Na1 Mn1 86.58(5) . . ? O2 Na1 Mn1 32.87(4) . . ? O5 Na1 Mn1 33.35(4) . . ? O12 Na1 Mn1 142.05(5) . . ? Mn2 Na1 Mn1 56.805(18) . . ? Mn4 Na1 Mn1 113.06(3) . . ? O15 Na1 H18 87.8(9) 2_655 . ? O16 Na1 H18 16.1(9) . . ? O8 Na1 H18 135.9(9) . . ? O2 Na1 H18 125.5(9) . . ? O5 Na1 H18 110.1(9) . . ? O12 Na1 H18 70.1(9) . . ? Mn2 Na1 H18 130.4(9) . . ? Mn4 Na1 H18 102.6(9) . . ? Mn1 Na1 H18 127.1(9) . . ? C1 O1 Mn1 128.06(18) . . ? C7 O2 Mn1 130.9(2) . . ? C7 O2 Na1 124.32(18) . . ? Mn1 O2 Na1 104.75(8) . . ? C9 O4 Mn1 111.94(14) . . ? C9 O4 Mn3 131.77(15) . 2_556 ? Mn1 O4 Mn3 110.02(8) . 2_556 ? C11 O5 Mn1 114.12(15) . . ? C11 O5 Mn2 130.12(14) . . ? Mn1 O5 Mn2 102.26(7) . . ? C11 O5 Na1 109.87(15) . . ? Mn1 O5 Na1 103.62(7) . . ? Mn2 O5 Na1 92.33(6) . . ? C13 O6 H6 109.5 . . ? C27 O7 Mn2 128.32(15) . . ? C27 O7 Mn4 112.60(14) . . ? Mn2 O7 Mn4 96.54(7) . . ? C27 O7 Mn3 115.07(14) . . ? Mn2 O7 Mn3 102.95(7) . . ? Mn4 O7 Mn3 95.19(6) . . ? C15 O8 Mn4 115.89(15) . . ? C15 O8 Mn2 127.19(15) . . ? Mn4 O8 Mn2 102.34(7) . . ? C15 O8 Na1 110.56(14) . . ? Mn4 O8 Na1 103.86(8) . . ? Mn2 O8 Na1 92.74(6) . . ? C30 O9 Mn2 126.28(15) . 2_556 ? C30 O9 Mn1 115.49(14) . 2_556 ? Mn2 O9 Mn1 96.71(7) 2_556 2_556 ? C30 O9 Mn3 115.49(15) . . ? Mn2 O9 Mn3 101.50(7) 2_556 . ? Mn1 O9 Mn3 95.88(7) 2_556 . ? C31 O10 Mn3 110.91(15) . . ? C31 O10 H14X 115(3) . . ? Mn3 O10 H14X 100(3) . . ? C17 O11 Mn4 113.64(14) . . ? C17 O11 Mn3 131.45(15) . . ? Mn4 O11 Mn3 105.07(7) . . ? C26 O12 Mn4 131.47(17) . . ? C26 O12 Na1 127.12(16) . . ? Mn4 O12 Na1 101.40(8) . . ? C20 O13 Mn4 128.63(17) . . ? C19 O15 Na1 126.43(19) . 2_655 ? C19 O15 H15 110(2) . . ? Na1 O15 H15 106(2) 2_655 . ? C33 O16 Na1 125.2(2) . . ? C33 O16 H18 104(3) . . ? Na1 O16 H18 95(3) . . ? C10 N1 C12 113.3(2) . . ? C10 N1 C8 113.3(2) . . ? C12 N1 C8 112.5(2) . . ? C10 N1 Mn1 100.62(14) . . ? C12 N1 Mn1 111.88(17) . . ? C8 N1 Mn1 104.28(14) . . ? N3 N2 Mn2 125.96(17) . 2_556 ? N3 N2 Mn2 121.81(16) . . ? Mn2 N2 Mn2 103.65(8) 2_556 . ? N3 N2 Mn3 110.98(17) . . ? Mn2 N2 Mn3 93.27(7) 2_556 . ? Mn2 N2 Mn3 92.32(7) . . ? N4 N3 N2 179.3(3) . . ? C18 N5 C14 113.6(2) . . ? C18 N5 C16 113.2(2) . . ? C14 N5 C16 112.5(2) . . ? C18 N5 Mn4 111.82(16) . . ? C14 N5 Mn4 100.40(14) . . ? C16 N5 Mn4 104.12(14) . . ? C29 N6 C32 110.8(2) . . ? C29 N6 C28 110.36(19) . . ? C32 N6 C28 111.6(2) . . ? C29 N6 Mn3 106.76(15) . . ? C32 N6 Mn3 110.00(15) . . ? C28 N6 Mn3 107.14(15) . . ? O1 C1 C2 118.0(3) . . ? O1 C1 C6 124.0(3) . . ? C2 C1 C6 118.0(3) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.9(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.4(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 119.0(3) . . ? C1 C6 C7 122.8(3) . . ? C5 C6 C7 118.1(3) . . ? O3 C7 O2 121.0(3) . . ? O3 C7 C6 119.7(3) . . ? O2 C7 C6 119.3(3) . . ? N1 C8 C9 109.3(2) . . ? N1 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N1 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? O4 C9 C8 108.6(2) . . ? O4 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? O4 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N1 C10 C11 110.8(2) . . ? N1 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? O5 C11 C10 110.3(2) . . ? O5 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? O5 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N1 C12 C13 114.7(3) . . ? N1 C12 H12A 108.6 . . ? C13 C12 H12A 108.6 . . ? N1 C12 H12B 108.6 . . ? C13 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O6 C13 C12 111.6(3) . . ? O6 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? O6 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? N5 C14 C15 111.0(2) . . ? N5 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N5 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? O8 C15 C14 110.4(2) . . ? O8 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? O8 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N5 C16 C17 109.3(2) . . ? N5 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? N5 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O11 C17 C16 109.1(2) . . ? O11 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? O11 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N5 C18 C19 114.8(2) . . ? N5 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? N5 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.5 . . ? O15 C19 C18 110.7(3) . . ? O15 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? O15 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? O13 C20 C21 117.2(3) . . ? O13 C20 C25 123.5(3) . . ? C21 C20 C25 119.3(3) . . ? C22 C21 C20 121.0(3) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 119.7(4) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.7(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C20 118.9(3) . . ? C24 C25 C26 117.6(3) . . ? C20 C25 C26 123.4(2) . . ? O14 C26 O12 120.0(3) . . ? O14 C26 C25 120.1(3) . . ? O12 C26 C25 120.0(2) . . ? O7 C27 C28 110.8(2) . . ? O7 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? O7 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? N6 C28 C27 111.0(2) . . ? N6 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? N6 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? N6 C29 C30 111.8(2) . . ? N6 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N6 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? O9 C30 C29 111.9(2) . . ? O9 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? O9 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? O10 C31 C32 110.0(2) . . ? O10 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O10 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? N6 C32 C31 111.0(2) . . ? N6 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? N6 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? O16 C33 H33A 109.5 . . ? O16 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O16 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 1.586 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.094 # Attachment '- 5_K2Mn8_1-D_final+sq.CIF' #========================================================================== data_748sq _database_code_depnum_ccdc_archive 'CCDC 834651' #TrackingRef '- 5_K2Mn8_1-D_final+sq.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains two unique halves of the cluster as well as solvent MeOH molecules. There is a disorderd water molecule coordinated to the K ion each set each at 0.5 occupancy. The lattice solvent molecules were preliminarily modelled as one fully occupied and seven partially occupied MeOH molecules which were refined with restrained bond (DFIX) and thermal (ISOR) parameters. Subsequently, these were removed and the associated electron density was accounted for using PLATON/SQUEEZE.that have been modelled at 0.5 All H atoms were placed in calculated positions, except for on the water molecules which were not included in the final model. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H114 K2 Mn8 N12 O37' _chemical_formula_weight 2221.44 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' K K 0.2009 0.2494 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.798(3) _cell_length_b 18.608(4) _cell_length_c 18.879(4) _cell_angle_alpha 77.060(3) _cell_angle_beta 75.811(5) _cell_angle_gamma 82.295(5) _cell_volume 4894.3(17) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 1.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22307 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.26 _reflns_number_total 13515 _reflns_number_gt 8765 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 structure was solved by direct methods. The asymmetric unit contains two unique halves of the cluster as well as solvent MeOH molecules. There is a disorderd water molecule coordinated to the K ion each set each at 0.5 occupancy. The lattice solvent molecules were preliminarily modelled as one fully occupied and seven partially occupied MeOH molecules which were refined with restrained bond (DFIX) and thermal (ISOR) parameters. Subsequently, these were removed and the associated electron density was accounted for using PLATON/SQUEEZE.that have been modelled at 0.5 All H atoms were placed in calculated positions, except for on the water molecules which were not included in the final model. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.124 0.500 1.00- 987.0 189 _platon_squeeze_details ; PLATON/SQUEEZE Spek, A.L. (1990), Acta Cryst. A46, C-34 ; _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^)+(0.1517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13515 _refine_ls_number_parameters 1072 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.1212 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2522 _refine_ls_wR_factor_gt 0.2316 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.85371(8) -0.04595(7) -0.15417(7) 0.0207(3) Uani 1 1 d . . . Mn2 Mn 0.88354(8) 0.02070(7) -0.01982(6) 0.0187(3) Uani 1 1 d . . . Mn3 Mn 0.92915(8) 0.05468(7) 0.14053(6) 0.0182(3) Uani 1 1 d . . . Mn4 Mn 0.73134(8) 0.10923(8) 0.08949(7) 0.0220(3) Uani 1 1 d . . . Mn5 Mn 0.16856(9) 0.58722(7) 0.61628(8) 0.0257(4) Uani 1 1 d . . . Mn6 Mn -0.02469(9) 0.63838(7) 0.55566(8) 0.0251(4) Uani 1 1 d . . . Mn7 Mn 0.11514(9) 0.47845(7) 0.52485(8) 0.0261(4) Uani 1 1 d . . . Mn8 Mn 0.24394(10) 0.34507(7) 0.45654(8) 0.0290(4) Uani 1 1 d . . . K1 K 0.62386(15) 0.06035(15) -0.06318(12) 0.0437(6) Uani 1 1 d . . . K2 K 0.37662(17) 0.43275(13) 0.56723(16) 0.0519(7) Uani 1 1 d . . . O1 O 0.9079(4) -0.0425(3) -0.2578(3) 0.0235(14) Uani 1 1 d . . . O2 O 0.7585(4) 0.0292(4) -0.1795(3) 0.0351(16) Uani 1 1 d . B . O3 O 0.6944(5) 0.1309(5) -0.2433(5) 0.066(2) Uani 1 1 d . B . O4 O 0.9516(4) -0.1186(3) -0.1319(3) 0.0230(14) Uani 1 1 d . . . O5 O 0.7936(4) -0.0454(3) -0.0512(3) 0.0275(15) Uani 1 1 d . B . O6 O 0.6884(5) -0.2809(4) -0.1441(4) 0.0481(19) Uani 1 1 d . . . H6 H 0.6441 -0.3078 -0.1354 0.058 Uiso 1 1 calc R . . O7 O 0.8236(4) 0.0081(3) 0.0970(3) 0.0198(13) Uani 1 1 d . . . O8 O 0.7830(4) 0.1162(3) -0.0158(3) 0.0265(15) Uani 1 1 d . B . O9 O 1.0548(4) -0.0287(3) 0.1376(3) 0.0189(13) Uani 1 1 d . . . O10 O 0.9036(4) 0.0836(3) 0.2592(3) 0.0292(15) Uani 1 1 d D . . H10 H 0.961(3) 0.086(5) 0.264(5) 0.035 Uiso 1 1 d D . . O11 O 0.8350(4) 0.1484(3) 0.1087(3) 0.0260(14) Uani 1 1 d . . . O12 O 0.6264(4) 0.0677(3) 0.0745(3) 0.0262(14) Uani 1 1 d . B . O13 O 0.6708(4) 0.1073(3) 0.1893(3) 0.0252(14) Uani 1 1 d . . . O14 O 0.4998(5) 0.0113(4) 0.0949(4) 0.0425(18) Uani 1 1 d . . . O15 O 0.4733(4) 0.3537(4) 0.1038(4) 0.0454(19) Uani 1 1 d . . . H15 H 0.4817 0.3582 0.1450 0.054 Uiso 1 1 calc R . . O17 O 0.3676(5) 0.2453(4) 0.6280(4) 0.051(2) Uani 1 1 d . A . O18 O 0.3150(4) 0.3146(3) 0.5329(4) 0.0377(17) Uani 1 1 d . A . O20 O 0.1614(4) 0.4826(3) 0.6246(4) 0.0321(16) Uani 1 1 d . A . O21 O 0.2345(4) 0.2438(3) 0.4559(3) 0.0267(15) Uani 1 1 d . . . O22 O -0.1062(4) 0.6377(3) 0.4692(3) 0.0252(14) Uani 1 1 d U . . O23 O -0.0695(5) 0.7539(4) 0.5861(4) 0.0358(17) Uani 1 1 d D . . H23' H -0.121(4) 0.758(5) 0.569(5) 0.043 Uiso 1 1 d D . . O24 O 0.1247(4) 0.5950(3) 0.5124(3) 0.0257(14) Uani 1 1 d . . . O25 O 0.1724(4) 0.3711(3) 0.3835(4) 0.0297(15) Uani 1 1 d . . . O26 O 0.5286(5) 0.3735(4) 0.2228(4) 0.049(2) Uani 1 1 d . . . H26 H 0.5829 0.3833 0.1990 0.059 Uiso 1 1 calc R . . O27 O 0.2543(4) 0.4460(3) 0.4626(4) 0.0355(17) Uani 1 1 d . A . O28 O 0.0366(4) 0.6091(3) 0.6509(3) 0.0286(15) Uani 1 1 d . . . O29 O 0.1859(4) 0.6853(3) 0.6170(4) 0.0274(15) Uani 1 1 d . . . O30 O 0.3013(4) 0.5694(3) 0.5745(4) 0.0324(16) Uani 1 1 d . A . O31 O 0.4426(5) 0.5899(4) 0.5103(4) 0.0440(19) Uani 1 1 d . . . O32 O 0.3089(8) 0.5710(7) 0.8668(8) 0.129(5) Uani 1 1 d . . . H32 H 0.3142 0.5532 0.9107 0.155 Uiso 1 1 calc R . . N1 N 0.7758(5) -0.1518(4) -0.1289(4) 0.0282(18) Uani 1 1 d . B . N2 N 1.0003(5) 0.0744(4) 0.0043(4) 0.0202(16) Uani 1 1 d . . . N3 N 1.0171(5) 0.1389(5) -0.0173(4) 0.0234(18) Uani 1 1 d . . . N4 N 1.0361(6) 0.2002(5) -0.0402(4) 0.039(2) Uani 1 1 d . . . N5 N 0.6957(5) 0.2342(4) 0.0511(4) 0.0285(18) Uani 1 1 d . . . N6 N 0.8776(5) -0.0551(4) 0.2311(3) 0.0193(16) Uani 1 1 d . . . N7 N 0.3639(5) 0.3738(4) 0.3510(5) 0.034(2) Uani 1 1 d . A . N8 N 0.0389(5) 0.7289(4) 0.4464(4) 0.0241(17) Uani 1 1 d . . . N9 N 0.1529(6) 0.5496(4) 0.7466(4) 0.036(2) Uani 1 1 d . . . N10 N -0.0415(6) 0.5039(4) 0.5750(5) 0.0287(19) Uani 1 1 d . . . N11 N -0.0833(6) 0.4823(4) 0.6375(5) 0.0265(18) Uani 1 1 d . . . N12 N -0.1260(7) 0.4611(5) 0.6984(5) 0.045(2) Uani 1 1 d . . . C1 C 0.8754(7) -0.0028(5) -0.3161(5) 0.029(2) Uani 1 1 d U B . C2 C 0.9199(7) -0.0195(5) -0.3855(5) 0.034(2) Uani 1 1 d . . . H2 H 0.9711 -0.0562 -0.3892 0.041 Uiso 1 1 calc R . . C3 C 0.8886(8) 0.0185(6) -0.4511(5) 0.047(3) Uani 1 1 d . . . H3 H 0.9174 0.0056 -0.4979 0.056 Uiso 1 1 calc R . . C4 C 0.8170(7) 0.0737(5) -0.4463(6) 0.039(3) Uani 1 1 d . . . H4 H 0.7975 0.1000 -0.4901 0.047 Uiso 1 1 calc R . . C5 C 0.7738(7) 0.0907(6) -0.3788(5) 0.038(3) Uani 1 1 d . B . H5 H 0.7240 0.1286 -0.3757 0.045 Uiso 1 1 calc R . . C6 C 0.8027(6) 0.0525(5) -0.3131(5) 0.025(2) Uani 1 1 d . . . C7 C 0.7493(7) 0.0741(5) -0.2428(6) 0.033(2) Uani 1 1 d . B . C8 C 0.8469(6) -0.2128(6) -0.1099(5) 0.034(2) Uani 1 1 d . . . H8A H 0.8383 -0.2569 -0.1280 0.041 Uiso 1 1 calc R . . H8B H 0.8395 -0.2266 -0.0551 0.041 Uiso 1 1 calc R . . C9 C 0.9441(7) -0.1875(5) -0.1461(5) 0.033(2) Uani 1 1 d . . . H9A H 0.9915 -0.2241 -0.1264 0.039 Uiso 1 1 calc R . . H9B H 0.9565 -0.1845 -0.2006 0.039 Uiso 1 1 calc R . . C10 C 0.7021(6) -0.1373(6) -0.0658(5) 0.032(2) Uani 1 1 d . . . H10A H 0.6728 -0.1836 -0.0396 0.038 Uiso 1 1 calc R B . H10B H 0.6532 -0.1010 -0.0838 0.038 Uiso 1 1 calc R . . C11 C 0.7412(6) -0.1066(6) -0.0110(5) 0.035(2) Uani 1 1 d . B . H11A H 0.6892 -0.0905 0.0278 0.042 Uiso 1 1 calc R . . H11B H 0.7820 -0.1457 0.0137 0.042 Uiso 1 1 calc R . . C12 C 0.7401(7) -0.1600(6) -0.1932(5) 0.035(2) Uani 1 1 d . . . H12A H 0.7930 -0.1803 -0.2287 0.042 Uiso 1 1 calc R B . H12B H 0.7204 -0.1099 -0.2186 0.042 Uiso 1 1 calc R . . C13 C 0.6604(7) -0.2075(6) -0.1783(6) 0.041(3) Uani 1 1 d . B . H13A H 0.6051 -0.1872 -0.1450 0.049 Uiso 1 1 calc R . . H13B H 0.6433 -0.2080 -0.2257 0.049 Uiso 1 1 calc R . . C14 C 0.7055(7) 0.2395(6) -0.0292(5) 0.042(3) Uani 1 1 d . B . H14A H 0.7118 0.2915 -0.0556 0.050 Uiso 1 1 calc R . . H14B H 0.6490 0.2231 -0.0382 0.050 Uiso 1 1 calc R . . C15 C 0.7909(7) 0.1913(5) -0.0585(6) 0.043(3) Uani 1 1 d . . . H15A H 0.7958 0.1920 -0.1118 0.051 Uiso 1 1 calc R B . H15B H 0.8480 0.2105 -0.0537 0.051 Uiso 1 1 calc R . . C16 C 0.7686(7) 0.2702(6) 0.0695(7) 0.046(3) Uani 1 1 d . . . H16A H 0.7407 0.3161 0.0873 0.055 Uiso 1 1 calc R . . H16B H 0.8188 0.2834 0.0245 0.055 Uiso 1 1 calc R . . C17 C 0.8094(6) 0.2166(5) 0.1303(6) 0.036(2) Uani 1 1 d . . . H17A H 0.8648 0.2363 0.1373 0.043 Uiso 1 1 calc R . . H17B H 0.7624 0.2107 0.1781 0.043 Uiso 1 1 calc R . . C18 C 0.6009(6) 0.2571(6) 0.0889(5) 0.034(2) Uani 1 1 d . . . H18A H 0.6005 0.2549 0.1418 0.041 Uiso 1 1 calc R . . H18B H 0.5584 0.2209 0.0876 0.041 Uiso 1 1 calc R . . C19 C 0.5619(7) 0.3338(6) 0.0570(5) 0.042(3) Uani 1 1 d . . . H19A H 0.6068 0.3702 0.0529 0.050 Uiso 1 1 calc R . . H19B H 0.5533 0.3349 0.0063 0.050 Uiso 1 1 calc R . . C20 C 0.5861(6) 0.0867(5) 0.2253(5) 0.024(2) Uani 1 1 d . B . C21 C 0.5539(6) 0.1041(5) 0.2971(4) 0.026(2) Uani 1 1 d . . . H21 H 0.5902 0.1312 0.3153 0.031 Uiso 1 1 calc R . . C22 C 0.4701(6) 0.0812(6) 0.3397(5) 0.037(3) Uani 1 1 d . . . H22 H 0.4487 0.0930 0.3878 0.045 Uiso 1 1 calc R . . C23 C 0.4144(7) 0.0410(6) 0.3149(5) 0.041(3) Uani 1 1 d . . . H23 H 0.3575 0.0239 0.3461 0.049 Uiso 1 1 calc R . . C24 C 0.4452(7) 0.0272(6) 0.2437(5) 0.036(2) Uani 1 1 d . B . H24 H 0.4080 0.0005 0.2259 0.044 Uiso 1 1 calc R . . C25 C 0.5292(6) 0.0511(5) 0.1966(5) 0.023(2) Uani 1 1 d U . . C26 C 0.5518(6) 0.0415(5) 0.1192(4) 0.021(2) Uani 1 1 d U B . C27 C 0.7842(6) -0.0557(5) 0.1397(4) 0.022(2) Uani 1 1 d . . . H27A H 0.8197 -0.0992 0.1210 0.026 Uiso 1 1 calc R . . H27B H 0.7190 -0.0541 0.1343 0.026 Uiso 1 1 calc R . . C28 C 0.7842(6) -0.0646(5) 0.2229(5) 0.026(2) Uani 1 1 d . . . H28A H 0.7382 -0.0273 0.2447 0.031 Uiso 1 1 calc R . . H28B H 0.7658 -0.1143 0.2500 0.031 Uiso 1 1 calc R . . C29 C 0.9443(5) -0.1157(5) 0.2106(4) 0.0189(19) Uani 1 1 d U . . H29A H 0.9310 -0.1304 0.1671 0.023 Uiso 1 1 calc R . . H29B H 0.9371 -0.1589 0.2525 0.023 Uiso 1 1 calc R . . C30 C 1.0452(6) -0.0943(5) 0.1912(4) 0.0197(19) Uani 1 1 d . . . H30A H 1.0621 -0.0875 0.2368 0.024 Uiso 1 1 calc R . . H30B H 1.0882 -0.1345 0.1719 0.024 Uiso 1 1 calc R . . C31 C 0.8750(6) -0.0446(5) 0.3080(4) 0.022(2) Uani 1 1 d . . . H31A H 0.9380 -0.0576 0.3187 0.026 Uiso 1 1 calc R . . H31B H 0.8314 -0.0779 0.3449 0.026 Uiso 1 1 calc R . . C32 C 0.8436(6) 0.0343(5) 0.3148(4) 0.023(2) Uani 1 1 d . . . H32A H 0.7784 0.0461 0.3085 0.027 Uiso 1 1 calc R . . H32B H 0.8452 0.0411 0.3650 0.027 Uiso 1 1 calc R . . C33 C 0.3373(7) 0.2499(5) 0.5720(5) 0.034(2) Uani 1 1 d . A . C34 C 0.3227(6) 0.1814(5) 0.5482(5) 0.022(2) Uani 1 1 d . . . C35 C 0.3636(6) 0.1149(5) 0.5820(5) 0.027(2) Uani 1 1 d . A . H35 H 0.3967 0.1147 0.6193 0.032 Uiso 1 1 calc R . . C36 C 0.3566(6) 0.0492(5) 0.5618(5) 0.025(2) Uani 1 1 d . . . H36 H 0.3869 0.0043 0.5835 0.030 Uiso 1 1 calc R A . C37 C 0.3062(6) 0.0497(5) 0.5108(5) 0.027(2) Uani 1 1 d . A . H37 H 0.2997 0.0043 0.4983 0.032 Uiso 1 1 calc R . . C38 C 0.2635(6) 0.1151(5) 0.4762(4) 0.022(2) Uani 1 1 d . . . H38 H 0.2269 0.1136 0.4416 0.026 Uiso 1 1 calc R A . C39 C 0.2746(6) 0.1830(5) 0.4924(5) 0.024(2) Uani 1 1 d . A . C40 C 0.2230(6) 0.3595(5) 0.3101(5) 0.032(2) Uani 1 1 d . . . H40A H 0.1847 0.3812 0.2730 0.039 Uiso 1 1 calc R . . H40B H 0.2359 0.3059 0.3105 0.039 Uiso 1 1 calc R . . C41 C 0.3141(6) 0.3959(5) 0.2892(6) 0.033(2) Uani 1 1 d . . . H41A H 0.3540 0.3810 0.2436 0.039 Uiso 1 1 calc R . . H41B H 0.3010 0.4504 0.2785 0.039 Uiso 1 1 calc R . . C42 C 0.4374(7) 0.3130(6) 0.3388(6) 0.041(3) Uani 1 1 d . . . H42A H 0.4147 0.2799 0.3137 0.049 Uiso 1 1 calc R . . H42B H 0.4443 0.2840 0.3883 0.049 Uiso 1 1 calc R . . C43 C 0.5321(7) 0.3325(6) 0.2947(6) 0.046(3) Uani 1 1 d . . . H43A H 0.5587 0.3620 0.3211 0.056 Uiso 1 1 calc R . . H43B H 0.5737 0.2867 0.2905 0.056 Uiso 1 1 calc R . . C44 C 0.3986(7) 0.4364(5) 0.3723(6) 0.039(3) Uani 1 1 d . . . H44A H 0.4364 0.4160 0.4100 0.046 Uiso 1 1 calc R A . H44B H 0.4397 0.4641 0.3278 0.046 Uiso 1 1 calc R . . C45 C 0.3210(7) 0.4879(5) 0.4028(6) 0.037(3) Uani 1 1 d . A . H45A H 0.3460 0.5245 0.4222 0.044 Uiso 1 1 calc R . . H45B H 0.2894 0.5150 0.3629 0.044 Uiso 1 1 calc R . . C46 C -0.0906(6) 0.6923(5) 0.4040(5) 0.026(2) Uani 1 1 d . . . H46A H -0.1321 0.7376 0.4120 0.031 Uiso 1 1 calc R . . H46B H -0.1058 0.6746 0.3629 0.031 Uiso 1 1 calc R . . C47 C 0.0121(7) 0.7107(5) 0.3824(5) 0.030(2) Uani 1 1 d . . . H47A H 0.0530 0.6678 0.3667 0.036 Uiso 1 1 calc R . . H47B H 0.0206 0.7533 0.3399 0.036 Uiso 1 1 calc R . . C48 C 0.0021(6) 0.8034(4) 0.4569(5) 0.026(2) Uani 1 1 d U . . H48A H -0.0585 0.8156 0.4416 0.031 Uiso 1 1 calc R . . H48B H 0.0460 0.8394 0.4249 0.031 Uiso 1 1 calc R . . C49 C -0.0119(7) 0.8096(5) 0.5382(5) 0.031(2) Uani 1 1 d . . . H49A H 0.0496 0.8036 0.5518 0.038 Uiso 1 1 calc R . . H49B H -0.0419 0.8592 0.5449 0.038 Uiso 1 1 calc R . . C50 C 0.1433(6) 0.7183(5) 0.4386(5) 0.025(2) Uani 1 1 d . . . H50A H 0.1745 0.7453 0.3890 0.029 Uiso 1 1 calc R . . H50B H 0.1602 0.7391 0.4771 0.029 Uiso 1 1 calc R . . C51 C 0.1768(6) 0.6377(5) 0.4471(5) 0.024(2) Uani 1 1 d . . . H51A H 0.1712 0.6195 0.4030 0.029 Uiso 1 1 calc R . . H51B H 0.2436 0.6315 0.4491 0.029 Uiso 1 1 calc R . . C52 C 0.3670(7) 0.6135(5) 0.5448(5) 0.030(2) Uani 1 1 d . A . C53 C 0.3498(6) 0.6926(5) 0.5509(5) 0.023(2) Uani 1 1 d . . . C54 C 0.4199(8) 0.7375(6) 0.5220(6) 0.042(3) Uani 1 1 d . A . H54 H 0.4763 0.7190 0.4928 0.050 Uiso 1 1 calc R . . C55 C 0.4130(8) 0.8106(5) 0.5331(6) 0.039(3) Uani 1 1 d . . . H55 H 0.4637 0.8408 0.5123 0.047 Uiso 1 1 calc R A . C56 C 0.3309(6) 0.8368(5) 0.5750(5) 0.030(2) Uani 1 1 d U A . H56 H 0.3247 0.8857 0.5839 0.035 Uiso 1 1 calc R . . C57 C 0.2576(6) 0.7932(4) 0.6043(5) 0.022(2) Uani 1 1 d . . . H57 H 0.2018 0.8119 0.6340 0.026 Uiso 1 1 calc R A . C58 C 0.2638(6) 0.7211(5) 0.5910(5) 0.024(2) Uani 1 1 d U A . C59 C 0.0167(6) 0.6346(5) 0.7200(5) 0.030(2) Uani 1 1 d . . . H59A H -0.0517 0.6432 0.7382 0.036 Uiso 1 1 calc R . . H59B H 0.0449 0.6818 0.7124 0.036 Uiso 1 1 calc R . . C60 C 0.0560(7) 0.5780(6) 0.7753(6) 0.043(3) Uani 1 1 d . . . H60A H 0.0543 0.5995 0.8191 0.052 Uiso 1 1 calc R . . H60B H 0.0160 0.5361 0.7924 0.052 Uiso 1 1 calc R . . C61 C 0.2262(8) 0.5810(6) 0.7729(6) 0.046(3) Uani 1 1 d . . . H61A H 0.2118 0.6352 0.7680 0.055 Uiso 1 1 calc R . . H61B H 0.2883 0.5723 0.7401 0.055 Uiso 1 1 calc R . . C62 C 0.2308(10) 0.5463(8) 0.8548(8) 0.077(4) Uani 1 1 d U . . H62A H 0.1736 0.5622 0.8895 0.093 Uiso 1 1 calc R . . H62B H 0.2365 0.4916 0.8627 0.093 Uiso 1 1 calc R . . C63 C 0.1684(9) 0.4693(5) 0.7545(7) 0.058(4) Uani 1 1 d . A . H63A H 0.1387 0.4453 0.8058 0.070 Uiso 1 1 calc R . . H63B H 0.2364 0.4544 0.7460 0.070 Uiso 1 1 calc R . . C64 C 0.1270(10) 0.4438(6) 0.6984(6) 0.056(3) Uani 1 1 d . . . H64A H 0.1434 0.3901 0.7010 0.067 Uiso 1 1 calc R A . H64B H 0.0580 0.4524 0.7116 0.067 Uiso 1 1 calc R . . O19 O 0.485(3) 0.3678(18) 0.6849(12) 0.199(19) Uani 0.50 1 d P A 13 O19' O 0.4175 0.4246 0.7134 0.050 Uani 0.50 1 d P A 14 O16 O 0.5105 0.2112 -0.0835 0.050 Uani 0.50 1 d P B 15 O16' O 0.4747(17) 0.1753(13) -0.1492(14) 0.121(8) Uani 0.50 1 d PU B 16 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 0.0138(7) 0.0354(8) 0.0124(7) -0.0055(6) -0.0016(5) -0.0015(6) Mn2 0.0103(7) 0.0336(8) 0.0099(6) -0.0041(6) 0.0007(5) 0.0002(6) Mn3 0.0100(6) 0.0304(8) 0.0116(7) -0.0026(6) 0.0006(5) -0.0004(6) Mn4 0.0109(7) 0.0390(9) 0.0146(7) -0.0082(6) 0.0005(5) 0.0016(6) Mn5 0.0289(8) 0.0118(7) 0.0445(9) -0.0103(6) -0.0199(7) 0.0005(6) Mn6 0.0283(8) 0.0113(7) 0.0423(9) -0.0070(6) -0.0194(7) -0.0006(6) Mn7 0.0324(8) 0.0095(7) 0.0442(9) -0.0074(6) -0.0229(7) 0.0014(6) Mn8 0.0307(8) 0.0133(7) 0.0521(10) -0.0121(7) -0.0229(7) 0.0012(6) K1 0.0249(12) 0.0834(19) 0.0279(12) -0.0242(12) -0.0004(9) -0.0105(12) K2 0.0397(14) 0.0367(14) 0.089(2) -0.0298(14) -0.0190(14) 0.0028(11) O1 0.025(3) 0.033(4) 0.011(3) -0.002(3) -0.004(3) 0.000(3) O2 0.014(3) 0.055(5) 0.035(4) -0.016(4) 0.001(3) 0.001(3) O3 0.041(5) 0.062(6) 0.080(6) -0.008(5) -0.006(4) 0.025(4) O4 0.017(3) 0.030(4) 0.020(3) -0.001(3) -0.004(3) -0.002(3) O5 0.016(3) 0.048(4) 0.016(3) -0.002(3) 0.004(2) -0.014(3) O6 0.036(4) 0.043(5) 0.071(5) -0.007(4) -0.025(4) -0.007(3) O7 0.012(3) 0.030(3) 0.015(3) -0.002(3) 0.002(2) -0.004(3) O8 0.021(3) 0.039(4) 0.012(3) -0.003(3) 0.002(2) 0.011(3) O9 0.013(3) 0.030(3) 0.012(3) -0.004(3) 0.000(2) -0.002(3) O10 0.022(3) 0.037(4) 0.027(3) -0.004(3) -0.003(3) -0.004(3) O11 0.010(3) 0.032(4) 0.033(4) -0.005(3) -0.001(3) -0.001(3) O12 0.018(3) 0.046(4) 0.019(3) -0.012(3) -0.007(3) -0.003(3) O13 0.008(3) 0.048(4) 0.022(3) -0.018(3) 0.005(2) -0.007(3) O14 0.031(4) 0.071(5) 0.034(4) -0.019(4) -0.009(3) -0.017(4) O15 0.026(4) 0.060(5) 0.053(5) -0.025(4) -0.007(3) 0.009(3) O17 0.064(5) 0.044(5) 0.063(5) -0.017(4) -0.044(4) -0.002(4) O18 0.033(4) 0.028(4) 0.067(5) -0.020(4) -0.031(4) 0.003(3) O20 0.045(4) 0.018(3) 0.046(4) -0.006(3) -0.035(3) -0.001(3) O21 0.040(4) 0.011(3) 0.040(4) -0.011(3) -0.029(3) 0.008(3) O22 0.033(3) 0.007(3) 0.041(4) -0.007(3) -0.014(3) -0.005(2) O23 0.037(4) 0.028(4) 0.054(4) -0.017(3) -0.025(4) 0.000(3) O24 0.029(4) 0.008(3) 0.043(4) -0.004(3) -0.017(3) 0.003(3) O25 0.028(4) 0.018(3) 0.051(4) -0.011(3) -0.022(3) -0.001(3) O26 0.031(4) 0.072(6) 0.044(5) -0.011(4) -0.008(3) -0.005(4) O27 0.036(4) 0.014(3) 0.066(5) -0.014(3) -0.023(4) -0.001(3) O28 0.026(4) 0.025(4) 0.040(4) -0.006(3) -0.015(3) -0.005(3) O29 0.016(3) 0.016(3) 0.052(4) -0.014(3) -0.004(3) 0.000(3) O30 0.028(4) 0.024(4) 0.055(4) -0.022(3) -0.023(3) 0.011(3) O31 0.029(4) 0.046(4) 0.064(5) -0.032(4) -0.012(4) 0.013(3) O32 0.093(9) 0.159(12) 0.159(12) -0.038(10) -0.049(8) -0.044(8) N1 0.026(4) 0.036(5) 0.024(4) -0.003(4) -0.008(3) -0.007(4) N2 0.017(4) 0.028(5) 0.017(4) -0.006(3) -0.005(3) -0.003(3) N3 0.005(4) 0.045(6) 0.018(4) -0.013(4) 0.002(3) 0.005(4) N4 0.044(5) 0.041(6) 0.025(5) 0.003(4) 0.001(4) -0.013(4) N5 0.014(4) 0.041(5) 0.025(4) -0.004(4) -0.002(3) 0.007(3) N6 0.017(4) 0.026(4) 0.008(3) 0.003(3) 0.004(3) -0.001(3) N7 0.031(5) 0.014(4) 0.062(6) -0.007(4) -0.018(4) -0.002(3) N8 0.025(4) 0.012(4) 0.038(5) -0.005(3) -0.013(3) -0.002(3) N9 0.051(6) 0.027(5) 0.041(5) -0.002(4) -0.028(4) -0.017(4) N10 0.038(5) 0.014(4) 0.047(6) -0.015(4) -0.034(4) 0.012(4) N11 0.035(5) 0.014(4) 0.037(6) -0.004(4) -0.025(4) 0.002(4) N12 0.067(7) 0.025(5) 0.049(6) -0.002(4) -0.032(5) 0.000(4) C1 0.038(5) 0.036(5) 0.022(5) -0.007(4) -0.014(4) -0.017(4) C2 0.059(7) 0.032(6) 0.014(5) -0.007(4) -0.008(5) -0.006(5) C3 0.070(8) 0.059(8) 0.014(5) -0.011(5) 0.000(5) -0.026(7) C4 0.046(7) 0.029(6) 0.046(7) 0.007(5) -0.022(5) -0.017(5) C5 0.045(6) 0.035(6) 0.036(6) 0.013(5) -0.017(5) -0.028(5) C6 0.024(5) 0.022(5) 0.030(5) 0.003(4) -0.016(4) -0.006(4) C7 0.033(6) 0.032(6) 0.042(6) -0.005(5) -0.028(5) -0.001(5) C8 0.019(5) 0.050(7) 0.028(5) -0.007(5) -0.003(4) 0.004(5) C9 0.033(6) 0.030(6) 0.037(6) -0.002(5) -0.016(5) 0.001(4) C10 0.018(5) 0.050(6) 0.027(5) -0.008(5) 0.001(4) -0.013(4) C11 0.024(5) 0.064(7) 0.016(5) -0.015(5) 0.008(4) -0.014(5) C12 0.029(6) 0.049(6) 0.032(6) -0.022(5) -0.011(4) 0.008(5) C13 0.024(6) 0.053(7) 0.055(7) -0.027(6) -0.015(5) 0.005(5) C14 0.042(6) 0.043(6) 0.028(6) -0.002(5) 0.003(5) 0.010(5) C15 0.036(6) 0.032(6) 0.040(6) 0.005(5) 0.005(5) 0.021(5) C16 0.024(6) 0.032(6) 0.078(8) -0.013(6) -0.007(5) 0.002(5) C17 0.016(5) 0.043(6) 0.049(6) -0.023(5) 0.003(4) 0.002(4) C18 0.028(5) 0.049(6) 0.025(5) -0.013(5) -0.001(4) 0.000(5) C19 0.025(6) 0.063(8) 0.037(6) -0.021(5) -0.008(5) 0.018(5) C20 0.015(5) 0.030(5) 0.028(5) -0.005(4) -0.010(4) 0.005(4) C21 0.020(5) 0.044(6) 0.017(5) -0.016(4) -0.006(4) 0.003(4) C22 0.027(6) 0.063(7) 0.018(5) -0.010(5) 0.003(4) 0.001(5) C23 0.019(5) 0.071(8) 0.029(6) -0.006(5) 0.005(4) -0.016(5) C24 0.032(6) 0.048(7) 0.037(6) -0.013(5) -0.013(5) -0.014(5) C25 0.011(4) 0.038(5) 0.020(4) -0.002(4) -0.008(3) 0.001(4) C26 0.011(4) 0.037(5) 0.014(4) -0.006(4) -0.006(3) 0.005(4) C27 0.011(4) 0.035(5) 0.019(5) -0.004(4) -0.001(4) -0.005(4) C28 0.014(5) 0.040(6) 0.025(5) -0.011(4) -0.003(4) -0.006(4) C29 0.017(4) 0.026(4) 0.009(4) -0.005(3) 0.008(3) -0.004(4) C30 0.018(5) 0.029(5) 0.011(4) -0.005(4) 0.002(3) -0.007(4) C31 0.023(5) 0.029(5) 0.015(4) -0.005(4) -0.004(4) -0.010(4) C32 0.026(5) 0.025(5) 0.016(5) -0.005(4) 0.003(4) -0.011(4) C33 0.033(6) 0.039(6) 0.032(6) -0.011(5) -0.015(5) 0.016(5) C34 0.010(4) 0.021(5) 0.031(5) 0.001(4) 0.002(4) -0.008(4) C35 0.012(5) 0.038(6) 0.024(5) -0.004(4) 0.007(4) 0.002(4) C36 0.014(5) 0.026(5) 0.027(5) 0.006(4) 0.002(4) -0.002(4) C37 0.026(5) 0.016(5) 0.029(5) -0.004(4) 0.005(4) 0.006(4) C38 0.023(5) 0.027(5) 0.011(4) -0.007(4) 0.008(4) -0.002(4) C39 0.013(5) 0.027(5) 0.031(5) -0.009(4) -0.002(4) 0.002(4) C40 0.024(5) 0.034(6) 0.043(6) -0.012(5) -0.014(5) 0.004(4) C41 0.030(6) 0.022(5) 0.052(6) -0.011(5) -0.015(5) -0.003(4) C42 0.036(6) 0.034(6) 0.059(7) -0.019(5) -0.020(5) 0.010(5) C43 0.042(7) 0.040(7) 0.068(8) -0.021(6) -0.021(6) -0.009(5) C44 0.032(6) 0.037(6) 0.063(7) -0.021(5) -0.037(5) 0.009(5) C45 0.041(6) 0.019(5) 0.058(7) -0.019(5) -0.014(5) -0.007(5) C46 0.027(5) 0.023(5) 0.035(5) -0.010(4) -0.016(4) -0.002(4) C47 0.048(6) 0.013(5) 0.036(6) -0.013(4) -0.017(5) 0.005(4) C48 0.027(5) 0.013(4) 0.044(5) -0.003(4) -0.020(4) -0.002(4) C49 0.033(6) 0.013(5) 0.053(6) -0.007(4) -0.017(5) -0.006(4) C50 0.018(5) 0.019(5) 0.045(6) -0.019(4) -0.012(4) 0.000(4) C51 0.021(5) 0.026(5) 0.024(5) -0.002(4) -0.006(4) -0.003(4) C52 0.023(6) 0.036(6) 0.035(6) -0.008(5) -0.012(5) -0.003(5) C53 0.031(5) 0.014(5) 0.029(5) -0.008(4) -0.014(4) 0.000(4) C54 0.049(7) 0.045(7) 0.037(6) -0.017(5) -0.019(5) 0.008(6) C55 0.058(7) 0.019(5) 0.044(6) -0.002(5) -0.020(6) -0.010(5) C56 0.031(5) 0.013(4) 0.047(5) 0.000(4) -0.018(4) -0.003(4) C57 0.031(5) 0.017(5) 0.025(5) -0.007(4) -0.017(4) -0.002(4) C58 0.023(5) 0.029(5) 0.033(5) -0.011(4) -0.022(4) -0.002(4) C59 0.025(5) 0.039(6) 0.026(5) -0.008(5) 0.003(4) -0.017(4) C60 0.045(7) 0.044(7) 0.042(6) 0.004(5) -0.016(5) -0.021(5) C61 0.051(7) 0.036(6) 0.063(8) -0.027(6) -0.019(6) -0.003(5) C62 0.081(8) 0.090(8) 0.090(8) -0.038(6) -0.042(6) -0.032(6) C63 0.104(10) 0.021(6) 0.077(9) -0.007(6) -0.076(8) -0.002(6) C64 0.100(10) 0.037(7) 0.046(7) -0.002(6) -0.047(7) -0.009(6) O19 0.34(5) 0.23(3) 0.062(15) 0.026(17) -0.05(2) -0.24(3) O19' 0.050 0.050 0.050 -0.010 -0.011 -0.004 O16 0.050 0.050 0.050 -0.010 -0.011 -0.004 O16' 0.115(11) 0.096(10) 0.128(11) -0.021(8) 0.010(8) 0.006(8) _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(6) . ? Mn1 O1 1.914(5) . ? Mn1 O2 1.916(6) . ? Mn1 O5 1.931(5) . ? Mn1 O9 2.183(6) 2_755 ? Mn1 N1 2.314(8) . ? Mn1 Mn2 3.2049(18) . ? Mn1 K1 3.910(3) . ? Mn2 O7 2.137(5) . ? Mn2 O8 2.162(6) . ? Mn2 O9 2.166(5) 2_755 ? Mn2 O5 2.187(6) . ? Mn2 N2 2.289(7) . ? Mn2 N2 2.317(7) 2_755 ? Mn2 Mn4 3.2084(17) . ? Mn2 K1 4.061(3) . ? Mn3 O11 2.151(6) . ? Mn3 O4 2.211(6) 2_755 ? Mn3 O9 2.254(5) . ? Mn3 O7 2.275(6) . ? Mn3 O10 2.349(6) . ? Mn3 N6 2.427(7) . ? Mn3 N2 2.491(7) . ? Mn4 O13 1.873(5) . ? Mn4 O11 1.926(6) . ? Mn4 O8 1.929(5) . ? Mn4 O12 1.930(6) . ? Mn4 O7 2.170(6) . ? Mn4 N5 2.305(8) . ? Mn4 K1 3.934(3) . ? Mn5 O29 1.881(6) . ? Mn5 O28 1.920(6) . ? Mn5 O20 1.933(6) . ? Mn5 O30 1.943(6) . ? Mn5 O24 2.182(6) . ? Mn5 N9 2.365(8) . ? Mn5 Mn7 3.2193(18) . ? Mn5 K2 4.003(3) . ? Mn6 O28 2.140(6) . ? Mn6 O25 2.215(6) 2_566 ? Mn6 O22 2.258(6) . ? Mn6 O24 2.266(6) . ? Mn6 O23 2.319(6) . ? Mn6 N8 2.428(7) . ? Mn6 N10 2.484(7) . ? Mn7 O24 2.149(6) . ? Mn7 O22 2.160(5) 2_566 ? Mn7 O20 2.175(6) . ? Mn7 O27 2.188(7) . ? Mn7 N10 2.307(8) . ? Mn7 N10 2.341(7) 2_566 ? Mn7 Mn8 3.2273(19) . ? Mn7 K2 4.082(3) . ? Mn8 O25 1.881(6) . ? Mn8 O21 1.911(5) . ? Mn8 O18 1.929(6) . ? Mn8 O27 1.935(6) . ? Mn8 O22 2.201(6) 2_566 ? Mn8 N7 2.334(8) . ? Mn8 K2 3.909(3) . ? K1 O12 2.643(6) . ? K1 O14 2.652(7) 2_655 ? K1 O2 2.692(6) . ? K1 O5 2.997(6) . ? K1 O16 3.068(3) . ? K1 O8 3.086(7) . ? K1 O14 3.107(7) . ? K1 C26 3.298(8) . ? K1 O3 3.317(9) . ? K1 O16' 3.32(3) . ? K1 C11 3.414(11) . ? K1 C7 3.415(10) . ? K2 O30 2.654(6) . ? K2 O31 2.744(7) 2_666 ? K2 O18 2.747(6) . ? K2 O19' 2.934(3) . ? K2 O27 2.941(7) . ? K2 O19 2.99(3) . ? K2 O31 3.083(8) . ? K2 O20 3.184(7) . ? K2 C52 3.284(10) . ? K2 C45 3.311(11) . ? K2 O17 3.429(8) . ? K2 C33 3.505(11) . ? O1 C1 1.337(10) . ? O2 C7 1.321(11) . ? O3 C7 1.244(11) . ? O4 C9 1.392(11) . ? O4 Mn3 2.211(6) 2_755 ? O5 C11 1.427(11) . ? O6 C13 1.429(12) . ? O6 H6 0.8400 . ? O7 C27 1.388(10) . ? O8 C15 1.453(11) . ? O9 C30 1.399(10) . ? O9 Mn2 2.166(5) 2_755 ? O9 Mn1 2.183(6) 2_755 ? O10 C32 1.436(10) . ? O10 H10 0.890(10) . ? O11 C17 1.395(11) . ? O12 C26 1.293(10) . ? O13 C20 1.333(10) . ? O14 C26 1.235(10) . ? O14 K1 2.652(7) 2_655 ? O15 C19 1.445(11) . ? O15 H15 0.8400 . ? O17 C33 1.228(11) . ? O18 C33 1.311(11) . ? O20 C64 1.423(13) . ? O21 C39 1.333(10) . ? O22 C46 1.402(10) . ? O22 Mn7 2.160(5) 2_566 ? O22 Mn8 2.201(6) 2_566 ? O23 C49 1.433(11) . ? O23 H23' 0.888(10) . ? O24 C51 1.417(10) . ? O25 C40 1.452(11) . ? O25 Mn6 2.215(6) 2_566 ? O26 C43 1.411(13) . ? O26 H26 0.8400 . ? O27 C45 1.457(12) . ? O28 C59 1.436(10) . ? O29 C58 1.340(10) . ? O30 C52 1.295(11) . ? O31 C52 1.228(11) . ? O31 K2 2.744(7) 2_666 ? O32 C62 1.384(15) . ? O32 H32 0.8400 . ? N1 C10 1.454(11) . ? N1 C12 1.481(11) . ? N1 C8 1.486(11) . ? N2 N3 1.217(11) . ? N2 Mn2 2.317(7) 2_755 ? N3 N4 1.172(11) . ? N5 C18 1.464(11) . ? N5 C14 1.468(12) . ? N5 C16 1.490(12) . ? N6 C29 1.452(10) . ? N6 C28 1.466(10) . ? N6 C31 1.498(10) . ? N7 C42 1.476(12) . ? N7 C41 1.484(12) . ? N7 C44 1.501(12) . ? N8 C48 1.457(10) . ? N8 C47 1.480(11) . ? N8 C50 1.506(10) . ? N9 C63 1.460(12) . ? N9 C60 1.473(13) . ? N9 C61 1.526(12) . ? N10 N11 1.198(11) . ? N10 Mn7 2.341(7) 2_566 ? N11 N12 1.176(12) . ? C1 C6 1.386(13) . ? C1 C2 1.396(12) . ? C2 C3 1.431(14) . ? C2 H2 0.9500 . ? C3 C4 1.375(15) . ? C3 H3 0.9500 . ? C4 C5 1.364(14) . ? C4 H4 0.9500 . ? C5 C6 1.417(12) . ? C5 H5 0.9500 . ? C6 C7 1.478(13) . ? C8 C9 1.521(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.540(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.502(14) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.511(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.530(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.514(14) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.404(12) . ? C20 C21 1.417(12) . ? C21 C22 1.366(13) . ? C21 H21 0.9500 . ? C22 C23 1.403(14) . ? C22 H22 0.9500 . ? C23 C24 1.380(13) . ? C23 H23 0.9500 . ? C24 C25 1.400(12) . ? C24 H24 0.9500 . ? C25 C26 1.463(11) . ? C27 C28 1.542(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.532(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.503(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.501(13) . ? C34 C35 1.392(12) . ? C34 C39 1.402(12) . ? C35 C36 1.384(13) . ? C35 H35 0.9500 . ? C36 C37 1.352(13) . ? C36 H36 0.9500 . ? C37 C38 1.396(12) . ? C37 H37 0.9500 . ? C38 C39 1.406(12) . ? C38 H38 0.9500 . ? C40 C41 1.516(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.489(14) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.483(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.538(13) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.526(13) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.500(11) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.484(12) . ? C53 C54 1.350(14) . ? C53 C58 1.414(12) . ? C54 C55 1.409(13) . ? C54 H54 0.9500 . ? C55 C56 1.373(14) . ? C55 H55 0.9500 . ? C56 C57 1.372(12) . ? C56 H56 0.9500 . ? C57 C58 1.406(12) . ? C57 H57 0.9500 . ? C59 C60 1.476(13) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.551(17) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.530(13) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? 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 O1 88.4(2) . . ? O4 Mn1 O2 177.9(3) . . ? O1 Mn1 O2 90.1(3) . . ? O4 Mn1 O5 94.8(2) . . ? O1 Mn1 O5 176.8(3) . . ? O2 Mn1 O5 86.7(3) . . ? O4 Mn1 O9 82.7(2) . 2_755 ? O1 Mn1 O9 96.4(2) . 2_755 ? O2 Mn1 O9 96.1(2) . 2_755 ? O5 Mn1 O9 84.0(2) . 2_755 ? O4 Mn1 N1 80.3(3) . . ? O1 Mn1 N1 98.9(3) . . ? O2 Mn1 N1 101.3(3) . . ? O5 Mn1 N1 81.6(3) . . ? O9 Mn1 N1 156.7(2) 2_755 . ? O4 Mn1 Mn2 85.42(18) . . ? O1 Mn1 Mn2 138.75(19) . . ? O2 Mn1 Mn2 94.9(2) . . ? O5 Mn1 Mn2 41.88(17) . . ? O9 Mn1 Mn2 42.32(14) 2_755 . ? N1 Mn1 Mn2 119.95(18) . . ? O4 Mn1 K1 143.12(17) . . ? O1 Mn1 K1 128.43(18) . . ? O2 Mn1 K1 38.58(19) . . ? O5 Mn1 K1 48.37(18) . . ? O9 Mn1 K1 94.11(15) 2_755 . ? N1 Mn1 K1 89.96(19) . . ? Mn2 Mn1 K1 68.80(4) . . ? O7 Mn2 O8 78.0(2) . . ? O7 Mn2 O9 177.7(2) . 2_755 ? O8 Mn2 O9 103.9(2) . 2_755 ? O7 Mn2 O5 100.1(2) . . ? O8 Mn2 O5 94.7(2) . . ? O9 Mn2 O5 78.7(2) 2_755 . ? O7 Mn2 N2 85.7(2) . . ? O8 Mn2 N2 95.6(3) . . ? O9 Mn2 N2 95.3(2) 2_755 . ? O5 Mn2 N2 169.1(2) . . ? O7 Mn2 N2 93.9(2) . 2_755 ? O8 Mn2 N2 168.3(2) . 2_755 ? O9 Mn2 N2 84.4(2) 2_755 2_755 ? O5 Mn2 N2 95.0(2) . 2_755 ? N2 Mn2 N2 75.2(3) . 2_755 ? O7 Mn2 Mn1 135.85(16) . . ? O8 Mn2 Mn1 104.28(16) . . ? O9 Mn2 Mn1 42.73(15) 2_755 . ? O5 Mn2 Mn1 36.11(14) . . ? N2 Mn2 Mn1 136.49(17) . . ? N2 Mn2 Mn1 87.41(17) 2_755 . ? O7 Mn2 Mn4 42.25(15) . . ? O8 Mn2 Mn4 35.83(14) . . ? O9 Mn2 Mn4 139.75(15) 2_755 . ? O5 Mn2 Mn4 100.72(15) . . ? N2 Mn2 Mn4 89.78(17) . . ? N2 Mn2 Mn4 135.15(17) 2_755 . ? Mn1 Mn2 Mn4 128.05(5) . . ? O7 Mn2 K1 90.18(15) . . ? O8 Mn2 K1 48.48(17) . . ? O9 Mn2 K1 90.29(15) 2_755 . ? O5 Mn2 K1 46.22(17) . . ? N2 Mn2 K1 143.79(19) . . ? N2 Mn2 K1 141.04(19) 2_755 . ? Mn1 Mn2 K1 63.84(4) . . ? Mn4 Mn2 K1 64.27(4) . . ? O11 Mn3 O4 96.3(2) . 2_755 ? O11 Mn3 O9 161.7(2) . . ? O4 Mn3 O9 74.7(2) 2_755 . ? O11 Mn3 O7 75.1(2) . . ? O4 Mn3 O7 155.7(2) 2_755 . ? O9 Mn3 O7 106.6(2) . . ? O11 Mn3 O10 89.7(2) . . ? O4 Mn3 O10 76.2(2) 2_755 . ? O9 Mn3 O10 103.2(2) . . ? O7 Mn3 O10 125.5(2) . . ? O11 Mn3 N6 123.1(2) . . ? O4 Mn3 N6 128.7(2) 2_755 . ? O9 Mn3 N6 73.8(2) . . ? O7 Mn3 N6 73.0(2) . . ? O10 Mn3 N6 73.0(2) . . ? O11 Mn3 N2 84.0(2) . . ? O4 Mn3 N2 78.3(2) 2_755 . ? O9 Mn3 N2 78.6(2) . . ? O7 Mn3 N2 78.2(2) . . ? O10 Mn3 N2 152.9(2) . . ? N6 Mn3 N2 131.9(2) . . ? O13 Mn4 O11 88.0(2) . . ? O13 Mn4 O8 174.5(3) . . ? O11 Mn4 O8 95.4(3) . . ? O13 Mn4 O12 89.9(2) . . ? O11 Mn4 O12 177.6(3) . . ? O8 Mn4 O12 86.8(3) . . ? O13 Mn4 O7 102.3(2) . . ? O11 Mn4 O7 82.2(2) . . ? O8 Mn4 O7 82.4(2) . . ? O12 Mn4 O7 97.0(2) . . ? O13 Mn4 N5 94.7(3) . . ? O11 Mn4 N5 79.7(3) . . ? O8 Mn4 N5 81.8(2) . . ? O12 Mn4 N5 101.8(3) . . ? O7 Mn4 N5 154.6(2) . . ? O13 Mn4 Mn2 143.8(2) . . ? O11 Mn4 Mn2 86.83(17) . . ? O8 Mn4 Mn2 41.01(17) . . ? O12 Mn4 Mn2 94.07(17) . . ? O7 Mn4 Mn2 41.47(14) . . ? N5 Mn4 Mn2 119.51(18) . . ? O13 Mn4 K1 125.93(18) . . ? O11 Mn4 K1 145.76(18) . . ? O8 Mn4 K1 50.42(19) . . ? O12 Mn4 K1 36.46(17) . . ? O7 Mn4 K1 93.13(15) . . ? N5 Mn4 K1 91.97(19) . . ? Mn2 Mn4 K1 68.44(5) . . ? O29 Mn5 O28 88.6(2) . . ? O29 Mn5 O20 172.5(3) . . ? O28 Mn5 O20 95.3(3) . . ? O29 Mn5 O30 90.1(3) . . ? O28 Mn5 O30 176.0(3) . . ? O20 Mn5 O30 86.4(3) . . ? O29 Mn5 O24 104.3(2) . . ? O28 Mn5 O24 81.1(2) . . ? O20 Mn5 O24 82.7(2) . . ? O30 Mn5 O24 95.5(2) . . ? O29 Mn5 N9 92.9(3) . . ? O28 Mn5 N9 79.2(3) . . ? O20 Mn5 N9 81.5(3) . . ? O30 Mn5 N9 104.7(3) . . ? O24 Mn5 N9 153.4(3) . . ? O29 Mn5 Mn7 145.8(2) . . ? O28 Mn5 Mn7 87.01(18) . . ? O20 Mn5 Mn7 41.16(17) . . ? O30 Mn5 Mn7 91.92(18) . . ? O24 Mn5 Mn7 41.60(14) . . ? N9 Mn5 Mn7 119.37(19) . . ? O29 Mn5 K2 124.36(18) . . ? O28 Mn5 K2 146.88(18) . . ? O20 Mn5 K2 51.6(2) . . ? O30 Mn5 K2 34.94(18) . . ? O24 Mn5 K2 92.58(15) . . ? N9 Mn5 K2 94.3(2) . . ? Mn7 Mn5 K2 67.85(5) . . ? O28 Mn6 O25 97.3(2) . 2_566 ? O28 Mn6 O22 163.6(2) . . ? O25 Mn6 O22 73.8(2) 2_566 . ? O28 Mn6 O24 74.7(2) . . ? O25 Mn6 O24 155.2(2) 2_566 . ? O22 Mn6 O24 107.6(2) . . ? O28 Mn6 O23 87.7(2) . . ? O25 Mn6 O23 77.0(2) 2_566 . ? O22 Mn6 O23 103.3(2) . . ? O24 Mn6 O23 125.0(2) . . ? O28 Mn6 N8 121.9(2) . . ? O25 Mn6 N8 128.6(2) 2_566 . ? O22 Mn6 N8 73.5(2) . . ? O24 Mn6 N8 73.5(2) . . ? O23 Mn6 N8 73.2(2) . . ? O28 Mn6 N10 85.4(2) . . ? O25 Mn6 N10 77.2(2) 2_566 . ? O22 Mn6 N10 79.3(2) . . ? O24 Mn6 N10 78.8(2) . . ? O23 Mn6 N10 152.2(3) . . ? N8 Mn6 N10 132.5(3) . . ? O24 Mn7 O22 176.9(2) . 2_566 ? O24 Mn7 O20 78.2(2) . . ? O22 Mn7 O20 104.8(2) 2_566 . ? O24 Mn7 O27 100.5(2) . . ? O22 Mn7 O27 78.2(2) 2_566 . ? O20 Mn7 O27 94.9(2) . . ? O24 Mn7 N10 85.2(2) . . ? O22 Mn7 N10 95.6(2) 2_566 . ? O20 Mn7 N10 95.1(3) . . ? O27 Mn7 N10 169.4(2) . . ? O24 Mn7 N10 92.8(2) . 2_566 ? O22 Mn7 N10 84.5(2) 2_566 2_566 ? O20 Mn7 N10 167.1(2) . 2_566 ? O27 Mn7 N10 95.8(3) . 2_566 ? N10 Mn7 N10 74.8(3) . 2_566 ? O24 Mn7 Mn5 42.37(16) . . ? O22 Mn7 Mn5 140.56(17) 2_566 . ? O20 Mn7 Mn5 35.81(15) . . ? O27 Mn7 Mn5 100.21(16) . . ? N10 Mn7 Mn5 90.03(18) . . ? N10 Mn7 Mn5 134.31(17) 2_566 . ? O24 Mn7 Mn8 135.61(17) . . ? O22 Mn7 Mn8 42.77(16) 2_566 . ? O20 Mn7 Mn8 105.94(17) . . ? O27 Mn7 Mn8 35.78(15) . . ? N10 Mn7 Mn8 136.59(18) . . ? N10 Mn7 Mn8 86.95(18) 2_566 . ? Mn5 Mn7 Mn8 128.56(5) . . ? O24 Mn7 K2 90.92(16) . . ? O22 Mn7 K2 90.10(16) 2_566 . ? O20 Mn7 K2 50.66(18) . . ? O27 Mn7 K2 44.21(17) . . ? N10 Mn7 K2 145.4(2) . . ? N10 Mn7 K2 139.7(2) 2_566 . ? Mn5 Mn7 K2 65.24(5) . . ? Mn8 Mn7 K2 63.40(5) . . ? O25 Mn8 O21 87.7(2) . . ? O25 Mn8 O18 177.7(3) . . ? O21 Mn8 O18 90.2(2) . . ? O25 Mn8 O27 95.0(3) . . ? O21 Mn8 O27 176.9(3) . . ? O18 Mn8 O27 87.0(3) . . ? O25 Mn8 O22 81.9(3) . 2_566 ? O21 Mn8 O22 96.3(2) . 2_566 ? O18 Mn8 O22 97.3(3) . 2_566 ? O27 Mn8 O22 82.8(2) . 2_566 ? O25 Mn8 N7 80.8(3) . . ? O21 Mn8 N7 100.1(3) . . ? O18 Mn8 N7 100.6(3) . . ? O27 Mn8 N7 81.7(3) . . ? O22 Mn8 N7 155.6(2) 2_566 . ? O25 Mn8 Mn7 83.87(18) . . ? O21 Mn8 Mn7 138.0(2) . . ? O18 Mn8 Mn7 97.01(19) . . ? O27 Mn8 Mn7 41.4(2) . . ? O22 Mn8 Mn7 41.78(14) 2_566 . ? N7 Mn8 Mn7 118.85(18) . . ? O25 Mn8 K2 141.58(18) . . ? O21 Mn8 K2 130.61(17) . . ? O18 Mn8 K2 40.58(19) . . ? O27 Mn8 K2 46.69(19) . . ? O22 Mn8 K2 94.12(15) 2_566 . ? N7 Mn8 K2 88.8(2) . . ? Mn7 Mn8 K2 69.03(5) . . ? O12 K1 O14 122.9(2) . 2_655 ? O12 K1 O2 132.8(2) . . ? O14 K1 O2 92.8(2) 2_655 . ? O12 K1 O5 83.37(17) . . ? O14 K1 O5 107.2(2) 2_655 . ? O2 K1 O5 55.03(18) . . ? O12 K1 O16 91.03(15) . . ? O14 K1 O16 94.77(17) 2_655 . ? O2 K1 O16 117.89(17) . . ? O5 K1 O16 156.81(14) . . ? O12 K1 O8 54.45(16) . . ? O14 K1 O8 169.9(2) 2_655 . ? O2 K1 O8 84.76(18) . . ? O5 K1 O8 63.42(16) . . ? O16 K1 O8 95.08(13) . . ? O12 K1 O14 43.64(18) . . ? O14 K1 O14 79.5(2) 2_655 . ? O2 K1 O14 150.5(2) . . ? O5 K1 O14 99.83(18) . . ? O16 K1 O14 91.28(15) . . ? O8 K1 O14 97.89(16) . . ? O12 K1 C26 21.76(19) . . ? O14 K1 C26 101.4(2) 2_655 . ? O2 K1 C26 147.8(2) . . ? O5 K1 C26 93.00(18) . . ? O16 K1 C26 89.79(15) . . ? O8 K1 C26 76.19(18) . . ? O14 K1 C26 21.97(19) . . ? O12 K1 O3 146.4(2) . . ? O14 K1 O3 89.5(2) 2_655 . ? O2 K1 O3 42.05(19) . . ? O5 K1 O3 95.96(17) . . ? O16 K1 O3 76.45(14) . . ? O8 K1 O3 95.16(19) . . ? O14 K1 O3 162.8(2) . . ? C26 K1 O3 163.2(2) . . ? O12 K1 O16' 119.1(4) . . ? O14 K1 O16' 68.2(5) 2_655 . ? O2 K1 O16' 101.5(4) . . ? O5 K1 O16' 156.4(4) . . ? O16 K1 O16' 31.4(4) . . ? O8 K1 O16' 122.0(5) . . ? O14 K1 O16' 101.9(4) . . ? C26 K1 O16' 110.6(4) . . ? O3 K1 O16' 61.5(4) . . ? O12 K1 C11 80.1(2) . . ? O14 K1 C11 88.4(2) 2_655 . ? O2 K1 C11 70.4(2) . . ? O5 K1 C11 24.63(18) . . ? O16 K1 C11 170.86(16) . . ? O8 K1 C11 81.5(2) . . ? O14 K1 C11 80.9(2) . . ? C26 K1 C11 81.2(2) . . ? O3 K1 C11 112.2(2) . . ? O16' K1 C11 155.1(5) . . ? O12 K1 C7 145.9(2) . . ? O14 K1 C7 89.2(2) 2_655 . ? O2 K1 C7 21.0(2) . . ? O5 K1 C7 75.78(19) . . ? O16 K1 C7 97.63(17) . . ? O8 K1 C7 91.87(19) . . ? O14 K1 C7 166.2(2) . . ? C26 K1 C7 166.5(2) . . ? O3 K1 C7 21.24(19) . . ? O16' K1 C7 80.9(4) . . ? C11 K1 C7 91.0(2) . . ? O30 K2 O31 120.0(2) . 2_666 ? O30 K2 O18 132.6(2) . . ? O31 K2 O18 94.7(2) 2_666 . ? O30 K2 O19' 87.19(15) . . ? O31 K2 O19' 97.62(16) 2_666 . ? O18 K2 O19' 121.53(17) . . ? O30 K2 O27 82.05(18) . . ? O31 K2 O27 107.3(2) 2_666 . ? O18 K2 O27 55.67(18) . . ? O19' K2 O27 155.01(17) . . ? O30 K2 O19 113.3(7) . . ? O31 K2 O19 75.4(7) 2_666 . ? O18 K2 O19 105.7(5) . . ? O19' K2 O19 28.3(7) . . ? O27 K2 O19 161.1(5) . . ? O30 K2 O31 43.87(19) . . ? O31 K2 O31 76.1(2) 2_666 . ? O18 K2 O31 146.7(2) . . ? O19' K2 O31 91.60(14) . . ? O27 K2 O31 96.04(19) . . ? O19 K2 O31 102.7(4) . . ? O30 K2 O20 53.12(18) . . ? O31 K2 O20 167.6(2) 2_666 . ? O18 K2 O20 86.17(18) . . ? O19' K2 O20 92.44(13) . . ? O27 K2 O20 63.12(18) . . ? O19 K2 O20 116.3(7) . . ? O31 K2 O20 96.46(17) . . ? O30 K2 C52 22.1(2) . . ? O31 K2 C52 98.0(2) 2_666 . ? O18 K2 C52 146.5(2) . . ? O19' K2 C52 87.34(17) . . ? O27 K2 C52 90.9(2) . . ? O19 K2 C52 107.4(5) . . ? O31 K2 C52 21.95(19) . . ? O20 K2 C52 75.1(2) . . ? O30 K2 C45 78.5(2) . . ? O31 K2 C45 86.6(2) 2_666 . ? O18 K2 C45 71.9(2) . . ? O19' K2 C45 165.25(17) . . ? O27 K2 C45 26.1(2) . . ? O19 K2 C45 161.6(7) . . ? O31 K2 C45 75.6(2) . . ? O20 K2 C45 81.9(2) . . ? C52 K2 C45 78.1(2) . . ? O30 K2 O17 149.7(2) . . ? O31 K2 O17 89.8(2) 2_666 . ? O18 K2 O17 40.01(18) . . ? O19' K2 O17 83.03(13) . . ? O27 K2 O17 95.01(17) . . ? O19 K2 O17 66.1(5) . . ? O31 K2 O17 164.20(19) . . ? O20 K2 O17 98.60(18) . . ? C52 K2 O17 168.3(2) . . ? C45 K2 O17 111.2(2) . . ? O30 K2 C33 146.7(2) . . ? O31 K2 C33 90.4(2) 2_666 . ? O18 K2 C33 19.8(2) . . ? O19' K2 C33 103.13(17) . . ? O27 K2 C33 75.4(2) . . ? O19 K2 C33 85.9(5) . . ? O31 K2 C33 161.3(2) . . ? O20 K2 C33 94.4(2) . . ? C52 K2 C33 165.7(2) . . ? C45 K2 C33 90.9(2) . . ? O17 K2 C33 20.36(18) . . ? C1 O1 Mn1 127.7(5) . . ? C7 O2 Mn1 132.5(6) . . ? C7 O2 K1 112.1(6) . . ? Mn1 O2 K1 115.1(3) . . ? C7 O3 K1 83.9(6) . . ? C9 O4 Mn1 114.2(5) . . ? C9 O4 Mn3 133.9(5) . 2_755 ? Mn1 O4 Mn3 104.8(3) . 2_755 ? C11 O5 Mn1 117.1(5) . . ? C11 O5 Mn2 132.8(5) . . ? Mn1 O5 Mn2 102.0(2) . . ? C11 O5 K1 94.3(5) . . ? Mn1 O5 K1 102.8(2) . . ? Mn2 O5 K1 102.0(2) . . ? C13 O6 H6 109.5 . . ? C27 O7 Mn2 122.9(5) . . ? C27 O7 Mn4 116.7(5) . . ? Mn2 O7 Mn4 96.3(2) . . ? C27 O7 Mn3 117.6(5) . . ? Mn2 O7 Mn3 103.3(2) . . ? Mn4 O7 Mn3 94.6(2) . . ? C15 O8 Mn4 114.5(5) . . ? C15 O8 Mn2 129.5(5) . . ? Mn4 O8 Mn2 103.2(2) . . ? C15 O8 K1 104.5(6) . . ? Mn4 O8 K1 100.8(2) . . ? Mn2 O8 K1 99.9(2) . . ? C30 O9 Mn2 125.7(5) . 2_755 ? C30 O9 Mn1 114.5(5) . 2_755 ? Mn2 O9 Mn1 94.9(2) 2_755 2_755 ? C30 O9 Mn3 116.8(4) . . ? Mn2 O9 Mn3 104.0(2) 2_755 . ? Mn1 O9 Mn3 94.8(2) 2_755 . ? C32 O10 Mn3 111.9(5) . . ? C32 O10 H10 119(6) . . ? Mn3 O10 H10 103(6) . . ? C17 O11 Mn4 111.9(5) . . ? C17 O11 Mn3 133.7(6) . . ? Mn4 O11 Mn3 106.4(3) . . ? C26 O12 Mn4 133.2(5) . . ? C26 O12 K1 109.0(5) . . ? Mn4 O12 K1 117.8(3) . . ? C20 O13 Mn4 129.0(5) . . ? C26 O14 K1 171.7(6) . 2_655 ? C26 O14 K1 87.8(5) . . ? K1 O14 K1 100.5(2) 2_655 . ? C19 O15 H15 109.5 . . ? C33 O17 K2 83.3(6) . . ? C33 O18 Mn8 133.0(6) . . ? C33 O18 K2 114.8(6) . . ? Mn8 O18 K2 112.2(3) . . ? C64 O20 Mn5 114.3(6) . . ? C64 O20 Mn7 127.2(6) . . ? Mn5 O20 Mn7 103.0(3) . . ? C64 O20 K2 110.6(6) . . ? Mn5 O20 K2 100.0(3) . . ? Mn7 O20 K2 97.4(2) . . ? C39 O21 Mn8 128.9(5) . . ? C46 O22 Mn7 126.1(5) . 2_566 ? C46 O22 Mn8 113.2(5) . 2_566 ? Mn7 O22 Mn8 95.5(2) 2_566 2_566 ? C46 O22 Mn6 117.4(5) . . ? Mn7 O22 Mn6 103.8(2) 2_566 . ? Mn8 O22 Mn6 94.6(2) 2_566 . ? C49 O23 Mn6 112.3(5) . . ? C49 O23 H23' 106(7) . . ? Mn6 O23 H23' 92(6) . . ? C51 O24 Mn7 122.4(5) . . ? C51 O24 Mn5 117.3(5) . . ? Mn7 O24 Mn5 96.0(2) . . ? C51 O24 Mn6 117.4(5) . . ? Mn7 O24 Mn6 103.4(2) . . ? Mn5 O24 Mn6 95.2(2) . . ? C40 O25 Mn8 114.1(5) . . ? C40 O25 Mn6 133.0(5) . 2_566 ? Mn8 O25 Mn6 106.0(3) . 2_566 ? C43 O26 H26 109.5 . . ? C45 O27 Mn8 117.0(5) . . ? C45 O27 Mn7 131.6(5) . . ? Mn8 O27 Mn7 102.9(3) . . ? C45 O27 K2 91.3(5) . . ? Mn8 O27 K2 104.7(2) . . ? Mn7 O27 K2 104.6(3) . . ? C59 O28 Mn5 111.2(5) . . ? C59 O28 Mn6 132.9(5) . . ? Mn5 O28 Mn6 107.8(3) . . ? C58 O29 Mn5 128.9(5) . . ? C52 O30 Mn5 132.2(6) . . ? C52 O30 K2 107.4(5) . . ? Mn5 O30 K2 120.3(3) . . ? C52 O31 K2 167.3(7) . 2_666 ? C52 O31 K2 88.2(6) . . ? K2 O31 K2 103.9(2) 2_666 . ? C62 O32 H32 109.5 . . ? C10 N1 C12 113.3(7) . . ? C10 N1 C8 114.4(7) . . ? C12 N1 C8 111.9(7) . . ? C10 N1 Mn1 99.9(5) . . ? C12 N1 Mn1 112.2(6) . . ? C8 N1 Mn1 104.0(6) . . ? N3 N2 Mn2 126.1(6) . . ? N3 N2 Mn2 122.4(5) . 2_755 ? Mn2 N2 Mn2 104.8(3) . 2_755 ? N3 N2 Mn3 108.2(5) . . ? Mn2 N2 Mn3 92.7(3) . . ? Mn2 N2 Mn3 92.8(2) 2_755 . ? N4 N3 N2 177.4(9) . . ? C18 N5 C14 112.9(7) . . ? C18 N5 C16 112.4(7) . . ? C14 N5 C16 113.9(8) . . ? C18 N5 Mn4 111.0(6) . . ? C14 N5 Mn4 101.2(5) . . ? C16 N5 Mn4 104.5(5) . . ? C29 N6 C28 111.2(7) . . ? C29 N6 C31 112.1(6) . . ? C28 N6 C31 111.3(6) . . ? C29 N6 Mn3 105.9(4) . . ? C28 N6 Mn3 106.3(5) . . ? C31 N6 Mn3 109.7(5) . . ? C42 N7 C41 112.1(8) . . ? C42 N7 C44 112.4(7) . . ? C41 N7 C44 114.9(7) . . ? C42 N7 Mn8 114.7(6) . . ? C41 N7 Mn8 103.5(6) . . ? C44 N7 Mn8 98.2(6) . . ? C48 N8 C47 111.5(6) . . ? C48 N8 C50 111.5(6) . . ? C47 N8 C50 111.2(7) . . ? C48 N8 Mn6 110.2(5) . . ? C47 N8 Mn6 106.8(5) . . ? C50 N8 Mn6 105.4(5) . . ? C63 N9 C60 115.3(9) . . ? C63 N9 C61 111.8(8) . . ? C60 N9 C61 114.0(8) . . ? C63 N9 Mn5 101.1(6) . . ? C60 N9 Mn5 102.0(5) . . ? C61 N9 Mn5 111.3(6) . . ? N11 N10 Mn7 127.2(6) . . ? N11 N10 Mn7 120.6(6) . 2_566 ? Mn7 N10 Mn7 105.2(3) . 2_566 ? N11 N10 Mn6 109.4(5) . . ? Mn7 N10 Mn6 92.6(3) . . ? Mn7 N10 Mn6 92.1(3) 2_566 . ? N12 N11 N10 178.5(9) . . ? O1 C1 C6 125.7(8) . . ? O1 C1 C2 116.0(9) . . ? C6 C1 C2 118.3(8) . . ? C1 C2 C3 120.3(10) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 119.9(9) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.0(10) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.7(10) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 120.8(9) . . ? C1 C6 C7 123.1(8) . . ? C5 C6 C7 116.1(8) . . ? O3 C7 O2 121.0(9) . . ? O3 C7 C6 121.1(9) . . ? O2 C7 C6 117.8(8) . . ? O3 C7 K1 74.9(6) . . ? O2 C7 K1 46.9(4) . . ? C6 C7 K1 160.5(6) . . ? N1 C8 C9 109.2(8) . . ? N1 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N1 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? O4 C9 C8 110.5(8) . . ? O4 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? O4 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N1 C10 C11 110.9(7) . . ? N1 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? O5 C11 C10 109.1(7) . . ? O5 C11 K1 61.1(5) . . ? C10 C11 K1 88.6(6) . . ? O5 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? K1 C11 H11A 64.2 . . ? O5 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? K1 C11 H11B 161.5 . . ? H11A C11 H11B 108.3 . . ? N1 C12 C13 118.2(8) . . ? N1 C12 H12A 107.8 . . ? C13 C12 H12A 107.8 . . ? N1 C12 H12B 107.8 . . ? C13 C12 H12B 107.8 . . ? H12A C12 H12B 107.1 . . ? O6 C13 C12 108.9(7) . . ? O6 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? O6 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N5 C14 C15 109.3(8) . . ? N5 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N5 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? O8 C15 C14 109.0(8) . . ? O8 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? O8 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N5 C16 C17 109.0(8) . . ? N5 C16 H16A 109.9 . . ? C17 C16 H16A 109.9 . . ? N5 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O11 C17 C16 108.8(8) . . ? O11 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? O11 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N5 C18 C19 115.8(8) . . ? N5 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? N5 C18 H18B 108.3 . . ? C19 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? O15 C19 C18 110.8(8) . . ? O15 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? O15 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? O13 C20 C25 124.9(8) . . ? O13 C20 C21 115.0(8) . . ? C25 C20 C21 120.1(8) . . ? C22 C21 C20 119.1(9) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 122.2(8) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C24 C23 C22 117.7(9) . . ? C24 C23 H23 121.1 . . ? C22 C23 H23 121.1 . . ? C23 C24 C25 122.5(9) . . ? C23 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C24 C25 C20 118.0(8) . . ? C24 C25 C26 119.1(8) . . ? C20 C25 C26 122.8(8) . . ? O14 C26 O12 119.2(7) . . ? O14 C26 C25 121.6(8) . . ? O12 C26 C25 119.1(7) . . ? O14 C26 K1 70.3(5) . . ? O12 C26 K1 49.3(4) . . ? C25 C26 K1 165.7(6) . . ? O7 C27 C28 112.0(7) . . ? O7 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? O7 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? N6 C28 C27 110.0(6) . . ? N6 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? N6 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? N6 C29 C30 111.6(7) . . ? N6 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N6 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? O9 C30 C29 110.5(7) . . ? O9 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? O9 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? N6 C31 C32 110.5(7) . . ? N6 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N6 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? O10 C32 C31 110.2(6) . . ? O10 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? O10 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? O17 C33 O18 120.8(9) . . ? O17 C33 C34 120.4(9) . . ? O18 C33 C34 118.7(8) . . ? O17 C33 K2 76.4(6) . . ? O18 C33 K2 45.4(4) . . ? C34 C33 K2 161.8(6) . . ? C35 C34 C39 120.5(8) . . ? C35 C34 C33 116.6(8) . . ? C39 C34 C33 122.8(8) . . ? C36 C35 C34 120.7(9) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C35 119.1(8) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C37 C38 121.9(9) . . ? C36 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C37 C38 C39 119.9(8) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? O21 C39 C34 125.1(8) . . ? O21 C39 C38 117.2(8) . . ? C34 C39 C38 117.7(8) . . ? O25 C40 C41 109.0(7) . . ? O25 C40 H40A 109.9 . . ? C41 C40 H40A 109.9 . . ? O25 C40 H40B 109.9 . . ? C41 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? N7 C41 C40 110.2(8) . . ? N7 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? N7 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? N7 C42 C43 118.1(9) . . ? N7 C42 H42A 107.8 . . ? C43 C42 H42A 107.8 . . ? N7 C42 H42B 107.8 . . ? C43 C42 H42B 107.8 . . ? H42A C42 H42B 107.1 . . ? O26 C43 C42 111.4(9) . . ? O26 C43 H43A 109.3 . . ? C42 C43 H43A 109.3 . . ? O26 C43 H43B 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C45 C44 N7 112.2(8) . . ? C45 C44 H44A 109.2 . . ? N7 C44 H44A 109.2 . . ? C45 C44 H44B 109.2 . . ? N7 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? O27 C45 C44 109.3(8) . . ? O27 C45 K2 62.6(5) . . ? C44 C45 K2 88.8(6) . . ? O27 C45 H45A 109.8 . . ? C44 C45 H45A 109.8 . . ? K2 C45 H45A 62.5 . . ? O27 C45 H45B 109.8 . . ? C44 C45 H45B 109.8 . . ? K2 C45 H45B 161.3 . . ? H45A C45 H45B 108.3 . . ? O22 C46 C47 110.3(7) . . ? O22 C46 H46A 109.6 . . ? C47 C46 H46A 109.6 . . ? O22 C46 H46B 109.6 . . ? C47 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? N8 C47 C46 110.2(7) . . ? N8 C47 H47A 109.6 . . ? C46 C47 H47A 109.6 . . ? N8 C47 H47B 109.6 . . ? C46 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? N8 C48 C49 111.0(7) . . ? N8 C48 H48A 109.4 . . ? C49 C48 H48A 109.4 . . ? N8 C48 H48B 109.4 . . ? C49 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? O23 C49 C48 110.4(7) . . ? O23 C49 H49A 109.6 . . ? C48 C49 H49A 109.6 . . ? O23 C49 H49B 109.6 . . ? C48 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? C51 C50 N8 110.7(6) . . ? C51 C50 H50A 109.5 . . ? N8 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? N8 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? O24 C51 C50 111.7(7) . . ? O24 C51 H51A 109.3 . . ? C50 C51 H51A 109.3 . . ? O24 C51 H51B 109.3 . . ? C50 C51 H51B 109.3 . . ? H51A C51 H51B 107.9 . . ? O31 C52 O30 119.5(9) . . ? O31 C52 C53 120.5(9) . . ? O30 C52 C53 120.0(8) . . ? O31 C52 K2 69.8(5) . . ? O30 C52 K2 50.5(4) . . ? C53 C52 K2 167.8(6) . . ? C54 C53 C58 118.8(8) . . ? C54 C53 C52 119.4(8) . . ? C58 C53 C52 121.7(8) . . ? C53 C54 C55 123.0(10) . . ? C53 C54 H54 118.5 . . ? C55 C54 H54 118.5 . . ? C56 C55 C54 117.9(10) . . ? C56 C55 H55 121.0 . . ? C54 C55 H55 121.0 . . ? C57 C56 C55 120.7(8) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 121.1(8) . . ? C56 C57 H57 119.5 . . ? C58 C57 H57 119.5 . . ? O29 C58 C57 116.3(8) . . ? O29 C58 C53 125.3(8) . . ? C57 C58 C53 118.4(8) . . ? O28 C59 C60 108.9(8) . . ? O28 C59 H59A 109.9 . . ? C60 C59 H59A 109.9 . . ? O28 C59 H59B 109.9 . . ? C60 C59 H59B 109.9 . . ? H59A C59 H59B 108.3 . . ? N9 C60 C59 113.7(8) . . ? N9 C60 H60A 108.8 . . ? C59 C60 H60A 108.8 . . ? N9 C60 H60B 108.8 . . ? C59 C60 H60B 108.8 . . ? H60A C60 H60B 107.7 . . ? N9 C61 C62 113.0(9) . . ? N9 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? N9 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? O32 C62 C61 106.3(12) . . ? O32 C62 H62A 110.5 . . ? C61 C62 H62A 110.5 . . ? O32 C62 H62B 110.5 . . ? C61 C62 H62B 110.5 . . ? H62A C62 H62B 108.7 . . ? N9 C63 C64 110.3(8) . . ? N9 C63 H63A 109.6 . . ? C64 C63 H63A 109.6 . . ? N9 C63 H63B 109.6 . . ? C64 C63 H63B 109.6 . . ? H63A C63 H63B 108.1 . . ? O20 C64 C63 111.2(10) . . ? O20 C64 H64A 109.4 . . ? C63 C64 H64A 109.4 . . ? O20 C64 H64B 109.4 . . ? C63 C64 H64B 109.4 . . ? H64A C64 H64B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 2.219 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.151