# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Shaowu Du' _publ_contact_author_email swdu@fjirsm.ac.cn loop_ _publ_author_name 'Shaowu Du' 'Chong-Bin Tian' 'Zhang-Zhen He' 'Ping Lin' 'Zhi-Hua Li' data_MN1 _database_code_depnum_ccdc_archive 'CCDC 763951' #TrackingRef '- cif data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H60 Cl0 Mn4 N0 O20' _chemical_formula_weight 1200.74 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' Cl Cl 0.1484 0.1585 '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 11.6608(6) _cell_length_b 39.3981(19) _cell_length_c 24.4617(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.297(3) _cell_angle_gamma 90.00 _cell_volume 11020.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13236 _cell_measurement_theta_min 3.1022 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.5000 _exptl_crystal_size_mid 0.5000 _exptl_crystal_size_min 0.4500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4960 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8392 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40296 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12506 _reflns_number_gt 11292 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1146P)^2^+46.9673P] 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 12506 _refine_ls_number_parameters 698 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1828 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.003 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 0.5000 0.209126(16) 0.2500 0.02520(16) Uani 1 2 d S . . Mn2 Mn 0.80595(4) 0.119682(11) 0.380486(18) 0.02555(13) Uani 1 1 d . . . Mn3 Mn 0.88221(5) 0.041689(12) 0.367143(19) 0.02932(14) Uani 1 1 d . . . Mn4 Mn 1.0000 0.031295(17) 0.2500 0.03150(18) Uani 1 2 d S . . Mn5 Mn 0.72126(5) 0.198828(12) 0.37166(2) 0.02932(14) Uani 1 1 d . . . O1 O 0.8967(3) 0.26470(8) 0.61939(13) 0.0584(9) Uani 1 1 d . . . O2 O 1.0272(3) 0.25014(6) 0.69456(10) 0.0391(6) Uani 1 1 d . . . O3 O 0.8051(3) 0.19542(7) 0.45524(12) 0.0529(8) Uani 1 1 d . . . O4 O 0.8939(3) 0.14618(8) 0.45039(11) 0.0439(7) Uani 1 1 d . . . O5 O 1.0730(3) -0.03809(8) 0.54371(11) 0.0502(7) Uani 1 1 d . . . O6 O 1.2097(3) -0.07624(7) 0.56804(11) 0.0446(7) Uani 1 1 d . . . O7 O 0.9852(3) 0.00269(7) 0.34502(13) 0.0489(7) Uani 1 1 d . . . O8 O 1.1120(3) -0.00935(7) 0.29322(10) 0.0422(6) Uani 1 1 d . . . O9 O 0.7251(2) 0.08861(7) 0.31203(10) 0.0382(6) Uani 1 1 d . . . O10 O 0.8122(2) 0.04608(6) 0.27750(10) 0.0332(5) Uani 1 1 d . . . O11 O 0.4891(3) 0.17008(6) 0.18741(11) 0.0413(6) Uani 1 1 d . . . O12 O 0.3602(2) 0.14776(6) 0.11880(10) 0.0319(5) Uani 1 1 d . . . O13 O 1.0328(2) 0.09313(6) 0.13117(10) 0.0292(5) Uani 1 1 d . . . O14 O 0.9403(2) 0.07162(6) 0.19403(11) 0.0366(6) Uani 1 1 d . . . O15 O 0.6978(2) 0.20151(6) 0.27462(10) 0.0332(5) Uani 1 1 d . . . O16 O 0.8164(2) 0.16264(6) 0.31899(10) 0.0353(5) Uani 1 1 d . . . O17 O 0.8464(5) 0.24019(12) 0.3639(2) 0.0899(14) Uani 1 1 d . . . H17 H 0.8725 0.2414 0.3304 0.108 Uiso 1 1 calc R . . O18 O 0.7401(4) 0.00511(11) 0.36331(17) 0.0754(12) Uani 1 1 d . . . H18 H 0.6992 0.0006 0.3275 0.090 Uiso 1 1 calc R . . O19 O 0.2526(15) 0.2774(3) 0.2367(5) 0.356(12) Uani 1 1 d . . . O20 O 0.7067(6) -0.02938(15) 0.2623(3) 0.117(2) Uani 1 1 d . . . C1 C 0.9708(3) 0.24458(8) 0.64644(14) 0.0313(7) Uani 1 1 d . . . C2 C 0.8740(3) 0.17244(9) 0.47573(13) 0.0319(7) Uani 1 1 d . . . C3 C 1.1433(4) -0.05864(9) 0.53116(14) 0.0375(8) Uani 1 1 d . . . C4 C 1.0704(3) -0.01423(8) 0.33633(13) 0.0313(7) Uani 1 1 d . . . C5 C 0.7402(3) 0.07051(8) 0.27158(13) 0.0282(6) Uani 1 1 d . . . C6 C 0.4553(3) 0.14625(8) 0.15482(13) 0.0282(6) Uani 1 1 d . . . C7 C 0.9613(3) 0.09543(8) 0.16444(12) 0.0264(6) Uani 1 1 d . . . C8 C 0.7685(3) 0.17714(8) 0.27402(13) 0.0280(6) Uani 1 1 d . . . C9 C 0.9895(3) 0.21236(8) 0.61632(13) 0.0273(6) Uani 1 1 d . . . C10 C 1.0668(3) 0.18746(9) 0.64151(14) 0.0332(7) Uani 1 1 d . . . H10A H 1.1093 0.1910 0.6774 0.040 Uiso 1 1 calc R . . C11 C 1.0816(4) 0.15717(10) 0.61380(15) 0.0386(8) Uani 1 1 d . . . C12 C 1.0174(3) 0.15288(9) 0.56023(15) 0.0357(8) Uani 1 1 d . . . H12A H 1.0259 0.1329 0.5412 0.043 Uiso 1 1 calc R . . C13 C 0.9409(3) 0.17756(8) 0.53431(13) 0.0296(7) Uani 1 1 d . . . C14 C 0.9270(3) 0.20734(8) 0.56248(13) 0.0293(6) Uani 1 1 d . . . H14A H 0.8758 0.2240 0.5453 0.035 Uiso 1 1 calc R . . C15 C 1.1661(5) 0.12979(12) 0.6431(2) 0.0571(13) Uani 1 1 d . . . C16 C 1.1957(11) 0.1041(3) 0.6023(3) 0.179(7) Uani 1 1 d . . . H16A H 1.2348 0.1153 0.5762 0.268 Uiso 1 1 calc R . . H16B H 1.1251 0.0938 0.5826 0.268 Uiso 1 1 calc R . . H16C H 1.2460 0.0870 0.6221 0.268 Uiso 1 1 calc R . . C17 C 1.1032(8) 0.1117(2) 0.6859(4) 0.122(3) Uani 1 1 d . . . H17A H 1.1531 0.0943 0.7051 0.183 Uiso 1 1 calc R . . H17B H 1.0316 0.1017 0.6666 0.183 Uiso 1 1 calc R . . H17C H 1.0864 0.1280 0.7124 0.183 Uiso 1 1 calc R . . C18 C 1.2777(6) 0.1450(2) 0.6757(4) 0.103(3) Uani 1 1 d . . . H18A H 1.3190 0.1562 0.6506 0.154 Uiso 1 1 calc R . . H18B H 1.3258 0.1274 0.6952 0.154 Uiso 1 1 calc R . . H18C H 1.2591 0.1612 0.7020 0.154 Uiso 1 1 calc R . . C19 C 1.1581(3) -0.06196(8) 0.47152(13) 0.0319(7) Uani 1 1 d . . . C20 C 1.2276(3) -0.08760(9) 0.45603(14) 0.0356(8) Uani 1 1 d . . . H20A H 1.2625 -0.1032 0.4826 0.043 Uiso 1 1 calc R . . C21 C 1.2459(3) -0.09034(8) 0.40170(15) 0.0337(7) Uani 1 1 d . . . C22 C 1.1931(3) -0.06600(9) 0.36338(14) 0.0326(7) Uani 1 1 d . . . H22A H 1.2048 -0.0670 0.3269 0.039 Uiso 1 1 calc R . . C23 C 1.1235(3) -0.04040(8) 0.37834(13) 0.0281(6) Uani 1 1 d . . . C24 C 1.1036(3) -0.03866(8) 0.43232(13) 0.0305(7) Uani 1 1 d . . . H24A H 1.0544 -0.0221 0.4421 0.037 Uiso 1 1 calc R . . C25 C 1.3191(4) -0.11874(11) 0.38317(19) 0.0478(10) Uani 1 1 d . . . C26 C 1.4097(7) -0.10384(18) 0.3541(4) 0.100(3) Uani 1 1 d . . . H26A H 1.3718 -0.0907 0.3227 0.150 Uiso 1 1 calc R . . H26B H 1.4539 -0.1218 0.3416 0.150 Uiso 1 1 calc R . . H26C H 1.4613 -0.0895 0.3796 0.150 Uiso 1 1 calc R . . C27 C 1.2368(6) -0.14247(15) 0.3442(3) 0.0741(17) Uani 1 1 d . . . H27A H 1.1970 -0.1299 0.3125 0.111 Uiso 1 1 calc R . . H27B H 1.1805 -0.1519 0.3637 0.111 Uiso 1 1 calc R . . H27C H 1.2813 -0.1604 0.3319 0.111 Uiso 1 1 calc R . . C28 C 1.3824(6) -0.13986(14) 0.4330(3) 0.0730(17) Uani 1 1 d . . . H28A H 1.4351 -0.1255 0.4580 0.110 Uiso 1 1 calc R . . H28B H 1.4257 -0.1578 0.4199 0.110 Uiso 1 1 calc R . . H28C H 1.3259 -0.1494 0.4524 0.110 Uiso 1 1 calc R . . C29 C 0.6689(3) 0.07849(8) 0.21540(12) 0.0268(6) Uani 1 1 d . . . C30 C 0.6766(3) 0.05923(8) 0.16823(14) 0.0313(7) Uani 1 1 d . . . H30A H 0.7252 0.0403 0.1719 0.038 Uiso 1 1 calc R . . C31 C 0.6127(3) 0.06797(9) 0.11572(14) 0.0336(7) Uani 1 1 d . . . C32 C 0.5369(3) 0.09551(8) 0.11198(14) 0.0322(7) Uani 1 1 d . . . H32A H 0.4897 0.1008 0.0778 0.039 Uiso 1 1 calc R . . C33 C 0.5302(3) 0.11546(8) 0.15849(13) 0.0272(6) Uani 1 1 d . . . C34 C 0.5982(3) 0.10718(8) 0.21002(13) 0.0277(6) Uani 1 1 d . . . H34A H 0.5964 0.1208 0.2409 0.033 Uiso 1 1 calc R . . C35 C 0.6344(4) 0.04838(11) 0.06416(16) 0.0474(10) Uani 1 1 d . . . C36 C 0.6132(6) 0.01051(13) 0.0714(2) 0.0688(15) Uani 1 1 d . . . H36A H 0.6268 -0.0016 0.0392 0.103 Uiso 1 1 calc R . . H36B H 0.5339 0.0070 0.0756 0.103 Uiso 1 1 calc R . . H36C H 0.6657 0.0023 0.1040 0.103 Uiso 1 1 calc R . . C37 C 0.5551(6) 0.06052(17) 0.0111(2) 0.083(2) Uani 1 1 d . . . H37A H 0.5683 0.0843 0.0059 0.124 Uiso 1 1 calc R . . H37B H 0.4750 0.0570 0.0138 0.124 Uiso 1 1 calc R . . H37C H 0.5719 0.0480 -0.0201 0.124 Uiso 1 1 calc R . . C38 C 0.7616(5) 0.05281(17) 0.0594(2) 0.0705(15) Uani 1 1 d . . . H38A H 0.7772 0.0764 0.0545 0.106 Uiso 1 1 calc R . . H38B H 0.7764 0.0402 0.0280 0.106 Uiso 1 1 calc R . . H38C H 0.8114 0.0447 0.0928 0.106 Uiso 1 1 calc R . . C39 C 0.8958(3) 0.12792(8) 0.16718(13) 0.0283(6) Uani 1 1 d . . . C40 C 0.8609(3) 0.14794(9) 0.11992(14) 0.0345(7) Uani 1 1 d . . . H40A H 0.8849 0.1422 0.0870 0.041 Uiso 1 1 calc R . . C41 C 0.7903(4) 0.17648(9) 0.12118(15) 0.0369(8) Uani 1 1 d . A . C42 C 0.7605(3) 0.18544(9) 0.17181(15) 0.0342(7) Uani 1 1 d . . . H42A H 0.7138 0.2044 0.1734 0.041 Uiso 1 1 calc R . . C43 C 0.7997(3) 0.16645(8) 0.22028(13) 0.0284(6) Uani 1 1 d . . . C44 C 0.8641(3) 0.13718(8) 0.21741(13) 0.0275(6) Uani 1 1 d . . . H44A H 0.8863 0.1237 0.2489 0.033 Uiso 1 1 calc R . . C45 C 0.7431(6) 0.19689(14) 0.06777(19) 0.0646(15) Uani 1 1 d . . . C46 C 0.754(3) 0.2355(3) 0.0831(8) 0.122(10) Uani 0.63(4) 1 d P A 1 H46A H 0.6873 0.2424 0.0980 0.183 Uiso 0.63(4) 1 calc PR A 1 H46B H 0.7569 0.2485 0.0502 0.183 Uiso 0.63(4) 1 calc PR A 1 H46C H 0.8240 0.2392 0.1104 0.183 Uiso 0.63(4) 1 calc PR A 1 C46' C 0.711(5) 0.1736(9) 0.0205(11) 0.18(3) Uani 0.36(3) 1 d P A 2 H46D H 0.6403 0.1618 0.0235 0.277 Uiso 0.36(3) 1 calc PR A 2 H46E H 0.7727 0.1574 0.0208 0.277 Uiso 0.36(3) 1 calc PR A 2 H46F H 0.6987 0.1862 -0.0137 0.277 Uiso 0.36(3) 1 calc PR A 2 C47 C 0.6084(15) 0.1902(7) 0.0532(6) 0.131(10) Uani 0.64(3) 1 d P A 1 H47A H 0.5856 0.1771 0.0823 0.197 Uiso 0.64(3) 1 calc PR A 1 H47B H 0.5895 0.1780 0.0186 0.197 Uiso 0.64(3) 1 calc PR A 1 H47C H 0.5675 0.2115 0.0495 0.197 Uiso 0.64(3) 1 calc PR A 1 C47' C 0.864(2) 0.2131(13) 0.0532(18) 0.128(19) Uani 0.37(4) 1 d P A 2 H47D H 0.9286 0.2079 0.0827 0.192 Uiso 0.37(4) 1 calc PR A 2 H47E H 0.8557 0.2373 0.0494 0.192 Uiso 0.37(4) 1 calc PR A 2 H47F H 0.8774 0.2036 0.0189 0.192 Uiso 0.37(4) 1 calc PR A 2 C48 C 0.800(4) 0.1899(8) 0.0221(9) 0.15(2) Uani 0.58(4) 1 d P A 1 H48A H 0.7557 0.1731 -0.0017 0.232 Uiso 0.58(4) 1 calc PR A 1 H48B H 0.8772 0.1815 0.0360 0.232 Uiso 0.58(4) 1 calc PR A 1 H48C H 0.8040 0.2103 0.0012 0.232 Uiso 0.58(4) 1 calc PR A 1 C48' C 0.660(3) 0.2221(9) 0.0723(8) 0.099(14) Uani 0.42(4) 1 d P A 2 H48D H 0.5912 0.2116 0.0807 0.148 Uiso 0.42(4) 1 calc PR A 2 H48E H 0.6403 0.2342 0.0378 0.148 Uiso 0.42(4) 1 calc PR A 2 H48F H 0.6923 0.2375 0.1017 0.148 Uiso 0.42(4) 1 calc PR A 2 C49 C 0.8905(12) 0.2648(3) 0.4045(6) 0.181(6) Uani 1 1 d . . . H49A H 0.9429 0.2797 0.3903 0.271 Uiso 1 1 calc R . . H49B H 0.9317 0.2537 0.4375 0.271 Uiso 1 1 calc R . . H49C H 0.8268 0.2777 0.4134 0.271 Uiso 1 1 calc R . . C50 C 0.7041(15) -0.0108(4) 0.4010(6) 0.244(11) Uani 1 1 d . . . H50A H 0.6388 -0.0248 0.3847 0.365 Uiso 1 1 calc R . . H50B H 0.6801 0.0050 0.4265 0.365 Uiso 1 1 calc R . . H50C H 0.7657 -0.0249 0.4207 0.365 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 0.0382(4) 0.0194(3) 0.0149(3) 0.000 -0.0021(2) 0.000 Mn2 0.0388(3) 0.0212(2) 0.0148(2) -0.00183(15) 0.00086(18) 0.00441(18) Mn3 0.0459(3) 0.0250(2) 0.0173(2) 0.00202(17) 0.0071(2) 0.0038(2) Mn4 0.0588(5) 0.0189(3) 0.0152(3) 0.000 0.0030(3) 0.000 Mn5 0.0406(3) 0.0234(2) 0.0203(2) -0.00326(17) -0.00321(19) 0.00551(19) O1 0.067(2) 0.0471(17) 0.0492(17) -0.0215(14) -0.0178(15) 0.0315(15) O2 0.0597(16) 0.0293(12) 0.0244(12) -0.0103(9) -0.0015(11) 0.0030(11) O3 0.074(2) 0.0422(15) 0.0295(14) -0.0101(11) -0.0221(13) 0.0129(14) O4 0.0514(16) 0.0501(16) 0.0252(12) -0.0173(11) -0.0047(11) 0.0056(13) O5 0.080(2) 0.0519(17) 0.0220(12) 0.0033(11) 0.0182(13) 0.0109(15) O6 0.0581(17) 0.0488(15) 0.0242(12) 0.0162(11) 0.0016(11) -0.0075(13) O7 0.0645(19) 0.0359(14) 0.0435(15) 0.0008(12) 0.0039(14) 0.0227(13) O8 0.0660(18) 0.0367(13) 0.0235(12) 0.0127(10) 0.0078(12) 0.0036(12) O9 0.0458(14) 0.0473(14) 0.0185(11) -0.0081(10) -0.0011(10) 0.0016(11) O10 0.0448(14) 0.0299(11) 0.0222(11) 0.0046(9) -0.0003(10) 0.0033(10) O11 0.0575(17) 0.0290(12) 0.0354(13) -0.0111(10) 0.0039(12) 0.0040(11) O12 0.0341(12) 0.0295(11) 0.0301(12) 0.0074(9) 0.0017(9) 0.0019(9) O13 0.0380(12) 0.0245(10) 0.0258(11) -0.0012(8) 0.0081(9) -0.0011(9) O14 0.0435(14) 0.0315(12) 0.0351(13) 0.0136(10) 0.0088(11) 0.0052(10) O15 0.0370(13) 0.0330(12) 0.0289(12) -0.0046(9) 0.0045(10) 0.0040(10) O16 0.0505(15) 0.0344(12) 0.0203(11) 0.0039(9) 0.0049(10) 0.0031(11) O17 0.108(3) 0.073(3) 0.085(3) -0.015(2) 0.011(3) -0.045(3) O18 0.088(3) 0.080(3) 0.060(2) 0.0020(19) 0.020(2) -0.041(2) O19 0.52(2) 0.176(9) 0.243(12) -0.128(9) -0.246(14) 0.214(12) O20 0.155(5) 0.106(4) 0.111(4) -0.050(3) 0.077(4) -0.061(4) C1 0.0404(18) 0.0263(15) 0.0250(15) -0.0052(12) 0.0012(13) 0.0037(13) C2 0.0424(18) 0.0330(16) 0.0171(14) -0.0050(12) -0.0020(12) -0.0015(14) C3 0.058(2) 0.0342(17) 0.0190(15) 0.0055(13) 0.0036(14) -0.0063(16) C4 0.0473(19) 0.0214(14) 0.0229(15) 0.0023(11) 0.0011(13) 0.0013(13) C5 0.0350(16) 0.0291(15) 0.0183(13) 0.0002(11) -0.0001(12) -0.0033(12) C6 0.0362(16) 0.0276(14) 0.0210(14) 0.0023(11) 0.0061(12) 0.0012(12) C7 0.0349(16) 0.0258(14) 0.0169(13) 0.0014(11) 0.0011(11) 0.0006(12) C8 0.0355(16) 0.0244(14) 0.0232(14) -0.0005(11) 0.0037(12) -0.0039(12) C9 0.0342(16) 0.0261(14) 0.0198(14) -0.0061(11) 0.0012(12) 0.0027(12) C10 0.0400(18) 0.0338(17) 0.0211(14) -0.0075(12) -0.0052(13) 0.0066(14) C11 0.049(2) 0.0356(18) 0.0275(17) -0.0042(14) -0.0026(15) 0.0150(16) C12 0.046(2) 0.0305(16) 0.0290(17) -0.0090(13) 0.0019(14) 0.0090(14) C13 0.0367(17) 0.0321(16) 0.0175(13) -0.0051(12) -0.0006(12) 0.0025(13) C14 0.0353(16) 0.0280(15) 0.0214(14) -0.0037(12) -0.0022(12) 0.0056(12) C15 0.069(3) 0.049(2) 0.043(2) -0.0049(18) -0.015(2) 0.029(2) C16 0.248(12) 0.169(9) 0.087(5) -0.047(6) -0.046(7) 0.180(10) C17 0.117(6) 0.091(5) 0.142(8) 0.062(5) -0.014(6) 0.023(5) C18 0.068(4) 0.092(5) 0.124(6) -0.001(4) -0.039(4) 0.035(3) C19 0.0469(19) 0.0279(15) 0.0191(14) 0.0047(12) 0.0021(13) -0.0005(14) C20 0.049(2) 0.0285(15) 0.0260(16) 0.0070(13) 0.0002(14) 0.0044(14) C21 0.0432(19) 0.0273(15) 0.0295(16) 0.0009(13) 0.0044(14) 0.0083(14) C22 0.0480(19) 0.0304(16) 0.0207(14) 0.0016(12) 0.0100(13) 0.0061(14) C23 0.0392(17) 0.0236(14) 0.0205(14) 0.0028(11) 0.0031(12) 0.0034(12) C24 0.0460(19) 0.0247(14) 0.0208(14) 0.0018(11) 0.0062(13) 0.0041(13) C25 0.056(2) 0.041(2) 0.047(2) -0.0011(17) 0.0112(19) 0.0202(18) C26 0.092(5) 0.076(4) 0.154(8) 0.021(4) 0.082(5) 0.035(4) C27 0.092(4) 0.059(3) 0.066(3) -0.026(3) 0.001(3) 0.027(3) C28 0.089(4) 0.051(3) 0.071(3) -0.004(2) -0.005(3) 0.037(3) C29 0.0362(16) 0.0240(14) 0.0178(13) -0.0015(11) -0.0006(12) -0.0017(12) C30 0.0403(18) 0.0271(15) 0.0227(15) -0.0046(12) -0.0027(13) 0.0033(13) C31 0.0447(19) 0.0311(16) 0.0214(15) -0.0081(12) -0.0023(13) 0.0016(14) C32 0.0400(18) 0.0297(15) 0.0229(15) -0.0022(12) -0.0041(13) 0.0019(13) C33 0.0340(16) 0.0251(14) 0.0212(14) -0.0013(11) 0.0019(12) -0.0008(12) C34 0.0337(16) 0.0280(15) 0.0203(14) -0.0045(11) 0.0025(12) -0.0001(12) C35 0.063(3) 0.046(2) 0.0271(18) -0.0154(16) -0.0065(17) 0.0147(19) C36 0.090(4) 0.046(3) 0.063(3) -0.026(2) -0.002(3) 0.010(2) C37 0.112(5) 0.092(4) 0.030(2) -0.027(2) -0.022(3) 0.049(4) C38 0.077(4) 0.090(4) 0.044(3) -0.023(3) 0.013(2) 0.011(3) C39 0.0349(16) 0.0255(14) 0.0235(15) 0.0043(11) 0.0033(12) 0.0005(12) C40 0.049(2) 0.0337(17) 0.0217(15) 0.0068(13) 0.0079(14) 0.0057(15) C41 0.049(2) 0.0360(18) 0.0265(16) 0.0132(14) 0.0089(15) 0.0107(15) C42 0.0444(19) 0.0306(16) 0.0288(16) 0.0090(13) 0.0102(14) 0.0082(14) C43 0.0346(16) 0.0286(15) 0.0219(14) 0.0017(12) 0.0048(12) 0.0009(12) C44 0.0337(16) 0.0278(14) 0.0198(14) 0.0044(11) 0.0026(12) -0.0003(12) C45 0.097(4) 0.066(3) 0.035(2) 0.030(2) 0.024(2) 0.038(3) C46 0.21(3) 0.064(7) 0.101(11) 0.051(7) 0.060(13) 0.038(10) C46' 0.33(7) 0.13(3) 0.040(14) -0.003(13) -0.09(3) 0.10(3) C47 0.130(12) 0.19(3) 0.060(8) 0.048(11) -0.010(7) 0.066(13) C47' 0.113(18) 0.18(4) 0.10(3) 0.12(3) 0.054(16) 0.044(19) C48 0.26(4) 0.17(3) 0.059(12) 0.071(15) 0.09(2) 0.15(3) C48' 0.14(2) 0.11(2) 0.048(9) 0.041(12) 0.014(12) 0.07(2) C49 0.161(11) 0.085(6) 0.271(18) 0.001(8) -0.018(11) -0.044(7) C50 0.31(2) 0.281(19) 0.190(13) -0.112(13) 0.165(14) -0.222(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O11 2.157(2) . ? Mn1 O11 2.157(2) 2_655 ? Mn1 O2 2.164(2) 7_656 ? Mn1 O2 2.164(2) 8_455 ? Mn1 O15 2.286(3) 2_655 ? Mn1 O15 2.286(3) . ? Mn2 O4 2.093(2) . ? Mn2 O9 2.139(2) . ? Mn2 O6 2.154(3) 5_756 ? Mn2 O13 2.218(2) 2_755 ? Mn2 O12 2.234(2) 2_655 ? Mn2 O16 2.283(2) . ? Mn2 Mn3 3.2331(7) . ? Mn3 O7 2.086(3) . ? Mn3 O5 2.145(3) 5_756 ? Mn3 O18 2.184(4) . ? Mn3 O10 2.192(2) . ? Mn3 O13 2.252(2) 2_755 ? Mn3 O6 2.487(3) 5_756 ? Mn4 O14 2.124(2) 2_755 ? Mn4 O14 2.124(2) . ? Mn4 O8 2.201(3) . ? Mn4 O8 2.201(3) 2_755 ? Mn4 O10 2.483(3) . ? Mn4 O10 2.483(3) 2_755 ? Mn5 O1 2.030(3) 7_656 ? Mn5 O3 2.091(3) . ? Mn5 O17 2.220(4) . ? Mn5 O12 2.256(2) 2_655 ? Mn5 O15 2.338(2) . ? Mn5 O16 2.342(3) . ? O1 C1 1.260(4) . ? O1 Mn5 2.030(3) 7_656 ? O2 C1 1.250(4) . ? O2 Mn1 2.164(2) 7_656 ? O3 C2 1.248(5) . ? O4 C2 1.251(4) . ? O5 C3 1.233(5) . ? O5 Mn3 2.145(3) 5_756 ? O6 C3 1.273(5) . ? O6 Mn2 2.154(3) 5_756 ? O6 Mn3 2.487(3) 5_756 ? O7 C4 1.249(5) . ? O8 C4 1.259(4) . ? O9 C5 1.260(4) . ? O10 C5 1.267(4) . ? O11 C6 1.245(4) . ? O12 C6 1.276(4) . ? O12 Mn2 2.234(2) 2_655 ? O12 Mn5 2.256(2) 2_655 ? O13 C7 1.278(4) . ? O13 Mn2 2.218(2) 2_755 ? O13 Mn3 2.252(2) 2_755 ? O14 C7 1.238(4) . ? O15 C8 1.268(4) . ? O16 C8 1.268(4) . ? O17 C49 1.411(12) . ? O17 H17 0.9300 . ? O18 C50 1.254(12) . ? O18 H18 0.9300 . ? C1 C9 1.505(4) . ? C2 C13 1.505(4) . ? C3 C19 1.508(5) . ? C4 C23 1.501(4) . ? C5 C29 1.493(4) . ? C6 C33 1.487(4) . ? C7 C39 1.499(4) . ? C8 C43 1.492(4) . ? C9 C14 1.389(4) . ? C9 C10 1.392(5) . ? C10 C11 1.400(5) . ? C10 H10A 0.9300 . ? C11 C12 1.386(5) . ? C11 C15 1.540(5) . ? C12 C13 1.386(5) . ? C12 H12A 0.9300 . ? C13 C14 1.386(4) . ? C14 H14A 0.9300 . ? C15 C16 1.506(8) . ? C15 C18 1.511(8) . ? C15 C17 1.564(11) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C24 1.388(4) . ? C19 C20 1.393(5) . ? C20 C21 1.391(5) . ? C20 H20A 0.9300 . ? C21 C22 1.397(5) . ? C21 C25 1.529(5) . ? C22 C23 1.387(5) . ? C22 H22A 0.9300 . ? C23 C24 1.387(4) . ? C24 H24A 0.9300 . ? C25 C26 1.503(8) . ? C25 C27 1.532(7) . ? C25 C28 1.540(7) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.390(4) . ? C29 C30 1.399(4) . ? C30 C31 1.396(4) . ? C30 H30A 0.9300 . ? C31 C32 1.391(5) . ? C31 C35 1.541(5) . ? C32 C33 1.398(4) . ? C32 H32A 0.9300 . ? C33 C34 1.390(4) . ? C34 H34A 0.9300 . ? C35 C37 1.516(6) . ? C35 C38 1.520(8) . ? C35 C36 1.528(7) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.393(4) . ? C39 C44 1.399(5) . ? C40 C41 1.397(5) . ? C40 H40A 0.9300 . ? C41 C42 1.396(5) . ? C41 C45 1.541(5) . ? C42 C43 1.401(4) . ? C42 H42A 0.9300 . ? C43 C44 1.386(5) . ? C44 H44A 0.9300 . ? C45 C48' 1.405(18) . ? C45 C48 1.432(15) . ? C45 C46' 1.47(3) . ? C45 C46 1.564(17) . ? C45 C47 1.56(2) . ? C45 C47' 1.65(3) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C46' H46D 0.9600 . ? C46' H46E 0.9600 . ? C46' H46F 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C47' H47D 0.9600 . ? C47' H47E 0.9600 . ? C47' H47F 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C48' H48D 0.9600 . ? C48' H48E 0.9600 . ? C48' H48F 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 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 O11 Mn1 O11 88.98(15) . 2_655 ? O11 Mn1 O2 168.05(11) . 7_656 ? O11 Mn1 O2 94.57(10) 2_655 7_656 ? O11 Mn1 O2 94.57(10) . 8_455 ? O11 Mn1 O2 168.05(11) 2_655 8_455 ? O2 Mn1 O2 84.28(15) 7_656 8_455 ? O11 Mn1 O15 78.65(10) . 2_655 ? O11 Mn1 O15 90.55(10) 2_655 2_655 ? O2 Mn1 O15 89.89(10) 7_656 2_655 ? O2 Mn1 O15 101.33(10) 8_455 2_655 ? O11 Mn1 O15 90.55(10) . . ? O11 Mn1 O15 78.65(10) 2_655 . ? O2 Mn1 O15 101.33(10) 7_656 . ? O2 Mn1 O15 89.89(10) 8_455 . ? O15 Mn1 O15 164.93(13) 2_655 . ? O4 Mn2 O9 174.77(11) . . ? O4 Mn2 O6 90.17(12) . 5_756 ? O9 Mn2 O6 85.87(11) . 5_756 ? O4 Mn2 O13 92.78(10) . 2_755 ? O9 Mn2 O13 83.35(10) . 2_755 ? O6 Mn2 O13 82.62(11) 5_756 2_755 ? O4 Mn2 O12 91.92(10) . 2_655 ? O9 Mn2 O12 92.26(10) . 2_655 ? O6 Mn2 O12 102.46(11) 5_756 2_655 ? O13 Mn2 O12 173.07(9) 2_755 2_655 ? O4 Mn2 O16 95.03(11) . . ? O9 Mn2 O16 88.89(10) . . ? O6 Mn2 O16 174.73(10) 5_756 . ? O13 Mn2 O16 96.26(9) 2_755 . ? O12 Mn2 O16 78.24(10) 2_655 . ? O4 Mn2 Mn3 117.15(8) . . ? O9 Mn2 Mn3 57.64(7) . . ? O6 Mn2 Mn3 50.23(9) 5_756 . ? O13 Mn2 Mn3 44.10(6) 2_755 . ? O12 Mn2 Mn3 136.68(6) 2_655 . ? O16 Mn2 Mn3 125.93(7) . . ? O7 Mn3 O5 100.20(12) . 5_756 ? O7 Mn3 O18 88.46(16) . . ? O5 Mn3 O18 91.81(14) 5_756 . ? O7 Mn3 O10 85.36(11) . . ? O5 Mn3 O10 172.33(12) 5_756 . ? O18 Mn3 O10 83.01(13) . . ? O7 Mn3 O13 113.21(12) . 2_755 ? O5 Mn3 O13 91.28(11) 5_756 2_755 ? O18 Mn3 O13 157.16(15) . 2_755 ? O10 Mn3 O13 91.36(9) . 2_755 ? O7 Mn3 O6 155.63(10) . 5_756 ? O5 Mn3 O6 55.78(10) 5_756 5_756 ? O18 Mn3 O6 88.30(14) . 5_756 ? O10 Mn3 O6 118.17(9) . 5_756 ? O13 Mn3 O6 74.86(9) 2_755 5_756 ? O7 Mn3 Mn2 155.52(10) . . ? O5 Mn3 Mn2 88.70(8) 5_756 . ? O18 Mn3 Mn2 114.21(13) . . ? O10 Mn3 Mn2 88.29(7) . . ? O13 Mn3 Mn2 43.26(6) 2_755 . ? O6 Mn3 Mn2 41.74(6) 5_756 . ? O14 Mn4 O14 83.13(15) 2_755 . ? O14 Mn4 O8 98.40(10) 2_755 . ? O14 Mn4 O8 160.46(10) . . ? O14 Mn4 O8 160.46(10) 2_755 2_755 ? O14 Mn4 O8 98.40(11) . 2_755 ? O8 Mn4 O8 86.67(16) . 2_755 ? O14 Mn4 O10 81.07(9) 2_755 . ? O14 Mn4 O10 78.71(9) . . ? O8 Mn4 O10 120.81(9) . . ? O8 Mn4 O10 80.15(10) 2_755 . ? O14 Mn4 O10 78.71(9) 2_755 2_755 ? O14 Mn4 O10 81.07(9) . 2_755 ? O8 Mn4 O10 80.15(10) . 2_755 ? O8 Mn4 O10 120.81(9) 2_755 2_755 ? O10 Mn4 O10 152.87(11) . 2_755 ? O1 Mn5 O3 97.87(12) 7_656 . ? O1 Mn5 O17 87.72(19) 7_656 . ? O3 Mn5 O17 86.66(16) . . ? O1 Mn5 O12 108.20(13) 7_656 2_655 ? O3 Mn5 O12 88.12(11) . 2_655 ? O17 Mn5 O12 163.79(16) . 2_655 ? O1 Mn5 O15 97.49(11) 7_656 . ? O3 Mn5 O15 159.25(13) . . ? O17 Mn5 O15 80.09(14) . . ? O12 Mn5 O15 100.22(9) 2_655 . ? O1 Mn5 O16 153.40(11) 7_656 . ? O3 Mn5 O16 108.53(11) . . ? O17 Mn5 O16 90.55(16) . . ? O12 Mn5 O16 76.60(9) 2_655 . ? O15 Mn5 O16 56.14(8) . . ? C1 O1 Mn5 142.9(3) . 7_656 ? C1 O2 Mn1 127.2(2) . 7_656 ? C2 O3 Mn5 125.5(2) . . ? C2 O4 Mn2 135.1(2) . . ? C3 O5 Mn3 99.7(2) . 5_756 ? C3 O6 Mn2 137.5(3) . 5_756 ? C3 O6 Mn3 82.8(2) . 5_756 ? Mn2 O6 Mn3 88.03(10) 5_756 5_756 ? C4 O7 Mn3 162.8(3) . . ? C4 O8 Mn4 102.9(2) . . ? C5 O9 Mn2 146.2(2) . . ? C5 O10 Mn3 106.4(2) . . ? C5 O10 Mn4 138.3(2) . . ? Mn3 O10 Mn4 94.42(9) . . ? C6 O11 Mn1 163.8(3) . . ? C6 O12 Mn2 127.6(2) . 2_655 ? C6 O12 Mn5 107.3(2) . 2_655 ? Mn2 O12 Mn5 93.30(9) 2_655 2_655 ? C7 O13 Mn2 136.4(2) . 2_755 ? C7 O13 Mn3 113.08(19) . 2_755 ? Mn2 O13 Mn3 92.64(9) 2_755 2_755 ? C7 O14 Mn4 150.1(2) . . ? C8 O15 Mn1 136.2(2) . . ? C8 O15 Mn5 91.74(19) . . ? Mn1 O15 Mn5 100.65(10) . . ? C8 O16 Mn2 146.5(2) . . ? C8 O16 Mn5 91.6(2) . . ? Mn2 O16 Mn5 89.81(9) . . ? C49 O17 Mn5 126.7(7) . . ? C49 O17 H17 116.6 . . ? Mn5 O17 H17 116.6 . . ? C50 O18 Mn3 131.3(7) . . ? C50 O18 H18 114.4 . . ? Mn3 O18 H18 114.4 . . ? O2 C1 O1 124.4(3) . . ? O2 C1 C9 120.6(3) . . ? O1 C1 C9 115.1(3) . . ? O3 C2 O4 124.6(3) . . ? O3 C2 C13 117.2(3) . . ? O4 C2 C13 118.1(3) . . ? O5 C3 O6 121.5(3) . . ? O5 C3 C19 120.3(3) . . ? O6 C3 C19 118.0(4) . . ? O7 C4 O8 120.7(3) . . ? O7 C4 C23 119.1(3) . . ? O8 C4 C23 120.2(3) . . ? O9 C5 O10 122.1(3) . . ? O9 C5 C29 117.7(3) . . ? O10 C5 C29 120.1(3) . . ? O11 C6 O12 122.0(3) . . ? O11 C6 C33 117.9(3) . . ? O12 C6 C33 120.0(3) . . ? O14 C7 O13 123.1(3) . . ? O14 C7 C39 117.4(3) . . ? O13 C7 C39 119.4(3) . . ? O16 C8 O15 120.5(3) . . ? O16 C8 C43 119.7(3) . . ? O15 C8 C43 119.7(3) . . ? C14 C9 C10 119.6(3) . . ? C14 C9 C1 119.0(3) . . ? C10 C9 C1 121.4(3) . . ? C9 C10 C11 121.1(3) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C12 C11 C10 117.8(3) . . ? C12 C11 C15 122.1(3) . . ? C10 C11 C15 120.1(3) . . ? C13 C12 C11 121.8(3) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? C12 C13 C14 119.6(3) . . ? C12 C13 C2 120.6(3) . . ? C14 C13 C2 119.9(3) . . ? C13 C14 C9 120.1(3) . . ? C13 C14 H14A 120.0 . . ? C9 C14 H14A 120.0 . . ? C16 C15 C18 109.3(7) . . ? C16 C15 C11 111.8(4) . . ? C18 C15 C11 111.9(4) . . ? C16 C15 C17 109.7(8) . . ? C18 C15 C17 107.2(6) . . ? C11 C15 C17 106.8(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 120.2(3) . . ? C24 C19 C3 119.2(3) . . ? C20 C19 C3 120.6(3) . . ? C21 C20 C19 121.5(3) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 117.2(3) . . ? C20 C21 C25 122.6(3) . . ? C22 C21 C25 120.1(3) . . ? C23 C22 C21 121.7(3) . . ? C23 C22 H22A 119.1 . . ? C21 C22 H22A 119.1 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 C4 119.6(3) . . ? C22 C23 C4 120.2(3) . . ? C23 C24 C19 119.0(3) . . ? C23 C24 H24A 120.5 . . ? C19 C24 H24A 120.5 . . ? C26 C25 C21 109.8(4) . . ? C26 C25 C27 110.9(5) . . ? C21 C25 C27 108.2(4) . . ? C26 C25 C28 108.3(5) . . ? C21 C25 C28 111.7(4) . . ? C27 C25 C28 108.0(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 119.7(3) . . ? C34 C29 C5 118.1(3) . . ? C30 C29 C5 122.1(3) . . ? C31 C30 C29 121.1(3) . . ? C31 C30 H30A 119.5 . . ? C29 C30 H30A 119.5 . . ? C32 C31 C30 118.1(3) . . ? C32 C31 C35 122.7(3) . . ? C30 C31 C35 119.1(3) . . ? C31 C32 C33 121.4(3) . . ? C31 C32 H32A 119.3 . . ? C33 C32 H32A 119.3 . . ? C34 C33 C32 119.6(3) . . ? C34 C33 C6 118.0(3) . . ? C32 C33 C6 122.4(3) . . ? C33 C34 C29 119.9(3) . . ? C33 C34 H34A 120.0 . . ? C29 C34 H34A 120.0 . . ? C37 C35 C38 109.8(5) . . ? C37 C35 C36 108.8(4) . . ? C38 C35 C36 107.7(4) . . ? C37 C35 C31 111.9(3) . . ? C38 C35 C31 108.9(3) . . ? C36 C35 C31 109.7(4) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 119.8(3) . . ? C40 C39 C7 121.0(3) . . ? C44 C39 C7 119.1(3) . . ? C39 C40 C41 121.0(3) . . ? C39 C40 H40A 119.5 . . ? C41 C40 H40A 119.5 . . ? C42 C41 C40 118.2(3) . . ? C42 C41 C45 120.7(3) . . ? C40 C41 C45 121.0(3) . . ? C41 C42 C43 121.3(3) . . ? C41 C42 H42A 119.3 . . ? C43 C42 H42A 119.3 . . ? C44 C43 C42 119.5(3) . . ? C44 C43 C8 120.5(3) . . ? C42 C43 C8 120.0(3) . . ? C43 C44 C39 120.0(3) . . ? C43 C44 H44A 120.0 . . ? C39 C44 H44A 120.0 . . ? C48' C45 C48 128.9(11) . . ? C48' C45 C46' 115(2) . . ? C48 C45 C46' 49(3) . . ? C48' C45 C41 116.0(8) . . ? C48 C45 C41 114.8(8) . . ? C46' C45 C41 109.6(12) . . ? C48' C45 C46 47.1(15) . . ? C48 C45 C46 110.3(16) . . ? C46' C45 C46 142.5(14) . . ? C41 C45 C46 107.8(8) . . ? C48' C45 C47 57(2) . . ? C48 C45 C47 113(2) . . ? C46' C45 C47 68(2) . . ? C41 C45 C47 106.3(6) . . ? C46 C45 C47 104.3(18) . . ? C48' C45 C47' 112.0(18) . . ? C48 C45 C47' 50.4(16) . . ? C46' C45 C47' 100(3) . . ? C41 C45 C47' 102.0(9) . . ? C46 C45 C47' 69.1(16) . . ? C47 C45 C47' 151.5(10) . . ? C45 C46 H46A 109.4 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C46' H46D 109.4 . . ? C45 C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? C45 C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C47' H47D 109.5 . . ? C45 C47' H47E 109.5 . . ? H47D C47' H47E 109.5 . . ? C45 C47' H47F 109.5 . . ? H47D C47' H47F 109.5 . . ? H47E C47' H47F 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C48' H48D 109.4 . . ? C45 C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? C45 C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? O17 C49 H49A 109.5 . . ? O17 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O17 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O18 C50 H50A 109.5 . . ? O18 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O18 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.863 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.096 #===END data_Mn2 _database_code_depnum_ccdc_archive 'CCDC 799836' #TrackingRef '- cif data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H66 Mn3 N0 O18' _chemical_formula_weight 1167.89 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.324(4) _cell_length_b 9.821(4) _cell_length_c 16.303(7) _cell_angle_alpha 87.715(12) _cell_angle_beta 77.376(13) _cell_angle_gamma 72.201(9) _cell_volume 1386.5(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3385 _cell_measurement_theta_min 3.0782 _cell_measurement_theta_max 27.4719 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.3500 _exptl_crystal_size_mid 0.3000 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 609 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4965 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10854 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5945 _reflns_number_gt 4495 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^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 5945 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.87487(4) 0.89190(4) 1.51399(3) 0.02314(14) Uani 1 1 d . . . Mn2 Mn 0.5000 1.0000 1.5000 0.02122(16) Uani 1 2 d S . . O1 O 0.8770(2) 0.6660(2) 1.52811(17) 0.0456(6) Uani 1 1 d . . . O2 O 0.6491(2) 0.8242(2) 1.55189(15) 0.0360(5) Uani 1 1 d . . . O3 O 0.6581(2) 0.1019(2) 1.53646(14) 0.0299(5) Uani 1 1 d . . . O4 O 0.8815(2) 0.14110(19) 1.50822(13) 0.0283(5) Uani 1 1 d . . . O5 O 0.8956(2) 0.9032(2) 1.38199(13) 0.0327(5) Uani 1 1 d . . . O6 O 0.6482(2) 0.9484(2) 1.37578(14) 0.0375(5) Uani 1 1 d . . . O7 O 0.6995(4) 0.8823(4) 0.98622(19) 0.0734(10) Uani 1 1 d . . . O8 O 0.5390(3) 1.0326(3) 1.08760(17) 0.0667(9) Uani 1 1 d . . . O9 O 0.8934(3) 0.9231(3) 1.64395(14) 0.0445(6) Uani 1 1 d . . . C1 C 0.7342(3) 0.6947(3) 1.5488(2) 0.0286(7) Uani 1 1 d . . . C2 C 0.6587(3) 0.5807(3) 1.57503(19) 0.0259(6) Uani 1 1 d . . . C3 C 0.5102(3) 0.6161(3) 1.6251(2) 0.0303(7) Uani 1 1 d . . . H3A H 0.4590 0.7111 1.6421 0.036 Uiso 1 1 calc R . . C4 C 0.4364(3) 0.5133(3) 1.65021(19) 0.0286(7) Uani 1 1 d . . . C5 C 0.5122(3) 0.3745(3) 1.61729(19) 0.0283(7) Uani 1 1 d . . . H5A H 0.4623 0.3050 1.6296 0.034 Uiso 1 1 calc R . . C6 C 0.6603(3) 0.3370(3) 1.56651(18) 0.0233(6) Uani 1 1 d . . . C7 C 0.7383(3) 0.4393(3) 1.54798(18) 0.0243(6) Uani 1 1 d . . . H7A H 0.8404 0.4139 1.5184 0.029 Uiso 1 1 calc R . . C8 C 0.2808(3) 0.5458(3) 1.7137(2) 0.0369(8) Uani 1 1 d . . . C9 C 0.3052(5) 0.4509(5) 1.7901(2) 0.0611(12) Uani 1 1 d . . . H9A H 0.3795 0.4729 1.8154 0.092 Uiso 1 1 calc R . . H9B H 0.3422 0.3521 1.7720 0.092 Uiso 1 1 calc R . . H9C H 0.2091 0.4685 1.8304 0.092 Uiso 1 1 calc R . . C10 C 0.2183(5) 0.7016(4) 1.7435(3) 0.0781(16) Uani 1 1 d . . . H10A H 0.2922 0.7256 1.7683 0.117 Uiso 1 1 calc R . . H10B H 0.1234 0.7163 1.7846 0.117 Uiso 1 1 calc R . . H10C H 0.1998 0.7614 1.6965 0.117 Uiso 1 1 calc R . . C11 C 0.1615(4) 0.5083(5) 1.6750(3) 0.0584(11) Uani 1 1 d . . . H11A H 0.1447 0.5663 1.6272 0.088 Uiso 1 1 calc R . . H11B H 0.0661 0.5261 1.7160 0.088 Uiso 1 1 calc R . . H11C H 0.1988 0.4092 1.6577 0.088 Uiso 1 1 calc R . . C12 C 0.7375(3) 0.1861(3) 1.53447(17) 0.0211(6) Uani 1 1 d . . . C13 C 0.7897(3) 0.9134(3) 1.34309(18) 0.0270(6) Uani 1 1 d . . . C14 C 0.8386(3) 0.8773(3) 1.25037(19) 0.0287(6) Uani 1 1 d . . . C15 C 0.7341(4) 0.9293(3) 1.19869(19) 0.0327(7) Uani 1 1 d . . . H15A H 0.6359 0.9906 1.2205 0.039 Uiso 1 1 calc R . . C16 C 0.7784(4) 0.8884(4) 1.1141(2) 0.0377(8) Uani 1 1 d . . . C17 C 0.9240(4) 0.7956(4) 1.0814(2) 0.0428(8) Uani 1 1 d . . . H17A H 0.9514 0.7696 1.0245 0.051 Uiso 1 1 calc R . . C18 C 1.0303(4) 0.7406(4) 1.1320(2) 0.0401(8) Uani 1 1 d . . . C19 C 0.9854(3) 0.7843(3) 1.2164(2) 0.0351(7) Uani 1 1 d . . . H19A H 1.0548 0.7508 1.2512 0.042 Uiso 1 1 calc R . . C20 C 1.1909(4) 0.6351(5) 1.0941(3) 0.0574(11) Uani 1 1 d . . . C21 C 1.1689(6) 0.5097(6) 1.0491(4) 0.114(3) Uani 1 1 d . . . H21A H 1.2680 0.4434 1.0256 0.172 Uiso 1 1 calc R . . H21B H 1.1153 0.5459 1.0050 0.172 Uiso 1 1 calc R . . H21C H 1.1099 0.4618 1.0889 0.172 Uiso 1 1 calc R . . C22 C 1.2803(6) 0.7124(7) 1.0332(5) 0.142(3) Uani 1 1 d . . . H22A H 1.2918 0.7907 1.0618 0.213 Uiso 1 1 calc R . . H22B H 1.2264 0.7482 0.9892 0.213 Uiso 1 1 calc R . . H22C H 1.3804 0.6479 1.0095 0.213 Uiso 1 1 calc R . . C23 C 1.2771(5) 0.5668(6) 1.1614(4) 0.0911(18) Uani 1 1 d . . . H23A H 1.2961 0.6394 1.1914 0.137 Uiso 1 1 calc R . . H23B H 1.3736 0.4988 1.1356 0.137 Uiso 1 1 calc R . . H23C H 1.2162 0.5188 1.1998 0.137 Uiso 1 1 calc R . . C24 C 0.6625(4) 0.9414(4) 1.0612(2) 0.0451(9) Uani 1 1 d . . . C25 C 0.7863(8) 0.9383(5) 1.7230(4) 0.124(3) Uani 1 1 d . . . H25A H 0.8596 0.9323 1.7588 0.149 Uiso 1 1 calc R . . C26 C 0.6914(7) 1.0742(5) 1.7482(4) 0.114(2) Uani 1 1 d . . . H26A H 0.7438 1.1426 1.7264 0.172 Uiso 1 1 calc R . . H26B H 0.6655 1.0818 1.8085 0.172 Uiso 1 1 calc R . . H26C H 0.5988 1.0930 1.7273 0.172 Uiso 1 1 calc R . . C27 C 0.7506(6) 0.8072(5) 1.7490(3) 0.0750(14) Uani 1 1 d . . . H27A H 0.8381 0.7265 1.7270 0.112 Uiso 1 1 calc R . . H27B H 0.6636 0.8032 1.7278 0.112 Uiso 1 1 calc R . . H27C H 0.7265 0.8052 1.8092 0.112 Uiso 1 1 calc R . . H7 H 0.669(12) 0.954(11) 0.964(7) 0.27(6) 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 0.0168(2) 0.0185(2) 0.0334(3) -0.00106(17) -0.00039(17) -0.00774(16) Mn2 0.0132(3) 0.0187(3) 0.0302(3) -0.0025(2) 0.0000(2) -0.0056(2) O1 0.0243(12) 0.0238(10) 0.0843(19) 0.0003(11) 0.0035(11) -0.0117(8) O2 0.0315(12) 0.0182(9) 0.0565(15) 0.0077(9) -0.0073(10) -0.0073(8) O3 0.0229(10) 0.0231(9) 0.0457(13) -0.0054(9) -0.0022(9) -0.0130(8) O4 0.0155(10) 0.0231(9) 0.0431(12) -0.0063(9) -0.0004(8) -0.0044(7) O5 0.0243(11) 0.0454(12) 0.0299(11) -0.0070(9) -0.0048(9) -0.0127(9) O6 0.0191(11) 0.0583(14) 0.0326(12) -0.0097(10) 0.0012(9) -0.0119(10) O7 0.069(2) 0.093(2) 0.0420(17) -0.0195(16) -0.0214(15) 0.0087(17) O8 0.0517(18) 0.088(2) 0.0439(16) -0.0091(15) -0.0179(13) 0.0088(15) O9 0.0460(14) 0.0511(14) 0.0315(13) 0.0034(10) 0.0024(10) -0.0156(11) C1 0.0271(16) 0.0173(12) 0.0397(17) -0.0011(11) -0.0029(13) -0.0071(11) C2 0.0219(14) 0.0183(12) 0.0360(16) 0.0013(11) -0.0012(12) -0.0076(10) C3 0.0236(15) 0.0185(13) 0.0442(18) -0.0056(12) -0.0006(13) -0.0036(11) C4 0.0225(15) 0.0217(13) 0.0366(17) -0.0022(12) 0.0026(12) -0.0054(11) C5 0.0227(15) 0.0211(13) 0.0400(17) 0.0012(12) 0.0019(12) -0.0109(11) C6 0.0193(14) 0.0169(12) 0.0329(15) -0.0003(11) -0.0029(11) -0.0062(10) C7 0.0188(14) 0.0167(12) 0.0353(16) -0.0004(11) 0.0008(11) -0.0068(10) C8 0.0239(16) 0.0309(15) 0.049(2) -0.0045(14) 0.0090(14) -0.0093(12) C9 0.047(2) 0.082(3) 0.044(2) 0.009(2) 0.0075(18) -0.017(2) C10 0.051(3) 0.043(2) 0.113(4) -0.029(2) 0.043(2) -0.0133(18) C11 0.0284(19) 0.081(3) 0.060(3) -0.005(2) 0.0074(17) -0.0203(19) C12 0.0195(13) 0.0157(11) 0.0292(15) 0.0015(10) -0.0031(11) -0.0087(10) C13 0.0255(15) 0.0282(14) 0.0292(15) -0.0019(12) -0.0036(12) -0.0120(11) C14 0.0244(15) 0.0325(15) 0.0314(16) -0.0037(12) -0.0002(12) -0.0152(12) C15 0.0267(16) 0.0364(16) 0.0314(17) -0.0050(13) -0.0007(12) -0.0077(12) C16 0.0361(19) 0.0461(19) 0.0297(17) 0.0011(14) -0.0047(13) -0.0124(14) C17 0.0385(19) 0.056(2) 0.0293(18) -0.0080(15) -0.0005(14) -0.0115(16) C18 0.0298(18) 0.0491(19) 0.0373(19) -0.0102(15) 0.0001(14) -0.0097(14) C19 0.0251(16) 0.0447(18) 0.0342(17) -0.0053(14) -0.0041(13) -0.0096(13) C20 0.0280(19) 0.080(3) 0.054(2) -0.026(2) 0.0018(17) -0.0053(18) C21 0.075(4) 0.100(4) 0.146(6) -0.081(4) -0.022(4) 0.015(3) C22 0.066(4) 0.122(5) 0.173(7) 0.024(5) 0.071(4) -0.006(3) C23 0.051(3) 0.091(4) 0.096(4) -0.027(3) -0.005(3) 0.026(3) C24 0.046(2) 0.054(2) 0.0316(19) 0.0027(16) -0.0075(15) -0.0099(17) C25 0.174(6) 0.055(3) 0.083(4) -0.002(3) 0.076(4) -0.020(3) C26 0.128(5) 0.065(3) 0.111(5) -0.017(3) 0.061(4) -0.030(3) C27 0.085(3) 0.058(3) 0.065(3) 0.002(2) 0.020(2) -0.023(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 O5 2.120(2) . ? Mn1 O4 2.144(2) 2_768 ? Mn1 O9 2.204(3) . ? Mn1 O1 2.215(2) . ? Mn1 O2 2.348(2) . ? Mn1 O3 2.380(2) 1_565 ? Mn1 O4 2.465(2) 1_565 ? Mn1 C1 2.633(3) . ? Mn2 O2 2.135(2) . ? Mn2 O2 2.135(2) 2_678 ? Mn2 O6 2.167(2) . ? Mn2 O6 2.167(2) 2_678 ? Mn2 O3 2.205(2) 1_565 ? Mn2 O3 2.205(2) 2_668 ? O1 C1 1.245(4) . ? O2 C1 1.272(3) . ? O3 C12 1.262(3) . ? O3 Mn2 2.205(2) 1_545 ? O3 Mn1 2.380(2) 1_545 ? O4 C12 1.258(3) . ? O4 Mn1 2.144(2) 2_768 ? O4 Mn1 2.465(2) 1_545 ? O5 C13 1.264(3) . ? O6 C13 1.254(3) . ? O7 C24 1.304(5) . ? O7 H7 0.78(11) . ? O8 C24 1.223(4) . ? O9 C25 1.429(5) . ? C1 C2 1.499(4) . ? C2 C3 1.392(4) . ? C2 C7 1.396(4) . ? C3 C4 1.389(4) . ? C3 H3A 0.9300 . ? C4 C5 1.396(4) . ? C4 C8 1.539(4) . ? C5 C6 1.394(4) . ? C5 H5A 0.9300 . ? C6 C7 1.398(4) . ? C6 C12 1.494(3) . ? C7 H7A 0.9300 . ? C8 C10 1.519(4) . ? C8 C11 1.532(5) . ? C8 C9 1.539(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C13 C14 1.504(4) . ? C14 C15 1.393(4) . ? C14 C19 1.399(4) . ? C15 C16 1.388(4) . ? C15 H15A 0.9300 . ? C16 C17 1.386(5) . ? C16 C24 1.488(5) . ? C17 C18 1.397(5) . ? C17 H17A 0.9300 . ? C18 C19 1.392(4) . ? C18 C20 1.548(5) . ? C19 H19A 0.9300 . ? C20 C22 1.490(7) . ? C20 C23 1.515(6) . ? C20 C21 1.546(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H7 1.58(11) . ? C25 C26 1.377(7) . ? C25 C27 1.450(6) . ? C25 H25A 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 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 O5 Mn1 O4 87.69(8) . 2_768 ? O5 Mn1 O9 163.40(9) . . ? O4 Mn1 O9 81.14(9) 2_768 . ? O5 Mn1 O1 98.29(9) . . ? O4 Mn1 O1 98.71(8) 2_768 . ? O9 Mn1 O1 95.53(10) . . ? O5 Mn1 O2 99.78(8) . . ? O4 Mn1 O2 155.20(7) 2_768 . ? O9 Mn1 O2 95.44(9) . . ? O1 Mn1 O2 56.97(7) . . ? O5 Mn1 O3 91.21(8) . 1_565 ? O4 Mn1 O3 132.59(7) 2_768 1_565 ? O9 Mn1 O3 87.43(8) . 1_565 ? O1 Mn1 O3 128.24(8) . 1_565 ? O2 Mn1 O3 71.29(7) . 1_565 ? O5 Mn1 O4 85.72(8) . 1_565 ? O4 Mn1 O4 79.21(7) 2_768 1_565 ? O9 Mn1 O4 80.17(8) . 1_565 ? O1 Mn1 O4 175.44(9) . 1_565 ? O2 Mn1 O4 124.66(6) . 1_565 ? O3 Mn1 O4 53.48(7) 1_565 1_565 ? O5 Mn1 C1 100.73(9) . . ? O4 Mn1 C1 126.62(8) 2_768 . ? O9 Mn1 C1 95.79(10) . . ? O1 Mn1 C1 28.10(8) . . ? O2 Mn1 C1 28.88(7) . . ? O3 Mn1 C1 100.14(8) 1_565 . ? O4 Mn1 C1 153.25(8) 1_565 . ? O2 Mn2 O2 180.00 . 2_678 ? O2 Mn2 O6 91.23(9) . . ? O2 Mn2 O6 88.77(9) 2_678 . ? O2 Mn2 O6 88.77(9) . 2_678 ? O2 Mn2 O6 91.23(9) 2_678 2_678 ? O6 Mn2 O6 180.000 . 2_678 ? O2 Mn2 O3 78.78(8) . 1_565 ? O2 Mn2 O3 101.22(8) 2_678 1_565 ? O6 Mn2 O3 90.55(8) . 1_565 ? O6 Mn2 O3 89.45(8) 2_678 1_565 ? O2 Mn2 O3 101.22(8) . 2_668 ? O2 Mn2 O3 78.78(8) 2_678 2_668 ? O6 Mn2 O3 89.45(8) . 2_668 ? O6 Mn2 O3 90.55(8) 2_678 2_668 ? O3 Mn2 O3 180.000 1_565 2_668 ? C1 O1 Mn1 94.94(16) . . ? C1 O2 Mn2 151.5(2) . . ? C1 O2 Mn1 88.10(17) . . ? Mn2 O2 Mn1 97.94(8) . . ? C12 O3 Mn2 159.2(2) . 1_545 ? C12 O3 Mn1 94.52(16) . 1_545 ? Mn2 O3 Mn1 95.10(8) 1_545 1_545 ? C12 O4 Mn1 164.72(19) . 2_768 ? C12 O4 Mn1 90.66(15) . 1_545 ? Mn1 O4 Mn1 100.79(7) 2_768 1_545 ? C13 O5 Mn1 126.24(19) . . ? C13 O6 Mn2 138.0(2) . . ? C24 O7 H7 95(8) . . ? C25 O9 Mn1 132.6(4) . . ? O1 C1 O2 120.0(3) . . ? O1 C1 C2 121.5(2) . . ? O2 C1 C2 118.5(3) . . ? O1 C1 Mn1 56.95(14) . . ? O2 C1 Mn1 63.03(15) . . ? C2 C1 Mn1 175.4(2) . . ? C3 C2 C7 120.6(2) . . ? C3 C2 C1 120.1(2) . . ? C7 C2 C1 119.3(2) . . ? C4 C3 C2 121.7(2) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 117.1(3) . . ? C3 C4 C8 122.9(2) . . ? C5 C4 C8 120.0(3) . . ? C6 C5 C4 121.9(3) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C7 120.0(2) . . ? C5 C6 C12 119.8(2) . . ? C7 C6 C12 120.2(2) . . ? C2 C7 C6 118.2(2) . . ? C2 C7 H7A 120.9 . . ? C6 C7 H7A 120.9 . . ? C10 C8 C11 109.0(3) . . ? C10 C8 C4 112.2(3) . . ? C11 C8 C4 110.5(3) . . ? C10 C8 C9 108.9(4) . . ? C11 C8 C9 108.1(3) . . ? C4 C8 C9 108.0(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O4 C12 O3 119.8(2) . . ? O4 C12 C6 120.5(2) . . ? O3 C12 C6 119.7(2) . . ? O6 C13 O5 125.3(3) . . ? O6 C13 C14 117.7(3) . . ? O5 C13 C14 116.9(3) . . ? C15 C14 C19 119.6(3) . . ? C15 C14 C13 119.9(3) . . ? C19 C14 C13 120.4(3) . . ? C16 C15 C14 119.1(3) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 C24 121.4(3) . . ? C15 C16 C24 117.8(3) . . ? C16 C17 C18 121.3(3) . . ? C16 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? C19 C18 C17 117.4(3) . . ? C19 C18 C20 122.4(3) . . ? C17 C18 C20 120.2(3) . . ? C18 C19 C14 121.8(3) . . ? C18 C19 H19A 119.1 . . ? C14 C19 H19A 119.1 . . ? C22 C20 C23 111.5(5) . . ? C22 C20 C21 110.4(5) . . ? C23 C20 C21 105.2(5) . . ? C22 C20 C18 108.8(4) . . ? C23 C20 C18 112.1(3) . . ? C21 C20 C18 108.8(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O8 C24 O7 122.6(3) . . ? O8 C24 C16 121.6(3) . . ? O7 C24 C16 115.8(3) . . ? O8 C24 H7 100(4) . . ? O7 C24 H7 30(4) . . ? C16 C24 H7 135(4) . . ? C26 C25 O9 117.1(4) . . ? C26 C25 C27 125.1(5) . . ? O9 C25 C27 113.1(4) . . ? C26 C25 H25A 97.2 . . ? O9 C25 H25A 97.2 . . ? C27 C25 H25A 97.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.543 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.079