# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Keith Murray' _publ_contact_author_email KEITH.MURRAY@SCI.MONASH.EDU.AU _publ_section_title ; Supertetrahedral icosanuclear and ring-like decanuclear mixed valent manganese(II/III) triethanolamine clusters ; loop_ _publ_author_name 'Keith Murray' 'Kevin J. Berry' 'Stuart K. Langley' 'Boujemaa Moubaraki' # Attachment 'StuartLangleyrepl-1 Mn20final.CIF' #========================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 759480' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C68 H112 Cl4 Mn20 N12 O44, 6(C H4 O), 4(O) ; _chemical_formula_sum 'C74 H144 Cl4 Mn20 N12 O54' _chemical_formula_weight 3306.54 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 30.711(4) _cell_length_b 30.711(4) _cell_length_c 13.202(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12452(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 88859 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.14 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6656 _exptl_absorpt_coefficient_mu 2.121 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77506 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX2' _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 88509 _diffrn_reflns_av_R_equivalents 0.0983 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.14 _reflns_number_total 5324 _reflns_number_gt 5264 _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 asymmetric unit contains five unique manganese ions as well as solvent MeOH and water molecules. One triethanolamine has it's carbon atoms (C8, C9 and C11) disordered over two positions. The solvent consists of three partially occupied MeOH molecules in which the bond lengths are restrained to 1.45 and a water molecule. Non H-atoms were refined anisotropically except for the water solvent molecule. H atoms were included in calculated positions, except for the H atoms found on the hydroxides which were refined freely and the H-atoms on the solvent waters. ; _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^)+(0.1034P)^2^+79.0480P] 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 5324 _refine_ls_number_parameters 430 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.2137 _refine_ls_wR_factor_gt 0.2049 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Mn2 Mn 0.98251(3) 0.30860(3) 0.03277(5) 0.0430(2) Uani 1 1 d . . . Mn3 Mn 0.88251(3) 0.27368(3) 0.02229(6) 0.0487(2) Uani 1 1 d . D . Mn4 Mn 0.95625(3) 0.24184(3) -0.13958(6) 0.0491(2) Uani 1 1 d . . . Mn1 Mn 0.91660(3) 0.32786(3) 0.21683(5) 0.0464(2) Uani 1 1 d . . . Mn5 Mn 0.86674(3) 0.19859(3) -0.14486(6) 0.0564(3) Uani 1 1 d . . . O6 O 1.03341(12) 0.30827(12) 0.1229(2) 0.0459(8) Uani 1 1 d . . . O2 O 0.96628(13) 0.33655(12) 0.2996(3) 0.0501(9) Uani 1 1 d . . . O7 O 1.0000 0.2500 -0.0387(3) 0.0454(11) Uani 1 2 d S . . O8 O 0.93420(13) 0.30523(13) -0.0702(3) 0.0496(9) Uani 1 1 d . D . O10 O 1.0000 0.2500 -0.2296(4) 0.0569(14) Uani 1 2 d S . . O5 O 1.01880(13) 0.34090(14) -0.0565(3) 0.0494(9) Uani 1 1 d . . . O1 O 0.89236(14) 0.37422(14) 0.2980(3) 0.0554(9) Uani 1 1 d . . . O3 O 0.96228(14) 0.37217(13) 0.1114(3) 0.0549(10) Uani 1 1 d . . . O4 O 0.86493(13) 0.32249(13) 0.1358(3) 0.0520(9) Uani 1 1 d . D . O11 O 0.91115(14) 0.23520(15) -0.2410(3) 0.0574(10) Uani 1 1 d . . . O13 O 0.83392(15) 0.24217(15) -0.0732(3) 0.0618(11) Uani 1 1 d . D . N2 N 0.84800(17) 0.33088(18) -0.0698(4) 0.0581(12) Uani 1 1 d . . . N3 N 0.8946(2) 0.14714(19) -0.2530(4) 0.0657(14) Uani 1 1 d . . . O12 O 0.8170(2) 0.1849(2) -0.2219(5) 0.0952(18) Uani 1 1 d . . . C13 C 0.9224(2) 0.2138(2) -0.3326(4) 0.0605(15) Uani 1 1 d . . . H13A H 0.9486 0.2275 -0.3627 0.073 Uiso 1 1 calc R . . H13B H 0.8982 0.2162 -0.3819 0.073 Uiso 1 1 calc R . . C12 C 0.9217(2) 0.3370(2) -0.1430(4) 0.0543(13) Uani 1 1 d . . . H12A H 0.9150 0.3224 -0.2081 0.065 Uiso 1 1 calc R A 1 H12B H 0.9461 0.3574 -0.1546 0.065 Uiso 1 1 calc R A 1 C7 C 0.8417(2) 0.3602(2) 0.1035(4) 0.0593(15) Uani 1 1 d . . . H7A H 0.8621 0.3850 0.0969 0.071 Uiso 1 1 calc R B 1 H7B H 0.8195 0.3680 0.1549 0.071 Uiso 1 1 calc R B 1 C17 C 0.9087(3) 0.1092(2) -0.1924(4) 0.0673(17) Uani 1 1 d . . . H17A H 0.9392 0.1135 -0.1704 0.081 Uiso 1 1 calc R . . H17B H 0.9077 0.0827 -0.2351 0.081 Uiso 1 1 calc R . . C14 C 0.9315(3) 0.1665(2) -0.3090(4) 0.0678(17) Uani 1 1 d . . . H14A H 0.9361 0.1503 -0.3729 0.081 Uiso 1 1 calc R . . H14B H 0.9583 0.1642 -0.2679 0.081 Uiso 1 1 calc R . . C10 C 0.8023(2) 0.2689(2) -0.1230(5) 0.0621(16) Uani 1 1 d . . . H10A H 0.7782 0.2758 -0.0757 0.075 Uiso 1 1 calc R C 1 H10B H 0.7900 0.2532 -0.1817 0.075 Uiso 1 1 calc R C 1 C15 C 0.8582(3) 0.1352(3) -0.3201(5) 0.075(2) Uani 1 1 d . . . H15A H 0.8448 0.1078 -0.2959 0.090 Uiso 1 1 calc R . . H15B H 0.8693 0.1303 -0.3895 0.090 Uiso 1 1 calc R . . C16 C 0.8245(3) 0.1703(4) -0.3221(7) 0.103(3) Uani 1 1 d . . . H16A H 0.8347 0.1948 -0.3646 0.123 Uiso 1 1 calc R . . H16B H 0.7972 0.1589 -0.3515 0.123 Uiso 1 1 calc R . . C9 C 0.8237(3) 0.3110(4) -0.1587(6) 0.062(3) Uani 0.671(12) 1 d P D 1 H9A H 0.8442 0.3048 -0.2148 0.075 Uiso 0.671(12) 1 calc PR D 1 H9B H 0.8013 0.3315 -0.1835 0.075 Uiso 0.671(12) 1 calc PR D 1 C11 C 0.8834(3) 0.3614(3) -0.1090(6) 0.056(2) Uani 0.671(12) 1 d P D 1 H11A H 0.8718 0.3788 -0.1660 0.067 Uiso 0.671(12) 1 calc PR D 1 H11B H 0.8921 0.3818 -0.0544 0.067 Uiso 0.671(12) 1 calc PR D 1 C8 C 0.8190(4) 0.3520(4) 0.0001(6) 0.058(2) Uani 0.671(12) 1 d P D 1 H8A H 0.7929 0.3335 0.0106 0.070 Uiso 0.671(12) 1 calc PR D 1 H8B H 0.8092 0.3801 -0.0288 0.070 Uiso 0.671(12) 1 calc PR D 1 Cl1 Cl 0.98576(10) 0.46021(7) -0.18809(15) 0.0992(7) Uani 1 1 d . . . N1 N 0.97244(19) 0.41752(16) -0.0219(4) 0.0592(12) Uani 1 1 d . . . C2 C 0.9332(3) 0.4439(2) 0.1227(5) 0.0718(19) Uani 1 1 d . . . H2 H 0.9219 0.4392 0.1888 0.086 Uiso 1 1 calc R . . C1 C 0.9558(2) 0.4109(2) 0.0716(4) 0.0568(14) Uani 1 1 d . . . C6 C 0.8527(2) 0.3695(3) 0.3514(4) 0.0657(17) Uani 1 1 d . . . H6A H 0.8306 0.3563 0.3065 0.079 Uiso 1 1 calc R . . H6B H 0.8420 0.3985 0.3729 0.079 Uiso 1 1 calc R . . C5 C 0.9655(3) 0.4560(2) -0.0642(5) 0.0725(19) Uani 1 1 d . . . C3 C 0.9278(3) 0.4828(3) 0.0753(6) 0.090(3) Uani 1 1 d . . . H3 H 0.9124 0.5055 0.1088 0.108 Uiso 1 1 calc R . . C4 C 0.9443(4) 0.4902(3) -0.0202(6) 0.093(3) Uani 1 1 d . . . H4 H 0.9412 0.5174 -0.0535 0.112 Uiso 1 1 calc R . . O1S O 0.7554(7) 0.1341(6) -0.1604(15) 0.144(7) Uani 0.50 1 d PD . . H1S H 0.7641 0.1170 -0.1150 0.172 Uiso 0.50 1 calc PR . . O4S O 0.7520(8) 0.0671(8) -0.3047(19) 0.348(11) Uiso 1 1 d . . . O3S O 0.7655(6) 0.4203(9) 0.479(2) 0.195(11) Uani 0.50 1 d PD . . H3S H 0.7617 0.4030 0.5271 0.234 Uiso 0.50 1 calc PR . . C3S C 0.7246(7) 0.4390(8) 0.450(2) 0.126(8) Uani 0.50 1 d PD . . H3S1 H 0.7178 0.4635 0.4950 0.189 Uiso 0.50 1 calc PR . . H3S2 H 0.7016 0.4170 0.4555 0.189 Uiso 0.50 1 calc PR . . H3S3 H 0.7263 0.4494 0.3799 0.189 Uiso 0.50 1 calc PR . . C2S C 0.6507(10) 0.0292(7) -0.321(2) 0.160(12) Uani 0.50 1 d PD . . H2S1 H 0.6279 0.0513 -0.3148 0.240 Uiso 0.50 1 calc PR . . H2S2 H 0.6383 0.0003 -0.3085 0.240 Uiso 0.50 1 calc PR . . H2S3 H 0.6633 0.0302 -0.3889 0.240 Uiso 0.50 1 calc PR . . O2S O 0.6842(9) 0.0377(11) -0.247(2) 0.227(13) Uani 0.50 1 d PD . . H2S H 0.7060 0.0443 -0.2732 0.273 Uiso 0.50 1 d P . . C11' C 0.8710(6) 0.3343(7) -0.1569(13) 0.058(5) Uani 0.329(12) 1 d P D 2 H11C H 0.8611 0.3606 -0.1934 0.070 Uiso 0.329(12) 1 calc PR D 2 H11D H 0.8642 0.3088 -0.2000 0.070 Uiso 0.329(12) 1 calc PR D 2 C9' C 0.8017(6) 0.3142(8) -0.0789(16) 0.070(6) Uani 0.329(12) 1 d P D 2 H9'1 H 0.7878 0.3137 -0.0113 0.084 Uiso 0.329(12) 1 calc PR D 2 H9'2 H 0.7846 0.3338 -0.1233 0.084 Uiso 0.329(12) 1 calc PR D 2 C8' C 0.8466(10) 0.3683(8) 0.0016(14) 0.067(6) Uani 0.329(12) 1 d P D 2 H8'1 H 0.8738 0.3851 -0.0073 0.081 Uiso 0.329(12) 1 calc PR D 2 H8'2 H 0.8223 0.3875 -0.0197 0.081 Uiso 0.329(12) 1 calc PR D 2 C1S C 0.7341(10) 0.1705(9) -0.115(2) 0.201(19) Uani 0.50 1 d PD . . H1S1 H 0.7299 0.1648 -0.0425 0.302 Uiso 0.50 1 calc PR . . H1S2 H 0.7058 0.1750 -0.1474 0.302 Uiso 0.50 1 calc PR . . H1S3 H 0.7522 0.1965 -0.1235 0.302 Uiso 0.50 1 calc PR . . H14 H 1.009(2) 0.365(2) -0.063(5) 0.054(19) 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 Mn2 0.0554(5) 0.0547(5) 0.0189(4) 0.0018(3) 0.0000(3) 0.0003(3) Mn3 0.0565(5) 0.0644(5) 0.0253(4) 0.0000(3) 0.0004(3) 0.0024(4) Mn4 0.0598(5) 0.0685(5) 0.0190(4) -0.0023(3) -0.0021(3) -0.0006(4) Mn1 0.0584(5) 0.0578(5) 0.0230(4) -0.0015(3) 0.0012(3) 0.0035(4) Mn5 0.0632(6) 0.0741(6) 0.0319(4) -0.0043(4) -0.0101(4) -0.0005(4) O6 0.058(2) 0.055(2) 0.0252(17) -0.0023(14) 0.0001(14) -0.0021(16) O2 0.062(2) 0.056(2) 0.0322(18) -0.0034(15) -0.0025(16) -0.0004(17) O7 0.059(3) 0.057(3) 0.020(2) 0.000 0.000 -0.001(2) O8 0.061(2) 0.063(2) 0.0254(16) 0.0029(15) -0.0009(15) 0.0037(17) O10 0.071(4) 0.083(4) 0.017(2) 0.000 0.000 -0.003(3) O5 0.062(2) 0.059(2) 0.0271(17) 0.0057(16) -0.0008(15) 0.0001(18) O1 0.062(2) 0.072(3) 0.0318(18) -0.0025(17) 0.0029(16) 0.0066(19) O3 0.075(3) 0.055(2) 0.0347(19) 0.0070(16) 0.0058(17) 0.0054(19) O4 0.064(2) 0.062(2) 0.0300(17) 0.0002(16) -0.0026(16) 0.0078(18) O11 0.071(3) 0.076(3) 0.0254(17) -0.0039(17) -0.0058(16) -0.001(2) O13 0.068(3) 0.083(3) 0.034(2) 0.0051(19) -0.0066(18) 0.003(2) N2 0.064(3) 0.077(3) 0.033(2) 0.004(2) -0.004(2) 0.008(2) N3 0.088(4) 0.080(4) 0.029(2) -0.004(2) -0.005(2) -0.001(3) O12 0.088(4) 0.119(5) 0.079(4) -0.021(3) -0.020(3) 0.009(3) C13 0.081(4) 0.080(4) 0.021(2) -0.003(2) -0.007(2) -0.003(3) C12 0.066(3) 0.066(3) 0.031(2) 0.006(2) -0.004(2) 0.000(3) C7 0.067(4) 0.071(4) 0.040(3) 0.002(3) -0.006(3) 0.014(3) C17 0.101(5) 0.071(4) 0.029(3) -0.005(3) -0.005(3) 0.000(3) C14 0.092(5) 0.086(5) 0.025(3) -0.007(3) -0.001(3) 0.006(4) C10 0.056(3) 0.093(5) 0.038(3) -0.004(3) -0.006(2) 0.007(3) C15 0.097(5) 0.096(5) 0.034(3) -0.011(3) -0.008(3) -0.004(4) C16 0.110(7) 0.128(8) 0.070(5) -0.010(5) -0.036(5) 0.000(6) C9 0.071(6) 0.091(7) 0.025(4) 0.000(4) -0.006(4) 0.014(5) C11 0.072(6) 0.068(6) 0.027(4) 0.005(4) -0.001(4) 0.012(4) C8 0.060(6) 0.082(7) 0.033(4) 0.002(4) 0.000(4) 0.014(5) Cl1 0.160(2) 0.0817(13) 0.0558(11) 0.0272(9) 0.0123(12) 0.0033(13) N1 0.080(3) 0.053(3) 0.044(3) 0.008(2) -0.002(2) -0.003(2) C2 0.102(5) 0.063(4) 0.050(4) 0.002(3) -0.002(3) 0.013(4) C1 0.075(4) 0.058(3) 0.038(3) 0.001(2) -0.005(3) -0.001(3) C6 0.072(4) 0.093(5) 0.032(3) -0.006(3) 0.008(3) 0.009(3) C5 0.105(6) 0.066(4) 0.046(3) 0.015(3) 0.000(3) -0.001(4) C3 0.142(8) 0.063(4) 0.064(5) 0.002(4) 0.004(5) 0.022(4) C4 0.150(8) 0.061(4) 0.068(5) 0.015(4) 0.007(5) 0.019(5) O1S 0.143(14) 0.141(14) 0.148(16) -0.010(12) -0.070(13) 0.005(11) O3S 0.118(14) 0.22(3) 0.24(3) -0.12(2) -0.015(15) 0.009(14) C3S 0.110(16) 0.137(19) 0.13(2) 0.028(15) -0.034(14) -0.035(14) C2S 0.25(4) 0.070(12) 0.16(3) 0.027(15) -0.03(3) -0.041(17) O2S 0.21(3) 0.29(4) 0.19(2) -0.04(2) 0.00(2) -0.06(2) C11' 0.070(12) 0.077(13) 0.028(8) 0.015(8) -0.002(7) 0.015(9) C9' 0.053(10) 0.107(17) 0.050(11) 0.011(11) -0.012(8) 0.010(10) C8' 0.082(17) 0.084(15) 0.036(9) -0.002(9) -0.002(10) 0.020(12) C1S 0.16(3) 0.34(5) 0.10(2) -0.04(3) 0.09(2) -0.08(3) _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 Mn2 O5 1.901(4) . ? Mn2 O6 1.928(4) 16_645 ? Mn2 O6 1.965(4) . ? Mn2 O8 2.014(4) . ? Mn2 O7 2.102(2) . ? Mn2 O3 2.297(4) . ? Mn3 O13 2.180(4) . ? Mn3 O4 2.188(4) . ? Mn3 O2 2.216(4) 16_645 ? Mn3 O8 2.225(4) . ? Mn3 O6 2.304(4) 16_645 ? Mn3 N2 2.385(5) . ? Mn3 O3 2.436(4) 16_645 ? Mn4 O10 1.811(3) . ? Mn4 O7 1.909(3) . ? Mn4 O11 1.937(4) . ? Mn4 O2 1.937(4) 16_645 ? Mn4 O8 2.256(4) . ? Mn1 O2 1.896(4) . ? Mn1 O4 1.920(4) . ? Mn1 O1 1.931(4) . ? Mn1 O6 1.965(4) 16_645 ? Mn1 O5 2.178(4) 16_645 ? Mn1 O3 2.400(4) . ? Mn1 Mn2 3.0257(12) 16_645 ? Mn5 O12 1.882(6) . ? Mn5 O13 1.924(5) . ? Mn5 O2 1.983(4) 16_645 ? Mn5 O1 2.167(4) 16_645 ? Mn5 O11 2.176(4) . ? Mn5 N3 2.296(6) . ? Mn5 Mn1 3.0636(12) 16_645 ? O6 Mn2 1.928(4) 14_665 ? O6 Mn1 1.965(4) 14_665 ? O6 Mn3 2.304(4) 14_665 ? O2 Mn4 1.937(4) 14_665 ? O2 Mn5 1.983(4) 14_665 ? O2 Mn3 2.216(4) 14_665 ? O7 Mn4 1.909(3) 3_755 ? O7 Mn2 2.102(2) 3_755 ? O8 C12 1.422(7) . ? O10 Mn4 1.811(3) 3_755 ? O5 Mn1 2.178(4) 14_665 ? O5 H14 0.81(7) . ? O1 C6 1.414(8) . ? O1 Mn5 2.167(4) 14_665 ? O3 C1 1.315(7) . ? O3 Mn3 2.436(4) 14_665 ? O4 C7 1.427(7) . ? O11 C13 1.419(7) . ? O13 C10 1.433(8) . ? N2 C11' 1.352(18) . ? N2 C8 1.438(10) . ? N2 C8' 1.49(2) . ? N2 C9' 1.52(2) . ? N2 C9 1.518(10) . ? N2 C11 1.526(11) . ? N3 C15 1.473(9) . ? N3 C14 1.476(9) . ? N3 C17 1.479(9) . ? O12 C16 1.416(11) . ? C13 C14 1.511(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C12 C11 1.464(11) . ? C12 C11' 1.57(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C7 C8' 1.38(2) . ? C7 C8 1.553(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C17 C6 1.494(9) 16_645 ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C10 C9' 1.51(3) . ? C10 C9 1.524(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C15 C16 1.492(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? Cl1 C5 1.755(7) . ? N1 C5 1.324(8) . ? N1 C1 1.351(8) . ? C2 C3 1.359(10) . ? C2 C1 1.401(9) . ? C2 H2 0.9500 . ? C6 C17 1.494(9) 14_665 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 C4 1.365(11) . ? C3 C4 1.378(12) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? O1S C1S 1.426(10) . ? O1S H1S 0.8400 . ? O3S C3S 1.432(10) . ? O3S H3S 0.8400 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C2S O2S 1.438(10) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? O2S H2S 0.7792 . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C9' H9'1 0.9900 . ? C9' H9'2 0.9900 . ? C8' H8'1 0.9900 . ? C8' H8'2 0.9900 . ? 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 O5 Mn2 O6 172.05(18) . 16_645 ? O5 Mn2 O6 84.93(16) . . ? O6 Mn2 O6 97.10(15) 16_645 . ? O5 Mn2 O8 92.32(16) . . ? O6 Mn2 O8 86.37(15) 16_645 . ? O6 Mn2 O8 173.87(15) . . ? O5 Mn2 O7 91.08(16) . . ? O6 Mn2 O7 96.44(14) 16_645 . ? O6 Mn2 O7 93.68(13) . . ? O8 Mn2 O7 80.88(14) . . ? O5 Mn2 O3 89.71(17) . . ? O6 Mn2 O3 82.74(15) 16_645 . ? O6 Mn2 O3 86.90(16) . . ? O8 Mn2 O3 98.59(16) . . ? O7 Mn2 O3 179.06(12) . . ? O13 Mn3 O4 122.11(17) . . ? O13 Mn3 O2 72.11(16) . 16_645 ? O4 Mn3 O2 160.81(14) . 16_645 ? O13 Mn3 O8 111.39(15) . . ? O4 Mn3 O8 104.69(15) . . ? O2 Mn3 O8 78.77(14) 16_645 . ? O13 Mn3 O6 160.89(16) . 16_645 ? O4 Mn3 O6 72.21(14) . 16_645 ? O2 Mn3 O6 91.26(14) 16_645 16_645 ? O8 Mn3 O6 73.13(13) . 16_645 ? O13 Mn3 N2 74.22(18) . . ? O4 Mn3 N2 74.63(16) . . ? O2 Mn3 N2 123.91(16) 16_645 . ? O8 Mn3 N2 73.53(16) . . ? O6 Mn3 N2 124.14(17) 16_645 . ? O13 Mn3 O3 88.88(15) . 16_645 ? O4 Mn3 O3 94.81(14) . 16_645 ? O2 Mn3 O3 71.33(14) 16_645 16_645 ? O8 Mn3 O3 136.48(14) . 16_645 ? O6 Mn3 O3 76.61(13) 16_645 16_645 ? N2 Mn3 O3 149.93(17) . 16_645 ? O10 Mn4 O7 85.26(15) . . ? O10 Mn4 O11 95.25(17) . . ? O7 Mn4 O11 178.34(15) . . ? O10 Mn4 O2 164.04(13) . 16_645 ? O7 Mn4 O2 95.92(15) . 16_645 ? O11 Mn4 O2 84.03(17) . 16_645 ? O10 Mn4 O8 111.70(11) . . ? O7 Mn4 O8 79.31(10) . . ? O11 Mn4 O8 99.04(17) . . ? O2 Mn4 O8 84.09(16) 16_645 . ? O2 Mn1 O4 176.43(17) . . ? O2 Mn1 O1 83.48(17) . . ? O4 Mn1 O1 93.08(17) . . ? O2 Mn1 O6 97.43(16) . 16_645 ? O4 Mn1 O6 85.94(16) . 16_645 ? O1 Mn1 O6 176.30(16) . 16_645 ? O2 Mn1 O5 83.63(16) . 16_645 ? O4 Mn1 O5 98.27(17) . 16_645 ? O1 Mn1 O5 105.76(16) . 16_645 ? O6 Mn1 O5 77.92(14) 16_645 16_645 ? O2 Mn1 O3 77.54(16) . . ? O4 Mn1 O3 102.04(16) . . ? O1 Mn1 O3 97.42(16) . . ? O6 Mn1 O3 79.32(15) 16_645 . ? O5 Mn1 O3 148.15(15) 16_645 . ? O2 Mn1 Mn2 86.14(12) . 16_645 ? O4 Mn1 Mn2 97.24(12) . 16_645 ? O1 Mn1 Mn2 144.05(13) . 16_645 ? O6 Mn1 Mn2 39.65(10) 16_645 16_645 ? O5 Mn1 Mn2 38.72(10) 16_645 16_645 ? O3 Mn1 Mn2 113.75(10) . 16_645 ? O12 Mn5 O13 89.8(2) . . ? O12 Mn5 O2 172.1(2) . 16_645 ? O13 Mn5 O2 82.91(17) . 16_645 ? O12 Mn5 O1 104.2(2) . 16_645 ? O13 Mn5 O1 109.34(17) . 16_645 ? O2 Mn5 O1 75.62(16) 16_645 16_645 ? O12 Mn5 O11 108.0(2) . . ? O13 Mn5 O11 104.83(18) . . ? O2 Mn5 O11 76.98(15) 16_645 . ? O1 Mn5 O11 132.50(17) 16_645 . ? O12 Mn5 N3 79.2(2) . . ? O13 Mn5 N3 168.57(19) . . ? O2 Mn5 N3 108.24(19) 16_645 . ? O1 Mn5 N3 76.74(17) 16_645 . ? O11 Mn5 N3 76.05(19) . . ? O12 Mn5 Mn1 142.5(2) . 16_645 ? O13 Mn5 Mn1 97.85(12) . 16_645 ? O2 Mn5 Mn1 36.85(11) 16_645 16_645 ? O1 Mn5 Mn1 38.78(11) 16_645 16_645 ? O11 Mn5 Mn1 105.37(11) . 16_645 ? N3 Mn5 Mn1 92.82(14) . 16_645 ? Mn2 O6 Mn2 135.5(2) 14_665 . ? Mn2 O6 Mn1 111.45(19) 14_665 14_665 ? Mn2 O6 Mn1 100.69(15) . 14_665 ? Mn2 O6 Mn3 100.19(13) 14_665 14_665 ? Mn2 O6 Mn3 104.86(17) . 14_665 ? Mn1 O6 Mn3 98.17(16) 14_665 14_665 ? Mn1 O2 Mn4 125.7(2) . 14_665 ? Mn1 O2 Mn5 104.29(19) . 14_665 ? Mn4 O2 Mn5 102.31(17) 14_665 14_665 ? Mn1 O2 Mn3 116.96(18) . 14_665 ? Mn4 O2 Mn3 103.37(18) 14_665 14_665 ? Mn5 O2 Mn3 100.33(17) 14_665 14_665 ? Mn4 O7 Mn4 91.5(2) . 3_755 ? Mn4 O7 Mn2 112.38(6) . 3_755 ? Mn4 O7 Mn2 104.22(5) 3_755 3_755 ? Mn4 O7 Mn2 104.22(5) . . ? Mn4 O7 Mn2 112.38(6) 3_755 . ? Mn2 O7 Mn2 126.7(2) 3_755 . ? C12 O8 Mn2 128.3(4) . . ? C12 O8 Mn3 118.4(3) . . ? Mn2 O8 Mn3 100.24(15) . . ? C12 O8 Mn4 113.5(3) . . ? Mn2 O8 Mn4 95.59(16) . . ? Mn3 O8 Mn4 93.51(15) . . ? Mn4 O10 Mn4 98.0(2) 3_755 . ? Mn2 O5 Mn1 95.52(16) . 14_665 ? Mn2 O5 H14 109(5) . . ? Mn1 O5 H14 118(5) 14_665 . ? C6 O1 Mn1 122.2(4) . . ? C6 O1 Mn5 113.9(3) . 14_665 ? Mn1 O1 Mn5 96.59(18) . 14_665 ? C1 O3 Mn2 129.0(4) . . ? C1 O3 Mn1 131.0(4) . . ? Mn2 O3 Mn1 86.45(14) . . ? C1 O3 Mn3 115.0(4) . 14_665 ? Mn2 O3 Mn3 91.45(15) . 14_665 ? Mn1 O3 Mn3 93.05(13) . 14_665 ? C7 O4 Mn1 120.7(4) . . ? C7 O4 Mn3 118.3(3) . . ? Mn1 O4 Mn3 103.68(18) . . ? C13 O11 Mn4 117.6(4) . . ? C13 O11 Mn5 114.3(4) . . ? Mn4 O11 Mn5 95.70(16) . . ? C10 O13 Mn5 121.9(4) . . ? C10 O13 Mn3 118.3(4) . . ? Mn5 O13 Mn3 103.6(2) . . ? C11' N2 C8 146.5(11) . . ? C11' N2 C8' 119.6(15) . . ? C8 N2 C8' 39.3(10) . . ? C11' N2 C9' 116.6(12) . . ? C8 N2 C9' 67.8(10) . . ? C8' N2 C9' 106.5(15) . . ? C11' N2 C9 68.4(10) . . ? C8 N2 C9 111.8(7) . . ? C8' N2 C9 141.8(11) . . ? C9' N2 C9 48.8(9) . . ? C11' N2 C11 45.0(10) . . ? C8 N2 C11 112.5(7) . . ? C8' N2 C11 76.2(12) . . ? C9' N2 C11 148.1(9) . . ? C9 N2 C11 109.6(6) . . ? C11' N2 Mn3 105.0(8) . . ? C8 N2 Mn3 106.3(5) . . ? C8' N2 Mn3 105.0(8) . . ? C9' N2 Mn3 102.0(9) . . ? C9 N2 Mn3 108.4(5) . . ? C11 N2 Mn3 108.0(4) . . ? C15 N3 C14 112.4(5) . . ? C15 N3 C17 110.6(6) . . ? C14 N3 C17 111.4(6) . . ? C15 N3 Mn5 105.1(4) . . ? C14 N3 Mn5 108.6(4) . . ? C17 N3 Mn5 108.4(3) . . ? C16 O12 Mn5 116.3(6) . . ? O11 C13 C14 108.3(5) . . ? O11 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? O11 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? O8 C12 C11 111.2(5) . . ? O8 C12 C11' 108.1(8) . . ? C11 C12 C11' 42.9(9) . . ? O8 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C11' C12 H12A 70.7 . . ? O8 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? C11' C12 H12B 140.2 . . ? H12A C12 H12B 108.0 . . ? C8' C7 O4 112.6(10) . . ? C8' C7 C8 38.7(12) . . ? O4 C7 C8 110.9(6) . . ? C8' C7 H7A 73.0 . . ? O4 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C8' C7 H7B 134.6 . . ? O4 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N3 C17 C6 111.7(6) . 16_645 ? N3 C17 H17A 109.3 . . ? C6 C17 H17A 109.3 16_645 . ? N3 C17 H17B 109.3 . . ? C6 C17 H17B 109.3 16_645 . ? H17A C17 H17B 107.9 . . ? N3 C14 C13 110.5(6) . . ? N3 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O13 C10 C9' 111.1(8) . . ? O13 C10 C9 109.6(6) . . ? C9' C10 C9 48.9(9) . . ? O13 C10 H10A 109.7 . . ? C9' C10 H10A 63.4 . . ? C9 C10 H10A 109.7 . . ? O13 C10 H10B 109.7 . . ? C9' C10 H10B 138.5 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N3 C15 C16 111.0(6) . . ? N3 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N3 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? O12 C16 C15 109.0(7) . . ? O12 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? O12 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? N2 C9 C10 108.3(6) . . ? N2 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? N2 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C12 C11 N2 111.2(7) . . ? C12 C11 H11A 109.4 . . ? N2 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? N2 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N2 C8 C7 111.0(7) . . ? N2 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N2 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C5 N1 C1 117.3(6) . . ? C3 C2 C1 118.4(7) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? O3 C1 N1 116.3(5) . . ? O3 C1 C2 122.5(6) . . ? N1 C1 C2 121.2(6) . . ? O1 C6 C17 110.3(6) . 14_665 ? O1 C6 H6A 109.6 . . ? C17 C6 H6A 109.6 14_665 . ? O1 C6 H6B 109.6 . . ? C17 C6 H6B 109.6 14_665 . ? H6A C6 H6B 108.1 . . ? N1 C5 C4 125.7(7) . . ? N1 C5 Cl1 113.8(6) . . ? C4 C5 Cl1 120.6(5) . . ? C2 C3 C4 121.3(8) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 116.1(7) . . ? C5 C4 H4 122.0 . . ? C3 C4 H4 122.0 . . ? C1S O1S H1S 109.5 . . ? C3S O3S H3S 109.5 . . ? 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 . . ? 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 . . ? C2S O2S H2S 111.2 . . ? N2 C11' C12 115.0(12) . . ? N2 C11' H11C 108.5 . . ? C12 C11' H11C 108.5 . . ? N2 C11' H11D 108.5 . . ? C12 C11' H11D 108.5 . . ? H11C C11' H11D 107.5 . . ? C10 C9' N2 109.3(13) . . ? C10 C9' H9'1 109.8 . . ? N2 C9' H9'1 109.8 . . ? C10 C9' H9'2 109.8 . . ? N2 C9' H9'2 109.8 . . ? H9'1 C9' H9'2 108.3 . . ? C7 C8' N2 118.9(18) . . ? C7 C8' H8'1 107.6 . . ? N2 C8' H8'1 107.6 . . ? C7 C8' H8'2 107.6 . . ? N2 C8' H8'2 107.6 . . ? H8'1 C8' H8'2 107.0 . . ? 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 0.988 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.625 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.111 data_2_Mn10_tpaa _database_code_depnum_ccdc_archive 'CCDC 759481' _publ_section_exptl_refinement ; The asymmetric unit contains half the cluster as well as 2 MeCN and 1 diethyl ether solvent molecules. All non H atoms were refined anisotropically. H-atoms are placed in calculated positions except for protonated hydrogens found on the teaH and teaH2 ligands, which were refined. ; _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety ; C156 H170 F8 Mn10 N6 O30, 2(C4 H10 O), 4(C2 H3 N) ; _chemical_formula_sum 'C172 H202 F8 Mn10 N10 O32' _chemical_formula_weight 3622.84 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' Mn Mn 0.3368 0.7283 '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' F F 0.0171 0.0103 '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 15.0189(3) _cell_length_b 16.8546(4) _cell_length_c 17.5974(4) _cell_angle_alpha 100.0530(10) _cell_angle_beta 105.1330(10) _cell_angle_gamma 99.4390(10) _cell_volume 4129.87(16) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9299 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 30.43 _exptl_crystal_description Block _exptl_crystal_colour brown _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1882 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_T_max 0.848 _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 Apex CCD' _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 68060 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.54 _reflns_number_total 24285 _reflns_number_gt 16560 _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 X-SEED _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 asymmetric unit contains half the cluster as well as 2 MeCN and 1 diethyl ether solvent molecules. All non H atoms were refined anisotropically. H-atoms are placed in calculated positions except for protonated hydrogens found on the teaH and teaH2 ligands, which were refined. ; _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^)+(0.0610P)^2^+1.8631P] 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 24285 _refine_ls_number_parameters 1065 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Mn3 Mn 0.07515(2) 0.00985(2) 0.25762(2) 0.01137(8) Uani 1 1 d . . . Mn1 Mn -0.11385(2) -0.01555(2) 0.445284(19) 0.01017(8) Uani 1 1 d . . . Mn4 Mn 0.11283(2) 0.14138(2) 0.423822(19) 0.01049(8) Uani 1 1 d . . . Mn2 Mn -0.06009(2) -0.15553(2) 0.256942(19) 0.01015(8) Uani 1 1 d . . . Mn5 Mn 0.13919(2) 0.23271(2) 0.61011(2) 0.01061(8) Uani 1 1 d . . . F2 F 0.02807(9) 0.03621(8) 0.44716(7) 0.0124(3) Uani 1 1 d . . . F4 F 0.17740(9) 0.07139(8) 0.37352(7) 0.0147(3) Uani 1 1 d . . . N1 N -0.27988(13) -0.02103(12) 0.40706(11) 0.0138(4) Uani 1 1 d . . . F3 F 0.06624(9) -0.08992(8) 0.32067(7) 0.0141(3) Uani 1 1 d . . . F1 F -0.11166(9) -0.11377(8) 0.35504(7) 0.0138(3) Uani 1 1 d . . . O12 O 0.19335(10) 0.14440(10) 0.52973(9) 0.0124(3) Uani 1 1 d . . . O13 O 0.05510(11) 0.20830(10) 0.48450(9) 0.0138(3) Uani 1 1 d . . . O10 O 0.20563(11) 0.25618(10) 0.41256(9) 0.0166(3) Uani 1 1 d . . . O6 O -0.07058(11) -0.06238(10) 0.21362(9) 0.0121(3) Uani 1 1 d . . . O2 O -0.13009(11) 0.09152(10) 0.52870(10) 0.0157(3) Uani 1 1 d . . . O7 O 0.10805(11) -0.09078(10) 0.17423(10) 0.0161(3) Uani 1 1 d . . . O9 O 0.02056(11) 0.11568(10) 0.31980(9) 0.0136(3) Uani 1 1 d . . . O15 O 0.25628(11) 0.27064(10) 0.72550(9) 0.0158(3) Uani 1 1 d . . . O5 O 0.00612(11) -0.20553(10) 0.17208(9) 0.0149(3) Uani 1 1 d . . . O14 O 0.24036(12) 0.33019(10) 0.57871(11) 0.0175(4) Uani 1 1 d . . . O4 O -0.05094(11) -0.24121(10) 0.30983(9) 0.0148(3) Uani 1 1 d . . . O1 O -0.14598(13) 0.05573(12) 0.34782(11) 0.0181(4) Uani 1 1 d . . . O8 O 0.18515(12) 0.08185(12) 0.21697(10) 0.0182(4) Uani 1 1 d . . . O3 O -0.19134(11) -0.20973(10) 0.19181(9) 0.0161(3) Uani 1 1 d . . . C42 C 0.14322(16) -0.29336(15) 0.14911(14) 0.0155(5) Uani 1 1 d . . . C9 C -0.43188(16) -0.33799(14) 0.13755(13) 0.0145(5) Uani 1 1 d . . . N3 N 0.06274(14) 0.34732(12) 0.59493(11) 0.0150(4) Uani 1 1 d . . . C29 C 0.12456(16) -0.22343(14) 0.10517(13) 0.0128(5) Uani 1 1 d . . . C10 C -0.46178(17) -0.30276(16) 0.20076(14) 0.0188(5) Uani 1 1 d . . . H10 H -0.4185 -0.2647 0.2450 0.023 Uiso 1 1 calc R . . O11 O 0.22832(13) 0.23794(11) 0.29017(10) 0.0244(4) Uani 1 1 d . . . C1 C -0.23332(17) 0.01171(16) 0.28949(14) 0.0191(5) Uani 1 1 d . . . H1A H -0.2303 -0.0447 0.2689 0.023 Uiso 1 1 calc R . . H1B H -0.2483 0.0383 0.2445 0.023 Uiso 1 1 calc R . . C78 C 0.04689(19) 0.37678(15) 0.67309(14) 0.0183(5) Uani 1 1 d . . . H78A H 0.0051 0.4149 0.6672 0.022 Uiso 1 1 calc R . . H78B H 0.1066 0.4062 0.7125 0.022 Uiso 1 1 calc R . . C21 C -0.34520(16) -0.26310(15) 0.06315(14) 0.0153(5) Uani 1 1 d . . . C8 C -0.33238(16) -0.31256(14) 0.12942(13) 0.0134(5) Uani 1 1 d . . . C27 C -0.00352(17) -0.30517(15) 0.29680(14) 0.0163(5) Uani 1 1 d . . . H27A H 0.0633 -0.2863 0.3259 0.020 Uiso 1 1 calc R . . H27B H -0.0103 -0.3225 0.2397 0.020 Uiso 1 1 calc R . . C61 C 0.34975(17) 0.50667(15) 0.45699(14) 0.0184(5) Uani 1 1 d . . . H61 H 0.4147 0.5103 0.4707 0.022 Uiso 1 1 calc R . . C7 C -0.25494(16) -0.25845(14) 0.20719(14) 0.0136(5) Uani 1 1 d . . . C5 C -0.32942(16) -0.10857(14) 0.38828(14) 0.0155(5) Uani 1 1 d . . . H5A H -0.3225 -0.1367 0.3378 0.019 Uiso 1 1 calc R . . H5B H -0.3963 -0.1114 0.3806 0.019 Uiso 1 1 calc R . . C36 C 0.05889(17) -0.25989(14) 0.01817(14) 0.0142(5) Uani 1 1 d . . . N2 N -0.01002(14) 0.06495(12) 0.15239(11) 0.0154(4) Uani 1 1 d . . . C28 C 0.07595(16) -0.16742(15) 0.15510(13) 0.0130(5) Uani 1 1 d . . . C70 C 0.49517(18) 0.34680(17) 0.60000(16) 0.0237(6) Uani 1 1 d . . . H70 H 0.5168 0.3767 0.6534 0.028 Uiso 1 1 calc R . . C30 C 0.21678(17) -0.17102(14) 0.10096(14) 0.0147(5) Uani 1 1 d . . . C12 C -0.62102(18) -0.38072(17) 0.13452(16) 0.0250(6) Uani 1 1 d . . . H12 H -0.6839 -0.3943 0.1336 0.030 Uiso 1 1 calc R . . C3 C -0.22240(17) 0.10831(15) 0.51264(15) 0.0178(5) Uani 1 1 d . . . H3A H -0.2294 0.1441 0.4749 0.021 Uiso 1 1 calc R . . H3B H -0.2306 0.1368 0.5624 0.021 Uiso 1 1 calc R . . C56 C 0.28861(16) 0.43002(15) 0.42084(13) 0.0148(5) Uani 1 1 d . . . C44 C 0.21391(18) -0.33315(18) 0.27295(16) 0.0255(6) Uani 1 1 d . . . H44 H 0.2490 -0.3181 0.3273 0.031 Uiso 1 1 calc R . . C74 C -0.00730(17) 0.25764(16) 0.45698(14) 0.0178(5) Uani 1 1 d . . . H74A H -0.0664 0.2230 0.4206 0.021 Uiso 1 1 calc R . . H74B H 0.0199 0.2937 0.4277 0.021 Uiso 1 1 calc R . . C75 C -0.02551(17) 0.30896(16) 0.52921(14) 0.0185(5) Uani 1 1 d . . . H75A H -0.0564 0.3518 0.5122 0.022 Uiso 1 1 calc R . . H75B H -0.0678 0.2739 0.5492 0.022 Uiso 1 1 calc R . . C14 C -0.49868(17) -0.39554(17) 0.07315(15) 0.0220(6) Uani 1 1 d . . . H14 H -0.4800 -0.4199 0.0300 0.026 Uiso 1 1 calc R . . C41 C 0.09788(19) -0.28870(16) -0.04198(15) 0.0205(5) Uani 1 1 d . . . H41 H 0.1631 -0.2830 -0.0293 0.025 Uiso 1 1 calc R . . C2 C -0.30638(16) 0.01373(16) 0.33446(14) 0.0175(5) Uani 1 1 d . . . H2A H -0.3119 0.0703 0.3508 0.021 Uiso 1 1 calc R . . H2B H -0.3674 -0.0180 0.2989 0.021 Uiso 1 1 calc R . . C31 C 0.21062(18) -0.10991(15) 0.05709(15) 0.0185(5) Uani 1 1 d . . . H31 H 0.1513 -0.1029 0.0302 0.022 Uiso 1 1 calc R . . C50 C -0.06601(17) 0.11838(15) 0.18538(13) 0.0153(5) Uani 1 1 d . . . H50A H -0.1230 0.0846 0.1889 0.018 Uiso 1 1 calc R . . H50B H -0.0845 0.1545 0.1496 0.018 Uiso 1 1 calc R . . C51 C -0.00766(17) 0.17024(15) 0.26930(13) 0.0155(5) Uani 1 1 d . . . H51A H 0.0476 0.2064 0.2657 0.019 Uiso 1 1 calc R . . H51B H -0.0451 0.2041 0.2918 0.019 Uiso 1 1 calc R . . C6 C -0.29304(15) -0.15325(15) 0.45344(14) 0.0148(5) Uani 1 1 d . . . H6A H -0.3076 -0.1306 0.5022 0.018 Uiso 1 1 calc R . . H6B H -0.3240 -0.2114 0.4357 0.018 Uiso 1 1 calc R . . C68 C 0.40075(16) 0.33157(15) 0.46187(14) 0.0165(5) Uani 1 1 d . . . C62 C 0.37268(17) 0.37860(15) 0.32914(14) 0.0163(5) Uani 1 1 d . . . C26 C -0.34742(19) -0.29394(17) -0.01609(15) 0.0246(6) Uani 1 1 d . . . H26 H -0.3388 -0.3472 -0.0312 0.029 Uiso 1 1 calc R . . C76 C 0.12286(18) 0.41310(15) 0.57378(15) 0.0205(5) Uani 1 1 d . . . H76A H 0.1133 0.4665 0.5970 0.025 Uiso 1 1 calc R . . H76B H 0.1049 0.4059 0.5155 0.025 Uiso 1 1 calc R . . C4 C -0.29767(17) 0.02889(15) 0.47734(14) 0.0180(5) Uani 1 1 d . . . H4A H -0.2977 -0.0028 0.5184 0.022 Uiso 1 1 calc R . . H4B H -0.3594 0.0419 0.4606 0.022 Uiso 1 1 calc R . . C43 C 0.19380(17) -0.27297(16) 0.23107(15) 0.0190(5) Uani 1 1 d . . . H43 H 0.2144 -0.2177 0.2581 0.023 Uiso 1 1 calc R . . C22 C -0.36238(17) -0.18424(16) 0.08191(15) 0.0195(5) Uani 1 1 d . . . H22 H -0.3634 -0.1630 0.1341 0.023 Uiso 1 1 calc R . . C45 C 0.1818(2) -0.41592(18) 0.23409(18) 0.0302(7) Uani 1 1 d . . . H45 H 0.1951 -0.4566 0.2621 0.036 Uiso 1 1 calc R . . C60 C 0.31642(19) 0.57766(16) 0.47299(16) 0.0241(6) Uani 1 1 d . . . H60 H 0.3588 0.6280 0.4980 0.029 Uiso 1 1 calc R . . C33 C 0.37944(19) -0.06934(17) 0.09069(17) 0.0289(6) Uani 1 1 d . . . H33 H 0.4334 -0.0350 0.0884 0.035 Uiso 1 1 calc R . . C77 C 0.22575(18) 0.41093(15) 0.60491(15) 0.0213(5) Uani 1 1 d . . . H77A H 0.2634 0.4505 0.5854 0.026 Uiso 1 1 calc R . . H77B H 0.2463 0.4265 0.6635 0.026 Uiso 1 1 calc R . . C32 C 0.29063(19) -0.05913(17) 0.05236(17) 0.0256(6) Uani 1 1 d . . . H32 H 0.2845 -0.0182 0.0234 0.031 Uiso 1 1 calc R . . C46 C 0.1299(2) -0.43724(18) 0.15341(18) 0.0296(6) Uani 1 1 d . . . H46 H 0.1074 -0.4927 0.1271 0.036 Uiso 1 1 calc R . . C58 C 0.15782(18) 0.49877(17) 0.41468(16) 0.0239(6) Uani 1 1 d . . . H58 H 0.0930 0.4959 0.3999 0.029 Uiso 1 1 calc R . . C49 C -0.12533(17) -0.06540(15) 0.13396(13) 0.0156(5) Uani 1 1 d . . . H49A H -0.1826 -0.0464 0.1354 0.019 Uiso 1 1 calc R . . H49B H -0.1434 -0.1219 0.1025 0.019 Uiso 1 1 calc R . . C52 C 0.05653(18) 0.11129(15) 0.11913(14) 0.0184(5) Uani 1 1 d . . . H52A H 0.0693 0.1697 0.1441 0.022 Uiso 1 1 calc R . . H52B H 0.0280 0.1042 0.0615 0.022 Uiso 1 1 calc R . . C57 C 0.19151(17) 0.42744(16) 0.39933(14) 0.0179(5) Uani 1 1 d . . . H57 H 0.1488 0.3772 0.3744 0.021 Uiso 1 1 calc R . . C15 C -0.28740(16) -0.38736(15) 0.11522(14) 0.0175(5) Uani 1 1 d . . . C48 C -0.06879(18) -0.01100(14) 0.09421(13) 0.0163(5) Uani 1 1 d . . . H48A H -0.0285 -0.0417 0.0720 0.020 Uiso 1 1 calc R . . H48B H -0.1120 0.0035 0.0500 0.020 Uiso 1 1 calc R . . C54 C 0.24646(16) 0.27602(15) 0.36155(14) 0.0157(5) Uani 1 1 d . . . C37 C -0.03916(17) -0.26968(15) -0.00348(14) 0.0184(5) Uani 1 1 d . . . H37 H -0.0674 -0.2511 0.0353 0.022 Uiso 1 1 calc R . . C13 C -0.59230(18) -0.41753(18) 0.07165(16) 0.0266(6) Uani 1 1 d . . . H13 H -0.6354 -0.4569 0.0284 0.032 Uiso 1 1 calc R . . C47 C 0.11102(18) -0.37643(16) 0.11119(16) 0.0208(5) Uani 1 1 d . . . H47 H 0.0763 -0.3917 0.0567 0.025 Uiso 1 1 calc R . . C24 C -0.3767(2) -0.16730(19) -0.05265(17) 0.0336(7) Uani 1 1 d . . . H24 H -0.3853 -0.1351 -0.0908 0.040 Uiso 1 1 calc R . . C55 C 0.32858(16) 0.35503(14) 0.39460(14) 0.0145(5) Uani 1 1 d . . . C35 C 0.30653(18) -0.18167(17) 0.13731(16) 0.0232(6) Uani 1 1 d . . . H35 H 0.3131 -0.2233 0.1655 0.028 Uiso 1 1 calc R . . C63 C 0.31632(18) 0.39751(16) 0.26146(15) 0.0205(5) Uani 1 1 d . . . H63 H 0.2512 0.3878 0.2524 0.025 Uiso 1 1 calc R . . C23 C -0.37797(19) -0.13670(17) 0.02524(16) 0.0265(6) Uani 1 1 d . . . H23 H -0.3893 -0.0843 0.0394 0.032 Uiso 1 1 calc R . . C72 C 0.49299(18) 0.23164(17) 0.49825(17) 0.0257(6) Uani 1 1 d . . . H72 H 0.5126 0.1833 0.4832 0.031 Uiso 1 1 calc R . . C64 C 0.3547(2) 0.43039(17) 0.20726(16) 0.0251(6) Uani 1 1 d . . . H64 H 0.3153 0.4429 0.1627 0.030 Uiso 1 1 calc R . . C67 C 0.46910(18) 0.39345(17) 0.34014(16) 0.0237(6) Uani 1 1 d . . . H67 H 0.5087 0.3817 0.3850 0.028 Uiso 1 1 calc R . . C38 C -0.09542(19) -0.30676(16) -0.08217(15) 0.0230(6) Uani 1 1 d . . . H38 H -0.1607 -0.3129 -0.0954 0.028 Uiso 1 1 calc R . . C20 C -0.21045(19) -0.38251(18) 0.08522(17) 0.0297(6) Uani 1 1 d . . . H20 H -0.1900 -0.3355 0.0681 0.036 Uiso 1 1 calc R . . C73 C 0.43224(18) 0.25979(16) 0.44123(16) 0.0214(5) Uani 1 1 d . . . H73 H 0.4117 0.2302 0.3877 0.026 Uiso 1 1 calc R . . C69 C 0.43263(17) 0.37426(16) 0.54202(15) 0.0193(5) Uani 1 1 d . . . H69 H 0.4120 0.4220 0.5574 0.023 Uiso 1 1 calc R . . C25 C -0.3625(2) -0.24582(19) -0.07308(17) 0.0353(7) Uani 1 1 d . . . H25 H -0.3629 -0.2671 -0.1257 0.042 Uiso 1 1 calc R . . C19 C -0.1636(2) -0.4465(2) 0.0802(2) 0.0442(9) Uani 1 1 d . . . H19 H -0.1131 -0.4427 0.0587 0.053 Uiso 1 1 calc R . . C18 C -0.1911(3) -0.5154(2) 0.1070(2) 0.0488(10) Uani 1 1 d . . . H18 H -0.1599 -0.5585 0.1034 0.059 Uiso 1 1 calc R . . C53 C 0.14836(18) 0.08269(16) 0.13352(14) 0.0206(5) Uani 1 1 d . . . H53A H 0.1378 0.0276 0.1004 0.025 Uiso 1 1 calc R . . H53B H 0.1939 0.1195 0.1181 0.025 Uiso 1 1 calc R . . C39 C -0.0549(2) -0.33440(16) -0.14054(15) 0.0240(6) Uani 1 1 d . . . H39 H -0.0925 -0.3587 -0.1932 0.029 Uiso 1 1 calc R . . C11 C -0.55595(18) -0.32353(17) 0.19897(16) 0.0236(6) Uani 1 1 d . . . H11 H -0.5752 -0.2987 0.2416 0.028 Uiso 1 1 calc R . . C59 C 0.22005(19) 0.57386(17) 0.45177(16) 0.0249(6) Uani 1 1 d . . . H59 H 0.1974 0.6215 0.4624 0.030 Uiso 1 1 calc R . . C40 C 0.0418(2) -0.32572(16) -0.12031(15) 0.0240(6) Uani 1 1 d . . . H40 H 0.0695 -0.3448 -0.1594 0.029 Uiso 1 1 calc R . . C16 C -0.3132(2) -0.45671(17) 0.14337(16) 0.0280(6) Uani 1 1 d . . . H16 H -0.3632 -0.4608 0.1654 0.034 Uiso 1 1 calc R . . C65 C 0.4510(2) 0.44478(18) 0.21904(16) 0.0285(6) Uani 1 1 d . . . H65 H 0.4770 0.4670 0.1828 0.034 Uiso 1 1 calc R . . C71 C 0.52491(18) 0.27555(18) 0.57829(17) 0.0269(6) Uani 1 1 d . . . H71 H 0.5662 0.2569 0.6170 0.032 Uiso 1 1 calc R . . C34 C 0.38692(19) -0.13101(18) 0.13227(18) 0.0303(6) Uani 1 1 d . . . H34 H 0.4464 -0.1390 0.1573 0.036 Uiso 1 1 calc R . . C66 C 0.50785(19) 0.42574(18) 0.28521(17) 0.0287(6) Uani 1 1 d . . . H66 H 0.5728 0.4345 0.2934 0.034 Uiso 1 1 calc R . . C17 C -0.2653(3) -0.5202(2) 0.13908(19) 0.0455(9) Uani 1 1 d . . . H17 H -0.2835 -0.5664 0.1582 0.055 Uiso 1 1 calc R . . C3S C -0.3800(2) 0.0565(2) 0.6554(2) 0.0424(8) Uani 1 1 d . . . O1S O 0.6909(3) 0.2784(3) 0.2891(2) 0.1133(14) Uani 1 1 d . . . N2S N -0.4084(3) 0.1019(3) 0.6217(2) 0.0817(13) Uani 1 1 d . . . C2S C 0.3623(3) -0.2233(3) -0.0844(3) 0.0939(19) Uani 1 1 d . . . H2S1 H 0.4205 -0.2248 -0.0461 0.141 Uiso 1 1 calc R . . H2S2 H 0.3492 -0.2664 -0.1320 0.141 Uiso 1 1 calc R . . H2S3 H 0.3117 -0.2314 -0.0607 0.141 Uiso 1 1 calc R . . N1S N 0.3819(4) -0.0781(4) -0.1186(3) 0.1162(18) Uani 1 1 d . . . C8S C 0.8455(5) 0.3527(4) 0.2987(3) 0.0966(19) Uani 1 1 d . . . H8S1 H 0.8547 0.3073 0.2623 0.145 Uiso 1 1 calc R . . H8S2 H 0.9046 0.3794 0.3390 0.145 Uiso 1 1 calc R . . H8S3 H 0.8225 0.3915 0.2690 0.145 Uiso 1 1 calc R . . C1S C 0.3707(4) -0.1452(4) -0.1057(3) 0.0853(16) Uani 1 1 d . . . C7S C 0.7771(4) 0.3219(4) 0.3378(3) 0.110(2) Uani 1 1 d . . . H7S1 H 0.8045 0.2872 0.3717 0.131 Uiso 1 1 calc R . . H7S2 H 0.7679 0.3688 0.3732 0.131 Uiso 1 1 calc R . . C5S C 0.6236(5) 0.2424(5) 0.3303(4) 0.121(2) Uani 1 1 d . . . H5S1 H 0.6102 0.2865 0.3660 0.145 Uiso 1 1 calc R . . H5S2 H 0.6523 0.2071 0.3627 0.145 Uiso 1 1 calc R . . C6S C 0.5294(5) 0.1911(5) 0.2663(4) 0.146(3) Uani 1 1 d . . . H6S1 H 0.5010 0.2261 0.2343 0.219 Uiso 1 1 calc R . . H6S2 H 0.4867 0.1690 0.2935 0.219 Uiso 1 1 calc R . . H6S3 H 0.5425 0.1466 0.2318 0.219 Uiso 1 1 calc R . . C4S C -0.3411(3) -0.0005(2) 0.6990(2) 0.0498(9) Uani 1 1 d . . . H4S1 H -0.3162 -0.0364 0.6653 0.075 Uiso 1 1 calc R . . H4S2 H -0.3898 -0.0327 0.7141 0.075 Uiso 1 1 calc R . . H4S3 H -0.2913 0.0296 0.7467 0.075 Uiso 1 1 calc R . . H3 H 0.232(2) 0.320(2) 0.528(2) 0.039(9) Uiso 1 1 d . . . H4 H 0.200(2) 0.127(2) 0.2413(18) 0.027(9) Uiso 1 1 d . . . H1 H -0.108(2) 0.0919(19) 0.5772(19) 0.036(9) Uiso 1 1 d . . . H2 H -0.109(2) 0.061(2) 0.333(2) 0.035(11) 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 Mn3 0.01317(16) 0.00994(18) 0.00975(16) 0.00160(13) 0.00410(13) -0.00132(13) Mn1 0.00948(16) 0.01044(17) 0.00932(16) 0.00173(13) 0.00211(13) 0.00031(13) Mn4 0.01155(16) 0.01012(17) 0.00854(16) 0.00132(13) 0.00319(13) -0.00056(13) Mn2 0.01107(16) 0.00888(17) 0.00963(16) 0.00239(13) 0.00346(13) -0.00107(13) Mn5 0.01084(16) 0.01022(17) 0.00942(16) 0.00164(13) 0.00306(13) -0.00080(13) F2 0.0115(6) 0.0134(7) 0.0110(6) 0.0038(5) 0.0030(5) -0.0012(5) F4 0.0143(6) 0.0151(7) 0.0135(6) 0.0009(5) 0.0053(5) 0.0006(5) N1 0.0133(9) 0.0142(10) 0.0133(9) 0.0032(8) 0.0041(8) 0.0007(8) F3 0.0148(6) 0.0148(7) 0.0112(6) 0.0038(5) 0.0034(5) -0.0010(5) F1 0.0173(7) 0.0113(7) 0.0117(6) 0.0013(5) 0.0058(5) -0.0004(5) O12 0.0093(7) 0.0149(8) 0.0115(8) 0.0021(6) 0.0028(6) 0.0004(6) O13 0.0150(8) 0.0135(8) 0.0126(8) 0.0020(7) 0.0036(6) 0.0039(7) O10 0.0178(8) 0.0148(9) 0.0156(8) 0.0049(7) 0.0057(7) -0.0032(7) O6 0.0126(7) 0.0126(8) 0.0084(7) 0.0025(6) 0.0011(6) -0.0015(6) O2 0.0154(8) 0.0186(9) 0.0117(8) 0.0025(7) 0.0021(7) 0.0043(7) O7 0.0197(8) 0.0116(9) 0.0180(8) 0.0026(7) 0.0095(7) 0.0005(7) O9 0.0170(8) 0.0124(8) 0.0100(7) 0.0034(6) 0.0029(6) 0.0000(6) O15 0.0131(8) 0.0192(9) 0.0132(8) 0.0027(7) 0.0040(6) -0.0010(7) O5 0.0169(8) 0.0125(8) 0.0163(8) 0.0025(7) 0.0087(7) 0.0006(7) O14 0.0209(9) 0.0151(9) 0.0150(9) 0.0016(7) 0.0075(7) -0.0015(7) O4 0.0178(8) 0.0135(8) 0.0185(8) 0.0069(7) 0.0111(7) 0.0054(7) O1 0.0109(8) 0.0257(10) 0.0186(9) 0.0089(8) 0.0048(7) 0.0015(7) O8 0.0222(9) 0.0139(10) 0.0155(9) 0.0008(8) 0.0068(7) -0.0032(7) O3 0.0141(8) 0.0167(9) 0.0135(8) 0.0037(7) 0.0020(7) -0.0045(7) C42 0.0139(11) 0.0167(12) 0.0209(12) 0.0083(10) 0.0107(10) 0.0039(9) C9 0.0138(11) 0.0145(12) 0.0131(11) 0.0042(9) 0.0019(9) -0.0010(9) N3 0.0212(10) 0.0119(10) 0.0132(10) 0.0027(8) 0.0090(8) 0.0013(8) C29 0.0119(10) 0.0121(12) 0.0151(11) 0.0028(9) 0.0060(9) 0.0016(9) C10 0.0152(11) 0.0213(14) 0.0155(12) 0.0002(10) 0.0012(10) 0.0014(10) O11 0.0314(10) 0.0184(10) 0.0169(9) -0.0013(7) 0.0079(8) -0.0073(8) C1 0.0176(12) 0.0249(14) 0.0138(12) 0.0073(10) 0.0014(10) 0.0041(10) C78 0.0311(14) 0.0127(12) 0.0149(12) 0.0029(10) 0.0123(10) 0.0065(10) C21 0.0102(10) 0.0176(13) 0.0141(11) 0.0025(10) 0.0022(9) -0.0042(9) C8 0.0117(10) 0.0139(12) 0.0107(11) -0.0003(9) 0.0017(9) -0.0017(9) C27 0.0214(12) 0.0159(12) 0.0159(12) 0.0052(10) 0.0106(10) 0.0067(10) C61 0.0172(12) 0.0162(13) 0.0214(13) 0.0057(10) 0.0064(10) -0.0003(10) C7 0.0118(10) 0.0114(12) 0.0153(11) 0.0014(9) 0.0030(9) 0.0001(9) C5 0.0113(10) 0.0145(12) 0.0170(12) 0.0004(10) 0.0023(9) -0.0007(9) C36 0.0198(12) 0.0088(11) 0.0154(11) 0.0051(9) 0.0070(10) 0.0017(9) N2 0.0215(10) 0.0128(10) 0.0119(9) 0.0033(8) 0.0066(8) 0.0004(8) C28 0.0129(10) 0.0150(12) 0.0102(11) 0.0033(9) 0.0022(9) 0.0023(9) C70 0.0179(12) 0.0293(15) 0.0220(13) 0.0099(12) 0.0041(10) -0.0018(11) C30 0.0185(12) 0.0127(12) 0.0141(11) 0.0015(9) 0.0083(9) 0.0028(9) C12 0.0141(12) 0.0323(16) 0.0298(15) 0.0138(13) 0.0056(11) 0.0023(11) C3 0.0184(12) 0.0155(13) 0.0184(12) 0.0005(10) 0.0045(10) 0.0057(10) C56 0.0176(11) 0.0140(12) 0.0129(11) 0.0068(9) 0.0055(9) -0.0016(9) C44 0.0213(13) 0.0415(18) 0.0232(13) 0.0182(13) 0.0117(11) 0.0130(12) C74 0.0183(12) 0.0218(13) 0.0142(11) 0.0055(10) 0.0037(10) 0.0075(10) C75 0.0182(12) 0.0203(13) 0.0172(12) 0.0038(10) 0.0048(10) 0.0064(10) C14 0.0177(12) 0.0266(15) 0.0171(12) 0.0009(11) 0.0041(10) -0.0022(11) C41 0.0226(13) 0.0207(14) 0.0193(12) 0.0033(11) 0.0077(10) 0.0068(11) C2 0.0130(11) 0.0219(13) 0.0163(12) 0.0065(10) 0.0008(9) 0.0038(10) C31 0.0209(12) 0.0178(13) 0.0197(12) 0.0045(10) 0.0105(10) 0.0044(10) C50 0.0202(12) 0.0156(12) 0.0111(11) 0.0051(9) 0.0045(9) 0.0043(10) C51 0.0219(12) 0.0124(12) 0.0118(11) 0.0045(9) 0.0038(9) 0.0028(9) C6 0.0099(10) 0.0147(12) 0.0180(12) 0.0029(10) 0.0048(9) -0.0020(9) C68 0.0127(11) 0.0167(12) 0.0201(12) 0.0071(10) 0.0063(9) -0.0021(9) C62 0.0206(12) 0.0107(12) 0.0169(12) 0.0025(9) 0.0080(10) -0.0020(9) C26 0.0327(15) 0.0209(14) 0.0199(13) 0.0031(11) 0.0119(12) 0.0005(11) C76 0.0294(14) 0.0125(12) 0.0215(13) 0.0058(10) 0.0120(11) 0.0007(10) C4 0.0175(12) 0.0189(13) 0.0184(12) 0.0030(10) 0.0068(10) 0.0053(10) C43 0.0177(12) 0.0232(14) 0.0203(12) 0.0096(11) 0.0096(10) 0.0049(10) C22 0.0173(12) 0.0198(13) 0.0182(12) 0.0020(10) 0.0034(10) 0.0003(10) C45 0.0342(16) 0.0334(17) 0.0426(17) 0.0292(14) 0.0241(14) 0.0191(13) C60 0.0282(14) 0.0154(13) 0.0271(14) 0.0047(11) 0.0096(12) -0.0019(11) C33 0.0236(14) 0.0240(15) 0.0401(16) 0.0057(13) 0.0183(13) -0.0046(11) C77 0.0287(14) 0.0130(12) 0.0195(13) -0.0006(10) 0.0118(11) -0.0056(10) C32 0.0311(15) 0.0196(14) 0.0331(15) 0.0119(12) 0.0193(13) 0.0028(11) C46 0.0335(15) 0.0189(14) 0.0444(17) 0.0146(13) 0.0196(14) 0.0068(12) C58 0.0197(13) 0.0299(16) 0.0291(14) 0.0184(12) 0.0100(11) 0.0082(11) C49 0.0190(12) 0.0137(12) 0.0109(11) 0.0030(9) 0.0010(9) 0.0002(9) C52 0.0291(13) 0.0149(13) 0.0120(11) 0.0039(10) 0.0091(10) 0.0013(10) C57 0.0174(12) 0.0178(13) 0.0186(12) 0.0081(10) 0.0064(10) -0.0018(10) C15 0.0144(11) 0.0163(13) 0.0148(11) -0.0040(10) -0.0005(9) 0.0005(9) C48 0.0238(12) 0.0133(12) 0.0091(11) 0.0019(9) 0.0018(9) 0.0026(10) C54 0.0148(11) 0.0127(12) 0.0184(12) 0.0059(10) 0.0039(9) -0.0012(9) C37 0.0214(12) 0.0179(13) 0.0160(12) 0.0043(10) 0.0079(10) 0.0007(10) C13 0.0163(12) 0.0311(16) 0.0230(14) 0.0031(12) -0.0004(11) -0.0072(11) C47 0.0214(12) 0.0179(13) 0.0264(13) 0.0083(11) 0.0098(11) 0.0054(10) C24 0.0380(17) 0.0317(17) 0.0285(15) 0.0181(13) 0.0040(13) -0.0018(13) C55 0.0140(11) 0.0121(12) 0.0152(11) 0.0032(9) 0.0047(9) -0.0036(9) C35 0.0194(12) 0.0258(15) 0.0283(14) 0.0098(12) 0.0113(11) 0.0057(11) C63 0.0180(12) 0.0221(14) 0.0215(13) 0.0064(11) 0.0074(10) 0.0008(10) C23 0.0229(13) 0.0227(15) 0.0308(15) 0.0088(12) 0.0029(12) 0.0015(11) C72 0.0216(13) 0.0221(14) 0.0380(16) 0.0126(12) 0.0139(12) 0.0033(11) C64 0.0296(14) 0.0254(15) 0.0200(13) 0.0081(11) 0.0084(11) 0.0009(12) C67 0.0208(13) 0.0281(15) 0.0215(13) 0.0081(11) 0.0077(11) -0.0016(11) C38 0.0208(13) 0.0214(14) 0.0219(13) 0.0065(11) 0.0016(11) -0.0027(11) C20 0.0189(13) 0.0287(16) 0.0349(16) -0.0050(13) 0.0070(12) 0.0022(11) C73 0.0201(12) 0.0191(14) 0.0255(13) 0.0072(11) 0.0086(11) 0.0010(10) C69 0.0156(11) 0.0185(13) 0.0217(13) 0.0052(10) 0.0056(10) -0.0029(10) C25 0.052(2) 0.0347(18) 0.0165(13) 0.0068(13) 0.0112(13) 0.0005(15) C19 0.0257(16) 0.044(2) 0.052(2) -0.0150(17) 0.0042(15) 0.0155(15) C18 0.053(2) 0.040(2) 0.0432(19) -0.0086(16) -0.0046(17) 0.0325(18) C53 0.0288(14) 0.0183(13) 0.0163(12) 0.0042(10) 0.0127(11) -0.0007(11) C39 0.0329(15) 0.0163(13) 0.0155(12) 0.0019(10) -0.0004(11) -0.0004(11) C11 0.0181(12) 0.0339(16) 0.0222(13) 0.0096(12) 0.0082(11) 0.0081(11) C59 0.0307(15) 0.0224(15) 0.0301(15) 0.0125(12) 0.0161(12) 0.0106(12) C40 0.0348(15) 0.0196(14) 0.0179(13) 0.0003(11) 0.0100(11) 0.0080(12) C16 0.0359(16) 0.0234(15) 0.0218(14) 0.0036(12) 0.0041(12) 0.0078(12) C65 0.0312(15) 0.0305(16) 0.0239(14) 0.0074(12) 0.0147(12) -0.0046(12) C71 0.0171(12) 0.0333(16) 0.0311(15) 0.0186(13) 0.0035(11) 0.0014(11) C34 0.0168(13) 0.0364(17) 0.0391(16) 0.0092(14) 0.0116(12) 0.0039(12) C66 0.0188(13) 0.0365(17) 0.0309(15) 0.0087(13) 0.0128(12) -0.0035(12) C17 0.067(2) 0.0291(18) 0.0369(18) 0.0074(15) 0.0015(17) 0.0226(17) C3S 0.0379(18) 0.051(2) 0.0427(19) 0.0070(17) 0.0171(16) 0.0176(17) O1S 0.127(4) 0.138(4) 0.076(2) 0.010(2) 0.033(3) 0.046(3) N2S 0.105(3) 0.092(3) 0.077(3) 0.039(2) 0.038(2) 0.065(3) C2S 0.074(3) 0.082(4) 0.099(4) -0.046(3) 0.052(3) -0.031(3) N1S 0.122(4) 0.155(6) 0.088(3) 0.045(4) 0.044(3) 0.040(4) C8S 0.136(5) 0.105(4) 0.086(4) 0.037(3) 0.054(4) 0.077(4) C1S 0.076(4) 0.099(5) 0.089(4) 0.027(4) 0.041(3) 0.010(3) C7S 0.081(4) 0.154(6) 0.061(3) -0.010(4) -0.029(3) 0.055(4) C5S 0.142(6) 0.144(6) 0.096(5) 0.009(4) 0.055(5) 0.076(5) C6S 0.143(7) 0.149(7) 0.123(6) -0.045(5) 0.062(5) 0.015(5) C4S 0.056(2) 0.051(2) 0.049(2) 0.0137(18) 0.0187(18) 0.0233(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn3 F4 2.1674(13) . ? Mn3 F3 2.1753(13) . ? Mn3 O6 2.1873(15) . ? Mn3 O8 2.2308(17) . ? Mn3 O7 2.2492(16) . ? Mn3 O9 2.3061(16) . ? Mn3 N2 2.3836(19) . ? Mn1 F1 2.0954(13) . ? Mn1 F2 2.1136(12) 2_556 ? Mn1 F2 2.1560(13) . ? Mn1 O2 2.2085(17) . ? Mn1 O1 2.2573(18) . ? Mn1 N1 2.3888(19) . ? Mn1 O12 2.4682(16) 2_556 ? Mn4 O13 1.8834(16) . ? Mn4 F4 1.8907(13) . ? Mn4 O9 1.9133(15) . ? Mn4 O12 1.9258(15) . ? Mn4 F2 2.1722(13) . ? Mn4 O10 2.2627(16) . ? Mn2 O4 1.8542(15) . ? Mn2 O6 1.8728(15) . ? Mn2 F3 1.9617(13) . ? Mn2 O3 1.9744(16) . ? Mn2 F1 2.1279(13) . ? Mn2 O5 2.1307(16) . ? Mn5 O13 2.1691(15) . ? Mn5 O4 2.1747(16) 2_556 ? Mn5 F1 2.2035(13) 2_556 ? Mn5 O15 2.2222(16) . ? Mn5 O12 2.2673(16) . ? Mn5 O14 2.2913(17) . ? Mn5 N3 2.423(2) . ? F2 Mn1 2.1136(12) 2_556 ? N1 C5 1.477(3) . ? N1 C4 1.480(3) . ? N1 C2 1.485(3) . ? F1 Mn5 2.2035(13) 2_556 ? O12 C6 1.425(3) 2_556 ? O12 Mn1 2.4682(16) 2_556 ? O13 C74 1.401(3) . ? O10 C54 1.272(3) . ? O6 C49 1.415(3) . ? O2 C3 1.426(3) . ? O2 H1 0.83(3) . ? O7 C28 1.254(3) . ? O9 C51 1.425(3) . ? O15 C7 1.242(3) 2_556 ? O5 C28 1.269(3) . ? O14 C77 1.430(3) . ? O14 H3 0.86(3) . ? O4 C27 1.404(3) . ? O4 Mn5 2.1747(16) 2_556 ? O1 C1 1.427(3) . ? O1 H2 0.68(3) . ? O8 C53 1.431(3) . ? O8 H4 0.77(3) . ? O3 C7 1.271(3) . ? C42 C47 1.387(4) . ? C42 C43 1.394(3) . ? C42 C29 1.542(3) . ? C9 C10 1.382(3) . ? C9 C14 1.391(3) . ? C9 C8 1.536(3) . ? N3 C78 1.472(3) . ? N3 C75 1.473(3) . ? N3 C76 1.474(3) . ? C29 C36 1.542(3) . ? C29 C30 1.542(3) . ? C29 C28 1.571(3) . ? C10 C11 1.391(3) . ? C10 H10 0.9300 . ? O11 C54 1.244(3) . ? C1 C2 1.513(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C78 C27 1.519(3) 2_556 ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C21 C26 1.390(3) . ? C21 C22 1.395(3) . ? C21 C8 1.538(3) . ? C8 C15 1.538(3) . ? C8 C7 1.563(3) . ? C27 C78 1.519(3) 2_556 ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C61 C60 1.383(4) . ? C61 C56 1.391(3) . ? C61 H61 0.9300 . ? C7 O15 1.242(3) 2_556 ? C5 C6 1.513(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C36 C41 1.392(3) . ? C36 C37 1.395(3) . ? N2 C52 1.470(3) . ? N2 C48 1.472(3) . ? N2 C50 1.475(3) . ? C70 C71 1.376(4) . ? C70 C69 1.395(3) . ? C70 H70 0.9300 . ? C30 C35 1.388(3) . ? C30 C31 1.392(3) . ? C12 C13 1.376(4) . ? C12 C11 1.379(4) . ? C12 H12 0.9300 . ? C3 C4 1.517(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C56 C57 1.399(3) . ? C56 C55 1.537(3) . ? C44 C43 1.381(3) . ? C44 C45 1.386(4) . ? C44 H44 0.9300 . ? C74 C75 1.521(3) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C14 C13 1.386(3) . ? C14 H14 0.9300 . ? C41 C40 1.386(4) . ? C41 H41 0.9300 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C31 C32 1.387(3) . ? C31 H31 0.9300 . ? C50 C51 1.528(3) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C6 O12 1.425(3) 2_556 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C68 C69 1.384(3) . ? C68 C73 1.394(4) . ? C68 C55 1.538(3) . ? C62 C67 1.384(3) . ? C62 C63 1.390(3) . ? C62 C55 1.548(3) . ? C26 C25 1.393(4) . ? C26 H26 0.9300 . ? C76 C77 1.508(4) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C43 H43 0.9300 . ? C22 C23 1.382(4) . ? C22 H22 0.9300 . ? C45 C46 1.380(4) . ? C45 H45 0.9300 . ? C60 C59 1.385(4) . ? C60 H60 0.9300 . ? C33 C34 1.375(4) . ? C33 C32 1.382(4) . ? C33 H33 0.9300 . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C32 H32 0.9300 . ? C46 C47 1.391(4) . ? C46 H46 0.9300 . ? C58 C59 1.381(4) . ? C58 C57 1.390(4) . ? C58 H58 0.9300 . ? C49 C48 1.526(3) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C52 C53 1.509(4) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C57 H57 0.9300 . ? C15 C16 1.384(4) . ? C15 C20 1.387(4) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C54 C55 1.565(3) . ? C37 C38 1.391(3) . ? C37 H37 0.9300 . ? C13 H13 0.9300 . ? C47 H47 0.9300 . ? C24 C25 1.376(4) . ? C24 C23 1.384(4) . ? C24 H24 0.9300 . ? C35 C34 1.392(4) . ? C35 H35 0.9300 . ? C63 C64 1.384(3) . ? C63 H63 0.9300 . ? C23 H23 0.9300 . ? C72 C73 1.376(4) . ? C72 C71 1.389(4) . ? C72 H72 0.9300 . ? C64 C65 1.381(4) . ? C64 H64 0.9300 . ? C67 C66 1.394(4) . ? C67 H67 0.9300 . ? C38 C39 1.376(4) . ? C38 H38 0.9300 . ? C20 C19 1.384(4) . ? C20 H20 0.9300 . ? C73 H73 0.9300 . ? C69 H69 0.9300 . ? C25 H25 0.9300 . ? C19 C18 1.370(5) . ? C19 H19 0.9300 . ? C18 C17 1.371(5) . ? C18 H18 0.9300 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C39 C40 1.378(4) . ? C39 H39 0.9300 . ? C11 H11 0.9300 . ? C59 H59 0.9300 . ? C40 H40 0.9300 . ? C16 C17 1.386(4) . ? C16 H16 0.9300 . ? C65 C66 1.374(4) . ? C65 H65 0.9300 . ? C71 H71 0.9300 . ? C34 H34 0.9300 . ? C66 H66 0.9300 . ? C17 H17 0.9300 . ? C3S N2S 1.119(5) . ? C3S C4S 1.435(5) . ? O1S C7S 1.356(6) . ? O1S C5S 1.500(8) . ? C2S C1S 1.427(8) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? N1S C1S 1.185(7) . ? C8S C7S 1.455(8) . ? C8S H8S1 0.9600 . ? C8S H8S2 0.9600 . ? C8S H8S3 0.9600 . ? C7S H7S1 0.9700 . ? C7S H7S2 0.9700 . ? C5S C6S 1.564(9) . ? C5S H5S1 0.9700 . ? C5S H5S2 0.9700 . ? C6S H6S1 0.9600 . ? C6S H6S2 0.9600 . ? C6S H6S3 0.9600 . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 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 F4 Mn3 F3 80.43(5) . . ? F4 Mn3 O6 137.14(5) . . ? F3 Mn3 O6 72.05(5) . . ? F4 Mn3 O8 79.82(6) . . ? F3 Mn3 O8 136.54(6) . . ? O6 Mn3 O8 141.84(6) . . ? F4 Mn3 O7 120.25(6) . . ? F3 Mn3 O7 78.69(5) . . ? O6 Mn3 O7 86.16(6) . . ? O8 Mn3 O7 78.58(6) . . ? F4 Mn3 O9 70.39(5) . . ? F3 Mn3 O9 108.73(5) . . ? O6 Mn3 O9 87.89(6) . . ? O8 Mn3 O9 100.38(6) . . ? O7 Mn3 O9 168.53(6) . . ? F4 Mn3 N2 130.66(6) . . ? F3 Mn3 N2 144.01(6) . . ? O6 Mn3 N2 72.17(6) . . ? O8 Mn3 N2 74.63(7) . . ? O7 Mn3 N2 95.16(6) . . ? O9 Mn3 N2 73.66(6) . . ? F1 Mn1 F2 103.94(5) . 2_556 ? F1 Mn1 F2 86.42(5) . . ? F2 Mn1 F2 76.14(5) 2_556 . ? F1 Mn1 O2 172.86(6) . . ? F2 Mn1 O2 83.11(6) 2_556 . ? F2 Mn1 O2 96.53(6) . . ? F1 Mn1 O1 87.17(6) . . ? F2 Mn1 O1 153.07(6) 2_556 . ? F2 Mn1 O1 80.25(6) . . ? O2 Mn1 O1 86.93(7) . . ? F1 Mn1 N1 99.03(6) . . ? F2 Mn1 N1 128.29(6) 2_556 . ? F2 Mn1 N1 151.59(6) . . ? O2 Mn1 N1 75.32(6) . . ? O1 Mn1 N1 72.27(7) . . ? F1 Mn1 O12 72.31(5) . 2_556 ? F2 Mn1 O12 71.83(5) 2_556 2_556 ? F2 Mn1 O12 135.32(5) . 2_556 ? O2 Mn1 O12 109.42(6) . 2_556 ? O1 Mn1 O12 135.08(6) . 2_556 ? N1 Mn1 O12 72.17(6) . 2_556 ? O13 Mn4 F4 173.79(6) . . ? O13 Mn4 O9 100.13(7) . . ? F4 Mn4 O9 85.44(6) . . ? O13 Mn4 O12 82.23(7) . . ? F4 Mn4 O12 91.76(6) . . ? O9 Mn4 O12 167.90(7) . . ? O13 Mn4 F2 86.87(6) . . ? F4 Mn4 F2 90.82(5) . . ? O9 Mn4 F2 85.98(6) . . ? O12 Mn4 F2 82.30(6) . . ? O13 Mn4 O10 89.67(7) . . ? F4 Mn4 O10 92.19(6) . . ? O9 Mn4 O10 98.91(6) . . ? O12 Mn4 O10 92.95(6) . . ? F2 Mn4 O10 174.45(5) . . ? O4 Mn2 O6 173.89(7) . . ? O4 Mn2 F3 94.20(6) . . ? O6 Mn2 F3 83.97(6) . . ? O4 Mn2 O3 91.33(7) . . ? O6 Mn2 O3 90.20(7) . . ? F3 Mn2 O3 173.60(6) . . ? O4 Mn2 F1 79.32(6) . . ? O6 Mn2 F1 94.81(6) . . ? F3 Mn2 F1 89.08(5) . . ? O3 Mn2 F1 88.78(6) . . ? O4 Mn2 O5 93.04(6) . . ? O6 Mn2 O5 92.66(6) . . ? F3 Mn2 O5 86.39(6) . . ? O3 Mn2 O5 96.55(7) . . ? F1 Mn2 O5 170.81(6) . . ? O13 Mn5 O4 111.16(6) . 2_556 ? O13 Mn5 F1 104.76(5) . 2_556 ? O4 Mn5 F1 71.24(5) 2_556 2_556 ? O13 Mn5 O15 164.49(6) . . ? O4 Mn5 O15 83.26(6) 2_556 . ? F1 Mn5 O15 84.87(5) 2_556 . ? O13 Mn5 O12 68.71(6) . . ? O4 Mn5 O12 144.50(6) 2_556 . ? F1 Mn5 O12 74.59(5) 2_556 . ? O15 Mn5 O12 103.15(6) . . ? O13 Mn5 O14 85.87(6) . . ? O4 Mn5 O14 132.65(6) 2_556 . ? F1 Mn5 O14 148.88(6) 2_556 . ? O15 Mn5 O14 79.88(6) . . ? O12 Mn5 O14 82.66(6) . . ? O13 Mn5 N3 72.91(6) . . ? O4 Mn5 N3 70.82(6) 2_556 . ? F1 Mn5 N3 137.78(6) 2_556 . ? O15 Mn5 N3 108.26(6) . . ? O12 Mn5 N3 135.67(6) . . ? O14 Mn5 N3 73.16(6) . . ? Mn1 F2 Mn1 103.86(5) 2_556 . ? Mn1 F2 Mn4 104.61(5) 2_556 . ? Mn1 F2 Mn4 142.47(6) . . ? Mn4 F4 Mn3 103.96(6) . . ? C5 N1 C4 112.29(18) . . ? C5 N1 C2 109.95(18) . . ? C4 N1 C2 111.33(18) . . ? C5 N1 Mn1 107.73(13) . . ? C4 N1 Mn1 105.98(13) . . ? C2 N1 Mn1 109.39(13) . . ? Mn2 F3 Mn3 99.67(5) . . ? Mn1 F1 Mn2 148.16(7) . . ? Mn1 F1 Mn5 111.26(5) . 2_556 ? Mn2 F1 Mn5 97.35(5) . 2_556 ? C6 O12 Mn4 122.01(13) 2_556 . ? C6 O12 Mn5 118.18(13) 2_556 . ? Mn4 O12 Mn5 101.79(7) . . ? C6 O12 Mn1 113.42(13) 2_556 2_556 ? Mn4 O12 Mn1 100.30(6) . 2_556 ? Mn5 O12 Mn1 96.99(6) . 2_556 ? C74 O13 Mn4 127.79(14) . . ? C74 O13 Mn5 121.90(13) . . ? Mn4 O13 Mn5 106.94(7) . . ? C54 O10 Mn4 136.32(15) . . ? C49 O6 Mn2 124.07(14) . . ? C49 O6 Mn3 118.83(13) . . ? Mn2 O6 Mn3 102.14(7) . . ? C3 O2 Mn1 116.09(14) . . ? C3 O2 H1 111(2) . . ? Mn1 O2 H1 114(2) . . ? C28 O7 Mn3 130.85(15) . . ? C51 O9 Mn4 128.49(14) . . ? C51 O9 Mn3 113.20(13) . . ? Mn4 O9 Mn3 98.28(7) . . ? C7 O15 Mn5 128.23(15) 2_556 . ? C28 O5 Mn2 126.21(15) . . ? C77 O14 Mn5 110.59(14) . . ? C77 O14 H3 110(2) . . ? Mn5 O14 H3 110(2) . . ? C27 O4 Mn2 127.54(13) . . ? C27 O4 Mn5 124.80(13) . 2_556 ? Mn2 O4 Mn5 107.44(7) . 2_556 ? C1 O1 Mn1 107.68(14) . . ? C1 O1 H2 114(3) . . ? Mn1 O1 H2 109(3) . . ? C53 O8 Mn3 110.23(14) . . ? C53 O8 H4 107(2) . . ? Mn3 O8 H4 110(2) . . ? C7 O3 Mn2 131.01(15) . . ? C47 C42 C43 117.8(2) . . ? C47 C42 C29 123.1(2) . . ? C43 C42 C29 119.1(2) . . ? C10 C9 C14 117.8(2) . . ? C10 C9 C8 124.7(2) . . ? C14 C9 C8 117.3(2) . . ? C78 N3 C75 113.19(19) . . ? C78 N3 C76 111.29(19) . . ? C75 N3 C76 112.21(19) . . ? C78 N3 Mn5 106.10(13) . . ? C75 N3 Mn5 102.97(14) . . ? C76 N3 Mn5 110.58(14) . . ? C36 C29 C30 108.39(18) . . ? C36 C29 C42 110.14(19) . . ? C30 C29 C42 112.01(18) . . ? C36 C29 C28 110.42(18) . . ? C30 C29 C28 109.44(18) . . ? C42 C29 C28 106.44(18) . . ? C9 C10 C11 120.7(2) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? O1 C1 C2 105.06(19) . . ? O1 C1 H1A 110.7 . . ? C2 C1 H1A 110.7 . . ? O1 C1 H1B 110.7 . . ? C2 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? N3 C78 C27 111.00(19) . 2_556 ? N3 C78 H78A 109.4 . . ? C27 C78 H78A 109.4 2_556 . ? N3 C78 H78B 109.4 . . ? C27 C78 H78B 109.4 2_556 . ? H78A C78 H78B 108.0 . . ? C26 C21 C22 117.5(2) . . ? C26 C21 C8 124.3(2) . . ? C22 C21 C8 118.1(2) . . ? C9 C8 C15 111.76(19) . . ? C9 C8 C21 104.74(18) . . ? C15 C8 C21 116.33(19) . . ? C9 C8 C7 116.14(19) . . ? C15 C8 C7 99.36(17) . . ? C21 C8 C7 108.94(18) . . ? O4 C27 C78 107.89(19) . 2_556 ? O4 C27 H27A 110.1 . . ? C78 C27 H27A 110.1 2_556 . ? O4 C27 H27B 110.1 . . ? C78 C27 H27B 110.1 2_556 . ? H27A C27 H27B 108.4 . . ? C60 C61 C56 121.7(2) . . ? C60 C61 H61 119.2 . . ? C56 C61 H61 119.2 . . ? O15 C7 O3 127.0(2) 2_556 . ? O15 C7 C8 119.7(2) 2_556 . ? O3 C7 C8 113.05(19) . . ? N1 C5 C6 113.41(19) . . ? N1 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N1 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C41 C36 C37 117.3(2) . . ? C41 C36 C29 119.0(2) . . ? C37 C36 C29 123.6(2) . . ? C52 N2 C48 112.24(18) . . ? C52 N2 C50 111.20(18) . . ? C48 N2 C50 113.09(19) . . ? C52 N2 Mn3 109.64(14) . . ? C48 N2 Mn3 101.27(13) . . ? C50 N2 Mn3 108.89(13) . . ? O7 C28 O5 126.0(2) . . ? O7 C28 C29 118.6(2) . . ? O5 C28 C29 115.4(2) . . ? C71 C70 C69 120.1(3) . . ? C71 C70 H70 119.9 . . ? C69 C70 H70 119.9 . . ? C35 C30 C31 117.3(2) . . ? C35 C30 C29 124.1(2) . . ? C31 C30 C29 118.6(2) . . ? C13 C12 C11 119.6(2) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? O2 C3 C4 110.80(19) . . ? O2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? O2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C61 C56 C57 117.5(2) . . ? C61 C56 C55 119.6(2) . . ? C57 C56 C55 122.3(2) . . ? C43 C44 C45 120.1(2) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? O13 C74 C75 109.05(18) . . ? O13 C74 H74A 109.9 . . ? C75 C74 H74A 109.9 . . ? O13 C74 H74B 109.9 . . ? C75 C74 H74B 109.9 . . ? H74A C74 H74B 108.3 . . ? N3 C75 C74 111.8(2) . . ? N3 C75 H75A 109.3 . . ? C74 C75 H75A 109.3 . . ? N3 C75 H75B 109.3 . . ? C74 C75 H75B 109.3 . . ? H75A C75 H75B 107.9 . . ? C13 C14 C9 121.8(2) . . ? C13 C14 H14 119.1 . . ? C9 C14 H14 119.1 . . ? C40 C41 C36 121.5(2) . . ? C40 C41 H41 119.3 . . ? C36 C41 H41 119.3 . . ? N1 C2 C1 110.97(18) . . ? N1 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C32 C31 C30 121.7(2) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? N2 C50 C51 109.95(19) . . ? N2 C50 H50A 109.7 . . ? C51 C50 H50A 109.7 . . ? N2 C50 H50B 109.7 . . ? C51 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? O9 C51 C50 108.37(18) . . ? O9 C51 H51A 110.0 . . ? C50 C51 H51A 110.0 . . ? O9 C51 H51B 110.0 . . ? C50 C51 H51B 110.0 . . ? H51A C51 H51B 108.4 . . ? O12 C6 C5 109.93(18) 2_556 . ? O12 C6 H6A 109.7 2_556 . ? C5 C6 H6A 109.7 . . ? O12 C6 H6B 109.7 2_556 . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C69 C68 C73 117.9(2) . . ? C69 C68 C55 124.6(2) . . ? C73 C68 C55 117.4(2) . . ? C67 C62 C63 117.3(2) . . ? C67 C62 C55 122.6(2) . . ? C63 C62 C55 119.4(2) . . ? C21 C26 C25 120.6(3) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? N3 C76 C77 110.8(2) . . ? N3 C76 H76A 109.5 . . ? C77 C76 H76A 109.5 . . ? N3 C76 H76B 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 108.1 . . ? N1 C4 C3 110.68(19) . . ? N1 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C44 C43 C42 121.4(3) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C23 C22 C21 121.9(2) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C46 C45 C44 119.3(2) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C61 C60 C59 120.1(2) . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C34 C33 C32 119.1(2) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? O14 C77 C76 110.8(2) . . ? O14 C77 H77A 109.5 . . ? C76 C77 H77A 109.5 . . ? O14 C77 H77B 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 108.1 . . ? C33 C32 C31 120.1(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C45 C46 C47 120.5(3) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C59 C58 C57 120.3(2) . . ? C59 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? O6 C49 C48 110.18(18) . . ? O6 C49 H49A 109.6 . . ? C48 C49 H49A 109.6 . . ? O6 C49 H49B 109.6 . . ? C48 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? N2 C52 C53 111.61(19) . . ? N2 C52 H52A 109.3 . . ? C53 C52 H52A 109.3 . . ? N2 C52 H52B 109.3 . . ? C53 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? C58 C57 C56 121.0(2) . . ? C58 C57 H57 119.5 . . ? C56 C57 H57 119.5 . . ? C16 C15 C20 117.8(2) . . ? C16 C15 C8 120.6(2) . . ? C20 C15 C8 120.9(2) . . ? N2 C48 C49 111.48(18) . . ? N2 C48 H48A 109.3 . . ? C49 C48 H48A 109.3 . . ? N2 C48 H48B 109.3 . . ? C49 C48 H48B 109.3 . . ? H48A C48 H48B 108.0 . . ? O11 C54 O10 126.2(2) . . ? O11 C54 C55 118.5(2) . . ? O10 C54 C55 115.2(2) . . ? C38 C37 C36 121.1(2) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C12 C13 C14 119.6(2) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C42 C47 C46 120.9(2) . . ? C42 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C25 C24 C23 119.3(3) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C56 C55 C68 116.14(19) . . ? C56 C55 C62 103.72(18) . . ? C68 C55 C62 111.46(19) . . ? C56 C55 C54 109.27(18) . . ? C68 C55 C54 103.48(18) . . ? C62 C55 C54 113.07(19) . . ? C30 C35 C34 121.0(2) . . ? C30 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C64 C63 C62 121.6(2) . . ? C64 C63 H63 119.2 . . ? C62 C63 H63 119.2 . . ? C22 C23 C24 119.8(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C73 C72 C71 119.9(3) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C65 C64 C63 120.3(2) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C62 C67 C66 121.2(2) . . ? C62 C67 H67 119.4 . . ? C66 C67 H67 119.4 . . ? C39 C38 C37 120.3(2) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C19 C20 C15 121.1(3) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C72 C73 C68 121.5(2) . . ? C72 C73 H73 119.2 . . ? C68 C73 H73 119.2 . . ? C68 C69 C70 121.0(2) . . ? C68 C69 H69 119.5 . . ? C70 C69 H69 119.5 . . ? C24 C25 C26 120.9(3) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C18 C19 C20 120.3(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C17 C18 C19 119.4(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? O8 C53 C52 110.23(19) . . ? O8 C53 H53A 109.6 . . ? C52 C53 H53A 109.6 . . ? O8 C53 H53B 109.6 . . ? C52 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? C38 C39 C40 119.5(2) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.3 . . ? C12 C11 C10 120.5(2) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C58 C59 C60 119.4(2) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.3 . . ? C39 C40 C41 120.2(2) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C66 C65 C64 118.9(2) . . ? C66 C65 H65 120.6 . . ? C64 C65 H65 120.6 . . ? C70 C71 C72 119.6(2) . . ? C70 C71 H71 120.2 . . ? C72 C71 H71 120.2 . . ? C33 C34 C35 120.8(3) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C65 C66 C67 120.6(2) . . ? C65 C66 H66 119.7 . . ? C67 C66 H66 119.7 . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? N2S C3S C4S 178.5(5) . . ? C7S O1S C5S 116.4(5) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C7S C8S H8S1 109.5 . . ? C7S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? C7S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? N1S C1S C2S 175.7(7) . . ? O1S C7S C8S 117.2(5) . . ? O1S C7S H7S1 108.0 . . ? C8S C7S H7S1 108.0 . . ? O1S C7S H7S2 108.0 . . ? C8S C7S H7S2 108.0 . . ? H7S1 C7S H7S2 107.3 . . ? O1S C5S C6S 110.4(5) . . ? O1S C5S H5S1 109.6 . . ? C6S C5S H5S1 109.6 . . ? O1S C5S H5S2 109.6 . . ? C6S C5S H5S2 109.6 . . ? H5S1 C5S H5S2 108.1 . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.021 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.095 # Attachment 'StuartLangleyrepl-3 Mn10(2-biphenyl)final2.cif' #========================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 759482' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H146 F8 Mn10 N10 O30' _chemical_formula_weight 2933.91 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' F F 0.0171 0.0103 '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 14.6314(4) _cell_length_b 20.7821(5) _cell_length_c 24.1056(6) _cell_angle_alpha 64.6900(10) _cell_angle_beta 89.4620(10) _cell_angle_gamma 77.6340(10) _cell_volume 6444.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 30.21 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3004 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.950 _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 Apex CCD' _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 75033 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.28 _reflns_number_total 31565 _reflns_number_gt 20982 _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 X-SEED _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 asymmetric unit contains two halves the cluster as well as 4 MeCN solvent molecules. Three of the phenyl rings of one cluster are disordered over two positions. All were refined freely - two were found to be 31/69 occupancy, while the third was found to be 75/25 occupancy. Each disordered ring was Restrained using AFIX 66 commands and the thermal parameters were restrained using SIMU, DELU and ISOR commands. One badly behaved MeCN lies close to a disordered phenyl ring and had it's thermal parameters fixed to 10.1. Bond restraints were placed on three of the solvent MeCN molecules, with partial occupancies applied for the disordered solvent MeCN molecules. All non H atoms were refined anisotropically, except for the MeCN mentioned in which the thermal parameter was fixed. H-atoms are placed in calculated positions except for protonated hydrogens on the teaH and teaH2 ligands which couldn't be found and were omitted. There are solvent accessible voids in the structure of 81 A3 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+3.3538P] 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 31565 _refine_ls_number_parameters 1751 _refine_ls_number_restraints 546 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1786 _refine_ls_wR_factor_gt 0.1567 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.078 _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 -0.10445(4) 1.20114(3) -0.01579(3) 0.01554(13) Uani 1 1 d . . . Mn2 Mn 0.03036(4) 1.06456(3) 0.10005(2) 0.01394(12) Uani 1 1 d . . . Mn3 Mn 0.17247(4) 0.91649(3) 0.19107(3) 0.01598(13) Uani 1 1 d . . . Mn4 Mn 0.17833(4) 0.79485(3) 0.14433(3) 0.01609(13) Uani 1 1 d . . . Mn5 Mn 0.05913(4) 1.06507(3) -0.03771(2) 0.01349(12) Uani 1 1 d . . . Mn6 Mn 0.33052(4) 0.08066(3) 0.63468(3) 0.01648(13) Uani 1 1 d . . . Mn7 Mn 0.32288(4) 0.20217(3) 0.49812(3) 0.01538(13) Uani 1 1 d . B . Mn8 Mn 0.39628(4) 0.20160(3) 0.37058(2) 0.01521(12) Uani 1 1 d . B . Mn9 Mn 0.52791(4) 0.06697(3) 0.35128(3) 0.01562(13) Uani 1 1 d . . . Mn10 Mn 0.56070(4) 0.06414(3) 0.48955(2) 0.01335(12) Uani 1 1 d . . . F1 F -0.05757(14) 1.15380(11) -0.08045(9) 0.0171(4) Uani 1 1 d . . . F2 F 0.02456(14) 0.99960(11) 0.05203(9) 0.0148(4) Uani 1 1 d . . . F3 F 0.16120(14) 1.02530(11) 0.11849(10) 0.0180(5) Uani 1 1 d . . . F4 F 0.20989(14) 0.89128(11) 0.11395(9) 0.0182(5) Uani 1 1 d . . . F5 F 0.65835(15) 0.02723(11) 0.36007(10) 0.0187(5) Uani 1 1 d . . . F6 F 0.44383(14) 0.15280(11) 0.46912(9) 0.0171(4) Uani 1 1 d . . . F7 F 0.29206(15) 0.10662(11) 0.53956(10) 0.0183(5) Uani 1 1 d . . . F8 F 0.47752(14) -0.00139(11) 0.55287(9) 0.0165(4) Uani 1 1 d . . . O1 O -0.09655(17) 1.10794(14) 0.07256(12) 0.0177(5) Uani 1 1 d . . . O2 O -0.0677(2) 1.26214(15) 0.03804(13) 0.0256(6) Uani 1 1 d . . . O3 O -0.0800(2) 1.30139(14) -0.09087(12) 0.0243(6) Uani 1 1 d . . . O4 O -0.22431(18) 1.22186(15) -0.07886(13) 0.0226(6) Uani 1 1 d . . . O5 O 0.04814(17) 1.13592(13) 0.01924(11) 0.0159(5) Uani 1 1 d . . . O6 O 0.0308(2) 1.14364(14) 0.13941(13) 0.0247(6) Uani 1 1 d . . . O7 O 0.1300(2) 1.09816(16) 0.22461(14) 0.0374(8) Uani 1 1 d . . . O8 O 0.01847(18) 0.98120(13) 0.17326(11) 0.0181(5) Uani 1 1 d . . . O9 O 0.2318(2) 0.96908(14) 0.24152(12) 0.0250(6) Uani 1 1 d . . . O10 O 0.31139(18) 0.83487(14) 0.23147(12) 0.0215(6) Uani 1 1 d . . . O11 O 0.12052(18) 0.82070(13) 0.20432(11) 0.0184(6) Uani 1 1 d . . . O12 O 0.30752(19) 0.74908(14) 0.19900(12) 0.0220(6) Uani 1 1 d . . . O13 O 0.1304(2) 0.70244(14) 0.17767(12) 0.0233(6) Uani 1 1 d . . . O14 O 0.18902(17) 0.97750(14) -0.00279(12) 0.0187(6) Uani 1 1 d . . . O15 O 0.09274(18) 1.08214(14) -0.13460(12) 0.0194(6) Uani 1 1 d . . . O16 O 0.2784(2) 0.02460(16) 0.72648(13) 0.0288(7) Uani 1 1 d . . . O17 O 0.38462(18) 0.17657(14) 0.57494(12) 0.0185(6) Uani 1 1 d . . . O18 O 0.19364(19) 0.16092(14) 0.61986(13) 0.0238(6) Uani 1 1 d . . . O19 O 0.19431(19) 0.24668(14) 0.52272(13) 0.0242(6) Uani 1 1 d . . . O20 O 0.27562(18) 0.21720(14) 0.42104(12) 0.0218(6) Uani 1 1 d . . . O21 O 0.3515(2) 0.30088(14) 0.46052(13) 0.0294(7) Uani 1 1 d . . . O22 O 0.41376(19) 0.30341(14) 0.37389(13) 0.0232(6) Uani 1 1 d . . . O23 O 0.4302(2) 0.26597(14) 0.27154(12) 0.0247(6) Uani 1 1 d . . . O24 O 0.40093(18) 0.11077(14) 0.34849(12) 0.0193(6) Uani 1 1 d . . . O25 O 0.54681(17) 0.13757(13) 0.37998(11) 0.0164(5) Uani 1 1 d . . . O26 O 0.69040(17) -0.02488(13) 0.51716(12) 0.0193(6) Uani 1 1 d . . . O27 O 0.59577(18) 0.07987(14) 0.57403(12) 0.0201(6) Uani 1 1 d . . . O28 O 0.5283(2) 0.14852(16) 0.25476(12) 0.0289(7) Uani 1 1 d . . . O29 O 0.6487(3) 0.1128(2) 0.20970(18) 0.0949(19) Uani 1 1 d . . . O30 O 0.51518(18) -0.01547(14) 0.33784(12) 0.0201(6) Uani 1 1 d . . . N1 N -0.2425(2) 1.22710(18) 0.02997(16) 0.0253(8) Uani 1 1 d . . . N2 N 0.1091(2) 0.87588(17) 0.28858(14) 0.0213(7) Uani 1 1 d . . . N3 N 0.1830(2) 1.12879(17) -0.06480(15) 0.0191(7) Uani 1 1 d . . . N4 N 0.3931(3) 0.12182(18) 0.70008(15) 0.0244(8) Uani 1 1 d . . . N5 N 0.2562(2) 0.23261(17) 0.30517(15) 0.0229(7) Uani 1 1 d . . . N6 N 0.6855(2) 0.12601(16) 0.46753(14) 0.0171(7) Uani 1 1 d . . . C1 C -0.1730(3) 1.1024(2) 0.10941(19) 0.0249(9) Uani 1 1 d . . . H1A H -0.1610 1.1149 0.1426 0.030 Uiso 1 1 calc R . . H1B H -0.1814 1.0527 0.1273 0.030 Uiso 1 1 calc R . . C2 C -0.2608(3) 1.1549(2) 0.0686(2) 0.0297(10) Uani 1 1 d . . . H2A H -0.2815 1.1350 0.0424 0.036 Uiso 1 1 calc R . . H2B H -0.3107 1.1602 0.0942 0.036 Uiso 1 1 calc R . . C3 C -0.1527(3) 1.3092(2) 0.0412(2) 0.0367(11) Uani 1 1 d . . . H3A H -0.1751 1.3480 0.0004 0.044 Uiso 1 1 calc R . . H3B H -0.1403 1.3314 0.0676 0.044 Uiso 1 1 calc R . . C4 C -0.2277(3) 1.2662(3) 0.0666(2) 0.0352(11) Uani 1 1 d . . . H4A H -0.2085 1.2312 0.1091 0.042 Uiso 1 1 calc R . . H4B H -0.2862 1.2994 0.0654 0.042 Uiso 1 1 calc R . . C5 C -0.3179(3) 1.2722(3) -0.0202(2) 0.0327(10) Uani 1 1 d . . . H5A H -0.3096 1.3219 -0.0402 0.039 Uiso 1 1 calc R . . H5B H -0.3781 1.2735 -0.0031 0.039 Uiso 1 1 calc R . . C6 C -0.3173(3) 1.2421(2) -0.0671(2) 0.0280(9) Uani 1 1 d . . . H6A H -0.3449 1.1999 -0.0515 0.034 Uiso 1 1 calc R . . H6B H -0.3540 1.2789 -0.1049 0.034 Uiso 1 1 calc R . . C7 C 0.1206(3) 1.1747(2) 0.01131(18) 0.0200(8) Uani 1 1 d . . . H7A H 0.1727 1.1446 0.0425 0.024 Uiso 1 1 calc R . . H7B H 0.0968 1.2191 0.0162 0.024 Uiso 1 1 calc R . . C8 C 0.1543(3) 1.1938(2) -0.05237(18) 0.0204(8) Uani 1 1 d . . . H8A H 0.1043 1.2293 -0.0831 0.024 Uiso 1 1 calc R . . H8B H 0.2072 1.2162 -0.0560 0.024 Uiso 1 1 calc R . . C9 C 0.2666(3) 1.0763(2) -0.0251(2) 0.0250(9) Uani 1 1 d . . . H9A H 0.2633 1.0734 0.0161 0.030 Uiso 1 1 calc R . . H9B H 0.3225 1.0932 -0.0411 0.030 Uiso 1 1 calc R . . C10 C 0.2736(3) 1.0008(2) -0.0222(2) 0.0238(9) Uani 1 1 d . . . H10A H 0.2840 1.0024 -0.0625 0.029 Uiso 1 1 calc R . . H10B H 0.3264 0.9661 0.0065 0.029 Uiso 1 1 calc R . . C11 C 0.1954(3) 1.1526(2) -0.13099(18) 0.0235(9) Uani 1 1 d . . . H11A H 0.2490 1.1194 -0.1359 0.028 Uiso 1 1 calc R . . H11B H 0.2080 1.2011 -0.1483 0.028 Uiso 1 1 calc R . . C12 C 0.1093(3) 1.1542(2) -0.16503(18) 0.0211(8) Uani 1 1 d . . . H12A H 0.0561 1.1901 -0.1635 0.025 Uiso 1 1 calc R . . H12B H 0.1193 1.1663 -0.2078 0.025 Uiso 1 1 calc R . . C13 C 0.0678(3) 1.1464(2) 0.18544(19) 0.0268(9) Uani 1 1 d . . . C14 C 0.0280(3) 1.2168(2) 0.1909(2) 0.0341(11) Uani 1 1 d . . . C15 C 0.0460(4) 1.2818(2) 0.1472(2) 0.0513(16) Uani 1 1 d . . . H15 H 0.0842 1.2818 0.1162 0.062 Uiso 1 1 calc R . . C16 C 0.0062(5) 1.3467(3) 0.1506(3) 0.064(2) Uani 1 1 d . . . H16 H 0.0179 1.3903 0.1215 0.077 Uiso 1 1 calc R . . C17 C -0.0491(4) 1.3478(3) 0.1952(3) 0.0597(18) Uani 1 1 d . . . H17 H -0.0752 1.3919 0.1967 0.072 Uiso 1 1 calc R . . C18 C -0.0674(4) 1.2832(3) 0.2391(3) 0.0537(16) Uani 1 1 d . . . H18 H -0.1064 1.2845 0.2695 0.064 Uiso 1 1 calc R . . C19 C -0.0282(3) 1.2164(3) 0.2382(2) 0.0361(11) Uani 1 1 d . . . C20 C -0.0500(3) 1.1471(3) 0.2850(3) 0.0409(13) Uani 1 1 d . . . C21 C -0.1274(5) 1.1258(5) 0.2757(3) 0.086(3) Uani 1 1 d . . . H21 H -0.1681 1.1553 0.2403 0.103 Uiso 1 1 calc R . . C22 C -0.1473(6) 1.0613(6) 0.3176(4) 0.116(4) Uani 1 1 d U . . H22 H -0.2008 1.0481 0.3097 0.139 Uiso 1 1 calc R . . C23 C -0.0936(5) 1.0194(4) 0.3672(4) 0.096(3) Uani 1 1 d U . . H23 H -0.1087 0.9763 0.3948 0.115 Uiso 1 1 calc R . . C24 C -0.0134(4) 1.0372(3) 0.3802(4) 0.103(3) Uani 1 1 d U . . H24 H 0.0255 1.0074 0.4164 0.123 Uiso 1 1 calc R . . C25 C 0.0067(4) 1.1018(3) 0.3369(4) 0.082(3) Uani 1 1 d . . . H25 H 0.0615 1.1141 0.3441 0.098 Uiso 1 1 calc R . . C26 C -0.0200(3) 0.9813(2) 0.22819(17) 0.0210(8) Uani 1 1 d . . . H26A H -0.0878 0.9988 0.2210 0.025 Uiso 1 1 calc R . . H26B H 0.0054 1.0132 0.2404 0.025 Uiso 1 1 calc R . . C27 C 0.0059(3) 0.9037(2) 0.27827(18) 0.0225(8) Uani 1 1 d . . . H27A H -0.0187 0.9022 0.3162 0.027 Uiso 1 1 calc R . . H27B H -0.0222 0.8725 0.2665 0.027 Uiso 1 1 calc R . . C28 C 0.2424(3) 0.9222(2) 0.30638(19) 0.0282(10) Uani 1 1 d . . . H28A H 0.2634 0.9465 0.3287 0.034 Uiso 1 1 calc R . . H28B H 0.2895 0.8776 0.3151 0.034 Uiso 1 1 calc R . . C29 C 0.1501(3) 0.9034(2) 0.32773(19) 0.0291(10) Uani 1 1 d . . . H29A H 0.1601 0.8664 0.3702 0.035 Uiso 1 1 calc R . . H29B H 0.1064 0.9467 0.3261 0.035 Uiso 1 1 calc R . . C30 C 0.1370(3) 0.7958(2) 0.31200(18) 0.0252(9) Uani 1 1 d . . . H30A H 0.1069 0.7733 0.3493 0.030 Uiso 1 1 calc R . . H30B H 0.2045 0.7796 0.3224 0.030 Uiso 1 1 calc R . . C31 C 0.1099(3) 0.7712(2) 0.26480(17) 0.0234(9) Uani 1 1 d . . . H31A H 0.1490 0.7232 0.2739 0.028 Uiso 1 1 calc R . . H31B H 0.0450 0.7671 0.2677 0.028 Uiso 1 1 calc R . . C32 C 0.0954(3) 0.6735(2) 0.14811(18) 0.0227(9) Uani 1 1 d . . . C33 C 0.0659(3) 0.6042(2) 0.1877(2) 0.0327(11) Uani 1 1 d . . . C34 C -0.0062(4) 0.6083(3) 0.2246(2) 0.0442(13) Uani 1 1 d . . . H34 H -0.0324 0.6528 0.2254 0.053 Uiso 1 1 calc R . . C35 C -0.0401(5) 0.5469(3) 0.2604(3) 0.0635(18) Uani 1 1 d . . . H35 H -0.0884 0.5497 0.2852 0.076 Uiso 1 1 calc R . . C36 C 0.0006(5) 0.4809(3) 0.2581(3) 0.0652(19) Uani 1 1 d . . . H36 H -0.0204 0.4390 0.2820 0.078 Uiso 1 1 calc R . . C37 C 0.0702(4) 0.4771(3) 0.2213(2) 0.0512(15) Uani 1 1 d . . . H37 H 0.0952 0.4327 0.2201 0.061 Uiso 1 1 calc R . . C38 C 0.1056(4) 0.5378(2) 0.1853(2) 0.0381(12) Uani 1 1 d . . . C39 C 0.1856(4) 0.5298(2) 0.1504(2) 0.0446(13) Uani 1 1 d . . . C40 C 0.2648(4) 0.5527(3) 0.1559(3) 0.0500(14) Uani 1 1 d . . . H40 H 0.2668 0.5748 0.1820 0.060 Uiso 1 1 calc R . . C41 C 0.3413(5) 0.5439(3) 0.1242(3) 0.0663(18) Uani 1 1 d . . . H41 H 0.3940 0.5600 0.1292 0.080 Uiso 1 1 calc R . . C42 C 0.3404(5) 0.5117(3) 0.0852(3) 0.076(2) Uani 1 1 d . . . H42 H 0.3918 0.5064 0.0632 0.091 Uiso 1 1 calc R . . C43 C 0.2643(6) 0.4877(3) 0.0789(4) 0.091(3) Uani 1 1 d . . . H43 H 0.2642 0.4656 0.0526 0.109 Uiso 1 1 calc R . . C44 C 0.1846(5) 0.4952(3) 0.1113(3) 0.0655(18) Uani 1 1 d . . . H44 H 0.1330 0.4777 0.1070 0.079 Uiso 1 1 calc R . . C45 C 0.3436(3) 0.7752(2) 0.22936(18) 0.0211(8) Uani 1 1 d . . . C46 C 0.4332(3) 0.7272(2) 0.2696(2) 0.0315(11) Uani 1 1 d . . . C47 C 0.4288(4) 0.7016(2) 0.3337(2) 0.0427(13) Uani 1 1 d . . . H47 H 0.3749 0.7189 0.3487 0.051 Uiso 1 1 calc R . . C48 C 0.5033(5) 0.6511(3) 0.3749(3) 0.0637(19) Uani 1 1 d . . . H48 H 0.4999 0.6342 0.4172 0.076 Uiso 1 1 calc R . . C49 C 0.5818(5) 0.6266(3) 0.3521(3) 0.071(2) Uani 1 1 d . . . H49 H 0.6316 0.5918 0.3794 0.085 Uiso 1 1 calc R . . C50 C 0.5892(4) 0.6518(3) 0.2901(3) 0.0640(19) Uani 1 1 d . . . H50 H 0.6442 0.6348 0.2760 0.077 Uiso 1 1 calc R . . C51 C 0.5138(3) 0.7037(3) 0.2473(3) 0.0456(14) Uani 1 1 d . . . C52 C 0.5263(4) 0.7325(4) 0.1817(3) 0.0569(15) Uani 1 1 d U . . C53 C 0.5635(5) 0.6879(5) 0.1530(4) 0.099(3) Uani 1 1 d U . . H53 H 0.5787 0.6375 0.1767 0.118 Uiso 1 1 calc R . . C54 C 0.5779(6) 0.7135(8) 0.0943(5) 0.141(4) Uani 1 1 d U . . H54 H 0.6022 0.6807 0.0781 0.169 Uiso 1 1 calc R . . C55 C 0.5586(5) 0.7858(7) 0.0569(4) 0.127(4) Uani 1 1 d U . . H55 H 0.5704 0.8025 0.0157 0.152 Uiso 1 1 calc R . . C56 C 0.5190(5) 0.8378(6) 0.0817(3) 0.104(3) Uani 1 1 d U . . H56 H 0.5045 0.8881 0.0573 0.125 Uiso 1 1 calc R . . C57 C 0.5042(4) 0.8072(4) 0.1448(3) 0.0632(16) Uani 1 1 d U . . H57 H 0.4786 0.8384 0.1622 0.076 Uiso 1 1 calc R . . C58 C 0.1613(3) 0.2208(2) 0.57505(19) 0.0236(9) Uani 1 1 d . B . C59 C 0.0765(3) 0.2722(2) 0.5826(2) 0.0308(10) Uani 1 1 d . . . C60 C 0.0849(4) 0.2941(2) 0.6284(2) 0.0401(12) Uani 1 1 d . B . H60 H 0.1381 0.2725 0.6564 0.048 Uiso 1 1 calc R . . C61 C 0.0152(4) 0.3479(3) 0.6333(3) 0.0537(16) Uani 1 1 d . . . H61 H 0.0220 0.3626 0.6642 0.064 Uiso 1 1 calc R B . C62 C -0.0640(4) 0.3792(3) 0.5923(3) 0.0635(19) Uani 1 1 d . B . H62 H -0.1110 0.4154 0.5951 0.076 Uiso 1 1 calc R . . C63 C -0.0731(4) 0.3573(3) 0.5479(3) 0.0563(17) Uani 1 1 d . . . H63 H -0.1268 0.3796 0.5202 0.068 Uiso 1 1 calc R B . C64 C -0.0056(3) 0.3026(2) 0.5414(2) 0.0376(12) Uani 1 1 d . B . C65 C -0.0228(3) 0.2764(3) 0.4954(2) 0.0382(12) Uani 1 1 d . . . C66 C -0.0623(3) 0.3255(3) 0.4353(2) 0.0445(13) Uani 1 1 d . B . H66 H -0.0728 0.3757 0.4227 0.053 Uiso 1 1 calc R . . C67 C -0.0856(4) 0.2985(3) 0.3949(3) 0.0554(15) Uani 1 1 d . . . H67 H -0.1127 0.3312 0.3554 0.066 Uiso 1 1 calc R B . C68 C -0.0696(4) 0.2253(3) 0.4120(3) 0.0570(16) Uani 1 1 d . B . H68 H -0.0851 0.2082 0.3843 0.068 Uiso 1 1 calc R . . C69 C -0.0296(4) 0.1761(3) 0.4715(3) 0.0501(14) Uani 1 1 d . . . H69 H -0.0186 0.1260 0.4835 0.060 Uiso 1 1 calc R B . C70 C -0.0067(3) 0.2012(3) 0.5122(2) 0.0402(12) Uani 1 1 d . B . H70 H 0.0200 0.1679 0.5517 0.048 Uiso 1 1 calc R . . C71 C 0.4015(3) 0.2242(2) 0.59892(19) 0.0251(9) Uani 1 1 d . B . H71A H 0.3668 0.2736 0.5726 0.030 Uiso 1 1 calc R . . H71B H 0.4679 0.2239 0.5992 0.030 Uiso 1 1 calc R . . C72 C 0.3721(3) 0.2016(2) 0.66443(18) 0.0225(9) Uani 1 1 d . B . H72A H 0.4049 0.2223 0.6852 0.027 Uiso 1 1 calc R . . H72B H 0.3052 0.2213 0.6625 0.027 Uiso 1 1 calc R . . C73 C 0.4957(3) 0.0902(2) 0.7125(2) 0.0333(11) Uani 1 1 d . . . H73A H 0.5178 0.0898 0.7504 0.040 Uiso 1 1 calc R . . H73B H 0.5273 0.1208 0.6794 0.040 Uiso 1 1 calc R . . C74 C 0.3443(5) 0.1003(3) 0.7559(2) 0.0617(19) Uani 1 1 d . B . H74A H 0.3874 0.0613 0.7896 0.074 Uiso 1 1 calc R A 3 H74B H 0.3276 0.1416 0.7659 0.074 Uiso 1 1 calc R A 3 C75 C 0.2632(6) 0.0766(4) 0.7523(3) 0.0191(18) Uani 0.50 1 d P B 3 H75A H 0.2135 0.1185 0.7269 0.023 Uiso 0.50 1 calc PR B 3 H75B H 0.2427 0.0543 0.7932 0.023 Uiso 0.50 1 calc PR B 3 C76 C 0.3767(3) 0.3329(2) 0.40638(19) 0.0222(8) Uani 1 1 d . B . C77 C 0.3514(3) 0.4152(2) 0.37812(18) 0.0239(9) Uani 1 1 d . . . C78 C 0.2607(4) 0.4510(3) 0.3501(2) 0.0389(12) Uani 1 1 d . B . H78 H 0.2168 0.4236 0.3529 0.047 Uiso 1 1 calc R . . C79 C 0.2341(4) 0.5263(3) 0.3184(2) 0.0446(13) Uani 1 1 d . . . H79 H 0.1728 0.5492 0.3007 0.054 Uiso 1 1 calc R B . C80 C 0.2978(4) 0.5663(3) 0.3132(2) 0.0491(14) Uani 1 1 d . B . H80 H 0.2806 0.6170 0.2911 0.059 Uiso 1 1 calc R . . C81 C 0.3865(4) 0.5331(3) 0.3399(3) 0.0637(18) Uani 1 1 d . . . H81 H 0.4298 0.5617 0.3347 0.076 Uiso 1 1 calc R B . C82 C 0.4161(4) 0.4563(2) 0.3754(3) 0.0494(15) Uani 1 1 d D B . C89 C 0.1822(3) 0.2422(2) 0.39498(19) 0.0269(9) Uani 1 1 d . B . H89A H 0.1483 0.2784 0.4077 0.032 Uiso 1 1 calc R . . H89B H 0.1513 0.2018 0.4087 0.032 Uiso 1 1 calc R . . C90 C 0.1824(3) 0.2758(2) 0.32540(19) 0.0291(10) Uani 1 1 d . B . H90A H 0.1217 0.2793 0.3071 0.035 Uiso 1 1 calc R . . H90B H 0.1920 0.3250 0.3109 0.035 Uiso 1 1 calc R . . C91 C 0.2369(3) 0.1606(2) 0.3187(2) 0.0258(9) Uani 1 1 d . B . H91A H 0.1870 0.1669 0.2894 0.031 Uiso 1 1 calc R . . H91B H 0.2158 0.1403 0.3597 0.031 Uiso 1 1 calc R . . C92 C 0.3243(3) 0.1074(2) 0.3153(2) 0.0270(9) Uani 1 1 d . B . H92A H 0.3145 0.0581 0.3331 0.032 Uiso 1 1 calc R . . H92B H 0.3369 0.1208 0.2727 0.032 Uiso 1 1 calc R . . C93 C 0.3464(3) 0.3139(2) 0.2342(2) 0.0332(10) Uani 1 1 d . B . H93A H 0.3223 0.3508 0.2486 0.040 Uiso 1 1 calc R C 7 H93B H 0.3607 0.3386 0.1919 0.040 Uiso 1 1 calc R C 7 C94 C 0.2651(5) 0.2716(4) 0.2411(3) 0.0236(14) Uani 0.687(4) 1 d P B 8 H94A H 0.2063 0.3061 0.2205 0.028 Uiso 0.687(4) 1 calc PR B 8 H94B H 0.2806 0.2379 0.2226 0.028 Uiso 0.687(4) 1 calc PR B 8 C95 C 0.6562(3) 0.1926(2) 0.40877(17) 0.0188(8) Uani 1 1 d . B . H95A H 0.7093 0.2147 0.3953 0.023 Uiso 1 1 calc R . . H95B H 0.6074 0.2277 0.4154 0.023 Uiso 1 1 calc R . . C96 C 0.6198(3) 0.1762(2) 0.35873(17) 0.0181(8) Uani 1 1 d . B . H96A H 0.5955 0.2216 0.3223 0.022 Uiso 1 1 calc R . . H96B H 0.6708 0.1468 0.3477 0.022 Uiso 1 1 calc R . . C97 C 0.7676(3) 0.0737(2) 0.46344(19) 0.0222(8) Uani 1 1 d . B . H97A H 0.8241 0.0904 0.4653 0.027 Uiso 1 1 calc R . . H97B H 0.7616 0.0718 0.4242 0.027 Uiso 1 1 calc R . . C98 C 0.7763(3) -0.0018(2) 0.51511(19) 0.0218(8) Uani 1 1 d . B . H98A H 0.8269 -0.0361 0.5090 0.026 Uiso 1 1 calc R . . H98B H 0.7914 -0.0014 0.5541 0.026 Uiso 1 1 calc R . . C99 C 0.7019(3) 0.1471(2) 0.51753(18) 0.0191(8) Uani 1 1 d . B . H99A H 0.7183 0.1942 0.5002 0.023 Uiso 1 1 calc R . . H99B H 0.7540 0.1113 0.5463 0.023 Uiso 1 1 calc R . . C100 C 0.6154(3) 0.1512(2) 0.55073(18) 0.0200(8) Uani 1 1 d . B . H10C H 0.6263 0.1635 0.5843 0.024 Uiso 1 1 calc R . . H10D H 0.5632 0.1880 0.5228 0.024 Uiso 1 1 calc R . . C101 C 0.5808(5) 0.1606(3) 0.2117(3) 0.072(2) Uani 1 1 d D B . C115 C 0.4791(3) -0.0135(2) 0.28200(19) 0.0315(10) Uani 1 1 d . . . H11C H 0.5065 0.0186 0.2471 0.038 Uiso 1 1 calc R . . H11D H 0.4115 0.0048 0.2758 0.038 Uiso 1 1 calc R . . C1' C 0.5962(7) 0.2458(3) 0.1774(4) 0.033(3) Uani 0.313(4) 1 d PGDU B 5 C2' C 0.6658(6) 0.2755(5) 0.1894(4) 0.037(3) Uani 0.313(4) 1 d PGU B 5 H2' H 0.7112 0.2469 0.2225 0.044 Uiso 0.313(4) 1 calc PR B 5 C3' C 0.6677(7) 0.3478(5) 0.1520(5) 0.055(4) Uani 0.313(4) 1 d PGU B 5 H3' H 0.7143 0.3677 0.1601 0.066 Uiso 0.313(4) 1 calc PR B 5 C4' C 0.5998(8) 0.3905(3) 0.1026(4) 0.059(5) Uani 0.313(4) 1 d PGU B 5 H4' H 0.6011 0.4389 0.0777 0.071 Uiso 0.313(4) 1 calc PR B 5 C5' C 0.5302(7) 0.3609(4) 0.0906(4) 0.033(5) Uiso 0.313(4) 1 d PGU B 5 H5' H 0.4848 0.3894 0.0575 0.039 Uiso 0.313(4) 1 calc PR B 5 C6' C 0.5283(6) 0.2885(5) 0.1280(4) 0.035(3) Uani 0.313(4) 1 d PGU B 5 C7' C 0.4523(6) 0.2640(6) 0.1124(5) 0.038(3) Uani 0.313(4) 1 d PGU B 5 C8' C 0.3640(7) 0.3115(5) 0.0926(5) 0.054(4) Uani 0.313(4) 1 d PGU B 5 H8' H 0.3560 0.3598 0.0864 0.065 Uiso 0.313(4) 1 calc PR B 5 C9' C 0.2878(6) 0.2867(7) 0.0822(6) 0.069(5) Uani 0.313(4) 1 d PGU B 5 H9' H 0.2288 0.3185 0.0690 0.083 Uiso 0.313(4) 1 calc PR B 5 C10' C 0.2999(7) 0.2145(7) 0.0915(6) 0.078(6) Uani 0.313(4) 1 d PGU B 5 H10' H 0.2489 0.1980 0.0846 0.094 Uiso 0.313(4) 1 calc PR B 5 C11' C 0.3882(8) 0.1671(5) 0.1113(5) 0.059(5) Uani 0.313(4) 1 d PGU B 5 H11' H 0.3962 0.1187 0.1176 0.070 Uiso 0.313(4) 1 calc PR B 5 C12' C 0.4644(6) 0.1918(5) 0.1218(5) 0.043(4) Uani 0.313(4) 1 d PGU B 5 H12' H 0.5234 0.1600 0.1350 0.052 Uiso 0.313(4) 1 calc PR B 5 C13' C 0.4875(6) 0.4328(5) 0.4347(4) 0.043(6) Uani 0.245(6) 1 d PGD B 1 C14' C 0.5588(6) 0.3749(5) 0.4377(5) 0.066(9) Uani 0.245(6) 1 d PGU B 1 H14' H 0.5501 0.3485 0.4160 0.079 Uiso 0.245(6) 1 calc PR B 1 C15' C 0.6430(7) 0.3563(8) 0.4731(8) 0.074(9) Uani 0.245(6) 1 d PGU B 1 H15' H 0.6907 0.3175 0.4751 0.089 Uiso 0.245(6) 1 calc PR B 1 C16' C 0.6560(8) 0.3957(7) 0.5055(7) 0.086(9) Uani 0.245(6) 1 d PGU B 1 H16' H 0.7124 0.3832 0.5292 0.103 Uiso 0.245(6) 1 calc PR B 1 C17' C 0.5848(8) 0.4536(6) 0.5025(5) 0.073(8) Uani 0.245(6) 1 d PGU B 1 H17' H 0.5935 0.4799 0.5242 0.088 Uiso 0.245(6) 1 calc PR B 1 C18' C 0.5005(8) 0.4722(7) 0.4671(6) 0.059(7) Uani 0.245(6) 1 d PGU B 1 H18' H 0.4528 0.5109 0.4652 0.071 Uiso 0.245(6) 1 calc PR B 1 C75' C 0.3029(8) 0.0419(6) 0.7766(5) 0.044(3) Uani 0.50 1 d P B 4 H75C H 0.2465 0.0530 0.7954 0.052 Uiso 0.50 1 calc PR B 4 H75D H 0.3456 -0.0005 0.8079 0.052 Uiso 0.50 1 calc PR B 4 C94' C 0.2842(10) 0.2789(9) 0.2362(6) 0.0236(13) Uani 0.313(4) 1 d PG B 7 H94C H 0.3068 0.2454 0.2182 0.028 Uiso 0.313(4) 1 calc PR B 7 H94D H 0.2280 0.3133 0.2111 0.028 Uiso 0.313(4) 1 calc PR B 7 C1D C 0.5382(3) 0.22449(17) 0.15340(16) 0.0253(13) Uani 0.687(4) 1 d PGU B 6 C2D C 0.5678(3) 0.2856(2) 0.14898(18) 0.0342(17) Uani 0.687(4) 1 d PGU B 6 H2D H 0.6112 0.2813 0.1791 0.041 Uiso 0.687(4) 1 calc PR B 6 C3D C 0.5325(4) 0.35333(18) 0.0996(2) 0.051(3) Uani 0.687(4) 1 d PGU B 6 H3D H 0.5523 0.3942 0.0966 0.061 Uiso 0.687(4) 1 calc PR B 6 C4D C 0.4677(3) 0.35988(18) 0.05457(18) 0.0418(17) Uani 0.687(4) 1 d PGU B 6 H4D H 0.4441 0.4052 0.0215 0.050 Uiso 0.687(4) 1 calc PR B 6 C5D C 0.4381(3) 0.2987(2) 0.05899(17) 0.0449(18) Uani 0.687(4) 1 d PGU B 6 H5D H 0.3948 0.3031 0.0289 0.054 Uiso 0.687(4) 1 calc PR B 6 C6D C 0.4734(3) 0.23103(19) 0.10840(19) 0.0311(16) Uani 0.687(4) 1 d PGU B 6 C7D C 0.4409(3) 0.1655(2) 0.1136(2) 0.0348(17) Uani 0.687(4) 1 d PGU B 6 C8D C 0.5000(3) 0.1106(2) 0.1032(2) 0.0437(18) Uani 0.687(4) 1 d PGU B 6 H8D H 0.5607 0.1144 0.0929 0.052 Uiso 0.687(4) 1 calc PR B 6 C9D C 0.4685(3) 0.0499(2) 0.1082(2) 0.0480(19) Uani 0.687(4) 1 d PGU B 6 H9D H 0.5081 0.0132 0.1012 0.058 Uiso 0.687(4) 1 calc PR B 6 C10D C 0.3778(3) 0.0443(2) 0.1235(2) 0.051(2) Uani 0.687(4) 1 d PGU B 6 H10E H 0.3568 0.0037 0.1268 0.061 Uiso 0.687(4) 1 calc PR B 6 C11D C 0.3187(3) 0.0992(3) 0.1339(2) 0.0451(18) Uani 0.687(4) 1 d PGU B 6 H11E H 0.2580 0.0954 0.1442 0.054 Uiso 0.687(4) 1 calc PR B 6 C12D C 0.3502(3) 0.1598(2) 0.1289(2) 0.043(2) Uani 0.687(4) 1 d PGU B 6 H12D H 0.3106 0.1965 0.1359 0.052 Uiso 0.687(4) 1 calc PR B 6 C13D C 0.5146(2) 0.4210(2) 0.4023(2) 0.0374(17) Uani 0.755(6) 1 d PG B 2 C14D C 0.5288(2) 0.3674(2) 0.46291(19) 0.0386(19) Uani 0.755(6) 1 d PGU B 2 H14D H 0.4777 0.3526 0.4838 0.046 Uiso 0.755(6) 1 calc PR B 2 C15D C 0.6192(3) 0.3360(2) 0.49231(18) 0.055(2) Uani 0.755(6) 1 d PGU B 2 H15D H 0.6287 0.3001 0.5328 0.065 Uiso 0.755(6) 1 calc PR B 2 C16D C 0.6955(2) 0.3581(2) 0.4611(3) 0.071(3) Uani 0.755(6) 1 d PG B 2 H16D H 0.7561 0.3371 0.4808 0.085 Uiso 0.755(6) 1 calc PR B 2 C17D C 0.6814(2) 0.4117(3) 0.4005(3) 0.075(3) Uani 0.755(6) 1 d PG B 2 H17D H 0.7324 0.4265 0.3797 0.091 Uiso 0.755(6) 1 calc PR B 2 C18D C 0.5909(3) 0.4431(2) 0.37113(19) 0.059(2) Uani 0.755(6) 1 d PG B 2 H18D H 0.5815 0.4790 0.3306 0.071 Uiso 0.755(6) 1 calc PR B 2 N1S N 0.1704(5) 0.4701(4) 0.5892(4) 0.103(2) Uani 1 1 d . F . N2S N 0.7063(8) 0.3636(7) 0.2659(5) 0.143(6) Uani 0.60 1 d P D 15 N3S N 0.5849(10) 0.5345(9) 0.0950(11) 0.128(8) Uani 0.40 1 d PD E 15 C1S C 0.1774(5) 0.4492(3) 0.5499(4) 0.077(2) Uani 1 1 d . . . C2S C 0.1808(7) 0.4270(4) 0.5012(4) 0.107(3) Uani 1 1 d . F 2 H2S1 H 0.1215 0.4476 0.4766 0.160 Uiso 1 1 calc R F 2 H2S2 H 0.1934 0.3745 0.5185 0.160 Uiso 1 1 calc R F 2 H2S3 H 0.2297 0.4438 0.4760 0.160 Uiso 1 1 calc R F 2 C3S C 0.6277(8) 0.3795(5) 0.2585(4) 0.065(3) Uani 0.60 1 d P D 15 C4S C 0.5285(5) 0.4027(4) 0.2521(3) 0.0290(17) Uani 0.60 1 d P D 15 H4S1 H 0.5038 0.3716 0.2882 0.044 Uiso 0.60 1 calc PR D 15 H4S2 H 0.5036 0.4001 0.2166 0.044 Uiso 0.60 1 calc PR D 15 H4S3 H 0.5109 0.4523 0.2471 0.044 Uiso 0.60 1 calc PR D 15 C5S C 0.6530(9) 0.5000(7) 0.1001(7) 0.059(4) Uani 0.40 1 d PD E 15 C6S C 0.7417(11) 0.4535(10) 0.1028(10) 0.095(7) Uani 0.40 1 d PD E 15 H6S1 H 0.7399 0.4369 0.0715 0.142 Uiso 0.40 1 d P G 15 H6S2 H 0.7560 0.4135 0.1424 0.142 Uiso 0.40 1 d P H 15 H6S3 H 0.7892 0.4818 0.0950 0.142 Uiso 0.40 1 d P I 15 N1V N 0.2109(12) 0.3638(18) -0.0058(15) 0.296(16) Uani 0.50 1 d PDU J 14 N2V N 0.0629(16) 0.4604(10) -0.0061(9) 0.175(9) Uani 0.50 1 d PDU K 15 C2V C 0.1341(11) 0.3760(11) -0.0150(9) 0.115(6) Uani 0.50 1 d PDU J 14 C3V C 0.0465(12) 0.3913(7) -0.0489(8) 0.115(8) Uani 0.50 1 d PDU J 14 H3V1 H 0.0664 0.4059 -0.0927 0.172 Uiso 0.50 1 d P L 14 H3V2 H 0.0008 0.4251 -0.0474 0.172 Uiso 0.50 1 d P M 14 H3V3 H 0.0314 0.3439 -0.0385 0.172 Uiso 0.50 1 d P N 14 C4V C 0.0674(14) 0.4236(9) -0.0293(7) 0.093(5) Uani 0.50 1 d PDU K 15 C5V C 0.093(2) 0.3845(17) -0.0664(15) 0.200 Uiso 0.50 1 d PD K 15 H5V1 H 0.1536 0.3508 -0.0502 0.300 Uiso 0.50 1 d P O 15 H5V2 H 0.1172 0.4269 -0.1068 0.300 Uiso 0.50 1 d P P 15 H5V3 H 0.0510 0.3725 -0.0812 0.300 Uiso 0.50 1 d P Q 15 N1X N 0.5346(5) -0.0069(4) 0.0834(4) 0.110 Uiso 1 1 d D R 8 C1X C 0.4609(6) -0.0149(5) 0.1034(4) 0.110 Uiso 1 1 d D R 8 C2X C 0.3723(6) -0.0297(5) 0.1291(4) 0.110 Uiso 1 1 d D R 8 H2X1 H 0.3412 -0.0477 0.1058 0.165 Uiso 1 1 calc R R 8 H2X2 H 0.3326 0.0146 0.1271 0.165 Uiso 1 1 calc R R 8 H2X3 H 0.3850 -0.0657 0.1713 0.165 Uiso 1 1 calc R R 8 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(3) 0.0178(3) 0.0148(3) -0.0101(2) 0.0011(2) -0.0034(2) Mn2 0.0148(3) 0.0173(3) 0.0123(3) -0.0086(2) 0.0009(2) -0.0042(2) Mn3 0.0186(3) 0.0179(3) 0.0141(3) -0.0092(2) -0.0007(2) -0.0045(2) Mn4 0.0184(3) 0.0180(3) 0.0152(3) -0.0104(2) -0.0007(2) -0.0037(2) Mn5 0.0132(3) 0.0173(3) 0.0133(3) -0.0087(2) 0.0026(2) -0.0059(2) Mn6 0.0200(3) 0.0189(3) 0.0139(3) -0.0096(2) 0.0035(2) -0.0060(2) Mn7 0.0172(3) 0.0172(3) 0.0136(3) -0.0082(2) 0.0033(2) -0.0047(2) Mn8 0.0178(3) 0.0175(3) 0.0110(3) -0.0071(2) 0.0000(2) -0.0036(2) Mn9 0.0194(3) 0.0184(3) 0.0114(3) -0.0088(2) -0.0001(2) -0.0042(2) Mn10 0.0138(3) 0.0167(3) 0.0123(3) -0.0085(2) -0.0003(2) -0.0045(2) F1 0.0179(11) 0.0204(11) 0.0166(11) -0.0119(9) 0.0005(9) -0.0033(9) F2 0.0166(11) 0.0191(10) 0.0120(10) -0.0089(9) 0.0016(8) -0.0062(8) F3 0.0170(11) 0.0211(11) 0.0192(11) -0.0118(9) -0.0004(9) -0.0042(9) F4 0.0205(12) 0.0205(11) 0.0162(11) -0.0100(9) 0.0005(9) -0.0055(9) F5 0.0207(12) 0.0205(11) 0.0170(11) -0.0097(9) 0.0035(9) -0.0056(9) F6 0.0172(11) 0.0212(11) 0.0125(11) -0.0078(9) -0.0006(8) -0.0023(9) F7 0.0213(12) 0.0185(10) 0.0183(11) -0.0107(9) 0.0018(9) -0.0056(9) F8 0.0206(11) 0.0213(11) 0.0128(10) -0.0105(9) 0.0023(8) -0.0089(9) O1 0.0148(13) 0.0241(14) 0.0173(14) -0.0111(12) 0.0057(10) -0.0064(11) O2 0.0293(16) 0.0257(15) 0.0264(16) -0.0184(13) -0.0019(12) -0.0005(12) O3 0.0341(17) 0.0208(14) 0.0190(15) -0.0087(12) -0.0030(12) -0.0076(12) O4 0.0153(14) 0.0338(15) 0.0246(15) -0.0200(13) -0.0016(11) -0.0020(12) O5 0.0150(13) 0.0190(13) 0.0169(13) -0.0090(11) 0.0027(10) -0.0078(10) O6 0.0310(16) 0.0264(15) 0.0224(15) -0.0168(13) -0.0028(12) -0.0044(12) O7 0.053(2) 0.0256(16) 0.0324(18) -0.0188(14) -0.0190(15) 0.0078(14) O8 0.0231(14) 0.0220(13) 0.0119(13) -0.0095(11) 0.0030(11) -0.0061(11) O9 0.0347(17) 0.0235(14) 0.0178(14) -0.0100(12) -0.0074(12) -0.0062(12) O10 0.0237(15) 0.0203(14) 0.0219(15) -0.0123(12) -0.0050(12) -0.0012(11) O11 0.0238(15) 0.0188(13) 0.0143(13) -0.0084(11) 0.0012(11) -0.0060(11) O12 0.0243(15) 0.0204(13) 0.0215(15) -0.0110(12) -0.0068(12) -0.0015(11) O13 0.0375(17) 0.0192(13) 0.0143(14) -0.0067(12) -0.0023(12) -0.0103(12) O14 0.0119(13) 0.0226(13) 0.0234(15) -0.0120(12) 0.0013(11) -0.0035(11) O15 0.0229(15) 0.0231(14) 0.0157(14) -0.0100(12) 0.0042(11) -0.0089(11) O16 0.0381(18) 0.0360(16) 0.0294(17) -0.0256(14) 0.0184(14) -0.0192(14) O17 0.0253(15) 0.0228(13) 0.0148(13) -0.0126(11) 0.0051(11) -0.0109(11) O18 0.0242(15) 0.0213(14) 0.0227(15) -0.0074(12) 0.0080(12) -0.0035(12) O19 0.0267(16) 0.0219(14) 0.0225(15) -0.0099(12) 0.0077(12) -0.0025(12) O20 0.0161(14) 0.0292(15) 0.0175(14) -0.0099(12) -0.0011(11) -0.0007(11) O21 0.052(2) 0.0202(14) 0.0219(16) -0.0120(13) 0.0170(14) -0.0142(13) O22 0.0272(16) 0.0210(14) 0.0242(15) -0.0115(12) 0.0102(12) -0.0083(12) O23 0.0289(16) 0.0246(14) 0.0129(14) -0.0034(12) 0.0003(11) -0.0013(12) O24 0.0180(14) 0.0237(14) 0.0195(14) -0.0129(12) -0.0037(11) -0.0038(11) O25 0.0193(14) 0.0179(13) 0.0155(13) -0.0091(11) 0.0030(10) -0.0077(10) O26 0.0135(13) 0.0216(13) 0.0234(15) -0.0107(12) -0.0016(11) -0.0033(11) O27 0.0230(15) 0.0266(14) 0.0152(14) -0.0101(12) 0.0010(11) -0.0128(12) O28 0.0346(17) 0.0360(16) 0.0121(14) -0.0096(13) 0.0046(12) -0.0022(13) O29 0.110(4) 0.059(3) 0.036(2) 0.020(2) 0.044(2) 0.049(2) O30 0.0260(15) 0.0255(14) 0.0139(13) -0.0128(12) -0.0017(11) -0.0068(12) N1 0.0215(18) 0.0313(19) 0.0207(18) -0.0137(16) 0.0005(14) 0.0042(15) N2 0.0295(19) 0.0228(17) 0.0142(16) -0.0104(14) -0.0010(14) -0.0062(14) N3 0.0180(17) 0.0240(17) 0.0190(17) -0.0113(14) 0.0011(13) -0.0079(13) N4 0.039(2) 0.0278(18) 0.0147(17) -0.0136(15) 0.0095(15) -0.0143(16) N5 0.0253(19) 0.0255(17) 0.0182(17) -0.0122(15) -0.0073(14) -0.0002(14) N6 0.0168(16) 0.0217(16) 0.0145(16) -0.0102(14) 0.0002(13) -0.0028(13) C1 0.020(2) 0.033(2) 0.019(2) -0.0105(18) 0.0046(16) -0.0041(17) C2 0.018(2) 0.040(2) 0.027(2) -0.013(2) 0.0060(17) -0.0005(18) C3 0.051(3) 0.029(2) 0.035(3) -0.025(2) -0.006(2) 0.005(2) C4 0.033(3) 0.045(3) 0.030(3) -0.027(2) -0.001(2) 0.010(2) C5 0.026(2) 0.041(3) 0.026(2) -0.019(2) 0.0005(18) 0.0129(19) C6 0.017(2) 0.037(2) 0.026(2) -0.014(2) -0.0022(17) 0.0008(18) C7 0.022(2) 0.0225(19) 0.025(2) -0.0159(17) 0.0035(16) -0.0123(16) C8 0.023(2) 0.0201(19) 0.024(2) -0.0123(17) 0.0054(16) -0.0108(16) C9 0.015(2) 0.028(2) 0.036(2) -0.016(2) 0.0003(17) -0.0067(16) C10 0.017(2) 0.028(2) 0.029(2) -0.0134(19) 0.0062(17) -0.0084(17) C11 0.024(2) 0.030(2) 0.024(2) -0.0143(18) 0.0129(17) -0.0143(17) C12 0.024(2) 0.024(2) 0.016(2) -0.0082(17) 0.0104(16) -0.0077(16) C13 0.039(3) 0.025(2) 0.024(2) -0.0180(19) -0.0016(19) -0.0071(19) C14 0.048(3) 0.025(2) 0.031(2) -0.018(2) -0.021(2) 0.001(2) C15 0.102(5) 0.025(2) 0.025(3) -0.012(2) -0.016(3) -0.008(3) C16 0.115(6) 0.025(3) 0.045(3) -0.015(3) -0.040(4) 0.000(3) C17 0.070(4) 0.035(3) 0.081(5) -0.042(3) -0.040(3) 0.014(3) C18 0.043(3) 0.051(3) 0.085(4) -0.057(3) -0.016(3) 0.013(2) C19 0.026(2) 0.041(3) 0.052(3) -0.035(2) -0.015(2) 0.004(2) C20 0.027(3) 0.049(3) 0.074(4) -0.050(3) 0.018(2) -0.015(2) C21 0.074(4) 0.196(8) 0.072(4) -0.109(5) 0.050(4) -0.095(5) C22 0.141(7) 0.228(10) 0.116(6) -0.150(7) 0.107(5) -0.159(7) C23 0.105(5) 0.085(5) 0.178(8) -0.111(6) 0.121(5) -0.073(4) C24 0.043(4) 0.038(3) 0.183(8) -0.009(4) 0.050(4) -0.010(3) C25 0.030(3) 0.035(3) 0.136(7) 0.006(4) -0.012(4) -0.011(2) C26 0.022(2) 0.029(2) 0.0153(19) -0.0122(17) 0.0069(16) -0.0074(17) C27 0.028(2) 0.024(2) 0.016(2) -0.0107(17) 0.0060(16) -0.0048(17) C28 0.039(3) 0.029(2) 0.020(2) -0.0141(19) -0.0070(18) -0.0077(19) C29 0.042(3) 0.032(2) 0.016(2) -0.0143(19) -0.0052(18) -0.004(2) C30 0.034(2) 0.021(2) 0.014(2) -0.0040(17) -0.0004(17) -0.0012(17) C31 0.034(2) 0.021(2) 0.0145(19) -0.0063(17) 0.0015(17) -0.0083(17) C32 0.033(2) 0.0189(19) 0.018(2) -0.0093(17) -0.0023(17) -0.0053(17) C33 0.050(3) 0.026(2) 0.023(2) -0.0076(19) -0.005(2) -0.017(2) C34 0.072(4) 0.037(3) 0.030(3) -0.013(2) 0.011(3) -0.030(3) C35 0.101(5) 0.061(4) 0.044(3) -0.020(3) 0.026(3) -0.056(4) C36 0.117(6) 0.045(3) 0.037(3) -0.006(3) 0.011(3) -0.051(4) C37 0.091(5) 0.023(2) 0.037(3) -0.005(2) -0.012(3) -0.024(3) C38 0.062(3) 0.026(2) 0.027(2) -0.011(2) -0.009(2) -0.012(2) C39 0.073(4) 0.016(2) 0.036(3) -0.007(2) -0.010(3) 0.000(2) C40 0.064(4) 0.032(3) 0.040(3) -0.009(2) -0.002(3) 0.005(3) C41 0.080(5) 0.036(3) 0.064(4) -0.015(3) -0.002(4) 0.010(3) C42 0.081(5) 0.046(4) 0.077(5) -0.017(4) 0.014(4) 0.012(3) C43 0.146(8) 0.048(4) 0.077(5) -0.043(4) 0.010(5) 0.015(4) C44 0.101(5) 0.034(3) 0.058(4) -0.026(3) -0.003(4) 0.003(3) C45 0.025(2) 0.0184(19) 0.019(2) -0.0088(17) -0.0043(16) -0.0026(16) C46 0.042(3) 0.018(2) 0.035(3) -0.0165(19) -0.019(2) 0.0036(18) C47 0.058(3) 0.031(2) 0.038(3) -0.017(2) -0.024(2) -0.002(2) C48 0.086(5) 0.043(3) 0.051(4) -0.019(3) -0.041(3) 0.005(3) C49 0.083(5) 0.041(3) 0.085(5) -0.035(3) -0.059(4) 0.013(3) C50 0.046(3) 0.061(4) 0.100(5) -0.063(4) -0.035(3) 0.020(3) C51 0.034(3) 0.054(3) 0.062(4) -0.046(3) -0.020(2) 0.010(2) C52 0.027(3) 0.091(4) 0.070(4) -0.055(3) -0.005(3) -0.004(3) C53 0.061(4) 0.163(7) 0.097(5) -0.101(5) -0.008(4) 0.022(5) C54 0.073(6) 0.272(10) 0.113(7) -0.129(8) 0.020(6) -0.012(7) C55 0.054(5) 0.307(11) 0.070(5) -0.108(6) 0.035(4) -0.088(6) C56 0.071(5) 0.209(8) 0.063(4) -0.057(5) 0.023(4) -0.100(5) C57 0.034(3) 0.126(5) 0.053(3) -0.049(4) 0.012(3) -0.045(3) C58 0.026(2) 0.024(2) 0.024(2) -0.0127(18) 0.0075(17) -0.0057(17) C59 0.036(3) 0.017(2) 0.030(2) -0.0030(19) 0.016(2) -0.0022(18) C60 0.055(3) 0.025(2) 0.033(3) -0.009(2) 0.022(2) -0.003(2) C61 0.087(4) 0.027(3) 0.043(3) -0.013(2) 0.040(3) -0.009(3) C62 0.080(4) 0.027(3) 0.051(4) -0.002(3) 0.035(3) 0.017(3) C63 0.045(3) 0.037(3) 0.052(4) 0.002(3) 0.022(3) 0.014(2) C64 0.027(3) 0.028(2) 0.035(3) 0.002(2) 0.016(2) 0.0043(19) C65 0.016(2) 0.038(3) 0.040(3) 0.000(2) 0.008(2) -0.0008(19) C66 0.033(3) 0.036(3) 0.041(3) -0.001(2) 0.003(2) 0.003(2) C67 0.032(3) 0.059(4) 0.047(3) 0.000(3) -0.009(3) -0.005(3) C68 0.036(3) 0.070(4) 0.055(4) -0.012(3) -0.006(3) -0.022(3) C69 0.033(3) 0.045(3) 0.062(4) -0.009(3) -0.001(3) -0.020(2) C70 0.022(2) 0.034(3) 0.044(3) 0.001(2) -0.001(2) -0.0017(19) C71 0.037(2) 0.026(2) 0.022(2) -0.0148(18) 0.0055(18) -0.0177(18) C72 0.027(2) 0.026(2) 0.025(2) -0.0189(18) 0.0054(17) -0.0097(17) C73 0.046(3) 0.031(2) 0.027(2) -0.018(2) -0.014(2) -0.006(2) C74 0.115(5) 0.084(4) 0.033(3) -0.046(3) 0.049(3) -0.074(4) C75 0.022(4) 0.022(4) 0.006(4) -0.004(3) -0.002(3) 0.005(3) C76 0.029(2) 0.0200(19) 0.022(2) -0.0117(17) 0.0070(17) -0.0099(17) C77 0.036(2) 0.0184(19) 0.018(2) -0.0082(17) 0.0060(17) -0.0060(17) C78 0.047(3) 0.034(2) 0.035(3) -0.015(2) -0.012(2) -0.009(2) C79 0.057(3) 0.035(3) 0.031(3) -0.010(2) -0.015(2) 0.003(2) C80 0.069(4) 0.025(2) 0.040(3) -0.008(2) -0.012(3) 0.002(2) C81 0.072(4) 0.023(3) 0.083(5) -0.007(3) -0.011(4) -0.019(3) C82 0.039(3) 0.023(2) 0.078(4) -0.014(3) -0.005(3) -0.009(2) C89 0.019(2) 0.038(2) 0.027(2) -0.019(2) -0.0017(17) -0.0026(18) C90 0.023(2) 0.035(2) 0.027(2) -0.017(2) -0.0093(18) 0.0036(18) C91 0.022(2) 0.029(2) 0.029(2) -0.0156(19) -0.0087(17) -0.0050(17) C92 0.029(2) 0.029(2) 0.025(2) -0.0166(19) -0.0106(18) -0.0018(18) C93 0.038(3) 0.030(2) 0.019(2) -0.0029(19) -0.0031(19) -0.001(2) C94 0.025(3) 0.027(3) 0.014(3) -0.006(2) -0.001(2) -0.004(2) C95 0.0210(19) 0.0219(18) 0.0168(18) -0.0092(16) 0.0022(15) -0.0099(15) C96 0.020(2) 0.0223(19) 0.0131(18) -0.0066(16) 0.0044(15) -0.0094(16) C97 0.018(2) 0.030(2) 0.023(2) -0.0148(18) 0.0054(16) -0.0067(17) C98 0.016(2) 0.024(2) 0.027(2) -0.0132(18) -0.0002(16) -0.0030(16) C99 0.018(2) 0.025(2) 0.020(2) -0.0111(17) 0.0011(15) -0.0116(16) C100 0.024(2) 0.024(2) 0.0165(19) -0.0131(17) -0.0013(16) -0.0043(16) C101 0.085(5) 0.052(3) 0.027(3) 0.008(3) 0.028(3) 0.033(3) C115 0.046(3) 0.033(2) 0.019(2) -0.0162(19) -0.0092(19) -0.004(2) C1' 0.046(8) 0.037(8) 0.014(7) -0.011(6) 0.013(5) -0.006(6) C2' 0.055(8) 0.034(6) 0.027(7) -0.019(5) 0.021(6) -0.012(6) C3' 0.088(12) 0.049(8) 0.041(9) -0.028(7) 0.029(8) -0.027(8) C4' 0.082(12) 0.032(8) 0.047(9) -0.009(7) 0.040(8) 0.002(7) C6' 0.033(7) 0.032(7) 0.027(8) -0.011(6) 0.012(5) 0.013(5) C7' 0.034(6) 0.048(8) 0.018(7) -0.013(7) 0.011(5) 0.014(6) C8' 0.039(7) 0.084(10) 0.030(8) -0.028(9) -0.009(7) 0.014(6) C9' 0.052(8) 0.105(11) 0.064(12) -0.060(11) -0.015(9) 0.008(9) C10' 0.056(9) 0.109(12) 0.078(13) -0.062(12) -0.032(10) 0.012(9) C11' 0.050(11) 0.104(11) 0.046(11) -0.064(10) -0.015(10) 0.002(8) C12' 0.041(8) 0.073(9) 0.020(8) -0.028(9) -0.004(7) -0.005(7) C13' 0.040(13) 0.043(12) 0.059(15) -0.029(12) 0.021(11) -0.025(10) C14' 0.046(14) 0.029(12) 0.11(2) -0.023(13) -0.036(15) -0.005(10) C15' 0.031(13) 0.041(13) 0.13(2) -0.020(14) -0.044(14) 0.003(12) C16' 0.033(13) 0.103(19) 0.12(2) -0.044(16) -0.024(14) -0.028(13) C17' 0.076(19) 0.09(2) 0.068(19) -0.034(16) 0.006(15) -0.042(16) C18' 0.065(16) 0.052(14) 0.066(17) -0.024(13) 0.001(13) -0.028(12) C75' 0.072(8) 0.065(7) 0.028(6) -0.038(6) 0.029(5) -0.047(6) C94' 0.025(2) 0.027(2) 0.014(2) -0.0059(19) -0.0010(18) -0.0040(18) C1D 0.031(3) 0.026(3) 0.017(3) -0.009(3) 0.008(2) -0.003(3) C2D 0.046(5) 0.031(4) 0.029(4) -0.014(3) 0.015(3) -0.016(3) C3D 0.070(6) 0.039(4) 0.038(4) -0.020(3) 0.019(4) 0.002(4) C4D 0.047(4) 0.031(3) 0.035(4) -0.010(3) 0.014(3) 0.003(3) C5D 0.045(4) 0.041(4) 0.025(4) 0.000(3) -0.003(3) 0.004(3) C6D 0.030(4) 0.031(4) 0.025(4) -0.011(3) 0.004(3) 0.005(3) C7D 0.035(4) 0.042(4) 0.020(4) -0.004(3) -0.007(3) -0.014(3) C8D 0.039(4) 0.045(4) 0.047(5) -0.016(4) 0.000(3) -0.016(3) C9D 0.053(4) 0.041(4) 0.054(5) -0.022(4) -0.009(4) -0.015(3) C10D 0.058(5) 0.049(4) 0.041(4) -0.007(4) -0.017(4) -0.033(4) C11D 0.047(4) 0.070(5) 0.019(3) -0.012(3) 0.000(3) -0.032(4) C12D 0.046(4) 0.071(5) 0.017(4) -0.016(4) 0.008(3) -0.025(4) C13D 0.027(3) 0.016(3) 0.072(5) -0.019(3) 0.010(3) -0.012(3) C14D 0.032(4) 0.031(4) 0.055(5) -0.019(3) 0.001(3) -0.012(3) C15D 0.041(5) 0.029(4) 0.091(7) -0.023(4) -0.003(4) -0.008(3) C16D 0.017(4) 0.050(5) 0.135(9) -0.033(5) -0.009(5) -0.003(4) C17D 0.038(5) 0.040(4) 0.143(10) -0.033(5) 0.023(5) -0.012(4) C18D 0.041(4) 0.031(4) 0.097(7) -0.018(4) 0.018(4) -0.011(3) N1S 0.087(5) 0.094(5) 0.128(7) -0.046(5) -0.006(4) -0.027(4) N2S 0.082(8) 0.154(11) 0.069(8) 0.031(7) 0.048(6) 0.045(8) N3S 0.068(11) 0.087(12) 0.20(2) -0.040(14) 0.045(13) -0.015(9) C1S 0.069(5) 0.044(4) 0.101(6) -0.015(4) 0.005(4) -0.016(3) C2S 0.181(9) 0.041(4) 0.095(6) -0.028(4) 0.059(6) -0.026(5) C3S 0.068(7) 0.051(6) 0.030(5) 0.016(4) 0.026(5) 0.003(5) C4S 0.051(5) 0.022(3) 0.021(4) -0.009(3) 0.025(3) -0.024(3) C5S 0.048(9) 0.049(8) 0.047(9) 0.008(7) 0.002(7) -0.006(7) C6S 0.065(12) 0.094(14) 0.085(14) -0.007(11) 0.016(10) -0.008(10) N1V 0.126(14) 0.37(3) 0.39(4) -0.20(3) -0.15(2) 0.049(19) N2V 0.24(3) 0.142(17) 0.116(16) -0.043(13) -0.022(16) -0.025(15) C2V 0.104(12) 0.114(14) 0.123(15) -0.051(12) -0.036(11) -0.017(11) C3V 0.163(14) 0.030(6) 0.127(13) -0.004(7) -0.110(12) -0.033(8) C4V 0.115(14) 0.090(12) 0.055(10) -0.018(9) -0.012(9) -0.016(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 2.164(3) . ? Mn1 O4 2.177(3) . ? Mn1 O3 2.197(3) . ? Mn1 F1 2.207(2) . ? Mn1 O2 2.301(3) . ? Mn1 O5 2.301(3) . ? Mn1 N1 2.363(3) . ? Mn2 O1 1.870(3) . ? Mn2 F3 1.888(2) . ? Mn2 O8 1.912(3) . ? Mn2 O5 1.936(2) . ? Mn2 F2 2.1346(19) . ? Mn2 O6 2.222(3) . ? Mn3 F3 2.160(2) . ? Mn3 F4 2.173(2) . ? Mn3 O11 2.178(2) . ? Mn3 O9 2.234(3) . ? Mn3 O10 2.259(3) . ? Mn3 O8 2.301(3) . ? Mn3 N2 2.387(3) . ? Mn4 O4 1.847(3) 2_575 ? Mn4 O11 1.882(3) . ? Mn4 F4 1.975(2) . ? Mn4 O13 2.018(3) . ? Mn4 O12 2.102(3) . ? Mn4 F1 2.114(2) 2_575 ? Mn5 F1 2.106(2) . ? Mn5 F2 2.1293(19) 2_575 ? Mn5 F2 2.132(2) . ? Mn5 O14 2.207(3) . ? Mn5 O15 2.273(3) . ? Mn5 O5 2.388(2) . ? Mn5 N3 2.394(3) . ? Mn6 F5 2.161(2) 2_656 ? Mn6 F7 2.168(2) . ? Mn6 O17 2.208(3) . ? Mn6 O16 2.232(3) . ? Mn6 O18 2.235(3) . ? Mn6 O30 2.307(3) 2_656 ? Mn6 N4 2.360(3) . ? Mn6 Mn9 3.1971(8) 2_656 ? Mn7 O20 1.861(3) . ? Mn7 O17 1.874(3) . ? Mn7 F7 1.955(2) . ? Mn7 O21 1.994(3) . ? Mn7 O19 2.109(3) . ? Mn7 F6 2.118(2) . ? Mn8 O24 2.158(2) . ? Mn8 O20 2.180(3) . ? Mn8 F6 2.196(2) . ? Mn8 O22 2.219(3) . ? Mn8 O25 2.274(3) . ? Mn8 O23 2.295(3) . ? Mn8 N5 2.393(3) . ? Mn9 O24 1.874(3) . ? Mn9 F5 1.885(2) . ? Mn9 O30 1.920(2) . ? Mn9 O25 1.937(2) . ? Mn9 F8 2.134(2) 2_656 ? Mn9 O28 2.218(3) . ? Mn9 Mn6 3.1971(8) 2_656 ? Mn10 F6 2.110(2) . ? Mn10 F8 2.1265(19) 2_656 ? Mn10 F8 2.136(2) . ? Mn10 O26 2.221(3) . ? Mn10 O27 2.276(3) . ? Mn10 N6 2.382(3) . ? Mn10 O25 2.403(3) . ? F1 Mn4 2.114(2) 2_575 ? F2 Mn5 2.1293(19) 2_575 ? F5 Mn6 2.161(2) 2_656 ? F8 Mn10 2.1265(19) 2_656 ? F8 Mn9 2.134(2) 2_656 ? O1 C1 1.415(5) . ? O2 C3 1.432(5) . ? O3 C32 1.252(5) 2_575 ? O4 C6 1.399(5) . ? O4 Mn4 1.847(3) 2_575 ? O5 C7 1.428(4) . ? O6 C13 1.267(4) . ? O7 C13 1.241(5) . ? O8 C26 1.434(4) . ? O9 C28 1.434(5) . ? O10 C45 1.251(4) . ? O11 C31 1.411(4) . ? O12 C45 1.256(4) . ? O13 C32 1.279(4) . ? O14 C10 1.427(4) . ? O15 C12 1.432(4) . ? O16 C75 1.440(8) . ? O16 C75' 1.468(9) . ? O17 C71 1.404(4) . ? O18 C58 1.244(5) . ? O19 C58 1.278(5) . ? O20 C89 1.402(5) . ? O21 C76 1.279(5) . ? O22 C76 1.242(5) . ? O23 C93 1.427(5) . ? O24 C92 1.414(4) . ? O25 C96 1.433(4) . ? O26 C98 1.431(4) . ? O27 C100 1.437(4) . ? O28 C101 1.254(6) . ? O29 C101 1.263(6) . ? O30 C115 1.431(4) . ? O30 Mn6 2.307(3) 2_656 ? N1 C2 1.471(5) . ? N1 C5 1.473(5) . ? N1 C4 1.475(5) . ? N2 C30 1.471(5) . ? N2 C27 1.479(5) . ? N2 C29 1.483(5) . ? N3 C9 1.470(5) . ? N3 C11 1.477(5) . ? N3 C8 1.481(5) . ? N4 C74 1.458(5) . ? N4 C72 1.467(5) . ? N4 C73 1.480(6) . ? N5 C94 1.424(7) . ? N5 C90 1.469(5) . ? N5 C91 1.478(5) . ? N5 C94' 1.626(14) . ? N6 C97 1.471(5) . ? N6 C95 1.479(5) . ? N6 C99 1.485(5) . ? C1 C2 1.522(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.522(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.510(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.518(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.522(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.498(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.517(6) . ? C14 C15 1.390(7) . ? C14 C19 1.397(7) . ? C15 C16 1.386(7) . ? C15 H15 0.9300 . ? C16 C17 1.344(9) . ? C16 H16 0.9300 . ? C17 C18 1.389(8) . ? C17 H17 0.9300 . ? C18 C19 1.393(6) . ? C18 H18 0.9300 . ? C19 C20 1.500(7) . ? C20 C25 1.349(8) . ? C20 C21 1.354(7) . ? C21 C22 1.380(11) . ? C21 H21 0.9300 . ? C22 C23 1.281(12) . ? C22 H22 0.9300 . ? C23 C24 1.379(10) . ? C23 H23 0.9300 . ? C24 C25 1.394(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.511(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.510(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.519(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O3 1.252(5) 2_575 ? C32 C33 1.502(6) . ? C33 C34 1.385(7) . ? C33 C38 1.405(6) . ? C34 C35 1.394(7) . ? C34 H34 0.9300 . ? C35 C36 1.399(8) . ? C35 H35 0.9300 . ? C36 C37 1.356(8) . ? C36 H36 0.9300 . ? C37 C38 1.395(7) . ? C37 H37 0.9300 . ? C38 C39 1.458(7) . ? C39 C40 1.371(8) . ? C39 C44 1.410(7) . ? C40 C41 1.373(8) . ? C40 H40 0.9300 . ? C41 C42 1.370(9) . ? C41 H41 0.9300 . ? C42 C43 1.348(10) . ? C42 H42 0.9300 . ? C43 C44 1.416(10) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.514(5) . ? C46 C51 1.373(7) . ? C46 C47 1.410(7) . ? C47 C48 1.383(7) . ? C47 H47 0.9300 . ? C48 C49 1.363(9) . ? C48 H48 0.9300 . ? C49 C50 1.367(9) . ? C49 H49 0.9300 . ? C50 C51 1.418(7) . ? C50 H50 0.9300 . ? C51 C52 1.458(8) . ? C52 C57 1.384(9) . ? C52 C53 1.399(8) . ? C53 C54 1.315(12) . ? C53 H53 0.9300 . ? C54 C55 1.347(14) . ? C54 H54 0.9300 . ? C55 C56 1.461(13) . ? C55 H55 0.9300 . ? C56 C57 1.410(9) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 C59 1.519(6) . ? C59 C60 1.376(7) . ? C59 C64 1.410(7) . ? C60 C61 1.389(6) . ? C60 H60 0.9300 . ? C61 C62 1.376(9) . ? C61 H61 0.9300 . ? C62 C63 1.347(9) . ? C62 H62 0.9300 . ? C63 C64 1.402(6) . ? C63 H63 0.9300 . ? C64 C65 1.473(7) . ? C65 C70 1.403(7) . ? C65 C66 1.404(7) . ? C66 C67 1.391(8) . ? C66 H66 0.9300 . ? C67 C68 1.361(8) . ? C67 H67 0.9300 . ? C68 C69 1.397(8) . ? C68 H68 0.9300 . ? C69 C70 1.366(8) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 C72 1.530(6) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C115 1.504(6) 2_656 ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75' 1.372(10) . ? C74 C75 1.396(9) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 C77 1.504(5) . ? C77 C82 1.389(6) . ? C77 C78 1.392(6) . ? C78 C79 1.380(6) . ? C78 H78 0.9300 . ? C79 C80 1.347(7) . ? C79 H79 0.9300 . ? C80 C81 1.353(8) . ? C80 H80 0.9300 . ? C81 C82 1.417(7) . ? C81 H81 0.9300 . ? C82 C13D 1.481(6) . ? C82 C13' 1.608(8) . ? C89 C90 1.517(6) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 C92 1.528(6) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 C94' 1.271(11) . ? C93 C94 1.592(7) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C95 C96 1.516(5) . ? C95 H95A 0.9700 . ? C95 H95B 0.9700 . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? C97 C98 1.509(5) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 H98A 0.9700 . ? C98 H98B 0.9700 . ? C99 C100 1.498(5) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 H10C 0.9700 . ? C100 H10D 0.9700 . ? C101 C1D 1.481(6) . ? C101 C1' 1.668(7) . ? C115 C73 1.504(6) 2_656 ? C115 H11C 0.9700 . ? C115 H11D 0.9700 . ? C1' C2' 1.3900 . ? C1' C6' 1.3900 . ? C2' C3' 1.3900 . ? C2' H2' 0.9300 . ? C3' C4' 1.3900 . ? C3' H3' 0.9300 . ? C4' C5' 1.3900 . ? C4' H4' 0.9300 . ? C5' C6' 1.3900 . ? C5' H5' 0.9300 . ? C6' C7' 1.431(11) . ? C7' C8' 1.3900 . ? C7' C12' 1.3900 . ? C8' C9' 1.3900 . ? C8' H8' 0.9300 . ? C9' C10' 1.3900 . ? C9' H9' 0.9300 . ? C10' C11' 1.3900 . ? C10' H10' 0.9300 . ? C11' C12' 1.3900 . ? C11' H11' 0.9300 . ? C12' H12' 0.9300 . ? C13' C14' 1.3900 . ? C13' C18' 1.3900 . ? C14' C15' 1.3900 . ? C14' H14' 0.9300 . ? C15' C16' 1.3900 . ? C15' H15' 0.9300 . ? C16' C17' 1.3900 . ? C16' H16' 0.9300 . ? C17' C18' 1.3900 . ? C17' H17' 0.9300 . ? C18' H18' 0.9300 . ? C75' H75C 0.9700 . ? C75' H75D 0.9700 . ? C94' H94C 0.9700 . ? C94' H94D 0.9700 . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C2D C3D 1.3900 . ? C2D H2D 0.9300 . ? C3D C4D 1.3900 . ? C3D H3D 0.9300 . ? C4D C5D 1.3900 . ? C4D H4D 0.9300 . ? C5D C6D 1.3900 . ? C5D H5D 0.9300 . ? C6D C7D 1.493(4) . ? C7D C8D 1.3900 . ? C7D C12D 1.3900 . ? C8D C9D 1.3900 . ? C8D H8D 0.9300 . ? C9D C10D 1.3900 . ? C9D H9D 0.9300 . ? C10D C11D 1.3900 . ? C10D H10E 0.9300 . ? C11D C12D 1.3900 . ? C11D H11E 0.9300 . ? C12D H12D 0.9300 . ? C13D C14D 1.3900 . ? C13D C18D 1.3900 . ? C14D C15D 1.3900 . ? C14D H14D 0.9300 . ? C15D C16D 1.3900 . ? C15D H15D 0.9300 . ? C16D C17D 1.3900 . ? C16D H16D 0.9300 . ? C17D C18D 1.3900 . ? C17D H17D 0.9300 . ? C18D H18D 0.9300 . ? N1S C1S 1.195(10) . ? N2S C3S 1.120(14) . ? N3S C5S 1.070(9) . ? C1S C2S 1.430(11) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3S C4S 1.415(12) . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? C5S C6S 1.426(9) . ? C6S H6S1 0.9547 . ? C6S H6S2 0.9474 . ? C6S H6S3 0.9722 . ? N1V C2V 1.100(9) . ? N2V C4V 1.116(9) . ? C2V C3V 1.426(9) . ? C2V H5V1 1.1775 . ? C3V H3V1 1.0247 . ? C3V H3V2 0.8715 . ? C3V H3V3 0.9814 . ? C3V H5V3 1.0075 . ? C4V C5V 1.444(10) . ? C4V H3V2 1.0606 . ? C5V H3V1 0.6594 . ? C5V H3V3 1.3390 . ? C5V H5V1 0.9732 . ? C5V H5V2 1.1180 . ? N1X C1X 1.194(7) . ? C1X C2X 1.467(8) . ? C2X H2X1 0.9600 . ? C2X H2X2 0.9600 . ? C2X H2X3 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 114.08(10) . . ? O1 Mn1 O3 162.91(10) . . ? O4 Mn1 O3 82.69(10) . . ? O1 Mn1 F1 105.01(9) . . ? O4 Mn1 F1 71.25(9) . . ? O3 Mn1 F1 82.85(9) . . ? O1 Mn1 O2 86.88(10) . . ? O4 Mn1 O2 132.93(10) . . ? O3 Mn1 O2 78.67(10) . . ? F1 Mn1 O2 146.18(9) . . ? O1 Mn1 O5 68.38(9) . . ? O4 Mn1 O5 144.48(9) . . ? O3 Mn1 O5 100.19(10) . . ? F1 Mn1 O5 74.00(8) . . ? O2 Mn1 O5 81.68(9) . . ? O1 Mn1 N1 73.41(11) . . ? O4 Mn1 N1 72.22(11) . . ? O3 Mn1 N1 110.89(11) . . ? F1 Mn1 N1 138.69(10) . . ? O2 Mn1 N1 74.85(11) . . ? O5 Mn1 N1 135.83(10) . . ? O1 Mn2 F3 173.62(11) . . ? O1 Mn2 O8 99.85(11) . . ? F3 Mn2 O8 85.69(10) . . ? O1 Mn2 O5 82.59(11) . . ? F3 Mn2 O5 91.38(10) . . ? O8 Mn2 O5 169.17(11) . . ? O1 Mn2 F2 87.34(9) . . ? F3 Mn2 F2 89.84(8) . . ? O8 Mn2 F2 86.75(9) . . ? O5 Mn2 F2 82.81(9) . . ? O1 Mn2 O6 89.00(11) . . ? F3 Mn2 O6 93.22(10) . . ? O8 Mn2 O6 99.50(10) . . ? O5 Mn2 O6 91.07(10) . . ? F2 Mn2 O6 173.23(9) . . ? F3 Mn3 F4 79.57(8) . . ? F3 Mn3 O11 136.70(9) . . ? F4 Mn3 O11 72.66(9) . . ? F3 Mn3 O9 78.96(9) . . ? F4 Mn3 O9 135.77(10) . . ? O11 Mn3 O9 143.03(10) . . ? F3 Mn3 O10 122.97(9) . . ? F4 Mn3 O10 79.87(9) . . ? O11 Mn3 O10 84.27(9) . . ? O9 Mn3 O10 80.20(10) . . ? F3 Mn3 O8 70.71(8) . . ? F4 Mn3 O8 109.45(8) . . ? O11 Mn3 O8 87.88(9) . . ? O9 Mn3 O8 99.13(10) . . ? O10 Mn3 O8 165.43(10) . . ? F3 Mn3 N2 130.87(10) . . ? F4 Mn3 N2 145.18(9) . . ? O11 Mn3 N2 72.83(10) . . ? O9 Mn3 N2 74.50(11) . . ? O10 Mn3 N2 92.28(11) . . ? O8 Mn3 N2 73.65(10) . . ? O4 Mn4 O11 173.32(12) 2_575 . ? O4 Mn4 F4 93.61(11) 2_575 . ? O11 Mn4 F4 83.82(10) . . ? O4 Mn4 O13 91.63(12) 2_575 . ? O11 Mn4 O13 90.42(11) . . ? F4 Mn4 O13 172.75(11) . . ? O4 Mn4 O12 94.86(11) 2_575 . ? O11 Mn4 O12 91.23(11) . . ? F4 Mn4 O12 88.09(9) . . ? O13 Mn4 O12 96.46(11) . . ? O4 Mn4 F1 79.96(10) 2_575 2_575 ? O11 Mn4 F1 93.76(10) . 2_575 ? F4 Mn4 F1 87.94(8) . 2_575 ? O13 Mn4 F1 88.05(9) . 2_575 ? O12 Mn4 F1 173.26(10) . 2_575 ? F1 Mn5 F2 85.99(8) . 2_575 ? F1 Mn5 F2 106.85(8) . . ? F2 Mn5 F2 75.48(8) 2_575 . ? F1 Mn5 O14 173.45(9) . . ? F2 Mn5 O14 95.77(8) 2_575 . ? F2 Mn5 O14 79.70(9) . . ? F1 Mn5 O15 86.16(9) . . ? F2 Mn5 O15 80.40(8) 2_575 . ? F2 Mn5 O15 151.48(8) . . ? O14 Mn5 O15 87.91(10) . . ? F1 Mn5 O5 74.00(8) . . ? F2 Mn5 O5 135.35(8) 2_575 . ? F2 Mn5 O5 73.00(8) . . ? O14 Mn5 O5 108.62(9) . . ? O15 Mn5 O5 135.52(9) . . ? F1 Mn5 N3 99.74(10) . . ? F2 Mn5 N3 151.06(10) 2_575 . ? F2 Mn5 N3 128.23(9) . . ? O14 Mn5 N3 75.71(10) . . ? O15 Mn5 N3 71.80(10) . . ? O5 Mn5 N3 72.92(10) . . ? F5 Mn6 F7 78.67(8) 2_656 . ? F5 Mn6 O17 134.53(9) 2_656 . ? F7 Mn6 O17 71.89(8) . . ? F5 Mn6 O16 79.10(9) 2_656 . ? F7 Mn6 O16 137.44(9) . . ? O17 Mn6 O16 144.40(9) . . ? F5 Mn6 O18 123.44(9) 2_656 . ? F7 Mn6 O18 81.20(9) . . ? O17 Mn6 O18 85.65(10) . . ? O16 Mn6 O18 81.50(10) . . ? F5 Mn6 O30 70.63(8) 2_656 2_656 ? F7 Mn6 O30 109.47(9) . 2_656 ? O17 Mn6 O30 87.30(10) . 2_656 ? O16 Mn6 O30 96.57(10) . 2_656 ? O18 Mn6 O30 164.64(10) . 2_656 ? F5 Mn6 N4 132.41(10) 2_656 . ? F7 Mn6 N4 144.54(10) . . ? O17 Mn6 N4 73.14(10) . . ? O16 Mn6 N4 73.94(11) . . ? O18 Mn6 N4 90.54(11) . . ? O30 Mn6 N4 74.35(11) 2_656 . ? F5 Mn6 Mn9 34.86(6) 2_656 2_656 ? F7 Mn6 Mn9 89.57(6) . 2_656 ? O17 Mn6 Mn9 110.29(7) . 2_656 ? O16 Mn6 Mn9 92.43(8) . 2_656 ? O18 Mn6 Mn9 158.21(7) . 2_656 ? O30 Mn6 Mn9 36.51(6) 2_656 2_656 ? N4 Mn6 Mn9 107.96(9) . 2_656 ? O20 Mn7 O17 171.64(12) . . ? O20 Mn7 F7 92.97(10) . . ? O17 Mn7 F7 84.24(10) . . ? O20 Mn7 O21 89.89(12) . . ? O17 Mn7 O21 93.25(11) . . ? F7 Mn7 O21 176.25(10) . . ? O20 Mn7 O19 95.87(11) . . ? O17 Mn7 O19 91.89(11) . . ? F7 Mn7 O19 87.41(10) . . ? O21 Mn7 O19 89.89(11) . . ? O20 Mn7 F6 79.47(10) . . ? O17 Mn7 F6 92.58(10) . . ? F7 Mn7 F6 89.14(8) . . ? O21 Mn7 F6 93.76(10) . . ? O19 Mn7 F6 174.06(10) . . ? O24 Mn8 O20 111.28(10) . . ? O24 Mn8 F6 105.76(9) . . ? O20 Mn8 F6 71.31(9) . . ? O24 Mn8 O22 165.66(10) . . ? O20 Mn8 O22 82.13(10) . . ? F6 Mn8 O22 82.91(9) . . ? O24 Mn8 O25 69.22(9) . . ? O20 Mn8 O25 144.34(10) . . ? F6 Mn8 O25 74.38(8) . . ? O22 Mn8 O25 103.14(9) . . ? O24 Mn8 O23 87.49(10) . . ? O20 Mn8 O23 132.93(10) . . ? F6 Mn8 O23 146.47(9) . . ? O22 Mn8 O23 79.30(10) . . ? O25 Mn8 O23 82.28(9) . . ? O24 Mn8 N5 73.62(10) . . ? O20 Mn8 N5 71.65(11) . . ? F6 Mn8 N5 139.57(10) . . ? O22 Mn8 N5 107.41(11) . . ? O25 Mn8 N5 136.07(10) . . ? O23 Mn8 N5 73.40(11) . . ? O24 Mn9 F5 173.69(10) . . ? O24 Mn9 O30 99.88(11) . . ? F5 Mn9 O30 85.62(10) . . ? O24 Mn9 O25 82.72(11) . . ? F5 Mn9 O25 91.34(10) . . ? O30 Mn9 O25 169.81(11) . . ? O24 Mn9 F8 87.47(10) . 2_656 ? F5 Mn9 F8 89.68(9) . 2_656 ? O30 Mn9 F8 87.52(9) . 2_656 ? O25 Mn9 F8 82.73(9) . 2_656 ? O24 Mn9 O28 88.61(11) . . ? F5 Mn9 O28 93.51(10) . . ? O30 Mn9 O28 100.11(11) . . ? O25 Mn9 O28 89.78(11) . . ? F8 Mn9 O28 171.93(9) 2_656 . ? O24 Mn9 Mn6 143.68(8) . 2_656 ? F5 Mn9 Mn6 40.95(6) . 2_656 ? O30 Mn9 Mn6 45.63(8) . 2_656 ? O25 Mn9 Mn6 129.10(8) . 2_656 ? F8 Mn9 Mn6 81.03(6) 2_656 2_656 ? O28 Mn9 Mn6 106.17(8) . 2_656 ? F6 Mn10 F8 105.49(8) . 2_656 ? F6 Mn10 F8 86.07(8) . . ? F8 Mn10 F8 75.38(9) 2_656 . ? F6 Mn10 O26 173.97(9) . . ? F8 Mn10 O26 80.52(9) 2_656 . ? F8 Mn10 O26 95.09(9) . . ? F6 Mn10 O27 86.35(9) . . ? F8 Mn10 O27 151.98(9) 2_656 . ? F8 Mn10 O27 80.34(8) . . ? O26 Mn10 O27 88.00(10) . . ? F6 Mn10 N6 100.67(9) . . ? F8 Mn10 N6 127.74(9) 2_656 . ? F8 Mn10 N6 151.48(9) . . ? O26 Mn10 N6 75.56(10) . . ? O27 Mn10 N6 72.57(10) . . ? F6 Mn10 O25 73.24(8) . . ? F8 Mn10 O25 72.71(8) 2_656 . ? F8 Mn10 O25 135.15(8) . . ? O26 Mn10 O25 109.61(9) . . ? O27 Mn10 O25 135.30(9) . . ? N6 Mn10 O25 72.82(9) . . ? Mn5 F1 Mn4 149.60(10) . 2_575 ? Mn5 F1 Mn1 109.16(9) . . ? Mn4 F1 Mn1 97.63(8) 2_575 . ? Mn5 F2 Mn5 104.52(8) 2_575 . ? Mn5 F2 Mn2 141.85(10) 2_575 . ? Mn5 F2 Mn2 103.01(8) . . ? Mn2 F3 Mn3 103.83(9) . . ? Mn4 F4 Mn3 99.30(9) . . ? Mn9 F5 Mn6 104.20(9) . 2_656 ? Mn10 F6 Mn7 148.99(11) . . ? Mn10 F6 Mn8 109.39(9) . . ? Mn7 F6 Mn8 97.78(8) . . ? Mn7 F7 Mn6 100.05(9) . . ? Mn10 F8 Mn9 103.50(8) 2_656 2_656 ? Mn10 F8 Mn10 104.62(9) 2_656 . ? Mn9 F8 Mn10 142.08(10) 2_656 . ? C1 O1 Mn2 126.7(2) . . ? C1 O1 Mn1 121.2(2) . . ? Mn2 O1 Mn1 107.97(11) . . ? C3 O2 Mn1 107.9(2) . . ? C32 O3 Mn1 131.1(2) 2_575 . ? C6 O4 Mn4 129.6(2) . 2_575 ? C6 O4 Mn1 122.8(2) . . ? Mn4 O4 Mn1 107.57(12) 2_575 . ? C7 O5 Mn2 120.7(2) . . ? C7 O5 Mn1 119.1(2) . . ? Mn2 O5 Mn1 100.55(10) . . ? C7 O5 Mn5 114.7(2) . . ? Mn2 O5 Mn5 100.61(10) . . ? Mn1 O5 Mn5 97.12(9) . . ? C13 O6 Mn2 139.7(3) . . ? C26 O8 Mn2 127.0(2) . . ? C26 O8 Mn3 112.7(2) . . ? Mn2 O8 Mn3 98.01(11) . . ? C28 O9 Mn3 109.4(2) . . ? C45 O10 Mn3 130.2(2) . . ? C31 O11 Mn4 125.5(2) . . ? C31 O11 Mn3 118.7(2) . . ? Mn4 O11 Mn3 102.13(11) . . ? C45 O12 Mn4 126.9(2) . . ? C32 O13 Mn4 128.9(2) . . ? C10 O14 Mn5 115.0(2) . . ? C12 O15 Mn5 106.5(2) . . ? C75 O16 Mn6 105.7(3) . . ? C75' O16 Mn6 118.7(4) . . ? C71 O17 Mn7 127.2(2) . . ? C71 O17 Mn6 118.8(2) . . ? Mn7 O17 Mn6 101.29(11) . . ? C58 O18 Mn6 129.5(3) . . ? C58 O19 Mn7 126.9(3) . . ? C89 O20 Mn7 128.9(2) . . ? C89 O20 Mn8 123.9(2) . . ? Mn7 O20 Mn8 106.85(12) . . ? C76 O21 Mn7 126.4(2) . . ? C76 O22 Mn8 129.1(2) . . ? C93 O23 Mn8 110.0(2) . . ? C92 O24 Mn9 126.8(2) . . ? C92 O24 Mn8 121.6(2) . . ? Mn9 O24 Mn8 107.09(11) . . ? C96 O25 Mn9 120.8(2) . . ? C96 O25 Mn8 119.5(2) . . ? Mn9 O25 Mn8 100.60(10) . . ? C96 O25 Mn10 114.2(2) . . ? Mn9 O25 Mn10 100.29(10) . . ? Mn8 O25 Mn10 97.40(9) . . ? C98 O26 Mn10 115.0(2) . . ? C100 O27 Mn10 105.7(2) . . ? C101 O28 Mn9 139.2(3) . . ? C115 O30 Mn9 126.6(2) . . ? C115 O30 Mn6 111.4(2) . 2_656 ? Mn9 O30 Mn6 97.86(10) . 2_656 ? C2 N1 C5 111.5(3) . . ? C2 N1 C4 112.0(3) . . ? C5 N1 C4 110.7(3) . . ? C2 N1 Mn1 104.4(2) . . ? C5 N1 Mn1 107.4(2) . . ? C4 N1 Mn1 110.5(3) . . ? C30 N2 C27 112.2(3) . . ? C30 N2 C29 113.4(3) . . ? C27 N2 C29 110.4(3) . . ? C30 N2 Mn3 102.1(2) . . ? C27 N2 Mn3 108.6(2) . . ? C29 N2 Mn3 109.7(2) . . ? C9 N3 C11 112.4(3) . . ? C9 N3 C8 112.6(3) . . ? C11 N3 C8 109.4(3) . . ? C9 N3 Mn5 105.3(2) . . ? C11 N3 Mn5 109.9(2) . . ? C8 N3 Mn5 107.0(2) . . ? C74 N4 C72 111.5(4) . . ? C74 N4 C73 112.8(4) . . ? C72 N4 C73 111.4(3) . . ? C74 N4 Mn6 107.9(3) . . ? C72 N4 Mn6 104.1(2) . . ? C73 N4 Mn6 108.7(2) . . ? C94 N5 C90 110.6(4) . . ? C94 N5 C91 110.6(4) . . ? C90 N5 C91 111.0(3) . . ? C90 N5 C94' 113.5(7) . . ? C91 N5 C94' 116.8(5) . . ? C94 N5 Mn8 114.4(3) . . ? C90 N5 Mn8 106.8(2) . . ? C91 N5 Mn8 103.3(2) . . ? C94' N5 Mn8 104.2(5) . . ? C97 N6 C95 112.7(3) . . ? C97 N6 C99 111.9(3) . . ? C95 N6 C99 109.5(3) . . ? C97 N6 Mn10 105.5(2) . . ? C95 N6 Mn10 107.5(2) . . ? C99 N6 Mn10 109.5(2) . . ? O1 C1 C2 108.1(3) . . ? O1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? O1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N1 C2 C1 111.0(3) . . ? N1 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? O2 C3 C4 110.5(3) . . ? O2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? O2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? N1 C4 C3 110.6(4) . . ? N1 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N1 C5 C6 111.2(3) . . ? N1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O4 C6 C5 108.6(3) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? O5 C7 C8 109.8(3) . . ? O5 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O5 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N3 C8 C7 112.2(3) . . ? N3 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N3 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N3 C9 C10 110.8(3) . . ? N3 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O14 C10 C9 110.0(3) . . ? O14 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? O14 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N3 C11 C12 110.8(3) . . ? N3 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? O15 C12 C11 105.9(3) . . ? O15 C12 H12A 110.6 . . ? C11 C12 H12A 110.6 . . ? O15 C12 H12B 110.6 . . ? C11 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? O7 C13 O6 126.7(4) . . ? O7 C13 C14 119.6(3) . . ? O6 C13 C14 113.6(4) . . ? C15 C14 C19 120.8(4) . . ? C15 C14 C13 119.0(5) . . ? C19 C14 C13 120.2(4) . . ? C16 C15 C14 119.0(6) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 121.3(6) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 120.2(5) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 120.8(6) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C14 118.0(5) . . ? C18 C19 C20 120.4(5) . . ? C14 C19 C20 121.6(4) . . ? C25 C20 C21 116.6(6) . . ? C25 C20 C19 122.6(4) . . ? C21 C20 C19 120.8(6) . . ? C20 C21 C22 121.5(8) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 121.3(6) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 120.8(7) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 117.3(8) . . ? C23 C24 H24 121.4 . . ? C25 C24 H24 121.4 . . ? C20 C25 C24 122.5(6) . . ? C20 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? O8 C26 C27 107.8(3) . . ? O8 C26 H26A 110.1 . . ? C27 C26 H26A 110.1 . . ? O8 C26 H26B 110.1 . . ? C27 C26 H26B 110.1 . . ? H26A C26 H26B 108.5 . . ? N2 C27 C26 110.5(3) . . ? N2 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? O9 C28 C29 110.3(3) . . ? O9 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? O9 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? N2 C29 C28 111.0(3) . . ? N2 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? N2 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? N2 C30 C31 111.6(3) . . ? N2 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? N2 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? O11 C31 C30 111.5(3) . . ? O11 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? O11 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? O3 C32 O13 126.9(4) 2_575 . ? O3 C32 C33 118.0(3) 2_575 . ? O13 C32 C33 115.0(3) . . ? C34 C33 C38 120.2(4) . . ? C34 C33 C32 117.9(4) . . ? C38 C33 C32 121.7(4) . . ? C33 C34 C35 121.1(5) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 118.1(6) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C37 C36 C35 120.8(5) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 122.0(5) . . ? C36 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C37 C38 C33 117.7(5) . . ? C37 C38 C39 120.1(4) . . ? C33 C38 C39 122.1(4) . . ? C40 C39 C44 118.0(6) . . ? C40 C39 C38 121.9(5) . . ? C44 C39 C38 120.1(5) . . ? C39 C40 C41 122.3(6) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C42 C41 C40 120.3(7) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 119.4(7) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 121.9(7) . . ? C42 C43 H43 119.1 . . ? C44 C43 H43 119.1 . . ? C39 C44 C43 118.2(7) . . ? C39 C44 H44 120.9 . . ? C43 C44 H44 120.9 . . ? O10 C45 O12 126.9(4) . . ? O10 C45 C46 117.2(3) . . ? O12 C45 C46 115.8(3) . . ? C51 C46 C47 119.7(4) . . ? C51 C46 C45 123.7(4) . . ? C47 C46 C45 116.4(4) . . ? C48 C47 C46 121.2(6) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C49 C48 C47 118.4(6) . . ? C49 C48 H48 120.8 . . ? C47 C48 H48 120.8 . . ? C48 C49 C50 121.8(5) . . ? C48 C49 H49 119.1 . . ? C50 C49 H49 119.1 . . ? C49 C50 C51 120.5(6) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C46 C51 C50 118.3(5) . . ? C46 C51 C52 122.8(4) . . ? C50 C51 C52 118.9(5) . . ? C57 C52 C53 116.5(7) . . ? C57 C52 C51 120.4(5) . . ? C53 C52 C51 123.1(7) . . ? C54 C53 C52 123.5(10) . . ? C54 C53 H53 118.3 . . ? C52 C53 H53 118.3 . . ? C53 C54 C55 121.9(10) . . ? C53 C54 H54 119.0 . . ? C55 C54 H54 119.0 . . ? C54 C55 C56 119.5(8) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C57 C56 C55 116.1(9) . . ? C57 C56 H56 122.0 . . ? C55 C56 H56 122.0 . . ? C52 C57 C56 122.5(7) . . ? C52 C57 H57 118.7 . . ? C56 C57 H57 118.7 . . ? O18 C58 O19 127.1(4) . . ? O18 C58 C59 118.3(4) . . ? O19 C58 C59 114.5(3) . . ? C60 C59 C64 119.8(4) . . ? C60 C59 C58 117.6(4) . . ? C64 C59 C58 122.3(4) . . ? C59 C60 C61 121.1(5) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.5 . . ? C62 C61 C60 119.4(5) . . ? C62 C61 H61 120.3 . . ? C60 C61 H61 120.3 . . ? C63 C62 C61 119.8(5) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 123.0(6) . . ? C62 C63 H63 118.5 . . ? C64 C63 H63 118.5 . . ? C63 C64 C59 116.8(5) . . ? C63 C64 C65 120.7(5) . . ? C59 C64 C65 122.5(4) . . ? C70 C65 C66 118.3(5) . . ? C70 C65 C64 120.3(4) . . ? C66 C65 C64 121.2(5) . . ? C67 C66 C65 119.5(5) . . ? C67 C66 H66 120.2 . . ? C65 C66 H66 120.2 . . ? C68 C67 C66 121.4(5) . . ? C68 C67 H67 119.3 . . ? C66 C67 H67 119.3 . . ? C67 C68 C69 119.5(6) . . ? C67 C68 H68 120.3 . . ? C69 C68 H68 120.3 . . ? C70 C69 C68 120.3(5) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C69 C70 C65 121.0(5) . . ? C69 C70 H70 119.5 . . ? C65 C70 H70 119.5 . . ? O17 C71 C72 111.3(3) . . ? O17 C71 H71A 109.4 . . ? C72 C71 H71A 109.4 . . ? O17 C71 H71B 109.4 . . ? C72 C71 H71B 109.4 . . ? H71A C71 H71B 108.0 . . ? N4 C72 C71 111.8(3) . . ? N4 C72 H72A 109.3 . . ? C71 C72 H72A 109.3 . . ? N4 C72 H72B 109.3 . . ? C71 C72 H72B 109.3 . . ? H72A C72 H72B 107.9 . . ? N4 C73 C115 112.1(3) . 2_656 ? N4 C73 H73A 109.2 . . ? C115 C73 H73A 109.2 2_656 . ? N4 C73 H73B 109.2 . . ? C115 C73 H73B 109.2 2_656 . ? H73A C73 H73B 107.9 . . ? C75' C74 N4 122.9(5) . . ? C75 C74 N4 114.9(5) . . ? C75' C74 H74A 74.6 . . ? C75 C74 H74A 108.5 . . ? N4 C74 H74A 108.5 . . ? C75' C74 H74B 125.2 . . ? C75 C74 H74B 108.5 . . ? N4 C74 H74B 108.5 . . ? H74A C74 H74B 107.5 . . ? C74 C75 O16 111.9(6) . . ? C74 C75 H75A 109.2 . . ? O16 C75 H75A 109.2 . . ? C74 C75 H75B 109.2 . . ? O16 C75 H75B 109.2 . . ? H75A C75 H75B 107.9 . . ? O22 C76 O21 126.9(3) . . ? O22 C76 C77 117.5(3) . . ? O21 C76 C77 115.5(3) . . ? C82 C77 C78 119.1(4) . . ? C82 C77 C76 122.9(4) . . ? C78 C77 C76 117.9(4) . . ? C79 C78 C77 121.6(5) . . ? C79 C78 H78 119.2 . . ? C77 C78 H78 119.2 . . ? C80 C79 C78 119.5(5) . . ? C80 C79 H79 120.2 . . ? C78 C79 H79 120.2 . . ? C79 C80 C81 120.2(5) . . ? C79 C80 H80 119.9 . . ? C81 C80 H80 119.9 . . ? C80 C81 C82 122.4(5) . . ? C80 C81 H81 118.8 . . ? C82 C81 H81 118.8 . . ? C77 C82 C81 116.9(5) . . ? C77 C82 C13D 121.3(4) . . ? C81 C82 C13D 121.4(4) . . ? C77 C82 C13' 120.0(5) . . ? C81 C82 C13' 113.7(5) . . ? O20 C89 C90 108.3(3) . . ? O20 C89 H89A 110.0 . . ? C90 C89 H89A 110.0 . . ? O20 C89 H89B 110.0 . . ? C90 C89 H89B 110.0 . . ? H89A C89 H89B 108.4 . . ? N5 C90 C89 112.1(3) . . ? N5 C90 H90A 109.2 . . ? C89 C90 H90A 109.2 . . ? N5 C90 H90B 109.2 . . ? C89 C90 H90B 109.2 . . ? H90A C90 H90B 107.9 . . ? N5 C91 C92 111.5(3) . . ? N5 C91 H91A 109.3 . . ? C92 C91 H91A 109.3 . . ? N5 C91 H91B 109.3 . . ? C92 C91 H91B 109.3 . . ? H91A C91 H91B 108.0 . . ? O24 C92 C91 108.1(3) . . ? O24 C92 H92A 110.1 . . ? C91 C92 H92A 110.1 . . ? O24 C92 H92B 110.1 . . ? C91 C92 H92B 110.1 . . ? H92A C92 H92B 108.4 . . ? C94' C93 O23 111.1(9) . . ? O23 C93 C94 111.3(4) . . ? C94' C93 H93A 109.4 . . ? O23 C93 H93A 109.4 . . ? C94 C93 H93A 105.2 . . ? C94' C93 H93B 109.4 . . ? O23 C93 H93B 109.4 . . ? C94 C93 H93B 113.2 . . ? H93A C93 H93B 108.0 . . ? N5 C94 C93 108.0(4) . . ? N5 C94 H94A 110.1 . . ? C93 C94 H94A 110.1 . . ? N5 C94 H94B 110.1 . . ? C93 C94 H94B 110.1 . . ? H94A C94 H94B 108.4 . . ? N6 C95 C96 112.1(3) . . ? N6 C95 H95A 109.2 . . ? C96 C95 H95A 109.2 . . ? N6 C95 H95B 109.2 . . ? C96 C95 H95B 109.2 . . ? H95A C95 H95B 107.9 . . ? O25 C96 C95 110.0(3) . . ? O25 C96 H96A 109.7 . . ? C95 C96 H96A 109.7 . . ? O25 C96 H96B 109.7 . . ? C95 C96 H96B 109.7 . . ? H96A C96 H96B 108.2 . . ? N6 C97 C98 111.2(3) . . ? N6 C97 H97A 109.4 . . ? C98 C97 H97A 109.4 . . ? N6 C97 H97B 109.4 . . ? C98 C97 H97B 109.4 . . ? H97A C97 H97B 108.0 . . ? O26 C98 C97 110.6(3) . . ? O26 C98 H98A 109.5 . . ? C97 C98 H98A 109.5 . . ? O26 C98 H98B 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 108.1 . . ? N6 C99 C100 110.1(3) . . ? N6 C99 H99A 109.6 . . ? C100 C99 H99A 109.6 . . ? N6 C99 H99B 109.6 . . ? C100 C99 H99B 109.6 . . ? H99A C99 H99B 108.1 . . ? O27 C100 C99 105.8(3) . . ? O27 C100 H10C 110.6 . . ? C99 C100 H10C 110.6 . . ? O27 C100 H10D 110.6 . . ? C99 C100 H10D 110.6 . . ? H10C C100 H10D 108.7 . . ? O28 C101 O29 123.7(4) . . ? O28 C101 C1D 114.0(5) . . ? O29 C101 C1D 118.6(4) . . ? O28 C101 C1' 115.4(5) . . ? O29 C101 C1' 114.0(6) . . ? C1D C101 C1' 47.5(4) . . ? O30 C115 C73 107.8(3) . 2_656 ? O30 C115 H11C 110.1 . . ? C73 C115 H11C 110.1 2_656 . ? O30 C115 H11D 110.1 . . ? C73 C115 H11D 110.1 2_656 . ? H11C C115 H11D 108.5 . . ? C2' C1' C6' 120.0 . . ? C2' C1' C101 130.0(6) . . ? C6' C1' C101 109.9(6) . . ? C1' C2' C3' 120.0 . . ? C1' C2' H2' 120.0 . . ? C3' C2' H2' 120.0 . . ? C4' C3' C2' 120.0 . . ? C4' C3' H3' 120.0 . . ? C2' C3' H3' 120.0 . . ? C3' C4' C5' 120.0 . . ? C3' C4' H4' 120.0 . . ? C5' C4' H4' 120.0 . . ? C4' C5' C6' 120.0 . . ? C4' C5' H5' 120.0 . . ? C6' C5' H5' 120.0 . . ? C5' C6' C1' 120.0 . . ? C5' C6' C7' 115.4(7) . . ? C1' C6' C7' 124.5(7) . . ? C8' C7' C12' 120.0 . . ? C8' C7' C6' 119.3(8) . . ? C12' C7' C6' 120.5(8) . . ? C7' C8' C9' 120.0 . . ? C7' C8' H8' 120.0 . . ? C9' C8' H8' 120.0 . . ? C10' C9' C8' 120.0 . . ? C10' C9' H9' 120.0 . . ? C8' C9' H9' 120.0 . . ? C11' C10' C9' 120.0 . . ? C11' C10' H10' 120.0 . . ? C9' C10' H10' 120.0 . . ? C12' C11' C10' 120.0 . . ? C12' C11' H11' 120.0 . . ? C10' C11' H11' 120.0 . . ? C11' C12' C7' 120.0 . . ? C11' C12' H12' 120.0 . . ? C7' C12' H12' 120.0 . . ? C14' C13' C18' 120.0 . . ? C14' C13' C82 107.4(4) . . ? C18' C13' C82 129.6(4) . . ? C13' C14' C15' 120.0 . . ? C13' C14' H14' 120.0 . . ? C15' C14' H14' 120.0 . . ? C16' C15' C14' 120.0 . . ? C16' C15' H15' 120.0 . . ? C14' C15' H15' 120.0 . . ? C15' C16' C17' 120.0 . . ? C15' C16' H16' 120.0 . . ? C17' C16' H16' 120.0 . . ? C18' C17' C16' 120.0 . . ? C18' C17' H17' 120.0 . . ? C16' C17' H17' 120.0 . . ? C17' C18' C13' 120.0 . . ? C17' C18' H18' 120.0 . . ? C13' C18' H18' 120.0 . . ? C74 C75' O16 111.7(7) . . ? C74 C75' H75C 109.3 . . ? O16 C75' H75C 109.3 . . ? C74 C75' H75D 109.3 . . ? O16 C75' H75D 109.3 . . ? H75C C75' H75D 107.9 . . ? C93 C94' N5 114.4(7) . . ? C93 C94' H94C 108.7 . . ? N5 C94' H94C 108.7 . . ? C93 C94' H94D 108.7 . . ? N5 C94' H94D 108.7 . . ? H94C C94' H94D 107.6 . . ? C2D C1D C6D 120.0 . . ? C2D C1D C101 109.6(4) . . ? C6D C1D C101 130.3(4) . . ? C1D C2D C3D 120.0 . . ? C1D C2D H2D 120.0 . . ? C3D C2D H2D 120.0 . . ? C4D C3D C2D 120.0 . . ? C4D C3D H3D 120.0 . . ? C2D C3D H3D 120.0 . . ? C5D C4D C3D 120.0 . . ? C5D C4D H4D 120.0 . . ? C3D C4D H4D 120.0 . . ? C4D C5D C6D 120.0 . . ? C4D C5D H5D 120.0 . . ? C6D C5D H5D 120.0 . . ? C5D C6D C1D 120.0 . . ? C5D C6D C7D 120.1(3) . . ? C1D C6D C7D 119.9(3) . . ? C8D C7D C12D 120.0 . . ? C8D C7D C6D 120.8(3) . . ? C12D C7D C6D 119.2(3) . . ? C7D C8D C9D 120.0 . . ? C7D C8D H8D 120.0 . . ? C9D C8D H8D 120.0 . . ? C10D C9D C8D 120.0 . . ? C10D C9D H9D 120.0 . . ? C8D C9D H9D 120.0 . . ? C9D C10D C11D 120.0 . . ? C9D C10D H10E 120.0 . . ? C11D C10D H10E 120.0 . . ? C10D C11D C12D 120.0 . . ? C10D C11D H11E 120.0 . . ? C12D C11D H11E 120.0 . . ? C11D C12D C7D 120.0 . . ? C11D C12D H12D 120.0 . . ? C7D C12D H12D 120.0 . . ? C14D C13D C18D 120.0 . . ? C14D C13D C82 117.2(3) . . ? C18D C13D C82 122.6(3) . . ? C13D C14D C15D 120.0 . . ? C13D C14D H14D 120.0 . . ? C15D C14D H14D 120.0 . . ? C14D C15D C16D 120.0 . . ? C14D C15D H15D 120.0 . . ? C16D C15D H15D 120.0 . . ? C17D C16D C15D 120.0 . . ? C17D C16D H16D 120.0 . . ? C15D C16D H16D 120.0 . . ? C16D C17D C18D 120.0 . . ? C16D C17D H17D 120.0 . . ? C18D C17D H17D 120.0 . . ? C17D C18D C13D 120.0 . . ? C17D C18D H18D 120.0 . . ? C13D C18D H18D 120.0 . . ? N1S C1S C2S 176.8(9) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 175.2(15) . . ? N3S C5S C6S 175(2) . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.8 . . ? H6S1 C6S H6S2 111.0 . . ? C5S C6S H6S3 108.1 . . ? H6S1 C6S H6S3 108.9 . . ? H6S2 C6S H6S3 109.5 . . ? C2V N1V H5V1 50.7 . . ? N1V C2V C3V 158(3) . . ? N1V C2V H5V1 83.1 . . ? C3V C2V H5V1 76.3 . . ? C2V C3V H3V1 101.1 . . ? C2V C3V H3V2 117.8 . . ? H3V1 C3V H3V2 111.3 . . ? C2V C3V H3V3 106.5 . . ? H3V1 C3V H3V3 102.8 . . ? H3V2 C3V H3V3 115.4 . . ? C2V C3V H5V3 113.7 . . ? H3V2 C3V H5V3 125.9 . . ? H3V3 C3V H5V3 61.7 . . ? N2V C4V C5V 165(3) . . ? N2V C4V H3V2 112.7 . . ? C5V C4V H3V2 77.7 . . ? C4V C5V H3V1 103.1 . . ? C4V C5V H3V3 88.2 . . ? H3V1 C5V H3V3 97.5 . . ? C4V C5V H5V1 109.3 . . ? H3V1 C5V H5V1 141.4 . . ? H3V3 C5V H5V1 103.8 . . ? C4V C5V H5V2 100.4 . . ? H3V1 C5V H5V2 56.4 . . ? H3V3 C5V H5V2 153.6 . . ? H5V1 C5V H5V2 96.9 . . ? C4V C5V H5V3 120.1 . . ? H3V1 C5V H5V3 55.4 . . ? H3V3 C5V H5V3 49.6 . . ? H5V1 C5V H5V3 119.7 . . ? H5V2 C5V H5V3 105.6 . . ? N1X C1X C2X 176.4(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F2 Mn5 F1 Mn4 -30.0(2) 2_575 . . 2_575 ? F2 Mn5 F1 Mn4 -103.5(2) . . . 2_575 ? O15 Mn5 F1 Mn4 50.6(2) . . . 2_575 ? O5 Mn5 F1 Mn4 -169.6(2) . . . 2_575 ? N3 Mn5 F1 Mn4 121.4(2) . . . 2_575 ? F2 Mn5 F1 Mn1 120.47(9) 2_575 . . . ? F2 Mn5 F1 Mn1 46.96(10) . . . . ? O15 Mn5 F1 Mn1 -158.91(10) . . . . ? O5 Mn5 F1 Mn1 -19.17(9) . . . . ? N3 Mn5 F1 Mn1 -88.12(11) . . . . ? O1 Mn1 F1 Mn5 -41.81(11) . . . . ? O4 Mn1 F1 Mn5 -152.61(12) . . . . ? O3 Mn1 F1 Mn5 122.72(11) . . . . ? O2 Mn1 F1 Mn5 65.60(19) . . . . ? O5 Mn1 F1 Mn5 19.92(9) . . . . ? N1 Mn1 F1 Mn5 -123.60(14) . . . . ? O1 Mn1 F1 Mn4 123.61(9) . . . 2_575 ? O4 Mn1 F1 Mn4 12.81(9) . . . 2_575 ? O3 Mn1 F1 Mn4 -71.87(10) . . . 2_575 ? O2 Mn1 F1 Mn4 -128.98(15) . . . 2_575 ? O5 Mn1 F1 Mn4 -174.66(10) . . . 2_575 ? N1 Mn1 F1 Mn4 41.82(17) . . . 2_575 ? F1 Mn5 F2 Mn5 81.15(9) . . . 2_575 ? F2 Mn5 F2 Mn5 0.000(1) 2_575 . . 2_575 ? O14 Mn5 F2 Mn5 -98.78(10) . . . 2_575 ? O15 Mn5 F2 Mn5 -33.1(2) . . . 2_575 ? O5 Mn5 F2 Mn5 147.96(11) . . . 2_575 ? N3 Mn5 F2 Mn5 -161.22(11) . . . 2_575 ? F1 Mn5 F2 Mn2 -72.18(9) . . . . ? F2 Mn5 F2 Mn2 -153.33(13) 2_575 . . . ? O14 Mn5 F2 Mn2 107.89(10) . . . . ? O15 Mn5 F2 Mn2 173.57(15) . . . . ? O5 Mn5 F2 Mn2 -5.36(8) . . . . ? N3 Mn5 F2 Mn2 45.45(14) . . . . ? O1 Mn2 F2 Mn5 -46.05(17) . . . 2_575 ? F3 Mn2 F2 Mn5 139.67(17) . . . 2_575 ? O8 Mn2 F2 Mn5 53.98(17) . . . 2_575 ? O5 Mn2 F2 Mn5 -128.91(18) . . . 2_575 ? O1 Mn2 F2 Mn5 89.24(10) . . . . ? F3 Mn2 F2 Mn5 -85.03(9) . . . . ? O8 Mn2 F2 Mn5 -170.72(11) . . . . ? O5 Mn2 F2 Mn5 6.38(10) . . . . ? O8 Mn2 F3 Mn3 11.10(10) . . . . ? O5 Mn2 F3 Mn3 -158.45(10) . . . . ? F2 Mn2 F3 Mn3 -75.65(9) . . . . ? O6 Mn2 F3 Mn3 110.40(10) . . . . ? F4 Mn3 F3 Mn2 105.30(10) . . . . ? O11 Mn3 F3 Mn2 54.89(16) . . . . ? O9 Mn3 F3 Mn2 -113.60(11) . . . . ? O10 Mn3 F3 Mn2 175.87(9) . . . . ? O8 Mn3 F3 Mn2 -9.73(9) . . . . ? N2 Mn3 F3 Mn2 -55.53(15) . . . . ? O4 Mn4 F4 Mn3 -174.77(10) 2_575 . . . ? O11 Mn4 F4 Mn3 11.43(10) . . . . ? O12 Mn4 F4 Mn3 -80.02(10) . . . . ? F1 Mn4 F4 Mn3 105.43(9) 2_575 . . . ? F3 Mn3 F4 Mn4 -156.65(10) . . . . ? O11 Mn3 F4 Mn4 -10.27(9) . . . . ? O9 Mn3 F4 Mn4 141.28(11) . . . . ? O10 Mn3 F4 Mn4 76.84(10) . . . . ? O8 Mn3 F4 Mn4 -91.56(10) . . . . ? N2 Mn3 F4 Mn4 -2.4(2) . . . . ? O30 Mn9 F5 Mn6 -10.92(10) . . . 2_656 ? O25 Mn9 F5 Mn6 159.34(10) . . . 2_656 ? F8 Mn9 F5 Mn6 76.62(9) 2_656 . . 2_656 ? O28 Mn9 F5 Mn6 -110.80(10) . . . 2_656 ? F8 Mn10 F6 Mn7 102.5(2) 2_656 . . . ? F8 Mn10 F6 Mn7 28.9(2) . . . . ? O27 Mn10 F6 Mn7 -51.6(2) . . . . ? N6 Mn10 F6 Mn7 -123.1(2) . . . . ? O25 Mn10 F6 Mn7 168.6(2) . . . . ? F8 Mn10 F6 Mn8 -47.24(11) 2_656 . . . ? F8 Mn10 F6 Mn8 -120.89(9) . . . . ? O27 Mn10 F6 Mn8 158.57(10) . . . . ? N6 Mn10 F6 Mn8 87.07(11) . . . . ? O25 Mn10 F6 Mn8 18.83(8) . . . . ? O20 Mn7 F6 Mn10 -134.9(2) . . . . ? O17 Mn7 F6 Mn10 42.5(2) . . . . ? F7 Mn7 F6 Mn10 -41.7(2) . . . . ? O21 Mn7 F6 Mn10 135.9(2) . . . . ? O20 Mn7 F6 Mn8 16.47(10) . . . . ? O17 Mn7 F6 Mn8 -166.16(9) . . . . ? F7 Mn7 F6 Mn8 109.65(9) . . . . ? O21 Mn7 F6 Mn8 -72.72(11) . . . . ? O24 Mn8 F6 Mn10 42.67(12) . . . . ? O20 Mn8 F6 Mn10 150.29(12) . . . . ? O22 Mn8 F6 Mn10 -125.66(11) . . . . ? O25 Mn8 F6 Mn10 -19.83(9) . . . . ? O23 Mn8 F6 Mn10 -67.43(18) . . . . ? N5 Mn8 F6 Mn10 125.74(14) . . . . ? O24 Mn8 F6 Mn7 -122.16(9) . . . . ? O20 Mn8 F6 Mn7 -14.54(9) . . . . ? O22 Mn8 F6 Mn7 69.51(9) . . . . ? O25 Mn8 F6 Mn7 175.34(10) . . . . ? O23 Mn8 F6 Mn7 127.74(15) . . . . ? N5 Mn8 F6 Mn7 -39.09(17) . . . . ? O20 Mn7 F7 Mn6 -175.15(10) . . . . ? O17 Mn7 F7 Mn6 12.76(10) . . . . ? O19 Mn7 F7 Mn6 -79.40(10) . . . . ? F6 Mn7 F7 Mn6 105.44(9) . . . . ? F5 Mn6 F7 Mn7 -156.20(10) 2_656 . . . ? O17 Mn6 F7 Mn7 -11.32(9) . . . . ? O16 Mn6 F7 Mn7 144.01(12) . . . . ? O18 Mn6 F7 Mn7 76.95(10) . . . . ? O30 Mn6 F7 Mn7 -91.64(10) 2_656 . . . ? N4 Mn6 F7 Mn7 -1.5(2) . . . . ? Mn9 Mn6 F7 Mn7 -122.86(7) 2_656 . . . ? F6 Mn10 F8 Mn10 107.13(9) . . . 2_656 ? F8 Mn10 F8 Mn10 0.0 2_656 . . 2_656 ? O26 Mn10 F8 Mn10 -78.81(10) . . . 2_656 ? O27 Mn10 F8 Mn10 -165.91(11) . . . 2_656 ? N6 Mn10 F8 Mn10 -147.66(17) . . . 2_656 ? O25 Mn10 F8 Mn10 45.75(14) . . . 2_656 ? F6 Mn10 F8 Mn9 -116.20(17) . . . 2_656 ? F8 Mn10 F8 Mn9 136.7(2) 2_656 . . 2_656 ? O26 Mn10 F8 Mn9 57.86(18) . . . 2_656 ? O27 Mn10 F8 Mn9 -29.24(17) . . . 2_656 ? N6 Mn10 F8 Mn9 -11.0(3) . . . 2_656 ? O25 Mn10 F8 Mn9 -177.58(13) . . . 2_656 ? O8 Mn2 O1 C1 27.6(3) . . . . ? O5 Mn2 O1 C1 -163.0(3) . . . . ? F2 Mn2 O1 C1 113.9(3) . . . . ? O6 Mn2 O1 C1 -71.8(3) . . . . ? O8 Mn2 O1 Mn1 -175.37(11) . . . . ? O5 Mn2 O1 Mn1 -6.05(11) . . . . ? F2 Mn2 O1 Mn1 -89.14(11) . . . . ? O6 Mn2 O1 Mn1 85.16(12) . . . . ? O4 Mn1 O1 C1 -54.6(3) . . . . ? O3 Mn1 O1 C1 113.8(4) . . . . ? F1 Mn1 O1 C1 -130.5(3) . . . . ? O2 Mn1 O1 C1 81.6(3) . . . . ? O5 Mn1 O1 C1 163.9(3) . . . . ? N1 Mn1 O1 C1 6.5(3) . . . . ? O4 Mn1 O1 Mn2 146.86(11) . . . . ? O3 Mn1 O1 Mn2 -44.7(4) . . . . ? F1 Mn1 O1 Mn2 71.02(12) . . . . ? O2 Mn1 O1 Mn2 -76.85(12) . . . . ? O5 Mn1 O1 Mn2 5.43(10) . . . . ? N1 Mn1 O1 Mn2 -151.97(15) . . . . ? O1 Mn1 O2 C3 -101.4(3) . . . . ? O4 Mn1 O2 C3 19.1(3) . . . . ? O3 Mn1 O2 C3 87.7(3) . . . . ? F1 Mn1 O2 C3 145.9(3) . . . . ? O5 Mn1 O2 C3 -170.0(3) . . . . ? N1 Mn1 O2 C3 -27.8(3) . . . . ? O1 Mn1 O3 C32 157.6(4) . . . 2_575 ? O4 Mn1 O3 C32 -33.1(4) . . . 2_575 ? F1 Mn1 O3 C32 38.9(4) . . . 2_575 ? O2 Mn1 O3 C32 -169.6(4) . . . 2_575 ? O5 Mn1 O3 C32 111.1(4) . . . 2_575 ? N1 Mn1 O3 C32 -100.8(4) . . . 2_575 ? O1 Mn1 O4 C6 64.6(3) . . . . ? O3 Mn1 O4 C6 -112.0(3) . . . . ? F1 Mn1 O4 C6 163.1(3) . . . . ? O2 Mn1 O4 C6 -44.9(3) . . . . ? O5 Mn1 O4 C6 150.7(3) . . . . ? N1 Mn1 O4 C6 2.8(3) . . . . ? O1 Mn1 O4 Mn4 -113.80(13) . . . 2_575 ? O3 Mn1 O4 Mn4 69.60(13) . . . 2_575 ? F1 Mn1 O4 Mn4 -15.29(11) . . . 2_575 ? O2 Mn1 O4 Mn4 136.66(13) . . . 2_575 ? O5 Mn1 O4 Mn4 -27.7(2) . . . 2_575 ? N1 Mn1 O4 Mn4 -175.65(16) . . . 2_575 ? O1 Mn2 O5 C7 138.8(3) . . . . ? F3 Mn2 O5 C7 -43.3(3) . . . . ? O8 Mn2 O5 C7 -117.4(6) . . . . ? F2 Mn2 O5 C7 -132.9(3) . . . . ? O6 Mn2 O5 C7 50.0(3) . . . . ? O1 Mn2 O5 Mn1 5.50(10) . . . . ? F3 Mn2 O5 Mn1 -176.60(9) . . . . ? O8 Mn2 O5 Mn1 109.3(6) . . . . ? F2 Mn2 O5 Mn1 93.74(9) . . . . ? O6 Mn2 O5 Mn1 -83.35(10) . . . . ? O1 Mn2 O5 Mn5 -93.89(11) . . . . ? F3 Mn2 O5 Mn5 84.01(10) . . . . ? O8 Mn2 O5 Mn5 9.9(6) . . . . ? F2 Mn2 O5 Mn5 -5.65(8) . . . . ? O6 Mn2 O5 Mn5 177.26(10) . . . . ? O1 Mn1 O5 C7 -139.4(3) . . . . ? O4 Mn1 O5 C7 119.1(3) . . . . ? O3 Mn1 O5 C7 27.4(2) . . . . ? F1 Mn1 O5 C7 106.8(2) . . . . ? O2 Mn1 O5 C7 -49.4(2) . . . . ? N1 Mn1 O5 C7 -107.4(3) . . . . ? O1 Mn1 O5 Mn2 -5.07(9) . . . . ? O4 Mn1 O5 Mn2 -106.63(17) . . . . ? O3 Mn1 O5 Mn2 161.69(10) . . . . ? F1 Mn1 O5 Mn2 -118.86(11) . . . . ? O2 Mn1 O5 Mn2 84.87(11) . . . . ? N1 Mn1 O5 Mn2 26.85(18) . . . . ? O1 Mn1 O5 Mn5 97.17(10) . . . . ? O4 Mn1 O5 Mn5 -4.4(2) . . . . ? O3 Mn1 O5 Mn5 -96.08(10) . . . . ? F1 Mn1 O5 Mn5 -16.63(8) . . . . ? O2 Mn1 O5 Mn5 -172.90(10) . . . . ? N1 Mn1 O5 Mn5 129.09(14) . . . . ? F1 Mn5 O5 C7 -109.2(2) . . . . ? F2 Mn5 O5 C7 -176.0(2) 2_575 . . . ? F2 Mn5 O5 C7 137.0(2) . . . . ? O14 Mn5 O5 C7 64.5(2) . . . . ? O15 Mn5 O5 C7 -42.2(3) . . . . ? N3 Mn5 O5 C7 -3.4(2) . . . . ? F1 Mn5 O5 Mn2 119.63(11) . . . . ? F2 Mn5 O5 Mn2 52.81(16) 2_575 . . . ? F2 Mn5 O5 Mn2 5.87(9) . . . . ? O14 Mn5 O5 Mn2 -66.66(12) . . . . ? O15 Mn5 O5 Mn2 -173.41(10) . . . . ? N3 Mn5 O5 Mn2 -134.57(13) . . . . ? F1 Mn5 O5 Mn1 17.44(8) . . . . ? F2 Mn5 O5 Mn1 -49.37(14) 2_575 . . . ? F2 Mn5 O5 Mn1 -96.32(9) . . . . ? O14 Mn5 O5 Mn1 -168.84(9) . . . . ? O15 Mn5 O5 Mn1 84.41(14) . . . . ? N3 Mn5 O5 Mn1 123.24(11) . . . . ? O1 Mn2 O6 C13 144.6(4) . . . . ? F3 Mn2 O6 C13 -41.4(4) . . . . ? O8 Mn2 O6 C13 44.8(4) . . . . ? O5 Mn2 O6 C13 -132.8(4) . . . . ? O1 Mn2 O8 C26 -66.9(3) . . . . ? F3 Mn2 O8 C26 116.3(3) . . . . ? O5 Mn2 O8 C26 -169.1(5) . . . . ? F2 Mn2 O8 C26 -153.7(3) . . . . ? O6 Mn2 O8 C26 23.7(3) . . . . ? O1 Mn2 O8 Mn3 166.61(10) . . . . ? F3 Mn2 O8 Mn3 -10.21(9) . . . . ? O5 Mn2 O8 Mn3 64.4(6) . . . . ? F2 Mn2 O8 Mn3 79.87(9) . . . . ? O6 Mn2 O8 Mn3 -102.76(10) . . . . ? F3 Mn3 O8 C26 -126.4(2) . . . . ? F4 Mn3 O8 C26 162.6(2) . . . . ? O11 Mn3 O8 C26 91.9(2) . . . . ? O9 Mn3 O8 C26 -51.6(2) . . . . ? O10 Mn3 O8 C26 34.6(5) . . . . ? N2 Mn3 O8 C26 19.2(2) . . . . ? F3 Mn3 O8 Mn2 9.42(8) . . . . ? F4 Mn3 O8 Mn2 -61.49(11) . . . . ? O11 Mn3 O8 Mn2 -132.25(11) . . . . ? O9 Mn3 O8 Mn2 84.25(11) . . . . ? O10 Mn3 O8 Mn2 170.4(3) . . . . ? N2 Mn3 O8 Mn2 155.02(12) . . . . ? F3 Mn3 O9 C28 169.4(3) . . . . ? F4 Mn3 O9 C28 -128.3(2) . . . . ? O11 Mn3 O9 C28 2.5(3) . . . . ? O10 Mn3 O9 C28 -64.0(3) . . . . ? O8 Mn3 O9 C28 101.2(3) . . . . ? N2 Mn3 O9 C28 31.1(3) . . . . ? F3 Mn3 O10 C45 -113.9(3) . . . . ? F4 Mn3 O10 C45 -43.5(3) . . . . ? O11 Mn3 O10 C45 29.9(3) . . . . ? O9 Mn3 O10 C45 176.2(4) . . . . ? O8 Mn3 O10 C45 87.6(5) . . . . ? N2 Mn3 O10 C45 102.4(3) . . . . ? F4 Mn4 O11 C31 -150.6(3) . . . . ? O13 Mn4 O11 C31 33.8(3) . . . . ? O12 Mn4 O11 C31 -62.7(3) . . . . ? F1 Mn4 O11 C31 121.9(3) 2_575 . . . ? F4 Mn4 O11 Mn3 -11.51(10) . . . . ? O13 Mn4 O11 Mn3 172.90(11) . . . . ? O12 Mn4 O11 Mn3 76.44(11) . . . . ? F1 Mn4 O11 Mn3 -99.03(10) 2_575 . . . ? F3 Mn3 O11 C31 -154.0(2) . . . . ? F4 Mn3 O11 C31 153.5(3) . . . . ? O9 Mn3 O11 C31 7.0(3) . . . . ? O10 Mn3 O11 C31 72.3(3) . . . . ? O8 Mn3 O11 C31 -95.4(3) . . . . ? N2 Mn3 O11 C31 -21.9(3) . . . . ? F3 Mn3 O11 Mn4 63.44(17) . . . . ? F4 Mn3 O11 Mn4 10.89(9) . . . . ? O9 Mn3 O11 Mn4 -135.57(15) . . . . ? O10 Mn3 O11 Mn4 -70.26(12) . . . . ? O8 Mn3 O11 Mn4 122.03(11) . . . . ? N2 Mn3 O11 Mn4 -164.44(14) . . . . ? O4 Mn4 O12 C45 135.1(3) 2_575 . . . ? O11 Mn4 O12 C45 -42.1(3) . . . . ? F4 Mn4 O12 C45 41.6(3) . . . . ? O13 Mn4 O12 C45 -132.7(3) . . . . ? O4 Mn4 O13 C32 -35.5(3) 2_575 . . . ? O11 Mn4 O13 C32 138.1(3) . . . . ? O12 Mn4 O13 C32 -130.6(3) . . . . ? F1 Mn4 O13 C32 44.4(3) 2_575 . . . ? F2 Mn5 O14 C10 142.0(2) 2_575 . . . ? F2 Mn5 O14 C10 -143.9(2) . . . . ? O15 Mn5 O14 C10 61.9(2) . . . . ? O5 Mn5 O14 C10 -76.0(3) . . . . ? N3 Mn5 O14 C10 -9.9(2) . . . . ? F1 Mn5 O15 C12 61.7(2) . . . . ? F2 Mn5 O15 C12 148.3(2) 2_575 . . . ? F2 Mn5 O15 C12 -179.3(2) . . . . ? O14 Mn5 O15 C12 -115.5(2) . . . . ? O5 Mn5 O15 C12 -0.7(3) . . . . ? N3 Mn5 O15 C12 -39.8(2) . . . . ? F5 Mn6 O16 C75 175.4(4) 2_656 . . . ? F7 Mn6 O16 C75 -125.0(4) . . . . ? O17 Mn6 O16 C75 12.1(4) . . . . ? O18 Mn6 O16 C75 -58.0(4) . . . . ? O30 Mn6 O16 C75 106.6(4) 2_656 . . . ? N4 Mn6 O16 C75 35.0(4) . . . . ? Mn9 Mn6 O16 C75 143.0(4) 2_656 . . . ? F5 Mn6 O16 C75' 142.9(6) 2_656 . . . ? F7 Mn6 O16 C75' -157.5(6) . . . . ? O17 Mn6 O16 C75' -20.5(7) . . . . ? O18 Mn6 O16 C75' -90.5(6) . . . . ? O30 Mn6 O16 C75' 74.1(6) 2_656 . . . ? N4 Mn6 O16 C75' 2.5(6) . . . . ? Mn9 Mn6 O16 C75' 110.5(6) 2_656 . . . ? O20 Mn7 O17 C71 136.3(8) . . . . ? F7 Mn7 O17 C71 -152.8(3) . . . . ? O21 Mn7 O17 C71 24.4(3) . . . . ? O19 Mn7 O17 C71 -65.6(3) . . . . ? F6 Mn7 O17 C71 118.3(3) . . . . ? F7 Mn7 O17 Mn6 -12.58(10) . . . . ? O21 Mn7 O17 Mn6 164.63(12) . . . . ? O19 Mn7 O17 Mn6 74.63(11) . . . . ? F6 Mn7 O17 Mn6 -101.45(10) . . . . ? F5 Mn6 O17 C71 -151.4(3) 2_656 . . . ? F7 Mn6 O17 C71 156.3(3) . . . . ? O16 Mn6 O17 C71 5.4(4) . . . . ? O18 Mn6 O17 C71 74.2(3) . . . . ? O30 Mn6 O17 C71 -92.2(3) 2_656 . . . ? N4 Mn6 O17 C71 -17.7(3) . . . . ? Mn9 Mn6 O17 C71 -121.1(3) 2_656 . . . ? F5 Mn6 O17 Mn7 64.17(16) 2_656 . . . ? F7 Mn6 O17 Mn7 11.87(9) . . . . ? O16 Mn6 O17 Mn7 -139.12(16) . . . . ? O18 Mn6 O17 Mn7 -70.29(12) . . . . ? O30 Mn6 O17 Mn7 123.37(11) 2_656 . . . ? N4 Mn6 O17 Mn7 -162.17(15) . . . . ? Mn9 Mn6 O17 Mn7 94.44(10) 2_656 . . . ? F5 Mn6 O18 C58 -113.5(3) 2_656 . . . ? F7 Mn6 O18 C58 -43.4(3) . . . . ? O17 Mn6 O18 C58 28.9(3) . . . . ? O16 Mn6 O18 C58 175.7(3) . . . . ? O30 Mn6 O18 C58 91.8(5) 2_656 . . . ? N4 Mn6 O18 C58 102.0(3) . . . . ? Mn9 Mn6 O18 C58 -109.3(3) 2_656 . . . ? O20 Mn7 O19 C58 137.2(3) . . . . ? O17 Mn7 O19 C58 -39.7(3) . . . . ? F7 Mn7 O19 C58 44.4(3) . . . . ? O21 Mn7 O19 C58 -133.0(3) . . . . ? F7 Mn7 O20 C89 81.3(3) . . . . ? O21 Mn7 O20 C89 -96.3(3) . . . . ? O19 Mn7 O20 C89 -6.4(3) . . . . ? F6 Mn7 O20 C89 169.9(3) . . . . ? F7 Mn7 O20 Mn8 -105.76(12) . . . . ? O21 Mn7 O20 Mn8 76.65(13) . . . . ? O19 Mn7 O20 Mn8 166.53(12) . . . . ? F6 Mn7 O20 Mn8 -17.19(10) . . . . ? O24 Mn8 O20 C89 -69.3(3) . . . . ? F6 Mn8 O20 C89 -169.4(3) . . . . ? O22 Mn8 O20 C89 105.5(3) . . . . ? O25 Mn8 O20 C89 -152.9(3) . . . . ? O23 Mn8 O20 C89 38.1(3) . . . . ? N5 Mn8 O20 C89 -5.9(3) . . . . ? O24 Mn8 O20 Mn7 117.34(12) . . . . ? F6 Mn8 O20 Mn7 17.21(10) . . . . ? O22 Mn8 O20 Mn7 -67.92(13) . . . . ? O25 Mn8 O20 Mn7 33.7(2) . . . . ? O23 Mn8 O20 Mn7 -135.31(12) . . . . ? N5 Mn8 O20 Mn7 -179.28(15) . . . . ? O20 Mn7 O21 C76 -33.3(3) . . . . ? O17 Mn7 O21 C76 138.9(3) . . . . ? O19 Mn7 O21 C76 -129.2(3) . . . . ? F6 Mn7 O21 C76 46.1(3) . . . . ? O24 Mn8 O22 C76 174.5(4) . . . . ? O20 Mn8 O22 C76 14.7(3) . . . . ? F6 Mn8 O22 C76 -57.3(3) . . . . ? O25 Mn8 O22 C76 -129.4(3) . . . . ? O23 Mn8 O22 C76 151.2(4) . . . . ? N5 Mn8 O22 C76 82.6(4) . . . . ? O24 Mn8 O23 C93 100.3(3) . . . . ? O20 Mn8 O23 C93 -16.8(3) . . . . ? F6 Mn8 O23 C93 -144.5(2) . . . . ? O22 Mn8 O23 C93 -85.3(3) . . . . ? O25 Mn8 O23 C93 169.7(3) . . . . ? N5 Mn8 O23 C93 26.6(2) . . . . ? O30 Mn9 O24 C92 -28.5(3) . . . . ? O25 Mn9 O24 C92 161.5(3) . . . . ? F8 Mn9 O24 C92 -115.6(3) 2_656 . . . ? O28 Mn9 O24 C92 71.5(3) . . . . ? Mn6 Mn9 O24 C92 -44.4(4) 2_656 . . . ? O30 Mn9 O24 Mn8 175.17(11) . . . . ? O25 Mn9 O24 Mn8 5.14(12) . . . . ? F8 Mn9 O24 Mn8 88.13(11) 2_656 . . . ? O28 Mn9 O24 Mn8 -84.81(12) . . . . ? Mn6 Mn9 O24 Mn8 159.25(5) 2_656 . . . ? O20 Mn8 O24 C92 55.8(3) . . . . ? F6 Mn8 O24 C92 131.5(3) . . . . ? O22 Mn8 O24 C92 -102.6(5) . . . . ? O25 Mn8 O24 C92 -162.5(3) . . . . ? O23 Mn8 O24 C92 -79.8(3) . . . . ? N5 Mn8 O24 C92 -6.3(3) . . . . ? O20 Mn8 O24 Mn9 -146.34(11) . . . . ? F6 Mn8 O24 Mn9 -70.67(13) . . . . ? O22 Mn8 O24 Mn9 55.2(5) . . . . ? O25 Mn8 O24 Mn9 -4.65(10) . . . . ? O23 Mn8 O24 Mn9 78.05(13) . . . . ? N5 Mn8 O24 Mn9 151.48(15) . . . . ? O24 Mn9 O25 C96 -138.8(3) . . . . ? F5 Mn9 O25 C96 43.4(2) . . . . ? O30 Mn9 O25 C96 115.8(6) . . . . ? F8 Mn9 O25 C96 132.9(2) 2_656 . . . ? O28 Mn9 O25 C96 -50.1(3) . . . . ? Mn6 Mn9 O25 C96 60.7(3) 2_656 . . . ? O24 Mn9 O25 Mn8 -4.74(11) . . . . ? F5 Mn9 O25 Mn8 177.39(10) . . . . ? O30 Mn9 O25 Mn8 -110.2(6) . . . . ? F8 Mn9 O25 Mn8 -93.10(10) 2_656 . . . ? O28 Mn9 O25 Mn8 83.89(11) . . . . ? Mn6 Mn9 O25 Mn8 -165.28(4) 2_656 . . . ? O24 Mn9 O25 Mn10 94.88(11) . . . . ? F5 Mn9 O25 Mn10 -82.99(10) . . . . ? O30 Mn9 O25 Mn10 -10.6(7) . . . . ? F8 Mn9 O25 Mn10 6.52(9) 2_656 . . . ? O28 Mn9 O25 Mn10 -176.49(11) . . . . ? Mn6 Mn9 O25 Mn10 -65.65(12) 2_656 . . . ? O24 Mn8 O25 C96 139.2(2) . . . . ? O20 Mn8 O25 C96 -122.9(2) . . . . ? F6 Mn8 O25 C96 -106.7(2) . . . . ? O22 Mn8 O25 C96 -28.1(2) . . . . ? O23 Mn8 O25 C96 49.0(2) . . . . ? N5 Mn8 O25 C96 105.2(2) . . . . ? O24 Mn8 O25 Mn9 4.37(10) . . . . ? O20 Mn8 O25 Mn9 102.25(17) . . . . ? F6 Mn8 O25 Mn9 118.43(11) . . . . ? O22 Mn8 O25 Mn9 -162.92(10) . . . . ? O23 Mn8 O25 Mn9 -85.87(11) . . . . ? N5 Mn8 O25 Mn9 -29.67(19) . . . . ? O24 Mn8 O25 Mn10 -97.61(10) . . . . ? O20 Mn8 O25 Mn10 0.27(19) . . . . ? F6 Mn8 O25 Mn10 16.46(7) . . . . ? O22 Mn8 O25 Mn10 95.10(10) . . . . ? O23 Mn8 O25 Mn10 172.15(10) . . . . ? N5 Mn8 O25 Mn10 -131.65(13) . . . . ? F6 Mn10 O25 C96 109.8(2) . . . . ? F8 Mn10 O25 C96 -137.5(2) 2_656 . . . ? F8 Mn10 O25 C96 175.9(2) . . . . ? O26 Mn10 O25 C96 -64.6(2) . . . . ? O27 Mn10 O25 C96 43.3(3) . . . . ? N6 Mn10 O25 C96 2.6(2) . . . . ? F6 Mn10 O25 Mn9 -119.50(11) . . . . ? F8 Mn10 O25 Mn9 -6.80(9) 2_656 . . . ? F8 Mn10 O25 Mn9 -53.34(16) . . . . ? O26 Mn10 O25 Mn9 66.10(12) . . . . ? O27 Mn10 O25 Mn9 174.01(10) . . . . ? N6 Mn10 O25 Mn9 133.31(13) . . . . ? F6 Mn10 O25 Mn8 -17.25(8) . . . . ? F8 Mn10 O25 Mn8 95.44(9) 2_656 . . . ? F8 Mn10 O25 Mn8 48.90(14) . . . . ? O26 Mn10 O25 Mn8 168.34(8) . . . . ? O27 Mn10 O25 Mn8 -83.75(14) . . . . ? N6 Mn10 O25 Mn8 -124.44(11) . . . . ? F8 Mn10 O26 C98 140.3(2) 2_656 . . . ? F8 Mn10 O26 C98 -145.5(2) . . . . ? O27 Mn10 O26 C98 -65.4(2) . . . . ? N6 Mn10 O26 C98 7.1(2) . . . . ? O25 Mn10 O26 C98 72.6(2) . . . . ? F6 Mn10 O27 C100 -63.7(2) . . . . ? F8 Mn10 O27 C100 179.5(2) 2_656 . . . ? F8 Mn10 O27 C100 -150.4(2) . . . . ? O26 Mn10 O27 C100 114.1(2) . . . . ? N6 Mn10 O27 C100 38.7(2) . . . . ? O25 Mn10 O27 C100 -2.1(3) . . . . ? O24 Mn9 O28 C101 -170.4(6) . . . . ? F5 Mn9 O28 C101 15.5(6) . . . . ? O30 Mn9 O28 C101 -70.6(6) . . . . ? O25 Mn9 O28 C101 106.9(6) . . . . ? Mn6 Mn9 O28 C101 -24.1(6) 2_656 . . . ? O24 Mn9 O30 C115 68.9(3) . . . . ? F5 Mn9 O30 C115 -114.2(3) . . . . ? O25 Mn9 O30 C115 172.9(6) . . . . ? F8 Mn9 O30 C115 155.9(3) 2_656 . . . ? O28 Mn9 O30 C115 -21.4(3) . . . . ? Mn6 Mn9 O30 C115 -124.2(3) 2_656 . . . ? O24 Mn9 O30 Mn6 -166.87(10) . . . 2_656 ? F5 Mn9 O30 Mn6 10.00(10) . . . 2_656 ? O25 Mn9 O30 Mn6 -62.9(7) . . . 2_656 ? F8 Mn9 O30 Mn6 -79.87(9) 2_656 . . 2_656 ? O28 Mn9 O30 Mn6 102.79(11) . . . 2_656 ? O1 Mn1 N1 C2 -29.8(2) . . . . ? O4 Mn1 N1 C2 93.1(3) . . . . ? O3 Mn1 N1 C2 167.7(2) . . . . ? F1 Mn1 N1 C2 64.3(3) . . . . ? O2 Mn1 N1 C2 -121.0(3) . . . . ? O5 Mn1 N1 C2 -60.6(3) . . . . ? O1 Mn1 N1 C5 -148.2(3) . . . . ? O4 Mn1 N1 C5 -25.4(3) . . . . ? O3 Mn1 N1 C5 49.2(3) . . . . ? F1 Mn1 N1 C5 -54.2(3) . . . . ? O2 Mn1 N1 C5 120.5(3) . . . . ? O5 Mn1 N1 C5 -179.1(2) . . . . ? O1 Mn1 N1 C4 90.9(3) . . . . ? O4 Mn1 N1 C4 -146.3(3) . . . . ? O3 Mn1 N1 C4 -71.7(3) . . . . ? F1 Mn1 N1 C4 -175.1(2) . . . . ? O2 Mn1 N1 C4 -0.4(3) . . . . ? O5 Mn1 N1 C4 60.0(3) . . . . ? F3 Mn3 N2 C30 175.4(2) . . . . ? F4 Mn3 N2 C30 29.8(3) . . . . ? O11 Mn3 N2 C30 37.6(2) . . . . ? O9 Mn3 N2 C30 -124.8(2) . . . . ? O10 Mn3 N2 C30 -45.6(2) . . . . ? O8 Mn3 N2 C30 130.5(2) . . . . ? F3 Mn3 N2 C27 56.7(3) . . . . ? F4 Mn3 N2 C27 -88.9(3) . . . . ? O11 Mn3 N2 C27 -81.1(2) . . . . ? O9 Mn3 N2 C27 116.5(2) . . . . ? O10 Mn3 N2 C27 -164.4(2) . . . . ? O8 Mn3 N2 C27 11.8(2) . . . . ? F3 Mn3 N2 C29 -64.1(3) . . . . ? F4 Mn3 N2 C29 150.4(2) . . . . ? O11 Mn3 N2 C29 158.2(3) . . . . ? O9 Mn3 N2 C29 -4.3(2) . . . . ? O10 Mn3 N2 C29 74.9(3) . . . . ? O8 Mn3 N2 C29 -108.9(3) . . . . ? F1 Mn5 N3 C9 166.2(2) . . . . ? F2 Mn5 N3 C9 -94.4(3) 2_575 . . . ? F2 Mn5 N3 C9 45.6(3) . . . . ? O14 Mn5 N3 C9 -18.6(2) . . . . ? O15 Mn5 N3 C9 -111.2(2) . . . . ? O5 Mn5 N3 C9 96.4(2) . . . . ? F1 Mn5 N3 C11 -72.6(2) . . . . ? F2 Mn5 N3 C11 26.9(4) 2_575 . . . ? F2 Mn5 N3 C11 166.8(2) . . . . ? O14 Mn5 N3 C11 102.6(3) . . . . ? O15 Mn5 N3 C11 10.1(2) . . . . ? O5 Mn5 N3 C11 -142.4(3) . . . . ? F1 Mn5 N3 C8 46.2(2) . . . . ? F2 Mn5 N3 C8 145.6(2) 2_575 . . . ? F2 Mn5 N3 C8 -74.5(3) . . . . ? O14 Mn5 N3 C8 -138.6(2) . . . . ? O15 Mn5 N3 C8 128.8(2) . . . . ? O5 Mn5 N3 C8 -23.6(2) . . . . ? F5 Mn6 N4 C74 -70.9(4) 2_656 . . . ? F7 Mn6 N4 C74 143.6(3) . . . . ? O17 Mn6 N4 C74 153.4(4) . . . . ? O16 Mn6 N4 C74 -12.8(4) . . . . ? O18 Mn6 N4 C74 68.2(4) . . . . ? O30 Mn6 N4 C74 -114.6(4) 2_656 . . . ? Mn9 Mn6 N4 C74 -100.1(4) 2_656 . . . ? F5 Mn6 N4 C72 170.6(2) 2_656 . . . ? F7 Mn6 N4 C72 25.1(3) . . . . ? O17 Mn6 N4 C72 34.9(2) . . . . ? O16 Mn6 N4 C72 -131.4(3) . . . . ? O18 Mn6 N4 C72 -50.4(2) . . . . ? O30 Mn6 N4 C72 126.8(2) 2_656 . . . ? Mn9 Mn6 N4 C72 141.3(2) 2_656 . . . ? F5 Mn6 N4 C73 51.8(3) 2_656 . . . ? F7 Mn6 N4 C73 -93.7(3) . . . . ? O17 Mn6 N4 C73 -83.9(3) . . . . ? O16 Mn6 N4 C73 109.8(3) . . . . ? O18 Mn6 N4 C73 -169.2(3) . . . . ? O30 Mn6 N4 C73 8.0(2) 2_656 . . . ? Mn9 Mn6 N4 C73 22.5(3) 2_656 . . . ? O24 Mn8 N5 C94 -90.8(4) . . . . ? O20 Mn8 N5 C94 149.4(4) . . . . ? F6 Mn8 N5 C94 173.9(4) . . . . ? O22 Mn8 N5 C94 74.2(4) . . . . ? O25 Mn8 N5 C94 -57.8(4) . . . . ? O23 Mn8 N5 C94 1.5(4) . . . . ? O24 Mn8 N5 C90 146.5(3) . . . . ? O20 Mn8 N5 C90 26.8(2) . . . . ? F6 Mn8 N5 C90 51.3(3) . . . . ? O22 Mn8 N5 C90 -48.4(3) . . . . ? O25 Mn8 N5 C90 179.6(2) . . . . ? O23 Mn8 N5 C90 -121.2(3) . . . . ? O24 Mn8 N5 C91 29.4(2) . . . . ? O20 Mn8 N5 C91 -90.3(3) . . . . ? F6 Mn8 N5 C91 -65.8(3) . . . . ? O22 Mn8 N5 C91 -165.6(2) . . . . ? O25 Mn8 N5 C91 62.5(3) . . . . ? O23 Mn8 N5 C91 121.7(3) . . . . ? O24 Mn8 N5 C94' -93.1(6) . . . . ? O20 Mn8 N5 C94' 147.1(6) . . . . ? F6 Mn8 N5 C94' 171.6(6) . . . . ? O22 Mn8 N5 C94' 71.9(6) . . . . ? O25 Mn8 N5 C94' -60.1(6) . . . . ? O23 Mn8 N5 C94' -0.8(6) . . . . ? F6 Mn10 N6 C97 -164.7(2) . . . . ? F8 Mn10 N6 C97 -45.4(3) 2_656 . . . ? F8 Mn10 N6 C97 93.7(3) . . . . ? O26 Mn10 N6 C97 20.1(2) . . . . ? O27 Mn10 N6 C97 112.6(2) . . . . ? O25 Mn10 N6 C97 -96.2(2) . . . . ? F6 Mn10 N6 C95 -44.2(2) . . . . ? F8 Mn10 N6 C95 75.1(2) 2_656 . . . ? F8 Mn10 N6 C95 -145.8(2) . . . . ? O26 Mn10 N6 C95 140.6(2) . . . . ? O27 Mn10 N6 C95 -126.9(2) . . . . ? O25 Mn10 N6 C95 24.3(2) . . . . ? F6 Mn10 N6 C99 74.7(2) . . . . ? F8 Mn10 N6 C99 -166.0(2) 2_656 . . . ? F8 Mn10 N6 C99 -26.9(3) . . . . ? O26 Mn10 N6 C99 -100.5(2) . . . . ? O27 Mn10 N6 C99 -8.0(2) . . . . ? O25 Mn10 N6 C99 143.2(2) . . . . ? Mn2 O1 C1 C2 172.2(2) . . . . ? Mn1 O1 C1 C2 17.9(4) . . . . ? C5 N1 C2 C1 165.7(3) . . . . ? C4 N1 C2 C1 -69.6(4) . . . . ? Mn1 N1 C2 C1 50.0(4) . . . . ? O1 C1 C2 N1 -46.5(4) . . . . ? Mn1 O2 C3 C4 52.8(4) . . . . ? C2 N1 C4 C3 143.1(4) . . . . ? C5 N1 C4 C3 -91.7(4) . . . . ? Mn1 N1 C4 C3 27.2(4) . . . . ? O2 C3 C4 N1 -54.8(5) . . . . ? C2 N1 C5 C6 -69.0(5) . . . . ? C4 N1 C5 C6 165.5(4) . . . . ? Mn1 N1 C5 C6 44.8(4) . . . . ? Mn4 O4 C6 C5 -161.9(3) 2_575 . . . ? Mn1 O4 C6 C5 20.1(5) . . . . ? N1 C5 C6 O4 -43.2(5) . . . . ? Mn2 O5 C7 C8 150.1(2) . . . . ? Mn1 O5 C7 C8 -84.8(3) . . . . ? Mn5 O5 C7 C8 29.5(4) . . . . ? C9 N3 C8 C7 -66.2(4) . . . . ? C11 N3 C8 C7 168.0(3) . . . . ? Mn5 N3 C8 C7 49.0(3) . . . . ? O5 C7 C8 N3 -53.8(4) . . . . ? C11 N3 C9 C10 -76.1(4) . . . . ? C8 N3 C9 C10 159.8(3) . . . . ? Mn5 N3 C9 C10 43.5(4) . . . . ? Mn5 O14 C10 C9 36.6(4) . . . . ? N3 C9 C10 O14 -55.2(4) . . . . ? C9 N3 C11 C12 136.8(3) . . . . ? C8 N3 C11 C12 -97.3(4) . . . . ? Mn5 N3 C11 C12 19.9(4) . . . . ? Mn5 O15 C12 C11 64.6(3) . . . . ? N3 C11 C12 O15 -56.0(4) . . . . ? Mn2 O6 C13 O7 7.4(8) . . . . ? Mn2 O6 C13 C14 -171.9(3) . . . . ? O7 C13 C14 C15 112.3(5) . . . . ? O6 C13 C14 C15 -68.4(6) . . . . ? O7 C13 C14 C19 -69.6(6) . . . . ? O6 C13 C14 C19 109.7(5) . . . . ? C19 C14 C15 C16 -1.0(7) . . . . ? C13 C14 C15 C16 177.1(4) . . . . ? C14 C15 C16 C17 0.1(8) . . . . ? C15 C16 C17 C18 0.1(8) . . . . ? C16 C17 C18 C19 0.8(8) . . . . ? C17 C18 C19 C14 -1.6(7) . . . . ? C17 C18 C19 C20 -178.7(4) . . . . ? C15 C14 C19 C18 1.7(7) . . . . ? C13 C14 C19 C18 -176.4(4) . . . . ? C15 C14 C19 C20 178.7(4) . . . . ? C13 C14 C19 C20 0.7(6) . . . . ? C18 C19 C20 C25 -96.5(7) . . . . ? C14 C19 C20 C25 86.6(7) . . . . ? C18 C19 C20 C21 85.8(6) . . . . ? C14 C19 C20 C21 -91.1(6) . . . . ? C25 C20 C21 C22 0.5(9) . . . . ? C19 C20 C21 C22 178.4(5) . . . . ? C20 C21 C22 C23 0.6(11) . . . . ? C21 C22 C23 C24 -0.3(11) . . . . ? C22 C23 C24 C25 -0.9(11) . . . . ? C21 C20 C25 C24 -1.9(10) . . . . ? C19 C20 C25 C24 -179.7(6) . . . . ? C23 C24 C25 C20 2.1(12) . . . . ? Mn2 O8 C26 C27 -166.8(2) . . . . ? Mn3 O8 C26 C27 -46.5(3) . . . . ? C30 N2 C27 C26 -152.4(3) . . . . ? C29 N2 C27 C26 80.1(4) . . . . ? Mn3 N2 C27 C26 -40.2(3) . . . . ? O8 C26 C27 N2 58.5(4) . . . . ? Mn3 O9 C28 C29 -54.8(4) . . . . ? C30 N2 C29 C28 91.6(4) . . . . ? C27 N2 C29 C28 -141.6(3) . . . . ? Mn3 N2 C29 C28 -21.9(4) . . . . ? O9 C28 C29 N2 51.1(4) . . . . ? C27 N2 C30 C31 65.3(4) . . . . ? C29 N2 C30 C31 -168.8(3) . . . . ? Mn3 N2 C30 C31 -50.8(4) . . . . ? Mn4 O11 C31 C30 133.9(3) . . . . ? Mn3 O11 C31 C30 0.8(4) . . . . ? N2 C30 C31 O11 36.8(5) . . . . ? Mn4 O13 C32 O3 -2.9(6) . . . 2_575 ? Mn4 O13 C32 C33 -179.5(3) . . . . ? O3 C32 C33 C34 -112.8(5) 2_575 . . . ? O13 C32 C33 C34 64.1(5) . . . . ? O3 C32 C33 C38 63.5(6) 2_575 . . . ? O13 C32 C33 C38 -119.6(5) . . . . ? C38 C33 C34 C35 0.8(8) . . . . ? C32 C33 C34 C35 177.1(5) . . . . ? C33 C34 C35 C36 -0.2(9) . . . . ? C34 C35 C36 C37 -0.8(9) . . . . ? C35 C36 C37 C38 1.1(9) . . . . ? C36 C37 C38 C33 -0.5(8) . . . . ? C36 C37 C38 C39 174.9(5) . . . . ? C34 C33 C38 C37 -0.5(7) . . . . ? C32 C33 C38 C37 -176.7(4) . . . . ? C34 C33 C38 C39 -175.8(5) . . . . ? C32 C33 C38 C39 8.0(7) . . . . ? C37 C38 C39 C40 -126.1(5) . . . . ? C33 C38 C39 C40 49.2(7) . . . . ? C37 C38 C39 C44 51.4(7) . . . . ? C33 C38 C39 C44 -133.4(5) . . . . ? C44 C39 C40 C41 1.1(8) . . . . ? C38 C39 C40 C41 178.6(5) . . . . ? C39 C40 C41 C42 0.2(8) . . . . ? C40 C41 C42 C43 -1.0(9) . . . . ? C41 C42 C43 C44 0.4(10) . . . . ? C40 C39 C44 C43 -1.6(8) . . . . ? C38 C39 C44 C43 -179.2(5) . . . . ? C42 C43 C44 C39 0.9(10) . . . . ? Mn3 O10 C45 O12 6.3(6) . . . . ? Mn3 O10 C45 C46 -170.7(3) . . . . ? Mn4 O12 C45 O10 -2.7(6) . . . . ? Mn4 O12 C45 C46 174.4(3) . . . . ? O10 C45 C46 C51 -122.5(5) . . . . ? O12 C45 C46 C51 60.1(6) . . . . ? O10 C45 C46 C47 62.7(5) . . . . ? O12 C45 C46 C47 -114.7(4) . . . . ? C51 C46 C47 C48 -2.1(7) . . . . ? C45 C46 C47 C48 172.9(4) . . . . ? C46 C47 C48 C49 0.2(8) . . . . ? C47 C48 C49 C50 1.5(9) . . . . ? C48 C49 C50 C51 -1.3(9) . . . . ? C47 C46 C51 C50 2.3(7) . . . . ? C45 C46 C51 C50 -172.3(4) . . . . ? C47 C46 C51 C52 -174.7(5) . . . . ? C45 C46 C51 C52 10.7(7) . . . . ? C49 C50 C51 C46 -0.6(8) . . . . ? C49 C50 C51 C52 176.5(5) . . . . ? C46 C51 C52 C57 47.3(7) . . . . ? C50 C51 C52 C57 -129.7(5) . . . . ? C46 C51 C52 C53 -134.9(6) . . . . ? C50 C51 C52 C53 48.2(8) . . . . ? C57 C52 C53 C54 0.2(11) . . . . ? C51 C52 C53 C54 -177.7(7) . . . . ? C52 C53 C54 C55 0.7(14) . . . . ? C53 C54 C55 C56 -1.0(14) . . . . ? C54 C55 C56 C57 0.3(10) . . . . ? C53 C52 C57 C56 -0.8(8) . . . . ? C51 C52 C57 C56 177.1(5) . . . . ? C55 C56 C57 C52 0.6(8) . . . . ? Mn6 O18 C58 O19 9.7(6) . . . . ? Mn6 O18 C58 C59 -166.6(3) . . . . ? Mn7 O19 C58 O18 -7.4(6) . . . . ? Mn7 O19 C58 C59 168.9(3) . . . . ? O18 C58 C59 C60 58.3(5) . . . . ? O19 C58 C59 C60 -118.4(4) . . . . ? O18 C58 C59 C64 -127.5(4) . . . . ? O19 C58 C59 C64 55.7(5) . . . . ? C64 C59 C60 C61 -2.5(7) . . . . ? C58 C59 C60 C61 171.9(4) . . . . ? C59 C60 C61 C62 0.7(7) . . . . ? C60 C61 C62 C63 0.1(8) . . . . ? C61 C62 C63 C64 0.8(9) . . . . ? C62 C63 C64 C59 -2.5(8) . . . . ? C62 C63 C64 C65 174.8(5) . . . . ? C60 C59 C64 C63 3.2(6) . . . . ? C58 C59 C64 C63 -170.8(4) . . . . ? C60 C59 C64 C65 -173.9(4) . . . . ? C58 C59 C64 C65 12.0(6) . . . . ? C63 C64 C65 C70 -131.4(5) . . . . ? C59 C64 C65 C70 45.6(6) . . . . ? C63 C64 C65 C66 43.7(6) . . . . ? C59 C64 C65 C66 -139.3(5) . . . . ? C70 C65 C66 C67 1.1(7) . . . . ? C64 C65 C66 C67 -174.1(4) . . . . ? C65 C66 C67 C68 -1.1(8) . . . . ? C66 C67 C68 C69 0.6(8) . . . . ? C67 C68 C69 C70 -0.1(8) . . . . ? C68 C69 C70 C65 0.2(8) . . . . ? C66 C65 C70 C69 -0.7(7) . . . . ? C64 C65 C70 C69 174.6(4) . . . . ? Mn7 O17 C71 C72 130.8(3) . . . . ? Mn6 O17 C71 C72 -3.5(4) . . . . ? C74 N4 C72 C71 -165.4(4) . . . . ? C73 N4 C72 C71 67.6(4) . . . . ? Mn6 N4 C72 C71 -49.3(4) . . . . ? O17 C71 C72 N4 37.6(5) . . . . ? C74 N4 C73 C115 83.3(4) . . . 2_656 ? C72 N4 C73 C115 -150.5(3) . . . 2_656 ? Mn6 N4 C73 C115 -36.3(4) . . . 2_656 ? C72 N4 C74 C75' 139.1(8) . . . . ? C73 N4 C74 C75' -94.8(9) . . . . ? Mn6 N4 C74 C75' 25.3(10) . . . . ? C72 N4 C74 C75 100.7(6) . . . . ? C73 N4 C74 C75 -133.1(6) . . . . ? Mn6 N4 C74 C75 -13.0(7) . . . . ? C75' C74 C75 O16 -65.0(9) . . . . ? N4 C74 C75 O16 47.4(8) . . . . ? C75' O16 C75 C74 62.4(9) . . . . ? Mn6 O16 C75 C74 -56.6(6) . . . . ? Mn8 O22 C76 O21 30.7(6) . . . . ? Mn8 O22 C76 C77 -144.2(3) . . . . ? Mn7 O21 C76 O22 -22.4(6) . . . . ? Mn7 O21 C76 C77 152.6(3) . . . . ? O22 C76 C77 C82 -82.4(6) . . . . ? O21 C76 C77 C82 102.1(5) . . . . ? O22 C76 C77 C78 93.4(5) . . . . ? O21 C76 C77 C78 -82.1(5) . . . . ? C82 C77 C78 C79 1.8(7) . . . . ? C76 C77 C78 C79 -174.2(4) . . . . ? C77 C78 C79 C80 1.3(8) . . . . ? C78 C79 C80 C81 -1.2(9) . . . . ? C79 C80 C81 C82 -1.8(10) . . . . ? C78 C77 C82 C81 -4.6(8) . . . . ? C76 C77 C82 C81 171.2(5) . . . . ? C78 C77 C82 C13D -177.6(5) . . . . ? C76 C77 C82 C13D -1.9(8) . . . . ? C78 C77 C82 C13' 139.9(6) . . . . ? C76 C77 C82 C13' -44.4(8) . . . . ? C80 C81 C82 C77 4.7(10) . . . . ? C80 C81 C82 C13D 177.8(6) . . . . ? C80 C81 C82 C13' -141.9(7) . . . . ? Mn7 O20 C89 C90 155.9(3) . . . . ? Mn8 O20 C89 C90 -16.0(4) . . . . ? C94 N5 C90 C89 -170.1(4) . . . . ? C91 N5 C90 C89 66.8(4) . . . . ? C94' N5 C90 C89 -159.3(4) . . . . ? Mn8 N5 C90 C89 -45.1(4) . . . . ? O20 C89 C90 N5 41.2(5) . . . . ? C94 N5 C91 C92 73.1(5) . . . . ? C90 N5 C91 C92 -163.8(3) . . . . ? C94' N5 C91 C92 64.0(7) . . . . ? Mn8 N5 C91 C92 -49.7(3) . . . . ? Mn9 O24 C92 C91 -171.3(3) . . . . ? Mn8 O24 C92 C91 -18.1(4) . . . . ? N5 C91 C92 O24 47.0(4) . . . . ? Mn8 O23 C93 C94' -55.6(7) . . . . ? Mn8 O23 C93 C94 -50.5(4) . . . . ? C90 N5 C94 C93 94.7(5) . . . . ? C91 N5 C94 C93 -141.9(4) . . . . ? C94' N5 C94 C93 -13(4) . . . . ? Mn8 N5 C94 C93 -25.9(6) . . . . ? C94' C93 C94 N5 139(13) . . . . ? O23 C93 C94 N5 51.2(6) . . . . ? C97 N6 C95 C96 66.1(4) . . . . ? C99 N6 C95 C96 -168.6(3) . . . . ? Mn10 N6 C95 C96 -49.7(3) . . . . ? Mn9 O25 C96 C95 -148.5(2) . . . . ? Mn8 O25 C96 C95 85.8(3) . . . . ? Mn10 O25 C96 C95 -28.8(3) . . . . ? N6 C95 C96 O25 53.7(4) . . . . ? C95 N6 C97 C98 -161.2(3) . . . . ? C99 N6 C97 C98 74.8(4) . . . . ? Mn10 N6 C97 C98 -44.2(3) . . . . ? Mn10 O26 C98 C97 -33.3(4) . . . . ? N6 C97 C98 O26 53.5(4) . . . . ? C97 N6 C99 C100 -139.5(3) . . . . ? C95 N6 C99 C100 94.8(4) . . . . ? Mn10 N6 C99 C100 -22.8(3) . . . . ? Mn10 O27 C100 C99 -64.7(3) . . . . ? N6 C99 C100 O27 58.5(4) . . . . ? Mn9 O28 C101 O29 17.9(12) . . . . ? Mn9 O28 C101 C1D 176.0(3) . . . . ? Mn9 O28 C101 C1' -131.4(5) . . . . ? Mn9 O30 C115 C73 166.1(3) . . . 2_656 ? Mn6 O30 C115 C73 47.8(4) 2_656 . . 2_656 ? O28 C101 C1' C2' 92.9(8) . . . . ? O29 C101 C1' C2' -59.4(9) . . . . ? C1D C101 C1' C2' -167.0(9) . . . . ? O28 C101 C1' C6' -90.5(7) . . . . ? O29 C101 C1' C6' 117.2(7) . . . . ? C1D C101 C1' C6' 9.6(5) . . . . ? C6' C1' C2' C3' 0.0 . . . . ? C101 C1' C2' C3' 176.3(8) . . . . ? C1' C2' C3' C4' 0.0 . . . . ? C2' C3' C4' C5' 0.0 . . . . ? C3' C4' C5' C6' 0.0 . . . . ? C4' C5' C6' C1' 0.0 . . . . ? C4' C5' C6' C7' 178.5(9) . . . . ? C2' C1' C6' C5' 0.0 . . . . ? C101 C1' C6' C5' -177.0(7) . . . . ? C2' C1' C6' C7' -178.4(10) . . . . ? C101 C1' C6' C7' 4.7(9) . . . . ? C5' C6' C7' C8' -38.0(9) . . . . ? C1' C6' C7' C8' 140.4(7) . . . . ? C5' C6' C7' C12' 147.2(6) . . . . ? C1' C6' C7' C12' -34.3(12) . . . . ? C12' C7' C8' C9' 0.0 . . . . ? C6' C7' C8' C9' -174.8(10) . . . . ? C7' C8' C9' C10' 0.0 . . . . ? C8' C9' C10' C11' 0.0 . . . . ? C9' C10' C11' C12' 0.0 . . . . ? C10' C11' C12' C7' 0.0 . . . . ? C8' C7' C12' C11' 0.0 . . . . ? C6' C7' C12' C11' 174.7(10) . . . . ? C77 C82 C13' C14' 78.1(9) . . . . ? C81 C82 C13' C14' -136.4(7) . . . . ? C13D C82 C13' C14' -25.1(6) . . . . ? C77 C82 C13' C18' -122.1(4) . . . . ? C81 C82 C13' C18' 23.4(7) . . . . ? C13D C82 C13' C18' 134.7(7) . . . . ? C18' C13' C14' C15' 0.0 . . . . ? C82 C13' C14' C15' 162.1(6) . . . . ? C13' C14' C15' C16' 0.0 . . . . ? C14' C15' C16' C17' 0.0 . . . . ? C15' C16' C17' C18' 0.0 . . . . ? C16' C17' C18' C13' 0.0 . . . . ? C14' C13' C18' C17' 0.0 . . . . ? C82 C13' C18' C17' -157.7(8) . . . . ? C75 C74 C75' O16 62.7(9) . . . . ? N4 C74 C75' O16 -24.0(13) . . . . ? C75 O16 C75' C74 -64.3(10) . . . . ? Mn6 O16 C75' C74 9.3(11) . . . . ? O23 C93 C94' N5 57.2(13) . . . . ? C94 C93 C94' N5 -37(12) . . . . ? C94 N5 C94' C93 162(6) . . . . ? C90 N5 C94' C93 86.4(13) . . . . ? C91 N5 C94' C93 -142.5(10) . . . . ? Mn8 N5 C94' C93 -29.4(13) . . . . ? O28 C101 C1D C2D 96.8(6) . . . . ? O29 C101 C1D C2D -103.9(7) . . . . ? C1' C101 C1D C2D -6.5(5) . . . . ? O28 C101 C1D C6D -79.0(6) . . . . ? O29 C101 C1D C6D 80.3(8) . . . . ? C1' C101 C1D C6D 177.7(7) . . . . ? C6D C1D C2D C3D 0.0 . . . . ? C101 C1D C2D C3D -176.3(4) . . . . ? C1D C2D C3D C4D 0.0 . . . . ? C2D C3D C4D C5D 0.0 . . . . ? C3D C4D C5D C6D 0.0 . . . . ? C4D C5D C6D C1D 0.0 . . . . ? C4D C5D C6D C7D 179.3(4) . . . . ? C2D C1D C6D C5D 0.0 . . . . ? C101 C1D C6D C5D 175.4(5) . . . . ? C2D C1D C6D C7D -179.3(4) . . . . ? C101 C1D C6D C7D -3.9(5) . . . . ? C5D C6D C7D C8D 108.3(3) . . . . ? C1D C6D C7D C8D -72.5(4) . . . . ? C5D C6D C7D C12D -71.7(4) . . . . ? C1D C6D C7D C12D 107.6(4) . . . . ? C12D C7D C8D C9D 0.0 . . . . ? C6D C7D C8D C9D -179.9(4) . . . . ? C7D C8D C9D C10D 0.0 . . . . ? C8D C9D C10D C11D 0.0 . . . . ? C9D C10D C11D C12D 0.0 . . . . ? C10D C11D C12D C7D 0.0 . . . . ? C8D C7D C12D C11D 0.0 . . . . ? C6D C7D C12D C11D 179.9(4) . . . . ? C77 C82 C13D C14D -51.2(6) . . . . ? C81 C82 C13D C14D 136.1(5) . . . . ? C13' C82 C13D C14D 48.1(7) . . . . ? C77 C82 C13D C18D 133.7(5) . . . . ? C81 C82 C13D C18D -39.0(7) . . . . ? C13' C82 C13D C18D -127.0(7) . . . . ? C18D C13D C14D C15D 0.0 . . . . ? C82 C13D C14D C15D -175.2(4) . . . . ? C13D C14D C15D C16D 0.0 . . . . ? C14D C15D C16D C17D 0.0 . . . . ? C15D C16D C17D C18D 0.0 . . . . ? C16D C17D C18D C13D 0.0 . . . . ? C14D C13D C18D C17D 0.0 . . . . ? C82 C13D C18D C17D 175.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.455 _refine_diff_density_min -1.801 _refine_diff_density_rms 0.123