# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 loop_ _publ_author_name _publ_author_address 'Gao Song' '' 'Chang-Long Zhou' '' _publ_contact_author_name 'Gao Song' _publ_contact_author_email gaosong@pku.edu.cn data_Mn3-GaoSongPKU _database_code_depnum_ccdc_archive 'CCDC 885723' #TrackingRef '- Mn3-SongGaoPKU-New.cif' 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 -0.006 0.011 1513 259 2 0.500 -0.054 0.539 1513 259 _platon_squeeze_details ; The disordered solvent molecules cannot be modeled even with restraits and were treated by SQUEEZE,PLATON. A total 522e per unit cell were accumulated which corresponds to 130e per Mn3 formula. The 130e might come from n-Propanol solvents and are not included in the formula. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Mn3Na-tBuSao _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H158 Mn3 N6 Na O16' _chemical_formula_weight 1912.1 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 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 37.563(8) _cell_length_b 15.648(3) _cell_length_c 23.292(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.34(3) _cell_angle_gamma 90.00 _cell_volume 13068(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110.05(10) _cell_measurement_reflns_used 12544 _cell_measurement_theta_min 3.5959 _cell_measurement_theta_max 73.7717 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4074 _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.41939 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110.05(10) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5992 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25367 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.5959 _diffrn_reflns_theta_max 73.7717 _reflns_number_total 12827 _reflns_number_gt 10765 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1008P)^2^+47.0058P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00072(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12827 _refine_ls_number_parameters 628 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1873 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.054 _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 0.0000 0.10625(4) 0.2500 0.02222(17) Uani 1 2 d S . . Na1 Na 0.0000 0.32955(13) 0.2500 0.0564(7) Uani 1 2 d S . . O6 O 0.03099(5) 0.20564(13) 0.23350(10) 0.0233(4) Uani 1 1 d . A . C1 C 0.13734(7) -0.03888(17) 0.35168(13) 0.0182(5) Uani 1 1 d . . . Mn2 Mn 0.097803(11) 0.11113(3) 0.295237(19) 0.01873(14) Uani 1 1 d . A . O5 O 0.03037(5) 0.09457(14) 0.33186(10) 0.0237(4) Uani 1 1 d . . . C2 C 0.12196(8) 0.23444(18) 0.48295(13) 0.0210(6) Uani 1 1 d . . . H2 H 0.1074 0.2163 0.5078 0.025 Uiso 1 1 calc R . . O1 O 0.12433(5) 0.20906(12) 0.32836(9) 0.0183(4) Uani 1 1 d . A . C3 C 0.15889(8) 0.26601(19) 0.13544(13) 0.0233(6) Uani 1 1 d . . . O2 O 0.12702(5) 0.09005(12) 0.24477(9) 0.0193(4) Uani 1 1 d . . . C4 C 0.07844(8) 0.22945(18) 0.19470(13) 0.0208(6) Uani 1 1 d . A . H4 H 0.0626 0.2718 0.1709 0.025 Uiso 1 1 calc R . . O3 O 0.12654(5) 0.04056(12) 0.35636(9) 0.0187(4) Uani 1 1 d . . . C5 C 0.07645(7) 0.16509(18) 0.39950(13) 0.0194(5) Uani 1 1 d . . . H5 H 0.0607 0.1614 0.4246 0.023 Uiso 1 1 calc R A . O4 O 0.03255(6) 0.02087(14) 0.22139(11) 0.0299(5) Uani 1 1 d . . . N3 N 0.06609(6) 0.18789(15) 0.23225(11) 0.0186(5) Uani 1 1 d . . . C6 C 0.12841(8) -0.17675(19) 0.30051(14) 0.0237(6) Uani 1 1 d . . . H6 H 0.1141 -0.2124 0.2691 0.028 Uiso 1 1 calc R . . N2 N 0.06500(6) 0.13058(15) 0.34724(11) 0.0187(5) Uani 1 1 d . A . C7 C 0.08086(8) -0.06752(19) 0.26490(14) 0.0247(6) Uani 1 1 d . . . H7 H 0.0658 -0.1108 0.2409 0.030 Uiso 1 1 calc R A . C8 C 0.16303(7) 0.29287(17) 0.40754(13) 0.0188(5) Uani 1 1 d . A . C9 C 0.11647(8) -0.09277(18) 0.30484(13) 0.0210(6) Uani 1 1 d . A . O10 O 0.0097(3) 0.3650(5) 0.3405(4) 0.066(2) Uani 0.50 1 d P A 1 C10 C 0.17217(8) 0.31480(18) 0.46814(13) 0.0206(6) Uani 1 1 d . . . H10 H 0.1927 0.3521 0.4838 0.025 Uiso 1 1 calc R . . N1 N 0.06771(6) 0.00891(16) 0.25906(12) 0.0228(5) Uani 1 1 d . A . C11 C 0.11162(7) 0.20924(17) 0.42288(13) 0.0189(5) Uani 1 1 d . A . C12 C 0.13301(7) 0.23526(17) 0.38520(12) 0.0161(5) Uani 1 1 d . . . O13 O 0.0232(2) 0.4701(6) 0.2291(4) 0.170(3) Uiso 1 1 d D A . C13 C 0.13713(8) 0.14544(17) 0.20917(12) 0.0179(5) Uani 1 1 d . A . C14 C 0.17971(8) -0.15540(19) 0.38810(13) 0.0222(6) Uani 1 1 d . . . H14 H 0.2014 -0.1776 0.4166 0.027 Uiso 1 1 calc R . . C15 C 0.15315(8) 0.28563(18) 0.50752(13) 0.0212(6) Uani 1 1 d . . . C16 C 0.12589(8) 0.27594(19) 0.14916(13) 0.0224(6) Uani 1 1 d . A . H16 H 0.1104 0.3237 0.1335 0.027 Uiso 1 1 calc R . . C17 C 0.16999(8) 0.13036(18) 0.19259(13) 0.0203(6) Uani 1 1 d . . . C18 C 0.16920(7) -0.07204(18) 0.39599(13) 0.0191(5) Uani 1 1 d . . . C19 C 0.11451(8) 0.21687(18) 0.18585(12) 0.0196(6) Uani 1 1 d . . . C20 C 0.17984(8) 0.1917(2) 0.15717(13) 0.0236(6) Uani 1 1 d . . . H20 H 0.2022 0.1832 0.1468 0.028 Uiso 1 1 calc R . . C21 C 0.18961(8) -0.01897(18) 0.45170(13) 0.0220(6) Uani 1 1 d . . . C22 C 0.16036(8) -0.20890(19) 0.34072(14) 0.0232(6) Uani 1 1 d . . . C23 C 0.16273(9) 0.0003(2) 0.48817(14) 0.0291(7) Uani 1 1 d . . . H23A H 0.1413 0.0324 0.4632 0.044 Uiso 1 1 calc R . . H23B H 0.1756 0.0343 0.5236 0.044 Uiso 1 1 calc R . . H23C H 0.1541 -0.0534 0.5011 0.044 Uiso 1 1 calc R . . C24 C 0.20812(9) 0.0429(2) 0.28062(15) 0.0284(7) Uani 1 1 d . . . H24A H 0.2220 -0.0106 0.2920 0.043 Uiso 1 1 calc R . . H24B H 0.1874 0.0445 0.2980 0.043 Uiso 1 1 calc R . . H24C H 0.2248 0.0914 0.2957 0.043 Uiso 1 1 calc R . . C25 C 0.20286(9) 0.2610(2) 0.33977(16) 0.0294(7) Uani 1 1 d . A . H25A H 0.2153 0.2866 0.3125 0.044 Uiso 1 1 calc R . . H25B H 0.1841 0.2198 0.3176 0.044 Uiso 1 1 calc R . . H25C H 0.2213 0.2318 0.3726 0.044 Uiso 1 1 calc R . . C26 C 0.21366(10) 0.3954(2) 0.39912(17) 0.0358(8) Uani 1 1 d . A . H26A H 0.2328 0.3655 0.4306 0.054 Uiso 1 1 calc R . . H26B H 0.2023 0.4400 0.4174 0.054 Uiso 1 1 calc R . . H26C H 0.2251 0.4215 0.3706 0.054 Uiso 1 1 calc R . . C27 C 0.16501(9) 0.3075(2) 0.57486(14) 0.0252(6) Uani 1 1 d . . . C28 C 0.15585(10) 0.3804(2) 0.31439(15) 0.0298(7) Uani 1 1 d . A . H28A H 0.1692 0.4071 0.2888 0.045 Uiso 1 1 calc R . . H28B H 0.1434 0.4247 0.3312 0.045 Uiso 1 1 calc R . . H28C H 0.1372 0.3405 0.2903 0.045 Uiso 1 1 calc R . . C29 C 0.20475(8) 0.0647(2) 0.43323(14) 0.0268(6) Uani 1 1 d . . . H29A H 0.2237 0.0515 0.4133 0.040 Uiso 1 1 calc R . . H29B H 0.2160 0.0994 0.4691 0.040 Uiso 1 1 calc R . . H29C H 0.1843 0.0966 0.4055 0.040 Uiso 1 1 calc R . . C30 C 0.18367(8) 0.33163(19) 0.36589(14) 0.0227(6) Uani 1 1 d . . . C31 C 0.22313(9) -0.0674(2) 0.49294(14) 0.0286(7) Uani 1 1 d . . . H31A H 0.2145 -0.1205 0.5067 0.043 Uiso 1 1 calc R . . H31B H 0.2355 -0.0318 0.5278 0.043 Uiso 1 1 calc R . . H31C H 0.2408 -0.0809 0.4707 0.043 Uiso 1 1 calc R . . C32 C 0.22605(11) 0.0443(3) 0.18690(18) 0.0395(8) Uani 1 1 d . . . H32A H 0.2172 0.0494 0.1430 0.059 Uiso 1 1 calc R . . H32B H 0.2390 -0.0104 0.1980 0.059 Uiso 1 1 calc R . . H32C H 0.2432 0.0912 0.2037 0.059 Uiso 1 1 calc R . . C33 C 0.19281(8) 0.0482(2) 0.21192(14) 0.0253(6) Uani 1 1 d . . . C34 C 0.16824(10) -0.0299(2) 0.18820(17) 0.0342(7) Uani 1 1 d . . . H34A H 0.1589 -0.0273 0.1442 0.051 Uiso 1 1 calc R . . H34B H 0.1471 -0.0302 0.2048 0.051 Uiso 1 1 calc R . . H34C H 0.1830 -0.0821 0.2004 0.051 Uiso 1 1 calc R . . C35 C 0.14440(11) 0.4003(3) 0.0719(2) 0.0441(9) Uani 1 1 d . . . H35A H 0.1535 0.4371 0.0452 0.066 Uiso 1 1 calc R . . H35B H 0.1399 0.4349 0.1041 0.066 Uiso 1 1 calc R . . H35C H 0.1211 0.3726 0.0488 0.066 Uiso 1 1 calc R . . C36 C 0.19748(10) 0.3715(2) 0.59173(16) 0.0338(7) Uani 1 1 d . . . H36A H 0.2040 0.3844 0.6348 0.051 Uiso 1 1 calc R . . H36B H 0.1900 0.4242 0.5685 0.051 Uiso 1 1 calc R . . H36C H 0.2191 0.3466 0.5826 0.051 Uiso 1 1 calc R . . C37 C 0.17368(9) 0.3320(2) 0.09935(16) 0.0300(7) Uani 1 1 d . . . C38 C 0.20838(11) 0.3757(2) 0.14195(19) 0.0415(9) Uani 1 1 d . . . H38A H 0.2191 0.4151 0.1189 0.062 Uiso 1 1 calc R . . H38B H 0.2269 0.3322 0.1611 0.062 Uiso 1 1 calc R . . H38C H 0.2012 0.4076 0.1730 0.062 Uiso 1 1 calc R . . C39 C 0.17243(10) -0.3016(2) 0.33527(16) 0.0328(7) Uani 1 1 d . . . C40 C 0.20944(11) -0.3241(2) 0.38162(17) 0.0380(8) Uani 1 1 d . . . H40A H 0.2151 -0.3846 0.3777 0.057 Uiso 1 1 calc R . . H40B H 0.2077 -0.3134 0.4221 0.057 Uiso 1 1 calc R . . H40C H 0.2293 -0.2888 0.3748 0.057 Uiso 1 1 calc R . . C41 C 0.18474(11) 0.2881(3) 0.04859(17) 0.0407(8) Uani 1 1 d . . . H41A H 0.1631 0.2577 0.0225 0.061 Uiso 1 1 calc R . . H41B H 0.2049 0.2474 0.0657 0.061 Uiso 1 1 calc R . . H41C H 0.1932 0.3311 0.0250 0.061 Uiso 1 1 calc R . . C42 C 0.17756(13) 0.2262(3) 0.61081(17) 0.0469(10) Uani 1 1 d . . . H42A H 0.1855 0.2397 0.6538 0.070 Uiso 1 1 calc R . . H42B H 0.1984 0.2010 0.5997 0.070 Uiso 1 1 calc R . . H42C H 0.1568 0.1855 0.6021 0.070 Uiso 1 1 calc R . . C43 C 0.13223(10) 0.3478(3) 0.59125(17) 0.0377(8) Uani 1 1 d . . . H43A H 0.1111 0.3080 0.5813 0.057 Uiso 1 1 calc R . . H43B H 0.1249 0.4009 0.5686 0.057 Uiso 1 1 calc R . . H43C H 0.1397 0.3602 0.6344 0.057 Uiso 1 1 calc R . . C44 C 0.14289(14) -0.3608(3) 0.3488(3) 0.0683(16) Uani 1 1 d . . . H44A H 0.1186 -0.3509 0.3190 0.102 Uiso 1 1 calc R . . H44B H 0.1412 -0.3485 0.3891 0.102 Uiso 1 1 calc R . . H44C H 0.1502 -0.4206 0.3468 0.102 Uiso 1 1 calc R . . C45 C 0.17586(18) -0.3171(4) 0.2738(2) 0.078(2) Uani 1 1 d . . . H45A H 0.1979 -0.2873 0.2697 0.118 Uiso 1 1 calc R . . H45B H 0.1536 -0.2955 0.2436 0.118 Uiso 1 1 calc R . . H45C H 0.1783 -0.3785 0.2678 0.118 Uiso 1 1 calc R . . C46 C 0.06823(16) 0.4217(4) 0.3861(3) 0.0804(17) Uani 1 1 d . . . H46A H 0.0750 0.4180 0.3482 0.096 Uiso 1 1 calc R B 1 H46B H 0.0744 0.3663 0.4073 0.096 Uiso 1 1 calc R B 1 C47 C 0.09153(18) 0.4953(4) 0.4267(3) 0.0829(18) Uani 1 1 d . . . H47A H 0.0746 0.5400 0.4322 0.124 Uiso 1 1 calc R . . H47B H 0.1090 0.5197 0.4071 0.124 Uiso 1 1 calc R . . H47C H 0.1055 0.4718 0.4660 0.124 Uiso 1 1 calc R . . C48 C 0.0427(2) 0.3855(5) 0.4072(4) 0.0465(19) Uani 0.50 1 d P A 2 H48A H 0.0268 0.4307 0.4165 0.056 Uiso 0.50 1 calc PR A 2 H48B H 0.0553 0.3553 0.4451 0.056 Uiso 0.50 1 calc PR A 2 O11 O 0.0196(2) 0.3262(4) 0.3656(3) 0.0506(16) Uani 0.50 1 d P A 2 C49 C 0.0585(3) 0.5266(8) 0.2268(6) 0.091(3) Uiso 0.60 1 d PD A 1 H49A H 0.0794 0.5243 0.2646 0.109 Uiso 0.60 1 calc PR A 1 H49B H 0.0674 0.5131 0.1919 0.109 Uiso 0.60 1 calc PR A 1 C50 C 0.0129(3) 0.6076(5) 0.2589(6) 0.074(3) Uani 0.60 1 d PD . 1 C52 C 0.0363(3) 0.6099(7) 0.2193(6) 0.098(4) Uani 0.60 1 d PD A 1 H52A H 0.0536 0.6592 0.2296 0.118 Uiso 0.60 1 calc PR A 1 H52B H 0.0207 0.6163 0.1770 0.118 Uiso 0.60 1 calc PR A 1 C53 C 0.0288(3) 0.4374(8) 0.3725(6) 0.072(3) Uani 0.50 1 d P A 1 H53A H 0.0221 0.4458 0.4101 0.086 Uiso 0.50 1 calc PR A 1 H53B H 0.0218 0.4896 0.3476 0.086 Uiso 0.50 1 calc PR A 1 C51 C 0.0799(5) 0.5178(10) 0.1840(7) 0.079(5) Uani 0.40 1 d PD A 2 H51A H 0.1058 0.5368 0.2040 0.095 Uiso 0.40 1 calc PR A 2 H51B H 0.0797 0.4795 0.1500 0.095 Uiso 0.40 1 calc PR A 2 C54 C 0.0637(3) 0.4770(9) 0.2259(10) 0.127(11) Uani 0.40 1 d PD A 2 H54A H 0.0777 0.5015 0.2654 0.153 Uiso 0.40 1 calc PR A 2 H54B H 0.0720 0.4169 0.2270 0.153 Uiso 0.40 1 calc PR A 2 C55 C 0.0548(9) 0.590(2) 0.1643(17) 0.181(13) Uiso 0.40 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0098(3) 0.0172(3) 0.0330(4) 0.000 -0.0037(2) 0.000 Na1 0.0210(9) 0.0176(9) 0.126(2) 0.000 0.0147(12) 0.000 O6 0.0100(9) 0.0225(10) 0.0345(11) 0.0050(9) 0.0021(8) 0.0043(7) C1 0.0121(12) 0.0155(12) 0.0246(14) 0.0022(11) 0.0014(10) -0.0021(10) Mn2 0.0113(2) 0.0168(2) 0.0234(2) 0.00135(16) -0.00205(16) -0.00107(15) O5 0.0075(8) 0.0253(10) 0.0310(11) 0.0050(9) -0.0054(8) -0.0081(8) C2 0.0158(12) 0.0194(13) 0.0263(14) 0.0011(11) 0.0041(11) -0.0008(10) O1 0.0135(9) 0.0151(9) 0.0238(10) -0.0004(8) 0.0020(7) -0.0030(7) C3 0.0231(14) 0.0205(14) 0.0241(14) -0.0013(11) 0.0037(11) -0.0007(11) O2 0.0154(9) 0.0149(9) 0.0247(10) 0.0016(8) 0.0013(8) 0.0019(7) C4 0.0177(13) 0.0158(13) 0.0244(14) 0.0047(11) -0.0005(11) 0.0042(10) O3 0.0120(8) 0.0137(9) 0.0242(10) 0.0014(8) -0.0042(7) -0.0006(7) C5 0.0114(12) 0.0190(13) 0.0257(14) 0.0016(11) 0.0023(10) -0.0028(10) O4 0.0122(9) 0.0226(11) 0.0394(13) 0.0019(9) -0.0162(9) -0.0017(8) N3 0.0090(10) 0.0179(11) 0.0238(12) -0.0003(9) -0.0030(8) 0.0030(8) C6 0.0225(14) 0.0179(13) 0.0253(14) -0.0007(11) -0.0011(11) -0.0026(11) N2 0.0076(10) 0.0177(11) 0.0281(12) 0.0024(10) 0.0013(9) -0.0047(8) C7 0.0179(13) 0.0179(13) 0.0302(15) 0.0020(12) -0.0056(11) -0.0046(11) C8 0.0146(12) 0.0142(12) 0.0248(14) 0.0003(10) 0.0018(10) -0.0008(10) C9 0.0154(13) 0.0177(13) 0.0239(14) 0.0035(11) -0.0031(11) -0.0027(10) O10 0.087(6) 0.043(4) 0.058(5) -0.018(4) 0.004(4) -0.011(4) C10 0.0150(12) 0.0154(12) 0.0283(15) -0.0022(11) 0.0019(11) -0.0026(10) N1 0.0095(10) 0.0199(12) 0.0304(13) 0.0045(10) -0.0072(9) -0.0028(9) C11 0.0111(12) 0.0154(12) 0.0265(14) -0.0007(11) 0.0000(10) -0.0016(10) C12 0.0105(11) 0.0143(12) 0.0200(13) 0.0007(10) -0.0008(10) 0.0009(9) C13 0.0183(13) 0.0159(13) 0.0164(12) -0.0017(10) 0.0006(10) -0.0006(10) C14 0.0167(13) 0.0220(14) 0.0240(14) 0.0064(11) 0.0001(11) 0.0019(11) C15 0.0187(13) 0.0182(13) 0.0226(14) -0.0021(11) -0.0002(11) -0.0001(10) C16 0.0214(14) 0.0179(13) 0.0248(14) 0.0037(11) 0.0022(11) 0.0019(11) C17 0.0174(13) 0.0182(13) 0.0224(14) -0.0027(11) 0.0016(10) 0.0036(10) C18 0.0121(12) 0.0190(13) 0.0235(14) 0.0053(11) 0.0011(10) -0.0020(10) C19 0.0176(13) 0.0189(13) 0.0194(13) 0.0002(11) 0.0009(10) 0.0023(10) C20 0.0207(14) 0.0255(15) 0.0239(14) 0.0000(12) 0.0055(11) 0.0019(11) C21 0.0170(13) 0.0190(13) 0.0244(14) 0.0036(11) -0.0022(11) -0.0002(11) C22 0.0222(14) 0.0174(13) 0.0266(15) 0.0033(11) 0.0021(11) 0.0036(11) C23 0.0287(16) 0.0303(16) 0.0260(15) -0.0003(13) 0.0046(12) 0.0008(13) C24 0.0233(14) 0.0269(15) 0.0330(17) 0.0037(13) 0.0053(12) 0.0084(12) C25 0.0198(14) 0.0307(16) 0.0393(18) -0.0019(14) 0.0112(13) -0.0023(12) C26 0.0337(18) 0.0382(19) 0.0367(18) -0.0084(15) 0.0124(15) -0.0230(15) C27 0.0273(15) 0.0226(14) 0.0233(15) -0.0022(12) 0.0038(12) -0.0036(12) C28 0.0362(17) 0.0190(14) 0.0348(17) 0.0020(13) 0.0115(14) -0.0054(13) C29 0.0203(14) 0.0235(15) 0.0277(15) 0.0031(12) -0.0063(11) -0.0070(11) C30 0.0186(13) 0.0205(14) 0.0284(15) -0.0046(12) 0.0063(11) -0.0084(11) C31 0.0227(14) 0.0266(15) 0.0265(15) 0.0042(13) -0.0083(12) 0.0000(12) C32 0.0374(19) 0.0379(19) 0.049(2) 0.0096(16) 0.0221(17) 0.0197(16) C33 0.0240(14) 0.0215(14) 0.0311(16) 0.0008(12) 0.0092(12) 0.0081(12) C34 0.0388(18) 0.0213(15) 0.0391(18) -0.0051(14) 0.0065(15) 0.0070(13) C35 0.040(2) 0.0343(19) 0.060(3) 0.0228(18) 0.0187(18) 0.0062(16) C36 0.0286(16) 0.0364(18) 0.0310(17) -0.0090(14) 0.0004(13) -0.0083(14) C37 0.0254(15) 0.0261(16) 0.0390(18) 0.0056(14) 0.0103(13) 0.0005(13) C38 0.0371(19) 0.0336(18) 0.052(2) 0.0042(17) 0.0096(17) -0.0104(15) C39 0.0313(17) 0.0229(16) 0.0363(18) -0.0018(13) -0.0018(14) 0.0097(13) C40 0.0406(19) 0.0307(18) 0.0380(19) 0.0037(15) 0.0046(15) 0.0168(15) C41 0.042(2) 0.044(2) 0.040(2) 0.0107(16) 0.0179(16) 0.0014(16) C42 0.069(3) 0.0311(19) 0.0294(18) 0.0036(15) -0.0030(18) -0.0034(18) C43 0.0345(18) 0.042(2) 0.0392(19) -0.0143(16) 0.0158(15) -0.0093(15) C44 0.049(3) 0.0194(18) 0.130(5) 0.000(2) 0.017(3) 0.0000(17) C45 0.109(5) 0.072(3) 0.041(2) -0.008(2) 0.001(3) 0.063(3) C46 0.058(3) 0.074(4) 0.108(5) -0.003(4) 0.024(3) 0.014(3) C47 0.074(4) 0.082(4) 0.084(4) -0.005(3) 0.010(3) -0.030(3) C48 0.039(4) 0.036(4) 0.060(5) 0.001(4) 0.009(4) -0.003(3) O11 0.059(4) 0.032(3) 0.048(4) -0.009(3) -0.003(3) -0.005(3) C50 0.073(6) 0.037(4) 0.125(9) 0.016(5) 0.049(8) -0.002(3) C52 0.098(9) 0.062(6) 0.124(10) 0.026(6) 0.016(7) -0.026(6) C53 0.068(7) 0.060(6) 0.082(8) -0.017(6) 0.013(6) 0.007(5) C51 0.121(13) 0.073(9) 0.072(9) 0.019(7) 0.071(9) 0.010(9) C54 0.028(6) 0.036(7) 0.28(3) -0.002(11) -0.007(10) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 1.917(2) . ? Mn1 O5 1.917(2) 2 ? Mn1 O6 2.047(2) 2 ? Mn1 O6 2.047(2) . ? Mn1 O4 2.052(2) . ? Mn1 O4 2.052(2) 2 ? Mn1 Na1 3.494(2) . ? Na1 O10 2.104(8) . ? Na1 O10 2.104(8) 2 ? Na1 O6 2.351(3) 2 ? Na1 O6 2.351(3) . ? Na1 O13 2.468(9) 2 ? Na1 O13 2.468(9) . ? Na1 O11 2.571(7) . ? Na1 O11 2.571(7) 2 ? O6 N3 1.356(3) . ? C1 O3 1.322(3) . ? C1 C9 1.416(4) . ? C1 C18 1.425(4) . ? Mn2 O2 1.861(2) . ? Mn2 O1 1.8649(19) . ? Mn2 O3 1.870(2) . ? Mn2 N2 1.992(2) . ? Mn2 N3 1.993(2) . ? Mn2 N1 1.995(2) . ? O5 N2 1.364(3) . ? C2 C11 1.393(4) . ? C2 C15 1.393(4) . ? O1 C12 1.330(3) . ? C3 C16 1.378(4) . ? C3 C20 1.410(4) . ? C3 C37 1.536(4) . ? O2 C13 1.331(3) . ? C4 N3 1.283(4) . ? C4 C19 1.443(4) . ? C5 N2 1.283(4) . ? C5 C11 1.446(4) . ? O4 N1 1.363(3) . ? C6 C22 1.378(4) . ? C6 C9 1.402(4) . ? C7 N1 1.286(4) . ? C7 C9 1.438(4) . ? C8 C10 1.392(4) . ? C8 C12 1.416(4) . ? C8 C30 1.536(4) . ? O10 C53 1.426(13) . ? C10 C15 1.397(4) . ? C11 C12 1.415(4) . ? O13 C54 1.546(15) . ? O13 C49 1.607(12) . ? C13 C19 1.411(4) . ? C13 C17 1.419(4) . ? C14 C18 1.391(4) . ? C14 C22 1.403(4) . ? C15 C27 1.536(4) . ? C16 C19 1.409(4) . ? C17 C20 1.386(4) . ? C17 C33 1.536(4) . ? C18 C21 1.539(4) . ? C21 C23 1.531(4) . ? C21 C31 1.537(4) . ? C21 C29 1.540(4) . ? C22 C39 1.537(4) . ? C24 C33 1.533(4) . ? C25 C30 1.540(4) . ? C26 C30 1.531(4) . ? C27 C42 1.518(5) . ? C27 C43 1.530(5) . ? C27 C36 1.536(4) . ? C28 C30 1.538(5) . ? C32 C33 1.528(4) . ? C33 C34 1.532(5) . ? C35 C37 1.530(5) . ? C37 C41 1.528(5) . ? C37 C38 1.543(5) . ? C39 C45 1.495(6) . ? C39 C40 1.525(5) . ? C39 C44 1.548(6) . ? C46 C48 1.328(11) . ? C46 C53 1.441(13) . ? C46 C47 1.579(9) . ? C48 O11 1.433(10) . ? C49 C52 1.529(13) . ? C50 C50 0.93(2) 2 ? C50 C52 1.454(13) . ? C51 C55 1.454(18) . ? C51 C54 1.447(16) . ? 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 O5 Mn1 O5 169.06(13) . 2 ? O5 Mn1 O6 95.10(9) . 2 ? O5 Mn1 O6 93.21(8) 2 2 ? O5 Mn1 O6 93.21(9) . . ? O5 Mn1 O6 95.10(9) 2 . ? O6 Mn1 O6 81.08(12) 2 . ? O5 Mn1 O4 91.46(9) . . ? O5 Mn1 O4 81.40(8) 2 . ? O6 Mn1 O4 169.49(9) 2 . ? O6 Mn1 O4 90.37(9) . . ? O5 Mn1 O4 81.40(8) . 2 ? O5 Mn1 O4 91.46(9) 2 2 ? O6 Mn1 O4 90.37(9) 2 2 ? O6 Mn1 O4 169.49(9) . 2 ? O4 Mn1 O4 98.74(13) . 2 ? O5 Mn1 Na1 95.47(7) . . ? O5 Mn1 Na1 95.47(7) 2 . ? O6 Mn1 Na1 40.54(6) 2 . ? O6 Mn1 Na1 40.54(6) . . ? O4 Mn1 Na1 130.63(7) . . ? O4 Mn1 Na1 130.63(7) 2 . ? O10 Na1 O10 149.5(5) . 2 ? O10 Na1 O6 90.0(2) . 2 ? O10 Na1 O6 115.7(3) 2 2 ? O10 Na1 O6 115.7(3) . . ? O10 Na1 O6 90.0(2) 2 . ? O6 Na1 O6 68.90(11) 2 . ? O10 Na1 O13 62.2(3) . 2 ? O10 Na1 O13 89.8(3) 2 2 ? O6 Na1 O13 118.8(2) 2 2 ? O6 Na1 O13 171.3(2) . 2 ? O10 Na1 O13 89.8(3) . . ? O10 Na1 O13 62.2(3) 2 . ? O6 Na1 O13 171.3(2) 2 . ? O6 Na1 O13 118.8(2) . . ? O13 Na1 O13 53.9(4) 2 . ? O10 Na1 O11 17.5(2) . . ? O10 Na1 O11 164.7(3) 2 . ? O6 Na1 O11 79.21(16) 2 . ? O6 Na1 O11 98.82(17) . . ? O13 Na1 O11 79.6(3) 2 . ? O13 Na1 O11 102.6(3) . . ? O10 Na1 O11 164.7(3) . 2 ? O10 Na1 O11 17.5(2) 2 2 ? O6 Na1 O11 98.82(17) 2 2 ? O6 Na1 O11 79.21(16) . 2 ? O13 Na1 O11 102.6(3) 2 2 ? O13 Na1 O11 79.6(3) . 2 ? O11 Na1 O11 177.6(3) . 2 ? O10 Na1 Mn1 105.3(2) . . ? O10 Na1 Mn1 105.3(2) 2 . ? O6 Na1 Mn1 34.45(6) 2 . ? O6 Na1 Mn1 34.45(6) . . ? O13 Na1 Mn1 153.0(2) 2 . ? O13 Na1 Mn1 153.0(2) . . ? O11 Na1 Mn1 88.82(16) . . ? O11 Na1 Mn1 88.82(16) 2 . ? N3 O6 Mn1 117.35(16) . . ? N3 O6 Na1 134.77(17) . . ? Mn1 O6 Na1 105.01(9) . . ? O3 C1 C9 120.7(2) . . ? O3 C1 C18 119.7(2) . . ? C9 C1 C18 119.6(3) . . ? O2 Mn2 O1 93.67(9) . . ? O2 Mn2 O3 93.49(9) . . ? O1 Mn2 O3 93.11(9) . . ? O2 Mn2 N2 177.72(9) . . ? O1 Mn2 N2 88.51(9) . . ? O3 Mn2 N2 87.06(9) . . ? O2 Mn2 N3 88.71(9) . . ? O1 Mn2 N3 86.43(9) . . ? O3 Mn2 N3 177.78(10) . . ? N2 Mn2 N3 90.75(10) . . ? O2 Mn2 N1 87.57(10) . . ? O1 Mn2 N1 177.89(9) . . ? O3 Mn2 N1 88.51(9) . . ? N2 Mn2 N1 90.23(10) . . ? N3 Mn2 N1 91.90(10) . . ? N2 O5 Mn1 117.40(17) . . ? C11 C2 C15 121.6(3) . . ? C12 O1 Mn2 127.38(17) . . ? C16 C3 C20 117.0(3) . . ? C16 C3 C37 123.2(3) . . ? C20 C3 C37 119.7(3) . . ? C13 O2 Mn2 127.56(18) . . ? N3 C4 C19 125.0(3) . . ? C1 O3 Mn2 127.90(18) . . ? N2 C5 C11 124.7(3) . . ? N1 O4 Mn1 115.93(18) . . ? C4 N3 O6 117.5(2) . . ? C4 N3 Mn2 123.30(19) . . ? O6 N3 Mn2 118.64(18) . . ? C22 C6 C9 121.7(3) . . ? C5 N2 O5 116.6(2) . . ? C5 N2 Mn2 123.21(18) . . ? O5 N2 Mn2 119.44(18) . . ? N1 C7 C9 125.3(3) . . ? C10 C8 C12 117.3(3) . . ? C10 C8 C30 121.6(2) . . ? C12 C8 C30 121.1(3) . . ? C6 C9 C1 119.9(3) . . ? C6 C9 C7 117.8(3) . . ? C1 C9 C7 121.9(3) . . ? C53 O10 Na1 130.0(8) . . ? C8 C10 C15 124.4(3) . . ? C7 N1 O4 117.6(2) . . ? C7 N1 Mn2 123.35(19) . . ? O4 N1 Mn2 118.69(18) . . ? C2 C11 C12 120.1(2) . . ? C2 C11 C5 117.6(3) . . ? C12 C11 C5 121.9(3) . . ? O1 C12 C11 120.8(2) . . ? O1 C12 C8 119.6(2) . . ? C11 C12 C8 119.5(3) . . ? C54 O13 C49 29.4(6) . . ? C54 O13 Na1 118.8(7) . . ? C49 O13 Na1 147.2(7) . . ? O2 C13 C19 120.3(2) . . ? O2 C13 C17 119.6(2) . . ? C19 C13 C17 120.0(3) . . ? C18 C14 C22 124.2(3) . . ? C2 C15 C10 116.8(3) . . ? C2 C15 C27 120.0(3) . . ? C10 C15 C27 123.2(3) . . ? C3 C16 C19 121.5(3) . . ? C20 C17 C13 117.1(3) . . ? C20 C17 C33 122.0(3) . . ? C13 C17 C33 120.9(3) . . ? C14 C18 C1 117.1(3) . . ? C14 C18 C21 121.9(2) . . ? C1 C18 C21 120.9(3) . . ? C16 C19 C13 119.8(3) . . ? C16 C19 C4 117.7(3) . . ? C13 C19 C4 122.4(3) . . ? C17 C20 C3 124.4(3) . . ? C23 C21 C31 107.7(3) . . ? C23 C21 C18 109.2(2) . . ? C31 C21 C18 111.7(2) . . ? C23 C21 C29 110.3(3) . . ? C31 C21 C29 107.0(2) . . ? C18 C21 C29 110.9(2) . . ? C6 C22 C14 117.3(3) . . ? C6 C22 C39 120.5(3) . . ? C14 C22 C39 122.1(3) . . ? C42 C27 C43 110.4(3) . . ? C42 C27 C15 108.9(3) . . ? C43 C27 C15 109.7(3) . . ? C42 C27 C36 108.2(3) . . ? C43 C27 C36 107.7(3) . . ? C15 C27 C36 111.9(3) . . ? C26 C30 C8 111.8(3) . . ? C26 C30 C28 107.3(3) . . ? C8 C30 C28 109.6(2) . . ? C26 C30 C25 107.9(3) . . ? C8 C30 C25 110.5(2) . . ? C28 C30 C25 109.7(3) . . ? C32 C33 C34 107.6(3) . . ? C32 C33 C24 107.5(3) . . ? C34 C33 C24 109.3(3) . . ? C32 C33 C17 111.7(3) . . ? C34 C33 C17 109.8(3) . . ? C24 C33 C17 110.8(2) . . ? C41 C37 C35 108.5(3) . . ? C41 C37 C3 110.3(3) . . ? C35 C37 C3 111.5(3) . . ? C41 C37 C38 108.9(3) . . ? C35 C37 C38 108.9(3) . . ? C3 C37 C38 108.7(3) . . ? C45 C39 C40 108.7(3) . . ? C45 C39 C22 110.1(3) . . ? C40 C39 C22 112.9(3) . . ? C45 C39 C44 111.7(4) . . ? C40 C39 C44 106.0(3) . . ? C22 C39 C44 107.5(3) . . ? C48 C46 C53 49.1(7) . . ? C48 C46 C47 114.9(7) . . ? C53 C46 C47 110.9(6) . . ? C46 C48 O11 112.6(8) . . ? C48 O11 Na1 128.4(6) . . ? C52 C49 O13 92.6(8) . . ? C50 C50 C52 117.4(19) 2 . ? C50 C52 C49 108.7(9) . . ? O10 C53 C46 107.6(9) . . ? C55 C51 C54 100.9(18) . . ? C51 C54 O13 133.0(14) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 73.91 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.822 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.091