# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_address ; State Key Lab of Rare Earth Resource Utilization Changchun Institute of Applied Chemistry CAS, Changchun 130022 P.R. China ; _publ_contact_author_name 'Dr Wuping Liao' _publ_contact_author_email wpliao@ciac.jl.cn _publ_section_title ; Mn4-Hinged Bithiacalix[4]arenes Accommodating Fullerenes ; #TrackingRef '- Compd_1-3-20110106.cif' _publ_contact_author 'Prof Dr Wuping Liao' _publ_author_name 'Wuping Liao' # Attachment '- Compd_1-3-20110106.cif' data_Compound_746727 _database_code_depnum_ccdc_archive 'CCDC 746727' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Mn4(C48H28O4S4)2)(CHCl3)2 _chemical_melting_point ? _chemical_formula_moiety 'C96 H56 Mn4 O8 S8, 2(CHCl3)' _chemical_formula_sum 'C98 H58 Cl6 Mn4 O8 S8' _chemical_formula_weight 2052.38 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number No.2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2061(6) _cell_length_b 13.6364(6) _cell_length_c 14.9448(7) _cell_angle_alpha 117.0520(10) _cell_angle_beta 90.3890(10) _cell_angle_gamma 113.0350(10) _cell_volume 2148.98(17) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5726 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7711 _exptl_absorpt_correction_T_max 0.8000 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10999 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7512 _reflns_number_gt 5887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Chloroform molecule was refined with two disordered parts (C49, Cl1 > Cl3 (0.56705) and C50, Cl4 > Cl6 (0.43295). Atoms C49 and C50, Cl1 > Cl3, and Cl4 > Cl6 were refined with the same ADPs, respectively. ; _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^)+(0.0790P)^2^+4.5291P] 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 7512 _refine_ls_number_parameters 566 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1615 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn -0.12879(6) 0.08631(6) 0.06658(5) 0.02600(19) Uani 1 1 d . . . Mn2 Mn -0.03576(5) 0.00486(6) -0.14948(5) 0.02651(19) Uani 1 1 d . . . S1 S -0.06893(10) 0.33094(11) 0.18041(9) 0.0315(3) Uani 1 1 d . . . S2 S 0.08024(10) 0.19450(11) -0.18068(9) 0.0307(3) Uani 1 1 d . . . S3 S 0.35115(9) 0.04933(10) -0.04092(9) 0.0260(3) Uani 1 1 d . . . S4 S 0.20164(10) 0.18468(10) 0.31971(9) 0.0287(3) Uani 1 1 d . . . O1 O -0.0271(3) 0.1615(3) -0.0145(3) 0.0436(9) Uani 1 1 d . . . O2 O 0.1369(3) 0.0572(3) -0.0957(3) 0.0444(9) Uani 1 1 d . . . O3 O 0.1833(3) 0.0431(3) 0.0934(2) 0.0311(7) Uani 1 1 d . . . O4 O 0.0173(3) 0.1571(3) 0.1799(3) 0.0435(9) Uani 1 1 d . . . C1 C 0.0205(4) 0.2766(4) 0.0072(4) 0.0311(10) Uani 1 1 d . . . C2 C 0.0145(4) 0.3709(4) 0.0973(4) 0.0314(10) Uani 1 1 d . . . C3 C 0.0682(4) 0.4927(4) 0.1206(4) 0.0374(12) Uani 1 1 d . . . H3A H 0.0616 0.5543 0.1814 0.045 Uiso 1 1 calc R . . C4 C 0.1321(4) 0.5260(4) 0.0556(4) 0.0390(12) Uani 1 1 d . . . C5 C 0.1345(4) 0.4333(5) -0.0346(4) 0.0369(12) Uani 1 1 d . . . H5A H 0.1752 0.4534 -0.0808 0.044 Uiso 1 1 calc R . . C6 C 0.0785(4) 0.3114(4) -0.0594(4) 0.0304(10) Uani 1 1 d . . . C7 C 0.2245(4) 0.1276(4) -0.1145(3) 0.0282(10) Uani 1 1 d . . . C8 C 0.2148(4) 0.2008(4) -0.1541(4) 0.0279(10) Uani 1 1 d . . . C9 C 0.3079(4) 0.2766(4) -0.1727(4) 0.0316(11) Uani 1 1 d . . . H9A H 0.2996 0.3271 -0.1970 0.038 Uiso 1 1 calc R . . C10 C 0.4128(4) 0.2796(4) -0.1564(4) 0.0298(10) Uani 1 1 d . . . C11 C 0.4241(4) 0.2069(4) -0.1188(3) 0.0275(10) Uani 1 1 d . . . H11A H 0.4952 0.2072 -0.1081 0.033 Uiso 1 1 calc R . . C12 C 0.3319(4) 0.1338(4) -0.0968(3) 0.0255(9) Uani 1 1 d . . . C13 C 0.2842(4) 0.1349(4) 0.1430(3) 0.0257(10) Uani 1 1 d . . . C14 C 0.3735(4) 0.1545(4) 0.0927(3) 0.0244(9) Uani 1 1 d . . . C15 C 0.4774(4) 0.2564(4) 0.1447(4) 0.0300(10) Uani 1 1 d . . . H23A H 0.5365 0.2677 0.1091 0.036 Uiso 1 1 calc R . . C16 C 0.4965(4) 0.3416(4) 0.2474(4) 0.0314(11) Uani 1 1 d . . . C17 C 0.4113(4) 0.3181(4) 0.2998(4) 0.0312(10) Uani 1 1 d . . . H21A H 0.4244 0.3731 0.3713 0.037 Uiso 1 1 calc R . . C18 C 0.3081(4) 0.2163(4) 0.2495(4) 0.0279(10) Uani 1 1 d . . . C19 C 0.0667(4) 0.2669(4) 0.2615(3) 0.0292(10) Uani 1 1 d . . . C20 C 0.1543(4) 0.2966(4) 0.3377(3) 0.0266(10) Uani 1 1 d . . . C21 C 0.2068(4) 0.4129(4) 0.4245(4) 0.0318(11) Uani 1 1 d . . . H17A H 0.2652 0.4302 0.4748 0.038 Uiso 1 1 calc R . . C22 C 0.1755(4) 0.5042(4) 0.4391(4) 0.0328(11) Uani 1 1 d . . . C23 C 0.0885(4) 0.4761(4) 0.3653(4) 0.0321(11) Uani 1 1 d . . . H15A H 0.0648 0.5370 0.3751 0.039 Uiso 1 1 calc R . . C24 C 0.0354(4) 0.3604(4) 0.2771(4) 0.0294(10) Uani 1 1 d . . . C25 C 0.1949(5) 0.6577(5) 0.0834(5) 0.0457(14) Uani 1 1 d . . . C26 C 0.2105(8) 0.7528(6) 0.1795(6) 0.084(3) Uani 1 1 d . . . H26A H 0.1769 0.7352 0.2297 0.101 Uiso 1 1 calc R . . C27 C 0.2750(9) 0.8752(7) 0.2052(8) 0.103(3) Uani 1 1 d . . . H27A H 0.2839 0.9396 0.2721 0.124 Uiso 1 1 calc R . . C28 C 0.3249(7) 0.9023(7) 0.1346(8) 0.081(3) Uani 1 1 d . . . H28A H 0.3704 0.9853 0.1526 0.097 Uiso 1 1 calc R . . C29 C 0.3094(5) 0.8109(7) 0.0395(7) 0.071(2) Uani 1 1 d . . . H29A H 0.3427 0.8298 -0.0103 0.085 Uiso 1 1 calc R . . C30 C 0.2458(5) 0.6897(5) 0.0129(6) 0.0543(16) Uani 1 1 d . . . H30A H 0.2365 0.6267 -0.0549 0.065 Uiso 1 1 calc R . . C31 C 0.5127(4) 0.3595(4) -0.1783(4) 0.0312(11) Uani 1 1 d . . . C32 C 0.5515(4) 0.4861(4) -0.1259(4) 0.0357(11) Uani 1 1 d . . . H32A H 0.5145 0.5226 -0.0759 0.043 Uiso 1 1 calc R . . C33 C 0.6447(4) 0.5595(5) -0.1467(4) 0.0399(12) Uani 1 1 d . . . H33A H 0.6728 0.6462 -0.1091 0.048 Uiso 1 1 calc R . . C34 C 0.6959(4) 0.5071(5) -0.2209(5) 0.0447(14) Uani 1 1 d . . . H34A H 0.7583 0.5577 -0.2358 0.054 Uiso 1 1 calc R . . C35 C 0.6576(5) 0.3814(6) -0.2744(5) 0.0478(14) Uani 1 1 d . . . H35A H 0.6933 0.3452 -0.3261 0.057 Uiso 1 1 calc R . . C36 C 0.5666(5) 0.3083(5) -0.2519(5) 0.0437(13) Uani 1 1 d . . . H36A H 0.5411 0.2219 -0.2876 0.052 Uiso 1 1 calc R . . C37 C 0.6035(4) 0.4583(5) 0.2986(4) 0.0362(12) Uani 1 1 d . . . C38 C 0.7064(4) 0.4589(5) 0.2813(4) 0.0439(13) Uani 1 1 d . . . H48A H 0.7098 0.3835 0.2392 0.053 Uiso 1 1 calc R . . C39 C 0.8056(5) 0.5691(6) 0.3252(5) 0.0522(15) Uani 1 1 d . . . H47A H 0.8761 0.5688 0.3136 0.063 Uiso 1 1 calc R . . C40 C 0.8000(5) 0.6777(5) 0.3850(4) 0.0520(15) Uani 1 1 d . . . H46A H 0.8669 0.7530 0.4143 0.062 Uiso 1 1 calc R . . C41 C 0.6973(5) 0.6788(5) 0.4031(4) 0.0463(14) Uani 1 1 d . . . H45A H 0.6943 0.7544 0.4455 0.056 Uiso 1 1 calc R . . C42 C 0.5992(4) 0.5691(5) 0.3590(4) 0.0398(12) Uani 1 1 d . . . H44A H 0.5287 0.5698 0.3702 0.048 Uiso 1 1 calc R . . C43 C 0.2383(4) 0.6303(4) 0.5294(4) 0.0357(11) Uani 1 1 d . . . C44 C 0.3556(5) 0.6841(5) 0.5556(4) 0.0471(14) Uani 1 1 d . . . H42A H 0.3943 0.6397 0.5157 0.057 Uiso 1 1 calc R . . C45 C 0.4179(6) 0.8024(5) 0.6395(5) 0.0570(16) Uani 1 1 d . . . H41A H 0.4980 0.8383 0.6556 0.068 Uiso 1 1 calc R . . C46 C 0.3622(6) 0.8662(6) 0.6985(5) 0.0611(18) Uani 1 1 d . . . H40A H 0.4036 0.9464 0.7558 0.073 Uiso 1 1 calc R . . C47 C 0.2443(6) 0.8125(5) 0.6738(4) 0.0584(17) Uani 1 1 d . . . H39A H 0.2056 0.8560 0.7151 0.070 Uiso 1 1 calc R . . C48 C 0.1828(5) 0.6953(5) 0.5887(4) 0.0465(14) Uani 1 1 d . . . H38A H 0.1027 0.6603 0.5715 0.056 Uiso 1 1 calc R . . C49 C -0.1509(10) 0.0092(13) -0.5550(9) 0.081(3) Uani 0.567(4) 1 d PD A 1 H49A H -0.1604 -0.0719 -0.6031 0.097 Uiso 0.567(4) 1 d PR A 1 Cl1 Cl -0.0642(3) 0.0970(4) -0.5992(3) 0.1001(11) Uani 0.567(4) 1 d PD A 1 Cl2 Cl -0.2862(3) -0.0033(5) -0.5620(4) 0.1001(11) Uani 0.567(4) 1 d PD A 1 Cl3 Cl -0.0955(3) 0.0369(4) -0.4367(3) 0.1001(11) Uani 0.567(4) 1 d PD A 1 C50 C -0.2381(12) 0.0836(15) -0.4981(10) 0.081(3) Uani 0.433(4) 1 d PD A 2 H50A H -0.2297 0.1455 -0.5107 0.097 Uiso 0.433(4) 1 d PR A 2 Cl4 Cl -0.1189(7) 0.1613(8) -0.4020(5) 0.143(2) Uani 0.433(4) 1 d PD A 2 Cl5 Cl -0.3593(7) 0.0270(7) -0.4653(5) 0.143(2) Uani 0.433(4) 1 d PD A 2 Cl6 Cl -0.2228(7) -0.0289(7) -0.6124(5) 0.143(2) Uani 0.433(4) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0220(4) 0.0208(3) 0.0270(4) 0.0111(3) 0.0045(3) 0.0030(3) Mn2 0.0220(4) 0.0229(4) 0.0279(4) 0.0127(3) 0.0056(3) 0.0037(3) S1 0.0226(6) 0.0268(6) 0.0373(7) 0.0119(5) 0.0061(5) 0.0086(5) S2 0.0239(6) 0.0336(6) 0.0344(6) 0.0217(5) 0.0055(5) 0.0068(5) S3 0.0248(6) 0.0207(5) 0.0286(6) 0.0115(5) 0.0066(5) 0.0074(4) S4 0.0285(6) 0.0263(6) 0.0264(6) 0.0137(5) 0.0059(5) 0.0067(5) O1 0.051(2) 0.0188(16) 0.039(2) 0.0100(15) 0.0203(17) -0.0002(16) O2 0.0202(17) 0.057(2) 0.073(3) 0.054(2) 0.0114(17) 0.0067(16) O3 0.0230(16) 0.0228(16) 0.0274(17) 0.0059(13) 0.0049(13) -0.0005(13) O4 0.042(2) 0.0261(18) 0.037(2) -0.0029(15) -0.0127(16) 0.0147(16) C1 0.023(2) 0.026(2) 0.039(3) 0.017(2) 0.003(2) 0.0043(19) C2 0.023(2) 0.026(2) 0.040(3) 0.016(2) 0.004(2) 0.0072(19) C3 0.033(3) 0.025(2) 0.048(3) 0.016(2) -0.001(2) 0.011(2) C4 0.033(3) 0.027(3) 0.056(3) 0.025(3) 0.000(2) 0.007(2) C5 0.029(3) 0.035(3) 0.052(3) 0.030(3) 0.005(2) 0.010(2) C6 0.024(2) 0.030(2) 0.037(3) 0.021(2) 0.004(2) 0.008(2) C7 0.025(2) 0.024(2) 0.029(2) 0.014(2) 0.0056(19) 0.0032(19) C8 0.023(2) 0.028(2) 0.031(2) 0.019(2) 0.0068(19) 0.0051(19) C9 0.031(3) 0.029(2) 0.036(3) 0.021(2) 0.010(2) 0.008(2) C10 0.025(2) 0.025(2) 0.034(3) 0.015(2) 0.011(2) 0.0053(19) C11 0.025(2) 0.024(2) 0.030(2) 0.013(2) 0.0085(19) 0.0075(19) C12 0.025(2) 0.022(2) 0.027(2) 0.0130(19) 0.0077(19) 0.0072(18) C13 0.023(2) 0.023(2) 0.032(2) 0.016(2) 0.0026(19) 0.0088(19) C14 0.023(2) 0.021(2) 0.026(2) 0.0119(19) 0.0040(18) 0.0067(18) C15 0.022(2) 0.029(2) 0.036(3) 0.018(2) 0.003(2) 0.007(2) C16 0.024(2) 0.024(2) 0.033(3) 0.011(2) -0.003(2) 0.0017(19) C17 0.028(2) 0.025(2) 0.030(2) 0.011(2) 0.003(2) 0.006(2) C18 0.023(2) 0.027(2) 0.031(2) 0.015(2) 0.0038(19) 0.0074(19) C19 0.022(2) 0.023(2) 0.028(2) 0.007(2) 0.0080(19) 0.0032(19) C20 0.026(2) 0.023(2) 0.023(2) 0.0105(19) 0.0063(18) 0.0058(19) C21 0.029(2) 0.026(2) 0.029(2) 0.012(2) 0.005(2) 0.004(2) C22 0.034(3) 0.025(2) 0.027(2) 0.010(2) 0.009(2) 0.005(2) C23 0.029(2) 0.024(2) 0.035(3) 0.011(2) 0.012(2) 0.008(2) C24 0.024(2) 0.027(2) 0.031(2) 0.013(2) 0.0090(19) 0.0073(19) C25 0.039(3) 0.027(3) 0.071(4) 0.029(3) -0.004(3) 0.010(2) C26 0.129(7) 0.039(4) 0.075(5) 0.033(4) 0.011(5) 0.023(4) C27 0.134(8) 0.034(4) 0.104(7) 0.023(4) -0.005(6) 0.019(5) C28 0.067(5) 0.045(4) 0.140(8) 0.060(5) 0.001(5) 0.017(4) C29 0.041(4) 0.058(4) 0.137(7) 0.070(5) 0.018(4) 0.017(3) C30 0.042(3) 0.042(3) 0.088(5) 0.040(3) 0.015(3) 0.018(3) C31 0.023(2) 0.033(3) 0.038(3) 0.023(2) 0.008(2) 0.007(2) C32 0.035(3) 0.034(3) 0.039(3) 0.022(2) 0.012(2) 0.012(2) C33 0.034(3) 0.033(3) 0.050(3) 0.029(3) 0.003(2) 0.003(2) C34 0.025(3) 0.057(4) 0.067(4) 0.047(3) 0.016(3) 0.010(2) C35 0.041(3) 0.056(4) 0.060(4) 0.038(3) 0.030(3) 0.024(3) C36 0.039(3) 0.036(3) 0.057(3) 0.027(3) 0.021(3) 0.014(2) C37 0.029(3) 0.035(3) 0.026(2) 0.013(2) -0.002(2) 0.000(2) C38 0.028(3) 0.041(3) 0.042(3) 0.015(3) 0.005(2) 0.004(2) C39 0.027(3) 0.054(4) 0.052(4) 0.023(3) 0.004(2) 0.001(3) C40 0.035(3) 0.041(3) 0.045(3) 0.018(3) -0.006(3) -0.010(3) C41 0.052(3) 0.028(3) 0.035(3) 0.013(2) -0.003(3) 0.000(2) C42 0.034(3) 0.036(3) 0.035(3) 0.015(2) 0.003(2) 0.006(2) C43 0.044(3) 0.025(2) 0.027(2) 0.010(2) 0.007(2) 0.008(2) C44 0.044(3) 0.032(3) 0.041(3) 0.006(2) -0.002(3) 0.009(2) C45 0.057(4) 0.034(3) 0.048(4) 0.011(3) -0.003(3) 0.004(3) C46 0.080(5) 0.035(3) 0.035(3) 0.003(3) -0.001(3) 0.012(3) C47 0.085(5) 0.041(3) 0.035(3) 0.009(3) 0.020(3) 0.025(3) C48 0.055(3) 0.033(3) 0.040(3) 0.016(2) 0.019(3) 0.012(3) C49 0.089(8) 0.076(7) 0.037(5) 0.020(5) -0.008(5) 0.009(6) Cl1 0.0719(15) 0.125(2) 0.0942(18) 0.0730(17) 0.0079(12) 0.0136(13) Cl2 0.0719(15) 0.125(2) 0.0942(18) 0.0730(17) 0.0079(12) 0.0136(13) Cl3 0.0719(15) 0.125(2) 0.0942(18) 0.0730(17) 0.0079(12) 0.0136(13) C50 0.089(8) 0.076(7) 0.037(5) 0.020(5) -0.008(5) 0.009(6) Cl4 0.140(4) 0.145(4) 0.074(2) 0.020(2) 0.030(2) 0.041(3) Cl5 0.140(4) 0.145(4) 0.074(2) 0.020(2) 0.030(2) 0.041(3) Cl6 0.140(4) 0.145(4) 0.074(2) 0.020(2) 0.030(2) 0.041(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 Mn1 O1 2.097(3) . ? Mn1 O3 2.120(3) 2 ? Mn1 O4 2.128(3) . ? Mn1 O2 2.154(3) 2 ? Mn1 S3 2.6983(12) 2 ? Mn1 S1 2.7209(13) . ? Mn2 O3 2.110(3) 2 ? Mn2 O1 2.129(3) . ? Mn2 O2 2.130(3) . ? Mn2 O4 2.158(4) 2 ? Mn2 S2 2.6940(13) . ? Mn2 S4 2.7319(13) 2 ? S1 C24 1.778(5) . ? S1 C2 1.794(5) . ? S2 C8 1.778(5) . ? S2 C6 1.797(5) . ? S3 C14 1.786(4) . ? S3 C12 1.786(5) . ? S3 Mn1 2.6983(12) 2 ? S4 C20 1.780(5) . ? S4 C18 1.794(5) . ? S4 Mn2 2.7320(13) 2 ? O1 C1 1.314(6) . ? O2 C7 1.311(5) . ? O2 Mn1 2.154(3) 2 ? O3 C13 1.314(5) . ? O3 Mn2 2.110(3) 2 ? O3 Mn1 2.120(3) 2 ? O4 C19 1.311(5) . ? O4 Mn2 2.158(4) 2 ? C1 C6 1.399(7) . ? C1 C2 1.407(7) . ? C2 C3 1.390(7) . ? C3 C4 1.405(8) . ? C3 H3A 0.9500 . ? C4 C5 1.377(8) . ? C4 C25 1.495(7) . ? C5 C6 1.387(6) . ? C5 H5A 0.9500 . ? C7 C12 1.404(6) . ? C7 C8 1.414(6) . ? C8 C9 1.391(6) . ? C9 C10 1.387(7) . ? C9 H9A 0.9500 . ? C10 C11 1.393(7) . ? C10 C31 1.496(6) . ? C11 C12 1.392(6) . ? C11 H11A 0.9500 . ? C13 C14 1.406(6) . ? C13 C18 1.406(6) . ? C14 C15 1.389(6) . ? C15 C16 1.383(7) . ? C15 H23A 0.9500 . ? C16 C17 1.392(7) . ? C16 C37 1.494(6) . ? C17 C18 1.381(6) . ? C17 H21A 0.9500 . ? C19 C24 1.412(7) . ? C19 C20 1.413(7) . ? C20 C21 1.391(6) . ? C21 C22 1.387(7) . ? C21 H17A 0.9500 . ? C22 C23 1.392(7) . ? C22 C43 1.491(6) . ? C23 C24 1.395(6) . ? C23 H15A 0.9500 . ? C25 C26 1.370(10) . ? C25 C30 1.399(9) . ? C26 C27 1.400(10) . ? C26 H26A 0.9500 . ? C27 C28 1.364(13) . ? C27 H27A 0.9500 . ? C28 C29 1.342(11) . ? C28 H28A 0.9500 . ? C29 C30 1.380(8) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.382(7) . ? C31 C32 1.388(7) . ? C32 C33 1.391(7) . ? C32 H32A 0.9500 . ? C33 C34 1.365(8) . ? C33 H33A 0.9500 . ? C34 C35 1.380(8) . ? C34 H34A 0.9500 . ? C35 C36 1.386(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.383(7) . ? C37 C42 1.388(7) . ? C38 C39 1.398(7) . ? C38 H48A 0.9500 . ? C39 C40 1.371(9) . ? C39 H47A 0.9500 . ? C40 C41 1.388(9) . ? C40 H46A 0.9500 . ? C41 C42 1.388(7) . ? C41 H45A 0.9500 . ? C42 H44A 0.9500 . ? C43 C48 1.383(8) . ? C43 C44 1.390(8) . ? C44 C45 1.399(8) . ? C44 H42A 0.9500 . ? C45 C46 1.373(9) . ? C45 H41A 0.9500 . ? C46 C47 1.397(10) . ? C46 H40A 0.9500 . ? C47 C48 1.397(8) . ? C47 H39A 0.9500 . ? C48 H38A 0.9500 . ? C49 Cl1 1.685(11) . ? C49 Cl3 1.722(11) . ? C49 Cl2 1.726(13) . ? C49 H49A 0.9600 . ? Cl2 H50A 1.6287 . ? C50 Cl5 1.669(14) . ? C50 Cl4 1.716(14) . ? C50 Cl6 1.781(14) . ? C50 H50A 0.9126 . ? Cl6 H49A 1.2214 . ? 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 O3 70.35(12) . 2 ? O1 Mn1 O4 90.13(16) . . ? O3 Mn1 O4 133.20(13) 2 . ? O1 Mn1 O2 129.83(15) . 2 ? O3 Mn1 O2 88.89(14) 2 2 ? O4 Mn1 O2 71.33(14) . 2 ? O1 Mn1 S3 136.22(12) . 2 ? O3 Mn1 S3 76.05(9) 2 2 ? O4 Mn1 S3 133.63(12) . 2 ? O2 Mn1 S3 75.30(9) 2 2 ? O1 Mn1 S1 75.93(9) . . ? O3 Mn1 S1 134.25(10) 2 . ? O4 Mn1 S1 75.37(10) . . ? O2 Mn1 S1 136.82(12) 2 . ? S3 Mn1 S1 111.49(4) 2 . ? O3 Mn2 O1 69.93(12) 2 . ? O3 Mn2 O2 134.40(14) 2 . ? O1 Mn2 O2 90.00(16) . . ? O3 Mn2 O4 94.20(14) 2 2 ? O1 Mn2 O4 134.98(15) . 2 ? O2 Mn2 O4 71.22(14) . 2 ? O3 Mn2 S2 132.55(10) 2 . ? O1 Mn2 S2 75.65(9) . . ? O2 Mn2 S2 75.54(9) . . ? O4 Mn2 S2 133.19(11) 2 . ? O3 Mn2 S4 74.88(9) 2 2 ? O1 Mn2 S4 134.56(12) . 2 ? O2 Mn2 S4 135.43(12) . 2 ? O4 Mn2 S4 74.35(9) 2 2 ? S2 Mn2 S4 110.89(4) . 2 ? C24 S1 C2 101.9(2) . . ? C24 S1 Mn1 95.21(15) . . ? C2 S1 Mn1 95.00(16) . . ? C8 S2 C6 102.1(2) . . ? C8 S2 Mn2 95.50(15) . . ? C6 S2 Mn2 95.88(15) . . ? C14 S3 C12 100.4(2) . . ? C14 S3 Mn1 95.39(14) . 2 ? C12 S3 Mn1 95.28(15) . 2 ? C20 S4 C18 100.3(2) . . ? C20 S4 Mn2 96.01(15) . 2 ? C18 S4 Mn2 95.38(15) . 2 ? C1 O1 Mn1 128.1(3) . . ? C1 O1 Mn2 127.9(3) . . ? Mn1 O1 Mn2 103.61(13) . . ? C7 O2 Mn2 126.3(3) . . ? C7 O2 Mn1 125.6(3) . 2 ? Mn2 O2 Mn1 103.27(13) . 2 ? C13 O3 Mn2 129.2(3) . 2 ? C13 O3 Mn1 127.3(3) . 2 ? Mn2 O3 Mn1 103.47(13) 2 2 ? C19 O4 Mn1 127.1(3) . . ? C19 O4 Mn2 128.1(3) . 2 ? Mn1 O4 Mn2 103.18(13) . 2 ? O1 C1 C6 121.5(4) . . ? O1 C1 C2 122.1(4) . . ? C6 C1 C2 116.4(4) . . ? C3 C2 C1 121.3(5) . . ? C3 C2 S1 119.8(4) . . ? C1 C2 S1 118.8(3) . . ? C2 C3 C4 120.9(5) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 117.8(4) . . ? C5 C4 C25 121.2(5) . . ? C3 C4 C25 121.0(5) . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C1 122.0(5) . . ? C5 C6 S2 119.1(4) . . ? C1 C6 S2 119.0(3) . . ? O2 C7 C12 121.9(4) . . ? O2 C7 C8 121.3(4) . . ? C12 C7 C8 116.8(4) . . ? C9 C8 C7 121.3(4) . . ? C9 C8 S2 119.7(4) . . ? C7 C8 S2 119.0(3) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 118.9(4) . . ? C9 C10 C31 120.8(4) . . ? C11 C10 C31 120.3(4) . . ? C12 C11 C10 120.5(4) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C7 121.6(4) . . ? C11 C12 S3 119.4(4) . . ? C7 C12 S3 118.9(3) . . ? O3 C13 C14 121.6(4) . . ? O3 C13 C18 121.3(4) . . ? C14 C13 C18 117.0(4) . . ? C15 C14 C13 120.9(4) . . ? C15 C14 S3 119.7(3) . . ? C13 C14 S3 119.3(3) . . ? C16 C15 C14 121.2(4) . . ? C16 C15 H23A 119.4 . . ? C14 C15 H23A 119.4 . . ? C15 C16 C17 118.1(4) . . ? C15 C16 C37 120.5(4) . . ? C17 C16 C37 121.3(4) . . ? C18 C17 C16 121.2(4) . . ? C18 C17 H21A 119.4 . . ? C16 C17 H21A 119.4 . . ? C17 C18 C13 121.1(4) . . ? C17 C18 S4 120.4(4) . . ? C13 C18 S4 118.6(3) . . ? O4 C19 C24 121.8(4) . . ? O4 C19 C20 121.0(4) . . ? C24 C19 C20 117.1(4) . . ? C21 C20 C19 121.2(4) . . ? C21 C20 S4 119.5(4) . . ? C19 C20 S4 119.2(3) . . ? C22 C21 C20 121.2(5) . . ? C22 C21 H17A 119.4 . . ? C20 C21 H17A 119.4 . . ? C21 C22 C23 118.3(4) . . ? C21 C22 C43 119.9(5) . . ? C23 C22 C43 121.7(5) . . ? C22 C23 C24 121.4(5) . . ? C22 C23 H15A 119.3 . . ? C24 C23 H15A 119.3 . . ? C23 C24 C19 120.7(4) . . ? C23 C24 S1 120.2(4) . . ? C19 C24 S1 119.1(3) . . ? C26 C25 C30 116.4(5) . . ? C26 C25 C4 122.6(6) . . ? C30 C25 C4 120.9(6) . . ? C25 C26 C27 121.4(8) . . ? C25 C26 H26A 119.3 . . ? C27 C26 H26A 119.3 . . ? C28 C27 C26 120.2(9) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 C27 119.5(7) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C28 C29 C30 121.0(8) . . ? C28 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? C29 C30 C25 121.4(7) . . ? C29 C30 H30A 119.3 . . ? C25 C30 H30A 119.3 . . ? C36 C31 C32 119.0(4) . . ? C36 C31 C10 120.5(4) . . ? C32 C31 C10 120.6(4) . . ? C31 C32 C33 120.0(5) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.2(5) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C35 120.5(5) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C34 C35 C36 119.3(5) . . ? C34 C35 H35A 120.3 . . ? C36 C35 H35A 120.3 . . ? C31 C36 C35 120.9(5) . . ? C31 C36 H36A 119.6 . . ? C35 C36 H36A 119.6 . . ? C38 C37 C42 119.2(5) . . ? C38 C37 C16 121.0(5) . . ? C42 C37 C16 119.7(5) . . ? C37 C38 C39 120.7(6) . . ? C37 C38 H48A 119.6 . . ? C39 C38 H48A 119.6 . . ? C40 C39 C38 119.4(6) . . ? C40 C39 H47A 120.3 . . ? C38 C39 H47A 120.3 . . ? C39 C40 C41 120.7(5) . . ? C39 C40 H46A 119.7 . . ? C41 C40 H46A 119.7 . . ? C42 C41 C40 119.7(5) . . ? C42 C41 H45A 120.2 . . ? C40 C41 H45A 120.2 . . ? C41 C42 C37 120.4(5) . . ? C41 C42 H44A 119.8 . . ? C37 C42 H44A 119.8 . . ? C48 C43 C44 118.8(5) . . ? C48 C43 C22 121.7(5) . . ? C44 C43 C22 119.5(5) . . ? C43 C44 C45 121.4(6) . . ? C43 C44 H42A 119.3 . . ? C45 C44 H42A 119.3 . . ? C46 C45 C44 119.5(6) . . ? C46 C45 H41A 120.2 . . ? C44 C45 H41A 120.2 . . ? C45 C46 C47 119.6(5) . . ? C45 C46 H40A 120.2 . . ? C47 C46 H40A 120.2 . . ? C46 C47 C48 120.5(6) . . ? C46 C47 H39A 119.8 . . ? C48 C47 H39A 119.8 . . ? C43 C48 C47 120.2(6) . . ? C43 C48 H38A 119.9 . . ? C47 C48 H38A 119.9 . . ? Cl1 C49 Cl3 115.5(7) . . ? Cl1 C49 Cl2 115.9(8) . . ? Cl3 C49 Cl2 111.1(7) . . ? Cl1 C49 H49A 103.4 . . ? Cl3 C49 H49A 105.0 . . ? Cl2 C49 H49A 104.4 . . ? C49 Cl2 H50A 87.4 . . ? Cl5 C50 Cl4 115.1(9) . . ? Cl5 C50 Cl6 112.8(9) . . ? Cl4 C50 Cl6 110.2(9) . . ? Cl5 C50 H50A 113.8 . . ? Cl4 C50 H50A 98.4 . . ? Cl6 C50 H50A 105.2 . . ? C50 Cl6 H49A 118.0 . . ? 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 O1 Mn1 S1 C24 -102.69(19) . . . . ? O3 Mn1 S1 C24 -145.97(19) 2 . . . ? O4 Mn1 S1 C24 -8.80(18) . . . . ? O2 Mn1 S1 C24 31.6(2) 2 . . . ? S3 Mn1 S1 C24 122.77(15) 2 . . . ? O1 Mn1 S1 C2 -0.2(2) . . . . ? O3 Mn1 S1 C2 -43.5(2) 2 . . . ? O4 Mn1 S1 C2 93.65(19) . . . . ? O2 Mn1 S1 C2 134.0(2) 2 . . . ? S3 Mn1 S1 C2 -134.77(16) 2 . . . ? O3 Mn2 S2 C8 148.26(19) 2 . . . ? O1 Mn2 S2 C8 104.0(2) . . . . ? O2 Mn2 S2 C8 10.18(19) . . . . ? O4 Mn2 S2 C8 -35.6(2) 2 . . . ? S4 Mn2 S2 C8 -123.38(16) 2 . . . ? O3 Mn2 S2 C6 45.4(2) 2 . . . ? O1 Mn2 S2 C6 1.13(19) . . . . ? O2 Mn2 S2 C6 -92.65(19) . . . . ? O4 Mn2 S2 C6 -138.4(2) 2 . . . ? S4 Mn2 S2 C6 133.79(16) 2 . . . ? O3 Mn1 O1 C1 146.5(5) 2 . . . ? O4 Mn1 O1 C1 -77.0(4) . . . . ? O2 Mn1 O1 C1 -142.4(4) 2 . . . ? S3 Mn1 O1 C1 104.4(4) 2 . . . ? S1 Mn1 O1 C1 -2.1(4) . . . . ? O3 Mn1 O1 Mn2 -26.90(15) 2 . . . ? O4 Mn1 O1 Mn2 109.66(17) . . . . ? O2 Mn1 O1 Mn2 44.2(3) 2 . . . ? S3 Mn1 O1 Mn2 -68.9(2) 2 . . . ? S1 Mn1 O1 Mn2 -175.47(18) . . . . ? O3 Mn2 O1 C1 -146.3(5) 2 . . . ? O2 Mn2 O1 C1 75.6(4) . . . . ? O4 Mn2 O1 C1 138.5(4) 2 . . . ? S2 Mn2 O1 C1 0.5(4) . . . . ? S4 Mn2 O1 C1 -104.8(4) 2 . . . ? O3 Mn2 O1 Mn1 27.11(15) 2 . . . ? O2 Mn2 O1 Mn1 -111.04(17) . . . . ? O4 Mn2 O1 Mn1 -48.1(3) 2 . . . ? S2 Mn2 O1 Mn1 173.90(18) . . . . ? S4 Mn2 O1 Mn1 68.6(2) 2 . . . ? O3 Mn2 O2 C7 -151.7(4) 2 . . . ? O1 Mn2 O2 C7 -90.4(4) . . . . ? O4 Mn2 O2 C7 131.3(4) 2 . . . ? S2 Mn2 O2 C7 -15.3(4) . . . . ? S4 Mn2 O2 C7 90.0(4) 2 . . . ? O3 Mn2 O2 Mn1 52.0(3) 2 . . 2 ? O1 Mn2 O2 Mn1 113.28(17) . . . 2 ? O4 Mn2 O2 Mn1 -25.02(16) 2 . . 2 ? S2 Mn2 O2 Mn1 -171.56(17) . . . 2 ? S4 Mn2 O2 Mn1 -66.3(2) 2 . . 2 ? O1 Mn1 O4 C19 86.4(4) . . . . ? O3 Mn1 O4 C19 149.0(3) 2 . . . ? O2 Mn1 O4 C19 -141.1(4) 2 . . . ? S3 Mn1 O4 C19 -95.0(4) 2 . . . ? S1 Mn1 O4 C19 11.0(4) . . . . ? O1 Mn1 O4 Mn2 -107.46(17) . . . 2 ? O3 Mn1 O4 Mn2 -44.8(3) 2 . . 2 ? O2 Mn1 O4 Mn2 25.02(15) 2 . . 2 ? S3 Mn1 O4 Mn2 71.21(19) 2 . . 2 ? S1 Mn1 O4 Mn2 177.12(17) . . . 2 ? Mn1 O1 C1 C6 -174.5(3) . . . . ? Mn2 O1 C1 C6 -2.7(7) . . . . ? Mn1 O1 C1 C2 4.5(7) . . . . ? Mn2 O1 C1 C2 176.3(3) . . . . ? O1 C1 C2 C3 178.0(5) . . . . ? C6 C1 C2 C3 -2.9(7) . . . . ? O1 C1 C2 S1 -4.4(7) . . . . ? C6 C1 C2 S1 174.7(4) . . . . ? C24 S1 C2 C3 -83.7(4) . . . . ? Mn1 S1 C2 C3 179.9(4) . . . . ? C24 S1 C2 C1 98.7(4) . . . . ? Mn1 S1 C2 C1 2.3(4) . . . . ? C1 C2 C3 C4 -1.1(8) . . . . ? S1 C2 C3 C4 -178.7(4) . . . . ? C2 C3 C4 C5 3.6(7) . . . . ? C2 C3 C4 C25 -176.8(5) . . . . ? C3 C4 C5 C6 -1.9(7) . . . . ? C25 C4 C5 C6 178.4(5) . . . . ? C4 C5 C6 C1 -2.3(8) . . . . ? C4 C5 C6 S2 177.5(4) . . . . ? O1 C1 C6 C5 -176.3(5) . . . . ? C2 C1 C6 C5 4.6(7) . . . . ? O1 C1 C6 S2 3.9(7) . . . . ? C2 C1 C6 S2 -175.2(3) . . . . ? C8 S2 C6 C5 80.4(4) . . . . ? Mn2 S2 C6 C5 177.3(4) . . . . ? C8 S2 C6 C1 -99.7(4) . . . . ? Mn2 S2 C6 C1 -2.8(4) . . . . ? Mn2 O2 C7 C12 -164.7(3) . . . . ? Mn1 O2 C7 C12 -13.5(6) 2 . . . ? Mn2 O2 C7 C8 15.1(7) . . . . ? Mn1 O2 C7 C8 166.3(3) 2 . . . ? O2 C7 C8 C9 179.1(4) . . . . ? C12 C7 C8 C9 -1.0(7) . . . . ? O2 C7 C8 S2 -1.1(6) . . . . ? C12 C7 C8 S2 178.7(3) . . . . ? C6 S2 C8 C9 -91.3(4) . . . . ? Mn2 S2 C8 C9 171.4(4) . . . . ? C6 S2 C8 C7 88.9(4) . . . . ? Mn2 S2 C8 C7 -8.3(4) . . . . ? C7 C8 C9 C10 2.2(7) . . . . ? S2 C8 C9 C10 -177.5(4) . . . . ? C8 C9 C10 C11 -1.3(7) . . . . ? C8 C9 C10 C31 178.9(4) . . . . ? C9 C10 C11 C12 -0.8(7) . . . . ? C31 C10 C11 C12 179.0(4) . . . . ? C10 C11 C12 C7 2.0(7) . . . . ? C10 C11 C12 S3 -176.0(3) . . . . ? O2 C7 C12 C11 178.8(4) . . . . ? C8 C7 C12 C11 -1.1(7) . . . . ? O2 C7 C12 S3 -3.2(6) . . . . ? C8 C7 C12 S3 176.9(3) . . . . ? C14 S3 C12 C11 94.1(4) . . . . ? Mn1 S3 C12 C11 -169.4(3) 2 . . . ? C14 S3 C12 C7 -84.0(4) . . . . ? Mn1 S3 C12 C7 12.5(4) 2 . . . ? Mn2 O3 C13 C14 -179.1(3) 2 . . . ? Mn1 O3 C13 C14 -3.2(6) 2 . . . ? Mn2 O3 C13 C18 2.4(6) 2 . . . ? Mn1 O3 C13 C18 178.3(3) 2 . . . ? O3 C13 C14 C15 175.8(4) . . . . ? C18 C13 C14 C15 -5.6(6) . . . . ? O3 C13 C14 S3 -2.2(6) . . . . ? C18 C13 C14 S3 176.4(3) . . . . ? C12 S3 C14 C15 -77.1(4) . . . . ? Mn1 S3 C14 C15 -173.5(4) 2 . . . ? C12 S3 C14 C13 101.0(4) . . . . ? Mn1 S3 C14 C13 4.6(4) 2 . . . ? C13 C14 C15 C16 0.0(7) . . . . ? S3 C14 C15 C16 178.0(4) . . . . ? C14 C15 C16 C17 4.7(7) . . . . ? C14 C15 C16 C37 -172.3(4) . . . . ? C15 C16 C17 C18 -3.7(7) . . . . ? C37 C16 C17 C18 173.3(5) . . . . ? C16 C17 C18 C13 -2.1(7) . . . . ? C16 C17 C18 S4 177.5(4) . . . . ? O3 C13 C18 C17 -174.8(4) . . . . ? C14 C13 C18 C17 6.6(7) . . . . ? O3 C13 C18 S4 5.6(6) . . . . ? C14 C13 C18 S4 -173.0(3) . . . . ? C20 S4 C18 C17 75.4(4) . . . . ? Mn2 S4 C18 C17 172.5(4) 2 . . . ? C20 S4 C18 C13 -105.0(4) . . . . ? Mn2 S4 C18 C13 -7.9(4) 2 . . . ? Mn1 O4 C19 C24 -8.6(6) . . . . ? Mn2 O4 C19 C24 -171.4(3) 2 . . . ? Mn1 O4 C19 C20 171.5(3) . . . . ? Mn2 O4 C19 C20 8.8(6) 2 . . . ? O4 C19 C20 C21 -179.9(4) . . . . ? C24 C19 C20 C21 0.3(6) . . . . ? O4 C19 C20 S4 2.5(6) . . . . ? C24 C19 C20 S4 -177.4(3) . . . . ? C18 S4 C20 C21 -89.4(4) . . . . ? Mn2 S4 C20 C21 174.0(3) 2 . . . ? C18 S4 C20 C19 88.3(4) . . . . ? Mn2 S4 C20 C19 -8.3(4) 2 . . . ? C19 C20 C21 C22 -0.4(7) . . . . ? S4 C20 C21 C22 177.3(4) . . . . ? C20 C21 C22 C23 1.0(7) . . . . ? C20 C21 C22 C43 -176.1(4) . . . . ? C21 C22 C23 C24 -1.6(7) . . . . ? C43 C22 C23 C24 175.4(4) . . . . ? C22 C23 C24 C19 1.6(7) . . . . ? C22 C23 C24 S1 -175.8(4) . . . . ? O4 C19 C24 C23 179.3(4) . . . . ? C20 C19 C24 C23 -0.9(6) . . . . ? O4 C19 C24 S1 -3.3(6) . . . . ? C20 C19 C24 S1 176.6(3) . . . . ? C2 S1 C24 C23 90.3(4) . . . . ? Mn1 S1 C24 C23 -173.4(4) . . . . ? C2 S1 C24 C19 -87.1(4) . . . . ? Mn1 S1 C24 C19 9.1(4) . . . . ? C5 C4 C25 C26 -168.5(6) . . . . ? C3 C4 C25 C26 11.9(9) . . . . ? C5 C4 C25 C30 8.3(8) . . . . ? C3 C4 C25 C30 -171.4(5) . . . . ? C30 C25 C26 C27 -0.5(12) . . . . ? C4 C25 C26 C27 176.4(8) . . . . ? C25 C26 C27 C28 -0.7(15) . . . . ? C26 C27 C28 C29 1.8(14) . . . . ? C27 C28 C29 C30 -1.6(12) . . . . ? C28 C29 C30 C25 0.3(10) . . . . ? C26 C25 C30 C29 0.7(9) . . . . ? C4 C25 C30 C29 -176.3(5) . . . . ? C9 C10 C31 C36 -118.0(6) . . . . ? C11 C10 C31 C36 62.1(7) . . . . ? C9 C10 C31 C32 61.1(7) . . . . ? C11 C10 C31 C32 -118.7(5) . . . . ? C36 C31 C32 C33 -1.1(8) . . . . ? C10 C31 C32 C33 179.7(5) . . . . ? C31 C32 C33 C34 2.2(8) . . . . ? C32 C33 C34 C35 -1.5(8) . . . . ? C33 C34 C35 C36 -0.2(9) . . . . ? C32 C31 C36 C35 -0.6(8) . . . . ? C10 C31 C36 C35 178.6(5) . . . . ? C34 C35 C36 C31 1.3(9) . . . . ? C15 C16 C37 C38 -42.2(7) . . . . ? C17 C16 C37 C38 140.9(5) . . . . ? C15 C16 C37 C42 133.5(5) . . . . ? C17 C16 C37 C42 -43.4(7) . . . . ? C42 C37 C38 C39 0.9(8) . . . . ? C16 C37 C38 C39 176.7(5) . . . . ? C37 C38 C39 C40 -0.7(9) . . . . ? C38 C39 C40 C41 0.7(9) . . . . ? C39 C40 C41 C42 -1.0(9) . . . . ? C40 C41 C42 C37 1.2(8) . . . . ? C38 C37 C42 C41 -1.2(8) . . . . ? C16 C37 C42 C41 -177.0(5) . . . . ? C21 C22 C43 C48 -135.7(5) . . . . ? C23 C22 C43 C48 47.3(7) . . . . ? C21 C22 C43 C44 43.9(7) . . . . ? C23 C22 C43 C44 -133.1(5) . . . . ? C48 C43 C44 C45 -0.6(9) . . . . ? C22 C43 C44 C45 179.8(5) . . . . ? C43 C44 C45 C46 1.0(10) . . . . ? C44 C45 C46 C47 -0.2(10) . . . . ? C45 C46 C47 C48 -1.0(10) . . . . ? C44 C43 C48 C47 -0.6(8) . . . . ? C22 C43 C48 C47 179.0(5) . . . . ? C46 C47 C48 C43 1.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.631 _refine_diff_density_min -1.709 _refine_diff_density_rms 0.100 ###END data_compound_746728 _database_code_depnum_ccdc_archive 'CCDC 746728' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Mn4(C48H28O4S4)2 _chemical_melting_point ? _chemical_formula_moiety Mn4(C48H56O4S4)2 _chemical_formula_sum 'C96 H56 Mn4 O8 S8' _chemical_formula_weight 1813.65 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number No.14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1007(8) _cell_length_b 21.8774(11) _cell_length_c 23.9036(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.0050(10) _cell_angle_gamma 90.00 _cell_volume 7799.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8766 _cell_measurement_theta_min 2.3889 _cell_measurement_theta_max 25.9644 _exptl_crystal_description sheet _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8045 _exptl_absorpt_correction_T_max 0.9308 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39674 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13720 _reflns_number_gt 8381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13720 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.29765(4) 0.20522(3) 0.27284(3) 0.02529(18) Uani 1 1 d . . . Mn2 Mn 0.24261(4) 0.08724(3) 0.34713(3) 0.02445(18) Uani 1 1 d . . . Mn3 Mn 0.21376(4) 0.00272(3) 0.23057(3) 0.02520(18) Uani 1 1 d . . . Mn4 Mn 0.26866(4) 0.12156(3) 0.15726(3) 0.02508(18) Uani 1 1 d . . . S1 S 0.09216(8) 0.10695(5) 0.39389(5) 0.0272(3) Uani 1 1 d . . . S2 S 0.04366(8) -0.03537(5) 0.20170(5) 0.0277(3) Uani 1 1 d . . . S3 S 0.13115(8) 0.16249(5) 0.07794(5) 0.0276(3) Uani 1 1 d . . . S4 S 0.19277(8) 0.30248(5) 0.27294(5) 0.0271(3) Uani 1 1 d . . . S5 S 0.37399(8) 0.04867(5) 0.42753(5) 0.0272(3) Uani 1 1 d . . . S6 S 0.32804(7) -0.09277(5) 0.23446(5) 0.0265(3) Uani 1 1 d . . . S7 S 0.42528(8) 0.10538(5) 0.11312(5) 0.0263(3) Uani 1 1 d . . . S8 S 0.46046(8) 0.24724(5) 0.30495(5) 0.0262(3) Uani 1 1 d . . . O1 O 0.20929(19) 0.17912(13) 0.32838(12) 0.0285(8) Uani 1 1 d . . . O2 O 0.13773(18) 0.05477(14) 0.28407(12) 0.0293(8) Uani 1 1 d . . . O3 O 0.16459(19) 0.05659(13) 0.15874(12) 0.0278(7) Uani 1 1 d . . . O4 O 0.19619(19) 0.18732(13) 0.20151(12) 0.0271(7) Uani 1 1 d . . . O5 O 0.36172(18) 0.13166(13) 0.32605(12) 0.0261(7) Uani 1 1 d . . . O6 O 0.28430(19) 0.00354(13) 0.31448(12) 0.0280(7) Uani 1 1 d . . . O7 O 0.32808(18) 0.03964(13) 0.19765(13) 0.0280(7) Uani 1 1 d . . . O8 O 0.36425(18) 0.17820(13) 0.20490(12) 0.0273(7) Uani 1 1 d . . . C1 C 0.1387(3) 0.2097(2) 0.33857(19) 0.0248(11) Uani 1 1 d . . . C2 C 0.1219(3) 0.2699(2) 0.31851(18) 0.0232(10) Uani 1 1 d . . . C3 C 0.0541(3) 0.3038(2) 0.33541(19) 0.0280(11) Uani 1 1 d . . . H3A H 0.0465 0.3451 0.3231 0.034 Uiso 1 1 calc R . . C4 C -0.0036(3) 0.2801(2) 0.3699(2) 0.0298(11) Uani 1 1 d . . . C5 C 0.0084(3) 0.2197(2) 0.38657(19) 0.0288(11) Uani 1 1 d . . . H5A H -0.0319 0.2017 0.4086 0.035 Uiso 1 1 calc R . . C6 C 0.0782(3) 0.1847(2) 0.37186(19) 0.0262(11) Uani 1 1 d . . . C7 C 0.0562(3) 0.0427(2) 0.29284(19) 0.0264(11) Uani 1 1 d . . . C8 C 0.0203(3) 0.0674(2) 0.33923(19) 0.0265(11) Uani 1 1 d . . . C9 C -0.0697(3) 0.0593(2) 0.3435(2) 0.0299(11) Uani 1 1 d . . . H9A H -0.0927 0.0776 0.3743 0.036 Uiso 1 1 calc R . . C10 C -0.1271(3) 0.0256(2) 0.3042(2) 0.0341(12) Uani 1 1 d . . . C11 C -0.0895(3) -0.0043(2) 0.2625(2) 0.0300(11) Uani 1 1 d . . . H11A H -0.1258 -0.0309 0.2371 0.036 Uiso 1 1 calc R . . C12 C -0.0009(3) 0.0035(2) 0.25692(19) 0.0263(11) Uani 1 1 d . . . C13 C 0.0804(3) 0.0611(2) 0.13366(19) 0.0256(11) Uani 1 1 d . . . C14 C 0.0157(3) 0.0190(2) 0.14561(19) 0.0259(11) Uani 1 1 d . . . C15 C -0.0708(3) 0.0206(2) 0.11697(19) 0.0302(11) Uani 1 1 d . . . H15A H -0.1120 -0.0100 0.1245 0.036 Uiso 1 1 calc R . . C16 C -0.0997(3) 0.0660(2) 0.0772(2) 0.0315(12) Uani 1 1 d . . . C17 C -0.0365(3) 0.1092(2) 0.06687(18) 0.0281(11) Uani 1 1 d . . . H17A H -0.0540 0.1412 0.0406 0.034 Uiso 1 1 calc R . . C18 C 0.0514(3) 0.1066(2) 0.09410(19) 0.0283(11) Uani 1 1 d . . . C19 C 0.1474(3) 0.2323(2) 0.1750(2) 0.0271(11) Uani 1 1 d . . . C20 C 0.1075(3) 0.2277(2) 0.11861(19) 0.0268(11) Uani 1 1 d . . . C21 C 0.0551(3) 0.2747(2) 0.0916(2) 0.0298(11) Uani 1 1 d . . . H21A H 0.0296 0.2703 0.0529 0.036 Uiso 1 1 calc R . . C22 C 0.0396(3) 0.3279(2) 0.1204(2) 0.0295(11) Uani 1 1 d . . . C23 C 0.0797(3) 0.3333(2) 0.17607(19) 0.0275(11) Uani 1 1 d . . . H23A H 0.0697 0.3695 0.1962 0.033 Uiso 1 1 calc R . . C24 C 0.1340(3) 0.2883(2) 0.20379(18) 0.0227(10) Uani 1 1 d . . . C25 C 0.4291(3) 0.1447(2) 0.36594(19) 0.0229(10) Uani 1 1 d . . . C26 C 0.4866(3) 0.1944(2) 0.36167(19) 0.0252(11) Uani 1 1 d . . . C27 C 0.5596(3) 0.2065(2) 0.40336(19) 0.0285(11) Uani 1 1 d . . . H27A H 0.5978 0.2399 0.3984 0.034 Uiso 1 1 calc R . . C28 C 0.5782(3) 0.1711(2) 0.4518(2) 0.0312(12) Uani 1 1 d . . . C29 C 0.5202(3) 0.1228(2) 0.45769(19) 0.0307(12) Uani 1 1 d . . . H29A H 0.5303 0.0984 0.4910 0.037 Uiso 1 1 calc R . . C30 C 0.4481(3) 0.1096(2) 0.41609(19) 0.0238(10) Uani 1 1 d . . . C31 C 0.3581(3) -0.0261(2) 0.33367(19) 0.0241(11) Uani 1 1 d . . . C32 C 0.4101(3) -0.0115(2) 0.38548(19) 0.0268(11) Uani 1 1 d . . . C33 C 0.4876(3) -0.0438(2) 0.4066(2) 0.0293(11) Uani 1 1 d . . . H33A H 0.5222 -0.0319 0.4416 0.035 Uiso 1 1 calc R . . C34 C 0.5152(3) -0.0940(2) 0.3767(2) 0.0316(12) Uani 1 1 d . . . C35 C 0.4633(3) -0.1092(2) 0.3254(2) 0.0307(12) Uani 1 1 d . . . H35A H 0.4795 -0.1438 0.3053 0.037 Uiso 1 1 calc R . . C36 C 0.3882(3) -0.0754(2) 0.30262(19) 0.0251(11) Uani 1 1 d . . . C37 C 0.3864(3) 0.0055(2) 0.17639(18) 0.0238(10) Uani 1 1 d . . . C38 C 0.3977(3) -0.0575(2) 0.18963(18) 0.0243(10) Uani 1 1 d . . . C39 C 0.4594(3) -0.0928(2) 0.16772(19) 0.0275(11) Uani 1 1 d . . . H39A H 0.4636 -0.1351 0.1768 0.033 Uiso 1 1 calc R . . C40 C 0.5160(3) -0.0686(2) 0.13258(19) 0.0287(11) Uani 1 1 d . . . C41 C 0.5062(3) -0.0066(2) 0.11901(19) 0.0276(11) Uani 1 1 d . . . H41A H 0.5446 0.0116 0.0958 0.033 Uiso 1 1 calc R . . C42 C 0.4418(3) 0.0288(2) 0.13878(18) 0.0252(11) Uani 1 1 d . . . C43 C 0.4515(3) 0.17866(19) 0.20708(19) 0.0237(10) Uani 1 1 d . . . C44 C 0.4941(3) 0.14855(19) 0.16691(18) 0.0241(11) Uani 1 1 d . . . C45 C 0.5872(3) 0.1524(2) 0.16801(19) 0.0273(11) Uani 1 1 d . . . H45A H 0.6135 0.1317 0.1398 0.033 Uiso 1 1 calc R . . C46 C 0.6419(3) 0.1858(2) 0.2096(2) 0.0289(11) Uani 1 1 d . . . C47 C 0.5999(3) 0.2150(2) 0.25065(19) 0.0283(11) Uani 1 1 d . . . H47A H 0.6351 0.2381 0.2796 0.034 Uiso 1 1 calc R . . C48 C 0.5078(3) 0.21088(19) 0.24978(18) 0.0238(10) Uani 1 1 d . . . C49 C -0.0767(3) 0.3182(2) 0.38559(19) 0.0302(11) Uani 1 1 d . . . C50 C -0.0595(3) 0.3763(2) 0.4078(2) 0.0372(13) Uani 1 1 d . . . H50A H 0.0005 0.3908 0.4155 0.045 Uiso 1 1 calc R . . C51 C -0.1292(4) 0.4135(2) 0.4190(2) 0.0400(13) Uani 1 1 d . . . H51A H -0.1170 0.4535 0.4335 0.048 Uiso 1 1 calc R . . C52 C -0.2147(4) 0.3926(2) 0.4094(2) 0.0414(14) Uani 1 1 d . . . H52A H -0.2623 0.4182 0.4169 0.050 Uiso 1 1 calc R . . C53 C -0.2330(3) 0.3345(3) 0.3886(2) 0.0446(14) Uani 1 1 d . . . H53A H -0.2930 0.3200 0.3823 0.054 Uiso 1 1 calc R . . C54 C -0.1643(3) 0.2974(2) 0.3768(2) 0.0396(13) Uani 1 1 d . . . H54A H -0.1773 0.2574 0.3625 0.047 Uiso 1 1 calc R . . C55 C -0.2250(3) 0.0238(2) 0.3049(2) 0.0375(13) Uani 1 1 d . . . C56 C -0.2676(4) 0.0676(3) 0.3295(3) 0.073(2) Uani 1 1 d . . . H56A H -0.2332 0.0990 0.3499 0.088 Uiso 1 1 calc R . . C57 C -0.3599(4) 0.0685(3) 0.3261(4) 0.085(2) Uani 1 1 d . . . H57A H -0.3873 0.1004 0.3444 0.103 Uiso 1 1 calc R . . C58 C -0.4105(4) 0.0260(3) 0.2980(3) 0.0644(19) Uani 1 1 d . . . H58A H -0.4740 0.0286 0.2934 0.077 Uiso 1 1 calc R . . C59 C -0.3687(4) -0.0234(4) 0.2750(3) 0.100(3) Uani 1 1 d . . . H59A H -0.4038 -0.0557 0.2566 0.120 Uiso 1 1 calc R . . C60 C -0.2768(4) -0.0247(4) 0.2792(3) 0.076(2) Uani 1 1 d . . . H60A H -0.2484 -0.0586 0.2646 0.091 Uiso 1 1 calc R . . C61 C -0.1949(3) 0.0689(2) 0.05159(19) 0.0341(12) Uani 1 1 d . . . C62 C -0.2394(3) 0.0163(3) 0.0302(2) 0.0432(14) Uani 1 1 d . . . H62A H -0.2079 -0.0213 0.0305 0.052 Uiso 1 1 calc R . . C63 C -0.3309(4) 0.0187(3) 0.0081(2) 0.0487(15) Uani 1 1 d . . . H63A H -0.3617 -0.0174 -0.0061 0.058 Uiso 1 1 calc R . . C64 C -0.3755(4) 0.0726(3) 0.0069(2) 0.0564(17) Uani 1 1 d . . . H64A H -0.4377 0.0738 -0.0079 0.068 Uiso 1 1 calc R . . C65 C -0.3323(3) 0.1258(3) 0.0268(2) 0.0478(15) Uani 1 1 d . . . H65A H -0.3641 0.1634 0.0253 0.057 Uiso 1 1 calc R . . C66 C -0.2415(3) 0.1235(3) 0.0489(2) 0.0424(14) Uani 1 1 d . . . H66A H -0.2111 0.1600 0.0623 0.051 Uiso 1 1 calc R . . C67 C -0.0195(3) 0.3769(2) 0.0918(2) 0.0349(12) Uani 1 1 d . . . C68 C -0.0159(3) 0.3949(2) 0.0368(2) 0.0413(13) Uani 1 1 d . . . H68A H 0.0275 0.3769 0.0170 0.050 Uiso 1 1 calc R . . C69 C -0.0732(4) 0.4380(3) 0.0101(2) 0.0529(16) Uani 1 1 d . . . H69A H -0.0683 0.4506 -0.0273 0.063 Uiso 1 1 calc R . . C70 C -0.1384(4) 0.4631(2) 0.0380(3) 0.0541(16) Uani 1 1 d . . . H70A H -0.1794 0.4922 0.0192 0.065 Uiso 1 1 calc R . . C71 C -0.1440(4) 0.4460(2) 0.0933(2) 0.0447(14) Uani 1 1 d . . . H71A H -0.1887 0.4631 0.1126 0.054 Uiso 1 1 calc R . . C72 C -0.0835(3) 0.4038(2) 0.1197(2) 0.0378(13) Uani 1 1 d . . . H72A H -0.0857 0.3930 0.1580 0.045 Uiso 1 1 calc R . . C73 C 0.5962(3) -0.1293(2) 0.4023(2) 0.0378(13) Uani 1 1 d . . . C74 C 0.6712(3) -0.0997(3) 0.4301(2) 0.0499(15) Uani 1 1 d . . . H74A H 0.6731 -0.0563 0.4306 0.060 Uiso 1 1 calc R . . C75 C 0.7439(4) -0.1329(3) 0.4572(3) 0.0597(17) Uani 1 1 d . . . H75A H 0.7952 -0.1122 0.4764 0.072 Uiso 1 1 calc R . . C76 C 0.7415(4) -0.1953(3) 0.4564(3) 0.0615(18) Uani 1 1 d . . . H76A H 0.7910 -0.2180 0.4754 0.074 Uiso 1 1 calc R . . C77 C 0.6674(4) -0.2259(3) 0.4281(2) 0.0559(17) Uani 1 1 d . . . H77A H 0.6662 -0.2693 0.4272 0.067 Uiso 1 1 calc R . . C78 C 0.5956(4) -0.1928(2) 0.4011(2) 0.0465(14) Uani 1 1 d . . . H78A H 0.5450 -0.2136 0.3814 0.056 Uiso 1 1 calc R . . C79 C 0.5854(3) -0.1069(2) 0.11050(19) 0.0284(11) Uani 1 1 d . . . C80 C 0.5613(3) -0.1613(2) 0.0832(2) 0.0393(13) Uani 1 1 d . . . H80A H 0.5004 -0.1741 0.0779 0.047 Uiso 1 1 calc R . . C81 C 0.6252(4) -0.1974(2) 0.0635(2) 0.0493(15) Uani 1 1 d . . . H81A H 0.6079 -0.2346 0.0444 0.059 Uiso 1 1 calc R . . C82 C 0.7133(4) -0.1796(3) 0.0715(2) 0.0491(15) Uani 1 1 d . . . H82A H 0.7572 -0.2049 0.0587 0.059 Uiso 1 1 calc R . . C83 C 0.7376(4) -0.1259(2) 0.0976(2) 0.0449(14) Uani 1 1 d . . . H83A H 0.7983 -0.1130 0.1021 0.054 Uiso 1 1 calc R . . C84 C 0.6741(3) -0.0896(2) 0.1180(2) 0.0383(13) Uani 1 1 d . . . H84A H 0.6921 -0.0526 0.1373 0.046 Uiso 1 1 calc R . . C85 C 0.7406(3) 0.1908(2) 0.21260(19) 0.0287(11) Uani 1 1 d . . . C86 C 0.7928(3) 0.1430(2) 0.1981(2) 0.0369(13) Uani 1 1 d . . . H86A H 0.7648 0.1057 0.1849 0.044 Uiso 1 1 calc R . . C87 C 0.8853(3) 0.1486(2) 0.2026(2) 0.0394(13) Uani 1 1 d . . . H87A H 0.9200 0.1150 0.1931 0.047 Uiso 1 1 calc R . . C88 C 0.9259(3) 0.2016(3) 0.2205(2) 0.0428(14) Uani 1 1 d . . . H88A H 0.9892 0.2051 0.2237 0.051 Uiso 1 1 calc R . . C89 C 0.8757(3) 0.2515(3) 0.2343(2) 0.0437(14) Uani 1 1 d . . . H89A H 0.9043 0.2892 0.2458 0.052 Uiso 1 1 calc R . . C90 C 0.7844(3) 0.2455(2) 0.2310(2) 0.0369(13) Uani 1 1 d . . . H90A H 0.7503 0.2789 0.2415 0.044 Uiso 1 1 calc R . . C91 C 0.6551(3) 0.1853(2) 0.4967(2) 0.0350(12) Uani 1 1 d . . . C92 C 0.7375(3) 0.2041(2) 0.4827(2) 0.0457(14) Uani 1 1 d . . . H92A H 0.7456 0.2057 0.4441 0.055 Uiso 1 1 calc R . . C93 C 0.8068(4) 0.2204(3) 0.5244(3) 0.0593(17) Uani 1 1 d . . . H93A H 0.8621 0.2337 0.5143 0.071 Uiso 1 1 calc R . . C94 C 0.7969(4) 0.2178(3) 0.5809(3) 0.0594(18) Uani 1 1 d . . . H94A H 0.8450 0.2285 0.6098 0.071 Uiso 1 1 calc R . . C95 C 0.7157(4) 0.1991(3) 0.5943(2) 0.0543(16) Uani 1 1 d . . . H95A H 0.7080 0.1973 0.6330 0.065 Uiso 1 1 calc R . . C96 C 0.6459(4) 0.1831(2) 0.5531(2) 0.0496(15) Uani 1 1 d . . . H96A H 0.5905 0.1705 0.5636 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0185(4) 0.0276(4) 0.0303(4) -0.0002(3) 0.0054(3) 0.0008(3) Mn2 0.0197(4) 0.0227(4) 0.0312(4) -0.0009(3) 0.0045(3) 0.0003(3) Mn3 0.0199(4) 0.0261(4) 0.0300(4) -0.0008(3) 0.0050(3) 0.0003(3) Mn4 0.0198(4) 0.0232(4) 0.0324(4) -0.0005(3) 0.0047(3) 0.0005(3) S1 0.0271(6) 0.0267(7) 0.0285(7) 0.0007(5) 0.0060(5) -0.0003(5) S2 0.0255(6) 0.0250(7) 0.0324(7) -0.0010(6) 0.0040(5) -0.0020(5) S3 0.0268(6) 0.0272(7) 0.0298(7) -0.0012(6) 0.0073(5) -0.0016(5) S4 0.0268(6) 0.0246(7) 0.0302(7) -0.0012(5) 0.0053(5) -0.0022(5) S5 0.0273(6) 0.0251(7) 0.0297(7) 0.0008(5) 0.0062(5) -0.0018(5) S6 0.0264(6) 0.0221(6) 0.0320(7) -0.0009(5) 0.0079(5) -0.0028(5) S7 0.0267(6) 0.0230(6) 0.0291(7) 0.0011(5) 0.0043(5) 0.0003(5) S8 0.0261(6) 0.0220(6) 0.0309(7) -0.0004(5) 0.0058(5) -0.0021(5) O1 0.0254(17) 0.0257(18) 0.037(2) 0.0036(15) 0.0127(14) 0.0075(14) O2 0.0164(16) 0.036(2) 0.0353(19) -0.0065(16) 0.0045(14) -0.0021(14) O3 0.0208(17) 0.0272(18) 0.0336(19) 0.0009(15) -0.0007(14) -0.0021(14) O4 0.0232(17) 0.0256(18) 0.0324(19) -0.0025(15) 0.0041(14) 0.0028(14) O5 0.0190(16) 0.0281(18) 0.0302(18) 0.0029(15) 0.0010(14) -0.0025(14) O6 0.0261(17) 0.0255(18) 0.0310(19) -0.0018(15) 0.0007(14) 0.0029(15) O7 0.0202(17) 0.0277(18) 0.038(2) 0.0016(15) 0.0107(14) 0.0042(14) O8 0.0157(16) 0.0325(19) 0.0348(19) -0.0059(15) 0.0071(14) -0.0036(14) C1 0.019(2) 0.026(3) 0.030(3) -0.009(2) 0.005(2) -0.002(2) C2 0.019(2) 0.023(3) 0.028(3) -0.001(2) 0.004(2) 0.003(2) C3 0.026(3) 0.024(3) 0.033(3) 0.000(2) 0.000(2) 0.005(2) C4 0.023(3) 0.033(3) 0.032(3) -0.007(2) 0.004(2) 0.003(2) C5 0.024(3) 0.036(3) 0.028(3) 0.000(2) 0.009(2) 0.004(2) C6 0.025(3) 0.023(3) 0.030(3) -0.001(2) 0.004(2) -0.002(2) C7 0.019(2) 0.027(3) 0.035(3) 0.007(2) 0.009(2) 0.003(2) C8 0.028(3) 0.023(3) 0.028(3) 0.000(2) 0.002(2) 0.001(2) C9 0.026(3) 0.033(3) 0.033(3) 0.003(2) 0.012(2) 0.003(2) C10 0.025(3) 0.032(3) 0.046(3) 0.006(3) 0.007(2) -0.003(2) C11 0.022(2) 0.032(3) 0.035(3) 0.006(2) 0.001(2) -0.005(2) C12 0.024(3) 0.026(3) 0.028(3) 0.003(2) 0.002(2) 0.002(2) C13 0.024(3) 0.023(3) 0.030(3) -0.007(2) 0.002(2) 0.000(2) C14 0.025(3) 0.026(3) 0.026(3) -0.001(2) 0.003(2) -0.002(2) C15 0.032(3) 0.027(3) 0.032(3) -0.002(2) 0.007(2) -0.006(2) C16 0.026(3) 0.037(3) 0.030(3) -0.001(2) 0.000(2) 0.000(2) C17 0.030(3) 0.030(3) 0.024(3) -0.001(2) 0.002(2) 0.000(2) C18 0.027(3) 0.030(3) 0.028(3) -0.006(2) 0.005(2) -0.001(2) C19 0.017(2) 0.025(3) 0.041(3) -0.001(2) 0.007(2) 0.002(2) C20 0.025(3) 0.029(3) 0.028(3) -0.002(2) 0.008(2) -0.001(2) C21 0.026(3) 0.033(3) 0.031(3) 0.000(2) 0.006(2) -0.001(2) C22 0.026(3) 0.030(3) 0.033(3) 0.009(2) 0.006(2) 0.003(2) C23 0.025(3) 0.028(3) 0.030(3) 0.001(2) 0.008(2) 0.002(2) C24 0.017(2) 0.024(3) 0.027(3) 0.003(2) 0.0044(19) -0.0013(19) C25 0.018(2) 0.023(3) 0.028(3) -0.003(2) 0.002(2) 0.002(2) C26 0.023(2) 0.024(3) 0.030(3) 0.001(2) 0.006(2) 0.003(2) C27 0.030(3) 0.024(3) 0.030(3) -0.005(2) 0.001(2) -0.006(2) C28 0.025(3) 0.033(3) 0.034(3) -0.005(2) 0.001(2) 0.001(2) C29 0.033(3) 0.032(3) 0.025(3) 0.004(2) -0.002(2) 0.002(2) C30 0.020(2) 0.025(3) 0.028(3) -0.003(2) 0.006(2) -0.001(2) C31 0.019(2) 0.023(3) 0.031(3) 0.004(2) 0.005(2) -0.002(2) C32 0.028(3) 0.023(3) 0.031(3) 0.000(2) 0.009(2) 0.000(2) C33 0.029(3) 0.024(3) 0.033(3) 0.000(2) 0.001(2) 0.001(2) C34 0.033(3) 0.026(3) 0.035(3) 0.010(2) 0.002(2) 0.008(2) C35 0.031(3) 0.024(3) 0.038(3) 0.004(2) 0.009(2) 0.002(2) C36 0.025(2) 0.021(3) 0.030(3) 0.001(2) 0.004(2) 0.000(2) C37 0.020(2) 0.022(3) 0.028(3) 0.000(2) 0.000(2) -0.003(2) C38 0.018(2) 0.027(3) 0.028(3) -0.004(2) 0.004(2) -0.006(2) C39 0.024(3) 0.020(3) 0.037(3) -0.002(2) 0.004(2) 0.003(2) C40 0.024(3) 0.032(3) 0.029(3) -0.002(2) 0.002(2) 0.003(2) C41 0.021(2) 0.034(3) 0.029(3) 0.002(2) 0.009(2) 0.002(2) C42 0.021(2) 0.025(3) 0.028(3) 0.000(2) -0.001(2) 0.001(2) C43 0.022(2) 0.018(2) 0.031(3) 0.004(2) 0.007(2) -0.001(2) C44 0.025(3) 0.019(2) 0.028(3) 0.002(2) 0.005(2) 0.000(2) C45 0.023(3) 0.026(3) 0.034(3) 0.000(2) 0.010(2) 0.003(2) C46 0.022(2) 0.031(3) 0.034(3) 0.003(2) 0.005(2) -0.005(2) C47 0.024(3) 0.029(3) 0.033(3) 0.002(2) 0.008(2) -0.003(2) C48 0.027(3) 0.018(2) 0.028(3) 0.000(2) 0.008(2) 0.000(2) C49 0.035(3) 0.027(3) 0.031(3) 0.004(2) 0.011(2) 0.009(2) C50 0.039(3) 0.031(3) 0.046(3) 0.005(3) 0.020(3) 0.000(2) C51 0.053(4) 0.031(3) 0.042(3) 0.002(3) 0.027(3) 0.005(3) C52 0.041(3) 0.043(4) 0.044(3) 0.009(3) 0.020(3) 0.022(3) C53 0.034(3) 0.052(4) 0.050(4) 0.009(3) 0.013(3) 0.004(3) C54 0.032(3) 0.038(3) 0.052(4) 0.000(3) 0.016(3) 0.007(3) C55 0.028(3) 0.046(3) 0.042(3) 0.004(3) 0.016(2) -0.005(3) C56 0.039(4) 0.055(4) 0.128(6) -0.036(4) 0.023(4) -0.014(3) C57 0.050(4) 0.055(4) 0.162(8) -0.019(5) 0.052(5) 0.004(4) C58 0.024(3) 0.099(6) 0.071(5) 0.024(4) 0.009(3) -0.004(4) C59 0.038(4) 0.197(10) 0.067(5) -0.053(5) 0.014(3) -0.035(5) C60 0.039(4) 0.131(7) 0.061(4) -0.037(4) 0.021(3) -0.022(4) C61 0.031(3) 0.043(3) 0.027(3) 0.006(2) 0.000(2) -0.005(3) C62 0.038(3) 0.051(4) 0.039(3) 0.013(3) -0.002(3) -0.013(3) C63 0.039(3) 0.061(4) 0.042(4) 0.013(3) -0.007(3) -0.020(3) C64 0.027(3) 0.094(5) 0.046(4) 0.022(4) 0.001(3) -0.004(3) C65 0.034(3) 0.066(4) 0.043(4) 0.005(3) 0.004(3) 0.003(3) C66 0.035(3) 0.052(4) 0.040(3) -0.003(3) 0.004(2) -0.002(3) C67 0.033(3) 0.031(3) 0.038(3) 0.002(3) 0.000(2) 0.005(2) C68 0.045(3) 0.040(3) 0.039(3) 0.007(3) 0.008(3) 0.005(3) C69 0.063(4) 0.049(4) 0.043(4) 0.009(3) 0.000(3) 0.007(3) C70 0.064(4) 0.033(3) 0.058(4) 0.004(3) -0.014(3) 0.020(3) C71 0.049(3) 0.033(3) 0.050(4) -0.007(3) 0.003(3) 0.010(3) C72 0.041(3) 0.034(3) 0.037(3) 0.003(3) 0.001(2) 0.007(3) C73 0.035(3) 0.039(3) 0.040(3) 0.005(3) 0.007(2) 0.015(3) C74 0.037(3) 0.052(4) 0.057(4) -0.009(3) -0.005(3) 0.012(3) C75 0.037(3) 0.070(5) 0.068(4) -0.011(4) -0.002(3) 0.017(3) C76 0.049(4) 0.074(5) 0.060(4) 0.005(4) 0.003(3) 0.037(4) C77 0.067(4) 0.046(4) 0.054(4) 0.007(3) 0.009(3) 0.029(3) C78 0.049(3) 0.036(3) 0.051(4) -0.007(3) -0.003(3) 0.015(3) C79 0.036(3) 0.024(3) 0.027(3) 0.002(2) 0.012(2) 0.007(2) C80 0.037(3) 0.039(3) 0.046(3) 0.002(3) 0.020(3) 0.003(3) C81 0.073(4) 0.030(3) 0.052(4) -0.007(3) 0.029(3) 0.004(3) C82 0.050(4) 0.050(4) 0.052(4) 0.006(3) 0.023(3) 0.022(3) C83 0.035(3) 0.043(4) 0.059(4) 0.008(3) 0.016(3) 0.009(3) C84 0.032(3) 0.035(3) 0.047(3) -0.001(3) 0.005(2) 0.007(2) C85 0.028(3) 0.031(3) 0.029(3) 0.004(2) 0.009(2) -0.003(2) C86 0.030(3) 0.037(3) 0.043(3) -0.003(3) 0.001(2) -0.002(2) C87 0.033(3) 0.042(3) 0.044(3) -0.004(3) 0.008(2) 0.011(3) C88 0.022(3) 0.065(4) 0.041(3) 0.002(3) 0.003(2) -0.001(3) C89 0.029(3) 0.065(4) 0.036(3) -0.004(3) 0.001(2) -0.017(3) C90 0.035(3) 0.039(3) 0.039(3) -0.008(3) 0.013(2) 0.002(2) C91 0.040(3) 0.030(3) 0.032(3) 0.004(2) -0.003(2) -0.003(2) C92 0.037(3) 0.050(4) 0.047(4) -0.002(3) 0.000(3) -0.007(3) C93 0.040(4) 0.062(4) 0.070(5) 0.006(4) -0.010(3) -0.012(3) C94 0.054(4) 0.046(4) 0.067(5) -0.001(3) -0.026(3) -0.013(3) C95 0.072(4) 0.053(4) 0.031(3) -0.001(3) -0.012(3) -0.012(3) C96 0.052(4) 0.048(4) 0.045(4) 0.002(3) -0.005(3) -0.018(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 Mn1 O1 2.103(3) . ? Mn1 O8 2.124(3) . ? Mn1 O4 2.142(3) . ? Mn1 O5 2.181(3) . ? Mn1 S8 2.6245(13) . ? Mn1 S4 2.6527(13) . ? Mn2 O1 2.103(3) . ? Mn2 O6 2.124(3) . ? Mn2 O2 2.130(3) . ? Mn2 O5 2.172(3) . ? Mn2 S5 2.6735(13) . ? Mn2 S1 2.7188(13) . ? Mn3 O6 2.119(3) . ? Mn3 O3 2.119(3) . ? Mn3 O7 2.163(3) . ? Mn3 O2 2.170(3) . ? Mn3 S2 2.6858(13) . ? Mn3 S6 2.7021(13) . ? Mn4 O8 2.098(3) . ? Mn4 O3 2.123(3) . ? Mn4 O7 2.163(3) . ? Mn4 O4 2.179(3) . ? Mn4 S3 2.7343(13) . ? Mn4 S7 2.7593(13) . ? S1 C6 1.783(4) . ? S1 C8 1.786(5) . ? S2 C12 1.788(5) . ? S2 C14 1.792(5) . ? S3 C20 1.793(5) . ? S3 C18 1.799(5) . ? S4 C24 1.777(4) . ? S4 C2 1.790(4) . ? S5 C30 1.789(4) . ? S5 C32 1.793(4) . ? S6 C36 1.778(5) . ? S6 C38 1.790(4) . ? S7 C42 1.788(4) . ? S7 C44 1.791(5) . ? S8 C26 1.779(5) . ? S8 C48 1.783(4) . ? O1 C1 1.314(5) . ? O2 C7 1.307(5) . ? O3 C13 1.322(5) . ? O4 C19 1.329(5) . ? O5 C25 1.312(5) . ? O6 C31 1.309(5) . ? O7 C37 1.316(5) . ? O8 C43 1.311(5) . ? C1 C6 1.412(6) . ? C1 C2 1.412(6) . ? C2 C3 1.375(6) . ? C3 C4 1.391(6) . ? C4 C5 1.385(6) . ? C4 C49 1.477(6) . ? C5 C6 1.391(6) . ? C7 C12 1.410(6) . ? C7 C8 1.415(6) . ? C8 C9 1.389(6) . ? C9 C10 1.387(6) . ? C10 C11 1.386(6) . ? C10 C55 1.481(6) . ? C11 C12 1.375(6) . ? C13 C18 1.395(6) . ? C13 C14 1.406(6) . ? C14 C15 1.376(6) . ? C15 C16 1.397(6) . ? C16 C17 1.393(6) . ? C16 C61 1.472(6) . ? C17 C18 1.385(6) . ? C19 C20 1.392(6) . ? C19 C24 1.434(6) . ? C20 C21 1.393(6) . ? C21 C22 1.391(6) . ? C22 C23 1.378(6) . ? C22 C67 1.490(6) . ? C23 C24 1.383(6) . ? C25 C26 1.405(6) . ? C25 C30 1.414(6) . ? C26 C27 1.391(6) . ? C27 C28 1.383(6) . ? C28 C29 1.394(6) . ? C28 C91 1.486(6) . ? C29 C30 1.385(6) . ? C31 C32 1.396(6) . ? C31 C36 1.424(6) . ? C32 C33 1.392(6) . ? C33 C34 1.408(6) . ? C34 C35 1.389(6) . ? C34 C73 1.495(6) . ? C35 C36 1.391(6) . ? C37 C42 1.415(6) . ? C37 C38 1.419(6) . ? C38 C39 1.375(6) . ? C39 C40 1.394(6) . ? C40 C41 1.396(6) . ? C40 C79 1.500(6) . ? C41 C42 1.384(6) . ? C43 C44 1.401(6) . ? C43 C48 1.411(6) . ? C44 C45 1.404(6) . ? C45 C46 1.395(6) . ? C46 C47 1.404(6) . ? C46 C85 1.485(6) . ? C47 C48 1.390(6) . ? C49 C54 1.384(6) . ? C49 C50 1.386(6) . ? C50 C51 1.390(6) . ? C51 C52 1.354(7) . ? C52 C53 1.377(7) . ? C53 C54 1.380(6) . ? C55 C56 1.340(7) . ? C55 C60 1.402(8) . ? C56 C57 1.384(8) . ? C57 C58 1.320(8) . ? C58 C59 1.405(9) . ? C59 C60 1.376(8) . ? C61 C66 1.384(7) . ? C61 C62 1.390(7) . ? C62 C63 1.400(7) . ? C63 C64 1.357(8) . ? C64 C65 1.382(8) . ? C65 C66 1.391(7) . ? C67 C68 1.382(6) . ? C67 C72 1.389(6) . ? C68 C69 1.368(7) . ? C69 C70 1.386(8) . ? C70 C71 1.390(7) . ? C71 C72 1.380(7) . ? C73 C74 1.381(7) . ? C73 C78 1.389(7) . ? C74 C75 1.388(7) . ? C75 C76 1.368(8) . ? C76 C77 1.386(8) . ? C77 C78 1.377(7) . ? C79 C84 1.376(6) . ? C79 C80 1.379(6) . ? C80 C81 1.387(7) . ? C81 C82 1.370(7) . ? C82 C83 1.354(7) . ? C83 C84 1.390(6) . ? C85 C86 1.386(6) . ? C85 C90 1.404(6) . ? C86 C87 1.390(6) . ? C87 C88 1.350(7) . ? C88 C89 1.399(7) . ? C89 C90 1.375(6) . ? C91 C96 1.377(7) . ? C91 C92 1.401(7) . ? C92 C93 1.374(7) . ? C93 C94 1.382(8) . ? C94 C95 1.377(8) . ? C95 C96 1.371(7) . ? 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 O8 146.13(12) . . ? O1 Mn1 O4 90.43(12) . . ? O8 Mn1 O4 72.89(11) . . ? O1 Mn1 O5 72.48(11) . . ? O8 Mn1 O5 91.18(11) . . ? O4 Mn1 O5 121.72(11) . . ? O1 Mn1 S8 124.63(9) . . ? O8 Mn1 S8 77.70(8) . . ? O4 Mn1 S8 144.81(9) . . ? O5 Mn1 S8 77.18(8) . . ? O1 Mn1 S4 77.26(8) . . ? O8 Mn1 S4 125.32(9) . . ? O4 Mn1 S4 78.15(8) . . ? O5 Mn1 S4 143.29(9) . . ? S8 Mn1 S4 104.53(4) . . ? O1 Mn2 O6 145.11(12) . . ? O1 Mn2 O2 92.37(12) . . ? O6 Mn2 O2 71.51(11) . . ? O1 Mn2 O5 72.67(11) . . ? O6 Mn2 O5 89.81(11) . . ? O2 Mn2 O5 122.41(11) . . ? O1 Mn2 S5 125.50(9) . . ? O6 Mn2 S5 76.28(8) . . ? O2 Mn2 S5 142.12(9) . . ? O5 Mn2 S5 76.10(8) . . ? O1 Mn2 S1 75.44(8) . . ? O6 Mn2 S1 127.05(9) . . ? O2 Mn2 S1 76.54(8) . . ? O5 Mn2 S1 143.14(9) . . ? S5 Mn2 S1 109.17(4) . . ? O6 Mn3 O3 145.38(12) . . ? O6 Mn3 O7 91.70(11) . . ? O3 Mn3 O7 72.29(11) . . ? O6 Mn3 O2 70.84(11) . . ? O3 Mn3 O2 92.01(12) . . ? O7 Mn3 O2 122.99(11) . . ? O6 Mn3 S2 124.39(9) . . ? O3 Mn3 S2 76.39(8) . . ? O7 Mn3 S2 143.91(9) . . ? O2 Mn3 S2 75.01(8) . . ? O6 Mn3 S6 75.54(8) . . ? O3 Mn3 S6 126.79(9) . . ? O7 Mn3 S6 76.08(8) . . ? O2 Mn3 S6 141.20(9) . . ? S2 Mn3 S6 110.42(4) . . ? O8 Mn4 O3 146.57(12) . . ? O8 Mn4 O7 92.58(11) . . ? O3 Mn4 O7 72.20(11) . . ? O8 Mn4 O4 72.64(11) . . ? O3 Mn4 O4 90.27(11) . . ? O7 Mn4 O4 122.36(11) . . ? O8 Mn4 S3 124.49(9) . . ? O3 Mn4 S3 75.35(8) . . ? O7 Mn4 S3 142.93(9) . . ? O4 Mn4 S3 74.68(8) . . ? O8 Mn4 S7 74.05(8) . . ? O3 Mn4 S7 126.97(9) . . ? O7 Mn4 S7 75.16(8) . . ? O4 Mn4 S7 142.74(8) . . ? S3 Mn4 S7 112.34(4) . . ? C6 S1 C8 102.5(2) . . ? C6 S1 Mn2 95.62(15) . . ? C8 S1 Mn2 94.21(15) . . ? C12 S2 C14 99.5(2) . . ? C12 S2 Mn3 96.79(15) . . ? C14 S2 Mn3 95.20(15) . . ? C20 S3 C18 103.1(2) . . ? C20 S3 Mn4 94.51(15) . . ? C18 S3 Mn4 95.14(16) . . ? C24 S4 C2 103.7(2) . . ? C24 S4 Mn1 94.05(15) . . ? C2 S4 Mn1 95.46(14) . . ? C30 S5 C32 102.1(2) . . ? C30 S5 Mn2 93.80(15) . . ? C32 S5 Mn2 94.92(15) . . ? C36 S6 C38 101.1(2) . . ? C36 S6 Mn3 95.65(15) . . ? C38 S6 Mn3 94.50(15) . . ? C42 S7 C44 102.4(2) . . ? C42 S7 Mn4 94.04(15) . . ? C44 S7 Mn4 95.36(14) . . ? C26 S8 C48 101.9(2) . . ? C26 S8 Mn1 94.63(15) . . ? C48 S8 Mn1 95.36(15) . . ? C1 O1 Mn1 126.4(3) . . ? C1 O1 Mn2 128.4(3) . . ? Mn1 O1 Mn2 103.88(12) . . ? C7 O2 Mn2 124.6(3) . . ? C7 O2 Mn3 125.9(3) . . ? Mn2 O2 Mn3 100.87(12) . . ? C13 O3 Mn3 126.8(3) . . ? C13 O3 Mn4 127.2(3) . . ? Mn3 O3 Mn4 102.68(12) . . ? C19 O4 Mn1 121.2(3) . . ? C19 O4 Mn4 122.7(3) . . ? Mn1 O4 Mn4 98.98(12) . . ? C25 O5 Mn2 120.3(3) . . ? C25 O5 Mn1 119.1(3) . . ? Mn2 O5 Mn1 99.06(11) . . ? C31 O6 Mn3 127.0(3) . . ? C31 O6 Mn2 125.7(3) . . ? Mn3 O6 Mn2 102.78(12) . . ? C37 O7 Mn4 123.6(3) . . ? C37 O7 Mn3 123.3(3) . . ? Mn4 O7 Mn3 99.95(11) . . ? C43 O8 Mn4 128.9(3) . . ? C43 O8 Mn1 124.1(3) . . ? Mn4 O8 Mn1 102.21(12) . . ? O1 C1 C6 121.5(4) . . ? O1 C1 C2 121.3(4) . . ? C6 C1 C2 117.1(4) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 S4 120.5(3) . . ? C1 C2 S4 119.1(3) . . ? C2 C3 C4 122.5(4) . . ? C5 C4 C3 117.4(4) . . ? C5 C4 C49 122.3(4) . . ? C3 C4 C49 120.2(4) . . ? C4 C5 C6 121.5(4) . . ? C5 C6 C1 120.8(4) . . ? C5 C6 S1 120.6(3) . . ? C1 C6 S1 118.6(3) . . ? O2 C7 C12 121.8(4) . . ? O2 C7 C8 122.3(4) . . ? C12 C7 C8 115.8(4) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 S1 119.8(3) . . ? C7 C8 S1 119.6(3) . . ? C10 C9 C8 122.2(4) . . ? C11 C10 C9 117.1(4) . . ? C11 C10 C55 121.2(5) . . ? C9 C10 C55 121.7(5) . . ? C12 C11 C10 121.7(4) . . ? C11 C12 C7 121.9(4) . . ? C11 C12 S2 119.8(4) . . ? C7 C12 S2 118.3(3) . . ? O3 C13 C18 122.5(4) . . ? O3 C13 C14 120.6(4) . . ? C18 C13 C14 116.9(4) . . ? C15 C14 C13 121.2(4) . . ? C15 C14 S2 118.9(3) . . ? C13 C14 S2 119.8(3) . . ? C14 C15 C16 121.9(4) . . ? C17 C16 C15 116.9(4) . . ? C17 C16 C61 123.3(4) . . ? C15 C16 C61 119.6(4) . . ? C18 C17 C16 121.5(4) . . ? C17 C18 C13 121.5(4) . . ? C17 C18 S3 119.7(4) . . ? C13 C18 S3 118.7(3) . . ? O4 C19 C20 122.1(4) . . ? O4 C19 C24 120.9(4) . . ? C20 C19 C24 117.0(4) . . ? C19 C20 C21 121.6(4) . . ? C19 C20 S3 119.3(3) . . ? C21 C20 S3 118.9(4) . . ? C22 C21 C20 121.1(4) . . ? C23 C22 C21 117.8(4) . . ? C23 C22 C67 121.5(4) . . ? C21 C22 C67 120.6(4) . . ? C22 C23 C24 122.7(4) . . ? C23 C24 C19 119.8(4) . . ? C23 C24 S4 119.6(3) . . ? C19 C24 S4 120.5(3) . . ? O5 C25 C26 122.2(4) . . ? O5 C25 C30 122.0(4) . . ? C26 C25 C30 115.8(4) . . ? C27 C26 C25 121.6(4) . . ? C27 C26 S8 118.6(3) . . ? C25 C26 S8 119.6(3) . . ? C28 C27 C26 121.8(4) . . ? C27 C28 C29 117.4(4) . . ? C27 C28 C91 121.5(4) . . ? C29 C28 C91 121.1(4) . . ? C30 C29 C28 121.4(4) . . ? C29 C30 C25 121.9(4) . . ? C29 C30 S5 119.1(3) . . ? C25 C30 S5 119.0(3) . . ? O6 C31 C32 121.9(4) . . ? O6 C31 C36 121.1(4) . . ? C32 C31 C36 117.0(4) . . ? C33 C32 C31 122.1(4) . . ? C33 C32 S5 118.8(4) . . ? C31 C32 S5 119.1(3) . . ? C32 C33 C34 120.6(4) . . ? C35 C34 C33 117.7(4) . . ? C35 C34 C73 123.4(4) . . ? C33 C34 C73 118.8(4) . . ? C34 C35 C36 122.1(4) . . ? C35 C36 C31 120.4(4) . . ? C35 C36 S6 120.9(4) . . ? C31 C36 S6 118.7(3) . . ? O7 C37 C42 122.6(4) . . ? O7 C37 C38 122.0(4) . . ? C42 C37 C38 115.4(4) . . ? C39 C38 C37 121.7(4) . . ? C39 C38 S6 118.9(3) . . ? C37 C38 S6 119.4(3) . . ? C38 C39 C40 122.1(4) . . ? C39 C40 C41 117.2(4) . . ? C39 C40 C79 121.8(4) . . ? C41 C40 C79 121.0(4) . . ? C42 C41 C40 121.2(4) . . ? C41 C42 C37 122.2(4) . . ? C41 C42 S7 118.3(3) . . ? C37 C42 S7 119.4(3) . . ? O8 C43 C44 122.4(4) . . ? O8 C43 C48 121.4(4) . . ? C44 C43 C48 116.2(4) . . ? C43 C44 C45 121.6(4) . . ? C43 C44 S7 117.6(3) . . ? C45 C44 S7 120.8(3) . . ? C46 C45 C44 121.6(4) . . ? C45 C46 C47 117.0(4) . . ? C45 C46 C85 123.5(4) . . ? C47 C46 C85 119.5(4) . . ? C48 C47 C46 121.3(4) . . ? C47 C48 C43 122.1(4) . . ? C47 C48 S8 118.4(3) . . ? C43 C48 S8 119.5(3) . . ? C54 C49 C50 118.5(4) . . ? C54 C49 C4 120.7(4) . . ? C50 C49 C4 120.8(4) . . ? C49 C50 C51 120.5(5) . . ? C52 C51 C50 120.1(5) . . ? C51 C52 C53 120.3(5) . . ? C52 C53 C54 120.1(5) . . ? C53 C54 C49 120.4(5) . . ? C56 C55 C60 117.4(5) . . ? C56 C55 C10 122.4(5) . . ? C60 C55 C10 120.3(5) . . ? C55 C56 C57 122.3(6) . . ? C58 C57 C56 121.0(6) . . ? C57 C58 C59 118.8(6) . . ? C60 C59 C58 119.8(7) . . ? C59 C60 C55 120.2(7) . . ? C66 C61 C62 119.0(5) . . ? C66 C61 C16 120.8(5) . . ? C62 C61 C16 120.1(5) . . ? C61 C62 C63 120.0(5) . . ? C64 C63 C62 119.9(5) . . ? C63 C64 C65 121.3(5) . . ? C64 C65 C66 119.0(6) . . ? C61 C66 C65 120.8(5) . . ? C68 C67 C72 118.1(5) . . ? C68 C67 C22 122.1(4) . . ? C72 C67 C22 119.8(4) . . ? C69 C68 C67 121.5(5) . . ? C68 C69 C70 119.7(5) . . ? C69 C70 C71 120.3(5) . . ? C72 C71 C70 118.7(5) . . ? C71 C72 C67 121.7(5) . . ? C74 C73 C78 118.7(5) . . ? C74 C73 C34 120.8(5) . . ? C78 C73 C34 120.4(5) . . ? C73 C74 C75 120.6(5) . . ? C76 C75 C74 119.8(6) . . ? C75 C76 C77 120.5(6) . . ? C78 C77 C76 119.4(6) . . ? C77 C78 C73 121.0(6) . . ? C84 C79 C80 118.5(4) . . ? C84 C79 C40 121.4(4) . . ? C80 C79 C40 120.1(4) . . ? C79 C80 C81 120.4(5) . . ? C82 C81 C80 120.2(5) . . ? C83 C82 C81 119.9(5) . . ? C82 C83 C84 120.3(5) . . ? C79 C84 C83 120.6(5) . . ? C86 C85 C90 117.6(4) . . ? C86 C85 C46 122.5(4) . . ? C90 C85 C46 119.9(4) . . ? C85 C86 C87 121.3(5) . . ? C88 C87 C86 120.0(5) . . ? C87 C88 C89 120.6(5) . . ? C90 C89 C88 119.2(5) . . ? C89 C90 C85 121.2(5) . . ? C96 C91 C92 118.3(5) . . ? C96 C91 C28 120.9(5) . . ? C92 C91 C28 120.7(5) . . ? C93 C92 C91 120.5(5) . . ? C92 C93 C94 120.7(6) . . ? C95 C94 C93 118.5(5) . . ? C96 C95 C94 121.4(6) . . ? C95 C96 C91 120.6(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.125 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.089 ###END data_compound_775185 _database_code_depnum_ccdc_archive 'CCDC 775185' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Mn4(C48H28O4S4)2)2 (C60)' _chemical_melting_point ? _chemical_formula_moiety 'C192 H112 Mn8 O16 S16, C60' _chemical_formula_sum 'C252 H112 Mn8 O16 S16' _chemical_formula_weight 4347.90 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_Int_Tables_number No.43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 56.211(3) _cell_length_b 29.8431(18) _cell_length_c 30.7930(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 51655(5) _cell_formula_units_Z 8 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used 9846 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 17664 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8915 _exptl_absorpt_correction_T_max 0.9059 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90912 _diffrn_reflns_av_R_equivalents 0.1546 _diffrn_reflns_av_sigmaI/netI 0.1423 _diffrn_reflns_limit_h_min -66 _diffrn_reflns_limit_h_max 66 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21881 _reflns_number_gt 12800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, the command 'omit 0 50' was used to omit the weak reflections above 50 degree. The command 'isor' was used to restrain the non-H atoms with NPD and ADP problems. These atoms are as follows: C26, C38, C55 > C60, C79 > C84, and C88 > C90. The command 'dfix' was also used to model the C60 molecule. The restraint commands lead to a relative high restraint number 326, but cannot be completely avoided. Suspect C-C bonds (especially in C60 molecule) are due to the weak high-angle diffractions and the disorders and these problems can't be solved by trials of refinement. The high Rint factor of compound might be due to the weak high-angle diffractions and the disorder of C60 and toluene molecules. Considering the large cell volume and large incorporated disordered toluene (the elcetron count to be 7028 within 20065 A3 void per cell), the present data is not good comparing to the ordinary ones and the resulted problems can not be completely solved by further refinement even with re-collected data. Those observations are familiar in calixarene-based compounds and more problems emerge by incorporating fullerene. ; _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^)+(0.1396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(9) _refine_ls_number_reflns 21881 _refine_ls_number_parameters 1210 _refine_ls_number_restraints 326 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.2144 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 3.017 _refine_ls_shift/su_max 0.002 _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 0.11660(7) 0.44621(14) 0.52276(15) 0.0340(11) Uani 1 1 d . . . Mn2 Mn 0.08496(7) 0.36088(14) 0.48624(15) 0.0337(11) Uani 1 1 d . . . Mn3 Mn 0.13273(7) 0.31940(14) 0.43959(15) 0.0348(11) Uani 1 1 d . . . Mn4 Mn 0.16464(8) 0.40410(14) 0.47704(15) 0.0358(11) Uani 1 1 d . . . S1 S 0.10283(12) 0.5255(2) 0.4900(3) 0.0346(17) Uani 1 1 d . . . S2 S 0.05060(13) 0.3837(3) 0.4302(3) 0.0388(19) Uani 1 1 d . . . S3 S 0.13075(13) 0.3166(2) 0.3515(3) 0.0367(18) Uani 1 1 d . . . S4 S 0.18365(13) 0.4572(2) 0.4152(3) 0.0389(19) Uani 1 1 d . . . S5 S 0.11941(12) 0.4522(2) 0.6084(2) 0.0326(17) Uani 1 1 d . . . S6 S 0.06647(13) 0.3101(2) 0.5500(3) 0.0358(18) Uani 1 1 d . . . S7 S 0.14583(13) 0.2398(2) 0.4717(3) 0.0370(18) Uani 1 1 d . . . S8 S 0.19933(13) 0.3810(2) 0.5313(3) 0.0384(19) Uani 1 1 d . . . O1 O 0.0924(3) 0.4295(6) 0.4700(7) 0.039(5) Uani 1 1 d . . . O2 O 0.0970(3) 0.3359(6) 0.4248(6) 0.034(5) Uani 1 1 d . . . O3 O 0.1465(4) 0.3837(7) 0.4172(7) 0.048(5) Uani 1 1 d . . . O4 O 0.1447(3) 0.4646(6) 0.4818(7) 0.037(5) Uani 1 1 d . . . O5 O 0.0950(3) 0.3941(6) 0.5433(6) 0.032(4) Uani 1 1 d . . . O6 O 0.1121(3) 0.3107(6) 0.4993(6) 0.034(5) Uani 1 1 d . . . O7 O 0.1621(3) 0.3344(6) 0.4777(7) 0.042(5) Uani 1 1 d . . . O8 O 0.1471(3) 0.4052(6) 0.5402(6) 0.032(4) Uani 1 1 d . . . C1 C 0.0777(5) 0.4567(10) 0.4536(12) 0.042(8) Uani 1 1 d . . . C2 C 0.0797(5) 0.5041(9) 0.4556(10) 0.036(7) Uani 1 1 d . . . C3 C 0.0650(5) 0.5337(10) 0.4342(9) 0.038(7) Uani 1 1 d . . . H3A H 0.0682 0.5649 0.4350 0.045 Uiso 1 1 calc R . . C4 C 0.0456(5) 0.5175(10) 0.4115(12) 0.046(8) Uani 1 1 d . . . C5 C 0.0416(5) 0.4725(10) 0.4101(11) 0.043(8) Uani 1 1 d . . . H5A H 0.0281 0.4619 0.3946 0.052 Uiso 1 1 calc R . . C6 C 0.0564(5) 0.4409(10) 0.4301(11) 0.043(8) Uani 1 1 d . . . C7 C 0.0886(5) 0.3465(9) 0.3873(9) 0.030(6) Uani 1 1 d . . . C8 C 0.0669(5) 0.3672(10) 0.3836(12) 0.046(8) Uani 1 1 d . . . C9 C 0.0578(5) 0.3801(11) 0.3410(9) 0.042(8) Uani 1 1 d . . . H9A H 0.0432 0.3957 0.3388 0.051 Uiso 1 1 calc R . . C10 C 0.0700(7) 0.3701(11) 0.3055(11) 0.056(9) Uani 1 1 d U . . C11 C 0.0933(6) 0.3479(12) 0.3109(12) 0.055(8) Uani 1 1 d DU . . H11A H 0.1025 0.3405 0.2861 0.066 Uiso 1 1 calc R . . C12 C 0.1011(5) 0.3389(10) 0.3480(10) 0.034(7) Uani 1 1 d U . . C13 C 0.1555(5) 0.3910(9) 0.3783(10) 0.034(7) Uani 1 1 d . . . C14 C 0.1489(5) 0.3659(9) 0.3441(10) 0.035(7) Uani 1 1 d . . . C15 C 0.1569(5) 0.3764(9) 0.3024(10) 0.034(7) Uani 1 1 d . . . H15A H 0.1516 0.3586 0.2788 0.041 Uiso 1 1 calc R . . C16 C 0.1720(5) 0.4114(9) 0.2942(9) 0.033(6) Uani 1 1 d . . . C17 C 0.1795(5) 0.4349(9) 0.3286(10) 0.038(7) Uani 1 1 d . . . H17A H 0.1908 0.4582 0.3241 0.046 Uiso 1 1 calc R . . C18 C 0.1715(5) 0.4267(9) 0.3705(10) 0.034(7) Uani 1 1 d . . . C19 C 0.1445(5) 0.4973(10) 0.4516(11) 0.039(8) Uani 1 1 d . . . C20 C 0.1612(5) 0.5004(10) 0.4195(10) 0.038(7) Uani 1 1 d . . . C21 C 0.1620(6) 0.5356(10) 0.3895(11) 0.048(8) Uani 1 1 d . . . H21A H 0.1742 0.5367 0.3684 0.058 Uiso 1 1 calc R . . C22 C 0.1451(6) 0.5682(10) 0.3908(12) 0.053(9) Uani 1 1 d . . . C23 C 0.1278(6) 0.5653(10) 0.4258(11) 0.048(8) Uani 1 1 d . . . H23A H 0.1165 0.5887 0.4298 0.057 Uiso 1 1 calc R . . C24 C 0.1278(5) 0.5292(10) 0.4530(10) 0.037(7) Uani 1 1 d . . . C25 C 0.0950(5) 0.3774(10) 0.5810(10) 0.035(7) Uani 1 1 d . . . C26 C 0.1057(4) 0.3992(9) 0.6183(9) 0.028(6) Uani 1 1 d U . . C27 C 0.1055(6) 0.3819(10) 0.6598(11) 0.044(8) Uani 1 1 d . . . H27A H 0.1137 0.3971 0.6823 0.053 Uiso 1 1 calc R . . C28 C 0.0933(5) 0.3426(10) 0.6688(11) 0.042(8) Uani 1 1 d . . . C29 C 0.0819(6) 0.3189(10) 0.6337(12) 0.051(9) Uani 1 1 d . . . H29A H 0.0740 0.2913 0.6388 0.062 Uiso 1 1 calc R . . C30 C 0.0826(5) 0.3372(9) 0.5928(9) 0.031(7) Uani 1 1 d . . . C31 C 0.1059(5) 0.2716(10) 0.5126(9) 0.032(7) Uani 1 1 d . . . C32 C 0.0856(5) 0.2638(9) 0.5371(10) 0.037(7) Uani 1 1 d . . . C33 C 0.0794(5) 0.2203(9) 0.5505(10) 0.042(8) Uani 1 1 d . . . H33A H 0.0654 0.2162 0.5673 0.051 Uiso 1 1 calc R . . C34 C 0.0928(6) 0.1840(10) 0.5402(12) 0.053(9) Uani 1 1 d . . . C35 C 0.1129(5) 0.1913(10) 0.5184(11) 0.044(8) Uani 1 1 d . . . H35A H 0.1227 0.1663 0.5120 0.053 Uiso 1 1 calc R . . C36 C 0.1202(5) 0.2327(9) 0.5045(10) 0.038(7) Uani 1 1 d . . . C37 C 0.1720(5) 0.3085(9) 0.5075(8) 0.027(6) Uani 1 1 d . . . C38 C 0.1667(5) 0.2633(9) 0.5100(8) 0.028(6) Uani 1 1 d U . . C39 C 0.1791(5) 0.2362(10) 0.5388(10) 0.040(8) Uani 1 1 d . . . H39A H 0.1747 0.2055 0.5401 0.048 Uiso 1 1 calc R . . C40 C 0.1969(5) 0.2495(9) 0.5648(10) 0.036(7) Uani 1 1 d . . . C41 C 0.2022(5) 0.2953(9) 0.5639(9) 0.035(7) Uani 1 1 d . . . H41A H 0.2141 0.3072 0.5826 0.042 Uiso 1 1 calc R . . C42 C 0.1900(5) 0.3236(9) 0.5352(9) 0.032(7) Uani 1 1 d . . . C43 C 0.1600(5) 0.4164(9) 0.5726(10) 0.034(7) Uani 1 1 d . . . C44 C 0.1848(5) 0.4067(8) 0.5772(9) 0.031(7) Uani 1 1 d . . . C45 C 0.1984(5) 0.4215(8) 0.6106(9) 0.029(6) Uani 1 1 d . . . H45A H 0.2149 0.4144 0.6112 0.035 Uiso 1 1 calc R . . C46 C 0.1886(5) 0.4469(10) 0.6445(10) 0.038(7) Uani 1 1 d . . . C47 C 0.1643(5) 0.4551(9) 0.6424(9) 0.037(7) Uani 1 1 d . . . H47A H 0.1572 0.4725 0.6648 0.044 Uiso 1 1 calc R . . C48 C 0.1502(5) 0.4393(10) 0.6094(10) 0.039(7) Uani 1 1 d . . . C49 C 0.0315(5) 0.5499(11) 0.3843(13) 0.050(9) Uani 1 1 d . . . C50 C 0.0241(7) 0.5359(14) 0.3416(13) 0.072(12) Uani 1 1 d . . . H50A H 0.0279 0.5068 0.3312 0.087 Uiso 1 1 calc R . . C51 C 0.0110(7) 0.5667(13) 0.3153(14) 0.072(12) Uani 1 1 d . . . H51A H 0.0064 0.5587 0.2867 0.086 Uiso 1 1 calc R . . C52 C 0.0050(6) 0.6094(14) 0.3324(18) 0.080(15) Uani 1 1 d . . . H52A H -0.0035 0.6304 0.3153 0.096 Uiso 1 1 calc R . . C53 C 0.0116(6) 0.6196(11) 0.3736(14) 0.056(9) Uani 1 1 d . . . H53A H 0.0077 0.6483 0.3850 0.067 Uiso 1 1 calc R . . C54 C 0.0238(6) 0.5894(11) 0.3992(13) 0.058(10) Uani 1 1 d . . . H54A H 0.0269 0.5970 0.4286 0.069 Uiso 1 1 calc R . . C55 C 0.0605(7) 0.3853(15) 0.2627(15) 0.083(12) Uani 1 1 d DU . . C56 C 0.0628(9) 0.3618(18) 0.221(2) 0.116(18) Uani 1 1 d DU . . H56A H 0.0722 0.3354 0.2213 0.140 Uiso 1 1 calc R . . C57 C 0.0528(10) 0.374(2) 0.182(2) 0.14(2) Uani 1 1 d DU . . H57A H 0.0557 0.3560 0.1569 0.163 Uiso 1 1 calc R . . C58 C 0.0390(14) 0.410(3) 0.180(3) 0.16(3) Uani 1 1 d DU . . H58A H 0.0308 0.4172 0.1535 0.194 Uiso 1 1 calc R . . C59 C 0.0369(14) 0.438(3) 0.217(3) 0.17(3) Uani 1 1 d DU . . H59A H 0.0289 0.4662 0.2147 0.203 Uiso 1 1 calc R . . C60 C 0.0462(9) 0.4262(18) 0.2582(17) 0.104(16) Uani 1 1 d DU . . H60A H 0.0433 0.4446 0.2828 0.125 Uiso 1 1 calc R . . C61 C 0.1798(6) 0.4225(10) 0.2503(12) 0.052(9) Uani 1 1 d . . . C62 C 0.1650(7) 0.4158(12) 0.2142(12) 0.060(10) Uani 1 1 d . . . H62A H 0.1494 0.4044 0.2180 0.072 Uiso 1 1 calc R . . C63 C 0.1736(8) 0.4263(12) 0.1718(12) 0.062(10) Uani 1 1 d . . . H63A H 0.1628 0.4237 0.1481 0.074 Uiso 1 1 calc R . . C64 C 0.1950(8) 0.4392(14) 0.1638(13) 0.075(12) Uani 1 1 d . . . H64A H 0.2003 0.4448 0.1350 0.090 Uiso 1 1 calc R . . C65 C 0.2106(7) 0.4448(13) 0.2001(12) 0.067(11) Uani 1 1 d . . . H65A H 0.2265 0.4548 0.1954 0.081 Uiso 1 1 calc R . . C66 C 0.2032(6) 0.4360(11) 0.2415(12) 0.057(9) Uani 1 1 d . . . H66A H 0.2141 0.4391 0.2648 0.069 Uiso 1 1 calc R . . C67 C 0.1448(7) 0.6081(12) 0.3613(14) 0.061(10) Uani 1 1 d . . . C68 C 0.1484(10) 0.6010(17) 0.321(2) 0.112(19) Uani 1 1 d . . . H68A H 0.1509 0.5707 0.3120 0.134 Uiso 1 1 calc R . . C69 C 0.1489(11) 0.6355(19) 0.285(2) 0.15(3) Uani 1 1 d . . . H69A H 0.1521 0.6295 0.2555 0.175 Uiso 1 1 calc R . . C70 C 0.1436(12) 0.6819(18) 0.3044(19) 0.12(2) Uani 1 1 d . . . H70A H 0.1442 0.7078 0.2864 0.147 Uiso 1 1 calc R . . C71 C 0.1383(12) 0.6858(16) 0.345(2) 0.13(2) Uani 1 1 d . . . H71A H 0.1333 0.7138 0.3562 0.150 Uiso 1 1 calc R . . C72 C 0.1399(9) 0.6487(12) 0.3712(16) 0.097(17) Uani 1 1 d . . . H72A H 0.1370 0.6541 0.4011 0.116 Uiso 1 1 calc R . . C73 C 0.0904(6) 0.3267(10) 0.7146(11) 0.049(8) Uani 1 1 d . . . C74 C 0.0846(7) 0.3556(13) 0.7471(13) 0.065(11) Uani 1 1 d . . . H74A H 0.0819 0.3863 0.7408 0.078 Uiso 1 1 calc R . . C75 C 0.0826(7) 0.3398(16) 0.7907(14) 0.073(12) Uani 1 1 d . . . H75A H 0.0793 0.3603 0.8135 0.088 Uiso 1 1 calc R . . C76 C 0.0853(7) 0.2985(15) 0.7991(13) 0.065(10) Uani 1 1 d U . . H76A H 0.0819 0.2880 0.8276 0.078 Uiso 1 1 calc R . . C77 C 0.0926(8) 0.2695(16) 0.7690(15) 0.086(13) Uani 1 1 d U . . H77A H 0.0957 0.2394 0.7774 0.103 Uiso 1 1 calc R . . C78 C 0.0959(8) 0.2822(13) 0.7246(15) 0.081(13) Uani 1 1 d . . . H78A H 0.1015 0.2617 0.7033 0.097 Uiso 1 1 calc R . . C79 C 0.0870(8) 0.1390(16) 0.5536(16) 0.097(14) Uani 1 1 d DU . . C80 C 0.1018(8) 0.1024(14) 0.5596(13) 0.084(12) Uani 1 1 d DU . . H80A H 0.1182 0.1075 0.5541 0.101 Uiso 1 1 calc R . . C81 C 0.0961(11) 0.0623(17) 0.5718(16) 0.107(16) Uani 1 1 d DU . . H81A H 0.1076 0.0390 0.5696 0.128 Uiso 1 1 calc R . . C82 C 0.0761(17) 0.053(3) 0.586(3) 0.17(3) Uani 1 1 d DU . . H82A H 0.0735 0.0268 0.6023 0.209 Uiso 1 1 calc R . . C83 C 0.0575(16) 0.083(3) 0.579(3) 0.16(3) Uani 1 1 d DU . . H83A H 0.0422 0.0749 0.5888 0.197 Uiso 1 1 calc R . . C84 C 0.0602(11) 0.127(2) 0.555(2) 0.13(2) Uani 1 1 d DU . . H84A H 0.0477 0.1440 0.5429 0.159 Uiso 1 1 calc R . . C85 C 0.2109(6) 0.2183(10) 0.5903(10) 0.041(7) Uani 1 1 d U . . C86 C 0.2204(7) 0.1795(13) 0.5741(14) 0.068(11) Uani 1 1 d . . . H86A H 0.2169 0.1726 0.5446 0.081 Uiso 1 1 calc R . . C87 C 0.2340(8) 0.1504(14) 0.5954(19) 0.091(15) Uani 1 1 d . . . H87A H 0.2401 0.1241 0.5821 0.109 Uiso 1 1 calc R . . C88 C 0.2386(10) 0.161(2) 0.637(2) 0.108(17) Uani 1 1 d U . . H88A H 0.2466 0.1385 0.6533 0.130 Uiso 1 1 calc R . . C89 C 0.2329(9) 0.2010(18) 0.6579(17) 0.099(15) Uani 1 1 d U . . H89A H 0.2388 0.2095 0.6856 0.119 Uiso 1 1 calc R . . C90 C 0.2165(10) 0.2283(18) 0.6314(19) 0.112(17) Uani 1 1 d U . . H90A H 0.2096 0.2542 0.6441 0.135 Uiso 1 1 calc R . . C91 C 0.2033(5) 0.4637(11) 0.6800(10) 0.044(8) Uani 1 1 d . . . C92 C 0.2191(7) 0.4326(14) 0.7033(15) 0.081(13) Uani 1 1 d . . . H92A H 0.2196 0.4017 0.6961 0.098 Uiso 1 1 calc R . . C93 C 0.2335(8) 0.4500(14) 0.7367(15) 0.084(14) Uani 1 1 d . . . H93A H 0.2434 0.4304 0.7530 0.101 Uiso 1 1 calc R . . C94 C 0.2335(6) 0.4949(16) 0.7459(14) 0.079(13) Uani 1 1 d . . . H94A H 0.2428 0.5058 0.7694 0.094 Uiso 1 1 calc R . . C95 C 0.2199(6) 0.5252(13) 0.7210(12) 0.058(9) Uani 1 1 d . . . H95A H 0.2214 0.5568 0.7245 0.069 Uiso 1 1 calc R . . C96 C 0.2050(5) 0.5073(12) 0.6923(10) 0.049(8) Uani 1 1 d . . . H96A H 0.1942 0.5275 0.6789 0.059 Uiso 1 1 calc R . . C1' C 0.3040(16) 0.301(2) 0.3715(17) 0.112(5) Uiso 0.50 1 d PD A -1 C5' C 0.3028(15) 0.2778(18) 0.4119(17) 0.112(5) Uiso 0.50 1 d PD A -1 C2' C 0.3042(13) 0.2294(18) 0.410(2) 0.112(5) Uiso 0.50 1 d PD A -1 C6' C 0.3053(18) 0.203(2) 0.3715(19) 0.112(5) Uiso 0.50 1 d PD A -1 C9' C 0.3065(17) 0.2773(19) 0.3307(19) 0.112(5) Uiso 0.50 1 d PD A -1 C10' C 0.3082(16) 0.2288(19) 0.3315(19) 0.112(5) Uiso 0.50 1 d PD A -1 C22' C 0.2909(15) 0.163(3) 0.3622(18) 0.112(5) Uiso 0.50 1 d PD A -1 C8' C 0.2890(14) 0.341(2) 0.3630(17) 0.112(5) Uiso 0.50 1 d PD A -1 C3' C 0.2867(10) 0.2925(18) 0.445(2) 0.112(5) Uiso 0.50 1 d PD A -1 C11' C 0.2767(10) 0.2527(17) 0.465(2) 0.112(5) Uiso 0.50 1 d PD A -1 C7' C 0.2872(15) 0.214(2) 0.443(3) 0.112(5) Uiso 0.50 1 d PD A -1 C4' C 0.2817(11) 0.340(2) 0.3179(17) 0.112(5) Uiso 0.50 1 d PD A -1 C21' C 0.2923(15) 0.301(2) 0.297(2) 0.112(5) Uiso 0.50 1 d PD A -1 C24' C 0.2805(12) 0.2754(19) 0.265(3) 0.112(5) Uiso 0.50 1 d PD A -1 C13' C 0.2569(12) 0.350(3) 0.307(2) 0.112(5) Uiso 0.50 1 d PD A -1 C18' C 0.2834(10) 0.166(2) 0.3174(18) 0.112(5) Uiso 0.50 1 d PD A -1 C16' C 0.2958(14) 0.204(2) 0.297(2) 0.112(5) Uiso 0.50 1 d PD A -1 C27' C 0.2820(14) 0.2269(19) 0.263(2) 0.112(5) Uiso 0.50 1 d PD A -1 C17F C 0.2590(12) 0.2094(18) 0.246(2) 0.112(5) Uiso 0.50 1 d PD A -1 C29' C 0.2732(12) 0.356(3) 0.3964(19) 0.112(5) Uiso 0.50 1 d PD A -1 C25' C 0.2720(12) 0.329(3) 0.436(2) 0.112(5) Uiso 0.50 1 d PD A -1 C30' C 0.2494(11) 0.371(3) 0.3866(19) 0.112(5) Uiso 0.50 1 d PD A -1 C19' C 0.2420(11) 0.363(4) 0.342(2) 0.112(5) Uiso 0.50 1 d PD A -1 C23F C 0.2424(11) 0.247(2) 0.245(3) 0.112(5) Uiso 0.50 1 d PD A -1 C23' C 0.2560(9) 0.2885(19) 0.253(3) 0.112(5) Uiso 0.50 1 d PD A -1 C28' C 0.2453(11) 0.328(3) 0.273(3) 0.112(5) Uiso 0.50 1 d PD A -1 C24F C 0.2183(14) 0.246(3) 0.262(4) 0.112(5) Uiso 0.50 1 d PD A -1 C17' C 0.2460(11) 0.178(4) 0.273(2) 0.112(5) Uiso 0.50 1 d PD A -1 C28F C 0.2596(11) 0.152(3) 0.304(2) 0.112(5) Uiso 0.50 1 d PD A -1 C19F C 0.2445(11) 0.139(4) 0.341(2) 0.112(5) Uiso 0.50 1 d PD A -1 C14F C 0.2741(10) 0.174(2) 0.437(2) 0.112(5) Uiso 0.50 1 d PD A -1 C30F C 0.2507(13) 0.133(3) 0.3856(19) 0.112(5) Uiso 0.50 1 d PD A -1 C26F C 0.2740(13) 0.150(3) 0.3952(19) 0.112(5) Uiso 0.50 1 d PD A -1 C9F C 0.194(2) 0.228(3) 0.321(3) 0.112(5) Uiso 0.50 1 d PD A -1 C21F C 0.2065(18) 0.213(3) 0.283(3) 0.112(5) Uiso 0.50 1 d PD A -1 C4F C 0.2208(13) 0.174(3) 0.287(2) 0.112(5) Uiso 0.50 1 d PD A -1 C13F C 0.2219(13) 0.150(3) 0.329(3) 0.112(5) Uiso 0.50 1 d PD A -1 C10F C 0.1904(16) 0.273(2) 0.317(3) 0.112(5) Uiso 0.50 1 d PD A -1 C16F C 0.2068(13) 0.285(3) 0.283(3) 0.112(5) Uiso 0.50 1 d PD A -1 C27F C 0.2217(14) 0.326(2) 0.292(3) 0.112(5) Uiso 0.50 1 d PD A -1 C18F C 0.2191(14) 0.351(3) 0.332(2) 0.112(5) Uiso 0.50 1 d PD A -1 C22F C 0.2055(16) 0.335(4) 0.367(2) 0.112(5) Uiso 0.50 1 d PD A -1 C6F C 0.191(2) 0.297(3) 0.356(3) 0.112(5) Uiso 0.50 1 d PD A -1 C15' C 0.2475(9) 0.328(2) 0.454(3) 0.112(5) Uiso 0.50 1 d PD A -1 C20' C 0.2361(11) 0.353(3) 0.4218(18) 0.112(5) Uiso 0.50 1 d PD A -1 C26' C 0.2123(13) 0.337(3) 0.412(2) 0.112(5) Uiso 0.50 1 d PD A -1 C15F C 0.2489(10) 0.175(2) 0.450(3) 0.112(5) Uiso 0.50 1 d PD A -1 C29F C 0.2357(10) 0.144(2) 0.422(3) 0.112(5) Uiso 0.50 1 d PD A -1 C14' C 0.2039(18) 0.295(2) 0.422(3) 0.112(5) Uiso 0.50 1 d PD A -1 C2F C 0.191(2) 0.269(2) 0.392(3) 0.112(5) Uiso 0.50 1 d PD A -1 C7F C 0.2109(8) 0.2726(15) 0.459(2) 0.112(5) Uiso 0.50 1 d PGD A -1 C3F C 0.2133(8) 0.2252(14) 0.4606(17) 0.112(5) Uiso 0.50 1 d PGD A -1 C11F C 0.2377(8) 0.2149(14) 0.4666(19) 0.112(5) Uiso 0.50 1 d PGD A -1 C12F C 0.2505(7) 0.2559(17) 0.469(2) 0.112(5) Uiso 0.50 1 d PGD A -1 C12' C 0.2339(9) 0.2915(14) 0.465(2) 0.112(5) Uiso 0.50 1 d PGD A -1 C5F C 0.2062(14) 0.201(2) 0.4257(18) 0.112(5) Uiso 0.50 1 d PGD A -1 C25F C 0.2148(12) 0.1623(19) 0.404(2) 0.112(5) Uiso 0.50 1 d PGD A -1 C8F C 0.2052(13) 0.162(2) 0.3616(17) 0.112(5) Uiso 0.50 1 d PGD A -1 C1F C 0.1906(12) 0.200(2) 0.3567(15) 0.112(5) Uiso 0.50 1 d PGD A -1 C20F C 0.1912(12) 0.2246(19) 0.3963(19) 0.112(5) Uiso 0.50 1 d PGD A -1 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 0.029(2) 0.038(3) 0.035(3) -0.0030(19) 0.001(2) -0.0007(18) Mn2 0.028(2) 0.032(2) 0.041(3) -0.002(2) 0.002(2) 0.0025(18) Mn3 0.028(2) 0.037(3) 0.040(3) -0.002(2) 0.003(2) 0.0009(18) Mn4 0.033(2) 0.039(3) 0.035(3) -0.004(2) 0.002(2) 0.0034(19) S1 0.033(4) 0.033(4) 0.038(5) -0.004(3) 0.006(3) 0.002(3) S2 0.029(4) 0.043(4) 0.044(5) -0.006(4) 0.000(4) -0.003(3) S3 0.038(4) 0.035(4) 0.037(5) -0.003(3) 0.005(3) 0.001(3) S4 0.029(4) 0.042(4) 0.046(5) -0.005(4) 0.001(4) 0.002(3) S5 0.028(4) 0.034(4) 0.035(5) -0.006(3) 0.002(3) 0.000(3) S6 0.028(4) 0.039(4) 0.040(5) -0.004(3) 0.004(3) -0.001(3) S7 0.034(4) 0.041(4) 0.036(5) -0.005(3) 0.000(3) 0.007(3) S8 0.028(4) 0.040(4) 0.047(5) -0.011(4) 0.007(4) 0.001(3) O1 0.034(11) 0.042(12) 0.041(13) -0.011(9) 0.000(9) -0.008(9) O2 0.030(10) 0.039(11) 0.034(12) -0.008(9) 0.005(9) 0.004(8) O3 0.046(13) 0.050(13) 0.048(15) -0.004(11) 0.001(11) 0.009(10) O4 0.038(11) 0.033(11) 0.042(13) -0.001(9) 0.001(10) 0.009(8) O5 0.037(11) 0.035(10) 0.023(11) 0.003(8) -0.006(9) -0.015(8) O6 0.031(10) 0.035(11) 0.037(12) -0.001(9) 0.004(9) 0.013(8) O7 0.038(11) 0.047(12) 0.040(13) -0.002(10) -0.011(10) 0.006(9) O8 0.026(10) 0.040(11) 0.032(12) -0.001(9) -0.003(9) 0.002(8) C1 0.011(14) 0.037(18) 0.08(3) -0.001(16) 0.005(15) 0.012(12) C2 0.033(16) 0.036(17) 0.04(2) -0.011(14) 0.016(14) -0.002(12) C3 0.051(19) 0.038(16) 0.023(17) -0.002(13) 0.007(14) -0.006(14) C4 0.029(16) 0.034(17) 0.07(3) 0.003(16) 0.007(16) 0.013(13) C5 0.016(14) 0.06(2) 0.06(2) -0.001(16) -0.004(14) -0.008(13) C6 0.041(18) 0.040(18) 0.05(2) -0.010(15) 0.011(16) 0.002(14) C7 0.031(16) 0.037(16) 0.021(17) -0.001(12) -0.010(13) 0.000(12) C8 0.041(18) 0.040(18) 0.06(2) -0.018(15) -0.013(16) 0.000(14) C9 0.037(17) 0.07(2) 0.019(17) -0.004(15) -0.004(13) 0.012(15) C10 0.08(2) 0.06(2) 0.026(18) -0.018(16) -0.019(18) 0.008(18) C11 0.050(18) 0.07(2) 0.046(19) -0.024(17) 0.006(16) -0.012(16) C12 0.030(16) 0.045(17) 0.028(17) -0.007(13) -0.002(13) 0.002(13) C13 0.014(13) 0.045(18) 0.04(2) 0.003(15) 0.010(13) 0.009(12) C14 0.041(17) 0.029(15) 0.03(2) -0.008(13) -0.003(14) 0.002(12) C15 0.035(16) 0.035(16) 0.033(18) -0.018(13) -0.010(14) 0.020(13) C16 0.033(15) 0.045(17) 0.020(16) -0.007(13) -0.007(12) 0.002(13) C17 0.052(19) 0.022(14) 0.04(2) 0.008(13) 0.014(15) 0.011(13) C18 0.028(15) 0.031(16) 0.04(2) -0.013(13) 0.009(14) 0.001(12) C19 0.032(17) 0.037(18) 0.05(2) -0.015(15) 0.003(15) 0.007(13) C20 0.044(19) 0.042(18) 0.028(18) 0.002(13) 0.004(15) -0.014(14) C21 0.06(2) 0.035(17) 0.05(2) -0.009(15) 0.015(17) -0.009(14) C22 0.06(2) 0.035(17) 0.06(2) 0.005(16) 0.030(19) 0.012(15) C23 0.040(18) 0.038(17) 0.06(2) 0.007(16) 0.000(17) -0.003(14) C24 0.016(14) 0.06(2) 0.038(19) -0.007(14) 0.012(13) -0.014(13) C25 0.030(16) 0.043(18) 0.031(19) -0.010(14) 0.003(14) -0.012(13) C26 0.016(12) 0.036(14) 0.032(16) -0.011(12) 0.011(11) 0.000(10) C27 0.047(19) 0.039(17) 0.05(2) -0.008(15) 0.005(16) -0.009(14) C28 0.038(17) 0.039(17) 0.05(2) 0.007(15) 0.001(15) 0.008(14) C29 0.07(2) 0.027(16) 0.06(2) 0.009(15) -0.002(19) 0.012(15) C30 0.023(14) 0.040(17) 0.028(18) 0.000(13) 0.005(13) 0.003(12) C31 0.032(16) 0.042(18) 0.023(17) -0.004(12) 0.002(13) -0.017(13) C32 0.029(16) 0.032(16) 0.05(2) -0.016(13) -0.008(14) 0.003(12) C33 0.042(18) 0.036(17) 0.05(2) -0.005(14) 0.020(15) -0.015(14) C34 0.042(19) 0.038(18) 0.08(3) 0.014(17) -0.006(18) 0.008(14) C35 0.025(16) 0.033(17) 0.07(2) 0.006(15) 0.008(16) 0.010(12) C36 0.044(18) 0.022(15) 0.05(2) -0.003(13) -0.002(15) 0.001(13) C37 0.023(14) 0.043(17) 0.014(15) -0.007(12) 0.006(12) 0.006(12) C38 0.040(15) 0.039(15) 0.005(13) -0.002(11) 0.002(11) 0.002(12) C39 0.039(17) 0.040(17) 0.04(2) -0.002(14) 0.012(15) 0.001(13) C40 0.036(17) 0.042(17) 0.029(17) 0.001(13) 0.001(14) -0.007(13) C41 0.040(16) 0.044(17) 0.020(16) -0.011(13) -0.009(13) 0.005(13) C42 0.031(15) 0.030(16) 0.036(18) 0.002(13) 0.005(13) 0.010(12) C43 0.026(15) 0.035(16) 0.04(2) -0.004(13) 0.009(14) -0.004(12) C44 0.032(15) 0.022(14) 0.038(19) -0.006(12) 0.011(13) 0.001(11) C45 0.026(14) 0.028(14) 0.034(17) 0.007(12) 0.002(12) 0.008(11) C46 0.022(14) 0.050(18) 0.042(19) 0.001(15) 0.010(13) -0.003(12) C47 0.041(17) 0.042(16) 0.028(17) -0.012(13) -0.005(14) 0.007(13) C48 0.028(16) 0.052(18) 0.035(19) -0.005(14) 0.009(13) -0.007(13) C49 0.019(15) 0.05(2) 0.08(3) 0.014(18) 0.011(16) 0.008(14) C50 0.08(3) 0.08(3) 0.06(3) 0.01(2) -0.05(2) 0.02(2) C51 0.07(3) 0.07(3) 0.07(3) -0.01(2) -0.02(2) 0.01(2) C52 0.03(2) 0.07(3) 0.14(5) 0.05(3) -0.01(2) 0.001(18) C53 0.042(19) 0.05(2) 0.08(3) 0.011(19) 0.00(2) 0.010(15) C54 0.05(2) 0.05(2) 0.07(3) 0.013(18) -0.023(19) 0.006(17) C55 0.07(2) 0.09(2) 0.08(2) 0.00(2) -0.014(19) 0.027(19) C56 0.11(3) 0.13(3) 0.11(3) -0.01(2) 0.00(2) 0.03(2) C57 0.13(3) 0.15(3) 0.13(3) 0.01(3) 0.01(3) 0.04(3) C58 0.17(4) 0.17(4) 0.15(4) -0.01(3) 0.00(3) 0.02(3) C59 0.18(4) 0.16(4) 0.16(4) -0.01(3) -0.02(3) 0.02(3) C60 0.11(3) 0.12(3) 0.09(3) -0.01(2) 0.00(2) 0.04(2) C61 0.045(19) 0.044(18) 0.07(3) -0.007(17) -0.011(18) 0.003(15) C62 0.06(2) 0.07(2) 0.05(3) -0.013(18) -0.014(19) -0.003(18) C63 0.08(3) 0.07(3) 0.03(2) 0.005(18) 0.00(2) 0.00(2) C64 0.09(3) 0.09(3) 0.05(3) 0.02(2) 0.02(2) -0.02(2) C65 0.06(2) 0.09(3) 0.05(2) -0.02(2) 0.02(2) -0.01(2) C66 0.05(2) 0.06(2) 0.06(2) 0.002(18) 0.011(18) -0.014(17) C67 0.06(2) 0.06(2) 0.06(3) 0.02(2) 0.03(2) -0.006(17) C68 0.13(4) 0.09(3) 0.12(5) 0.07(3) -0.02(4) 0.00(3) C69 0.16(6) 0.10(4) 0.17(6) 0.08(4) 0.08(5) 0.02(4) C70 0.19(6) 0.09(4) 0.09(4) 0.05(3) 0.06(4) 0.05(4) C71 0.18(6) 0.05(3) 0.14(6) 0.02(3) 0.03(5) 0.00(3) C72 0.17(5) 0.03(2) 0.09(3) 0.03(2) 0.04(3) 0.02(2) C73 0.06(2) 0.043(18) 0.05(2) -0.001(16) -0.005(17) -0.012(15) C74 0.07(3) 0.07(3) 0.05(3) -0.01(2) 0.00(2) 0.00(2) C75 0.08(3) 0.09(3) 0.05(3) 0.02(2) 0.02(2) 0.00(2) C76 0.06(2) 0.09(3) 0.05(2) 0.027(19) 0.002(19) 0.00(2) C77 0.10(4) 0.08(3) 0.08(3) 0.03(2) -0.01(3) 0.01(2) C78 0.09(3) 0.06(2) 0.10(4) 0.04(2) -0.02(3) 0.02(2) C79 0.08(2) 0.09(2) 0.12(3) 0.00(2) 0.03(2) -0.01(2) C80 0.07(2) 0.07(2) 0.11(3) 0.03(2) 0.03(2) 0.017(18) C81 0.10(3) 0.09(3) 0.13(3) 0.03(2) 0.01(2) 0.01(2) C82 0.18(4) 0.17(4) 0.18(4) 0.01(3) 0.00(3) 0.00(3) C83 0.16(4) 0.15(3) 0.19(4) 0.01(3) 0.01(3) -0.01(3) C84 0.12(3) 0.13(3) 0.15(3) 0.02(3) 0.01(3) -0.01(2) C85 0.046(18) 0.046(19) 0.031(18) 0.011(14) 0.002(15) -0.007(15) C86 0.07(3) 0.07(3) 0.06(3) 0.01(2) 0.01(2) 0.01(2) C87 0.09(3) 0.06(3) 0.13(5) 0.01(3) -0.04(3) 0.02(2) C88 0.11(3) 0.11(3) 0.10(3) 0.02(2) -0.02(2) 0.01(2) C89 0.10(3) 0.11(3) 0.08(3) 0.03(2) -0.02(2) 0.01(2) C90 0.13(3) 0.10(3) 0.10(3) 0.00(2) -0.03(2) 0.00(2) C91 0.036(17) 0.06(2) 0.038(19) -0.016(16) 0.010(14) -0.007(15) C92 0.06(3) 0.07(3) 0.11(4) -0.02(2) -0.01(2) 0.01(2) C93 0.08(3) 0.06(3) 0.11(4) 0.00(2) -0.06(3) 0.01(2) C94 0.04(2) 0.11(4) 0.08(3) -0.03(3) 0.00(2) -0.02(2) C95 0.037(18) 0.07(2) 0.07(3) -0.007(19) -0.014(18) 0.007(17) C96 0.032(17) 0.07(2) 0.04(2) -0.015(17) 0.002(15) 0.024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 2.073(18) . ? Mn1 O4 2.09(2) . ? Mn1 O8 2.176(18) . ? Mn1 O1 2.18(2) . ? Mn1 S5 2.646(9) . ? Mn1 S1 2.685(8) . ? Mn2 O5 2.094(18) . ? Mn2 O2 2.142(19) . ? Mn2 O1 2.15(2) . ? Mn2 O6 2.175(17) . ? Mn2 S2 2.679(9) . ? Mn2 S6 2.689(9) . ? Mn3 O7 2.08(2) . ? Mn3 O2 2.117(19) . ? Mn3 O3 2.18(2) . ? Mn3 O6 2.188(19) . ? Mn3 S7 2.677(8) . ? Mn3 S3 2.715(9) . ? Mn4 O7 2.09(2) . ? Mn4 O4 2.131(18) . ? Mn4 O8 2.179(19) . ? Mn4 O3 2.19(2) . ? Mn4 S8 2.659(9) . ? Mn4 S4 2.699(9) . ? S1 C2 1.79(3) . ? S1 C24 1.81(3) . ? S2 C6 1.74(3) . ? S2 C8 1.77(3) . ? S3 C12 1.80(3) . ? S3 C14 1.81(3) . ? S4 C18 1.79(3) . ? S4 C20 1.81(3) . ? S5 C48 1.77(3) . ? S5 C26 1.79(3) . ? S6 C30 1.79(3) . ? S6 C32 1.80(3) . ? S7 C36 1.77(3) . ? S7 C38 1.80(3) . ? S8 C42 1.80(3) . ? S8 C44 1.80(3) . ? O1 C1 1.26(3) . ? O2 C7 1.29(3) . ? O3 C13 1.32(3) . ? O4 C19 1.35(4) . ? O5 C25 1.26(3) . ? O6 C31 1.29(3) . ? O7 C37 1.32(3) . ? O8 C43 1.28(3) . ? C1 C2 1.42(4) . ? C1 C6 1.48(4) . ? C2 C3 1.38(4) . ? C3 C4 1.38(4) . ? C3 H3A 0.9500 . ? C4 C5 1.36(4) . ? C4 C49 1.50(4) . ? C5 C6 1.40(4) . ? C5 H5A 0.9500 . ? C7 C8 1.37(4) . ? C7 C12 1.42(4) . ? C8 C9 1.46(4) . ? C9 C10 1.32(4) . ? C9 H9A 0.9500 . ? C10 C11 1.48(5) . ? C10 C55 1.49(5) . ? C11 C12 1.25(4) . ? C11 H11A 0.9500 . ? C13 C14 1.35(4) . ? C13 C18 1.41(4) . ? C14 C15 1.39(4) . ? C15 C16 1.37(4) . ? C15 H15A 0.9500 . ? C16 C17 1.34(4) . ? C16 C61 1.46(5) . ? C17 C18 1.39(4) . ? C17 H17A 0.9500 . ? C19 C24 1.34(4) . ? C19 C20 1.37(4) . ? C20 C21 1.40(4) . ? C21 C22 1.36(4) . ? C21 H21A 0.9500 . ? C22 C23 1.45(4) . ? C22 C67 1.50(5) . ? C23 C24 1.36(4) . ? C23 H23A 0.9500 . ? C25 C30 1.43(4) . ? C25 C26 1.45(4) . ? C26 C27 1.38(4) . ? C27 C28 1.39(4) . ? C27 H27A 0.9500 . ? C28 C29 1.44(5) . ? C28 C73 1.50(5) . ? C29 C30 1.37(4) . ? C29 H29A 0.9500 . ? C31 C32 1.39(4) . ? C31 C36 1.43(4) . ? C32 C33 1.41(4) . ? C33 C34 1.36(4) . ? C33 H33A 0.9500 . ? C34 C35 1.33(4) . ? C34 C79 1.44(5) . ? C35 C36 1.37(4) . ? C35 H35A 0.9500 . ? C37 C38 1.38(4) . ? C37 C42 1.40(4) . ? C38 C39 1.39(4) . ? C39 C40 1.34(4) . ? C39 H39A 0.9500 . ? C40 C41 1.40(4) . ? C40 C85 1.45(4) . ? C41 C42 1.40(4) . ? C41 H41A 0.9500 . ? C43 C44 1.43(4) . ? C43 C48 1.43(4) . ? C44 C45 1.35(4) . ? C45 C46 1.40(4) . ? C45 H45A 0.9500 . ? C46 C47 1.38(4) . ? C46 C91 1.46(4) . ? C47 C48 1.37(4) . ? C47 H47A 0.9500 . ? C49 C54 1.34(5) . ? C49 C50 1.44(5) . ? C50 C51 1.43(5) . ? C50 H50A 0.9500 . ? C51 C52 1.42(6) . ? C51 H51A 0.9500 . ? C52 C53 1.35(6) . ? C52 H52A 0.9500 . ? C53 C54 1.38(5) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C55 C56 1.46(7) . ? C55 C60 1.47(6) . ? C56 C57 1.37(8) . ? C56 H56A 0.9500 . ? C57 C58 1.34(8) . ? C57 H57A 0.9500 . ? C58 C59 1.44(9) . ? C58 H58A 0.9500 . ? C59 C60 1.40(8) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? C61 C66 1.40(4) . ? C61 C62 1.40(5) . ? C62 C63 1.43(5) . ? C62 H62A 0.9500 . ? C63 C64 1.29(5) . ? C63 H63A 0.9500 . ? C64 C65 1.43(5) . ? C64 H64A 0.9500 . ? C65 C66 1.36(5) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C67 C72 1.28(5) . ? C67 C68 1.29(6) . ? C68 C69 1.50(6) . ? C68 H68A 0.9500 . ? C69 C70 1.54(8) . ? C69 H69A 0.9500 . ? C70 C71 1.28(7) . ? C70 H70A 0.9500 . ? C71 C72 1.38(6) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C73 C74 1.36(5) . ? C73 C78 1.40(5) . ? C74 C75 1.43(5) . ? C74 H74A 0.9500 . ? C75 C76 1.27(5) . ? C75 H75A 0.9500 . ? C76 C77 1.33(6) . ? C76 H76A 0.9500 . ? C77 C78 1.43(6) . ? C77 H77A 0.9500 . ? C78 H78A 0.9500 . ? C79 C80 1.38(6) . ? C79 C84 1.55(7) . ? C80 C81 1.30(6) . ? C80 H80A 0.9500 . ? C81 C82 1.24(9) . ? C81 H81A 0.9500 . ? C82 C83 1.38(10) . ? C82 H82A 0.9500 . ? C83 C84 1.51(9) . ? C83 H83A 0.9500 . ? C84 H84A 0.9500 . ? C85 C90 1.34(6) . ? C85 C86 1.37(5) . ? C86 C87 1.33(5) . ? C86 H86A 0.9500 . ? C87 C88 1.33(7) . ? C87 H87A 0.9500 . ? C88 C89 1.41(7) . ? C88 H88A 0.9500 . ? C89 C90 1.48(7) . ? C89 H89A 0.9500 . ? C90 H90A 0.9500 . ? C91 C96 1.36(4) . ? C91 C92 1.47(5) . ? C92 C93 1.41(5) . ? C92 H92A 0.9500 . ? C93 C94 1.37(5) . ? C93 H93A 0.9500 . ? C94 C95 1.41(5) . ? C94 H94A 0.9500 . ? C95 C96 1.33(4) . ? C95 H95A 0.9500 . ? C96 H96A 0.9500 . ? C1' C5' 1.43(4) . ? C1' C9' 1.45(4) . ? C1' C8' 1.48(4) . ? C5' C3' 1.43(4) . ? C5' C2' 1.45(4) . ? C2' C6' 1.42(4) . ? C2' C7' 1.46(4) . ? C6' C10' 1.47(4) . ? C6' C22' 1.47(4) . ? C9' C10' 1.45(4) . ? C9' C21' 1.48(4) . ? C10' C16' 1.47(4) . ? C22' C26F 1.44(4) . ? C22' C18' 1.45(4) . ? C8' C29' 1.43(4) . ? C8' C4' 1.45(4) . ? C3' C25' 1.39(4) . ? C3' C11' 1.45(4) . ? C11' C7' 1.46(4) . ? C11' C12F 1.48(5) . ? C7' C14F 1.43(4) . ? C4' C21' 1.44(4) . ? C4' C13' 1.46(4) . ? C21' C24' 1.43(4) . ? C24' C27' 1.45(4) . ? C24' C23' 1.47(4) . ? C13' C28' 1.41(5) . ? C13' C19' 1.42(5) . ? C18' C28F 1.45(4) . ? C18' C16' 1.47(4) . ? C16' C27' 1.47(4) . ? C27' C17F 1.49(4) . ? C17F C17' 1.44(6) . ? C17F C23F 1.45(6) . ? C29' C30' 1.44(4) . ? C29' C25' 1.48(4) . ? C25' C15' 1.47(4) . ? C30' C20' 1.43(4) . ? C30' C19' 1.44(4) . ? C19' C18F 1.37(6) . ? C23F C24F 1.45(6) . ? C23F C23' 1.48(4) . ? C23' C28' 1.46(4) . ? C28' C27F 1.45(6) . ? C24F C21F 1.37(6) . ? C24F C16F 1.48(6) . ? C17' C28F 1.45(4) . ? C17' C4F 1.48(6) . ? C28F C19F 1.47(4) . ? C19F C13F 1.36(6) . ? C19F C30F 1.43(6) . ? C14F C26F 1.46(4) . ? C14F C15F 1.47(4) . ? C30F C26F 1.44(4) . ? C30F C29F 1.45(6) . ? C9F C10F 1.37(6) . ? C9F C1F 1.40(6) . ? C9F C21F 1.42(6) . ? C21F C4F 1.41(6) . ? C4F C13F 1.50(4) . ? C13F C8F 1.41(5) . ? C10F C6F 1.39(6) . ? C10F C16F 1.45(6) . ? C16F C27F 1.49(4) . ? C27F C18F 1.45(6) . ? C18F C22F 1.40(4) . ? C22F C6F 1.43(4) . ? C22F C26' 1.44(6) . ? C6F C2F 1.40(6) . ? C15' C12' 1.36(4) . ? C15' C20' 1.39(4) . ? C20' C26' 1.44(4) . ? C26' C14' 1.38(5) . ? C15F C11F 1.44(4) . ? C15F C29F 1.45(4) . ? C29F C25F 1.41(5) . ? C14' C7F 1.39(4) . ? C14' C2F 1.40(6) . ? C2F C20F 1.33(6) . ? C7F C3F 1.4200 . ? C7F C12' 1.4200 . ? C3F C5F 1.35(3) . ? C3F C11F 1.4200 . ? C11F C12F 1.4200 . ? C12F C12' 1.4200 . ? C5F C20F 1.4200 . ? C5F C25F 1.4200 . ? C25F C8F 1.4200 . ? C8F C1F 1.4200 . ? C1F C20F 1.4200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 O4 145.4(8) . . ? O5 Mn1 O8 88.0(7) . . ? O4 Mn1 O8 72.6(7) . . ? O5 Mn1 O1 71.9(7) . . ? O4 Mn1 O1 94.7(8) . . ? O8 Mn1 O1 123.2(7) . . ? O5 Mn1 S5 77.4(5) . . ? O4 Mn1 S5 122.5(6) . . ? O8 Mn1 S5 75.2(5) . . ? O1 Mn1 S5 142.7(6) . . ? O5 Mn1 S1 127.3(6) . . ? O4 Mn1 S1 76.1(5) . . ? O8 Mn1 S1 144.6(5) . . ? O1 Mn1 S1 75.0(6) . . ? S5 Mn1 S1 109.4(3) . . ? O5 Mn2 O2 145.1(7) . . ? O5 Mn2 O1 72.1(7) . . ? O2 Mn2 O1 93.7(8) . . ? O5 Mn2 O6 89.0(7) . . ? O2 Mn2 O6 72.6(7) . . ? O1 Mn2 O6 124.3(7) . . ? O5 Mn2 S2 127.9(6) . . ? O2 Mn2 S2 75.4(5) . . ? O1 Mn2 S2 75.3(6) . . ? O6 Mn2 S2 143.1(6) . . ? O5 Mn2 S6 76.0(5) . . ? O2 Mn2 S6 124.8(6) . . ? O1 Mn2 S6 141.5(6) . . ? O6 Mn2 S6 75.4(5) . . ? S2 Mn2 S6 109.6(3) . . ? O7 Mn3 O2 145.7(8) . . ? O7 Mn3 O3 72.9(8) . . ? O2 Mn3 O3 93.7(8) . . ? O7 Mn3 O6 88.4(8) . . ? O2 Mn3 O6 72.8(7) . . ? O3 Mn3 O6 123.9(8) . . ? O7 Mn3 S7 76.3(6) . . ? O2 Mn3 S7 123.2(6) . . ? O3 Mn3 S7 143.1(6) . . ? O6 Mn3 S7 74.4(5) . . ? O7 Mn3 S3 127.2(6) . . ? O2 Mn3 S3 75.8(6) . . ? O3 Mn3 S3 74.1(6) . . ? O6 Mn3 S3 144.4(5) . . ? S7 Mn3 S3 110.6(3) . . ? O7 Mn4 O4 144.0(8) . . ? O7 Mn4 O8 88.6(8) . . ? O4 Mn4 O8 71.9(7) . . ? O7 Mn4 O3 72.5(8) . . ? O4 Mn4 O3 92.8(8) . . ? O8 Mn4 O3 122.9(8) . . ? O7 Mn4 S8 77.6(6) . . ? O4 Mn4 S8 124.2(6) . . ? O8 Mn4 S8 76.9(5) . . ? O3 Mn4 S8 142.9(6) . . ? O7 Mn4 S4 128.3(6) . . ? O4 Mn4 S4 76.1(6) . . ? O8 Mn4 S4 143.1(5) . . ? O3 Mn4 S4 75.8(6) . . ? S8 Mn4 S4 107.8(3) . . ? C2 S1 C24 102.1(13) . . ? C2 S1 Mn1 96.8(10) . . ? C24 S1 Mn1 93.9(11) . . ? C6 S2 C8 100.2(15) . . ? C6 S2 Mn2 96.6(11) . . ? C8 S2 Mn2 94.4(11) . . ? C12 S3 C14 102.3(13) . . ? C12 S3 Mn3 95.0(10) . . ? C14 S3 Mn3 94.5(10) . . ? C18 S4 C20 98.8(13) . . ? C18 S4 Mn4 95.3(10) . . ? C20 S4 Mn4 95.1(10) . . ? C48 S5 C26 103.2(13) . . ? C48 S5 Mn1 93.6(10) . . ? C26 S5 Mn1 94.9(9) . . ? C30 S6 C32 101.9(13) . . ? C30 S6 Mn2 95.0(9) . . ? C32 S6 Mn2 92.3(11) . . ? C36 S7 C38 101.6(13) . . ? C36 S7 Mn3 95.3(10) . . ? C38 S7 Mn3 94.2(9) . . ? C42 S8 C44 102.8(13) . . ? C42 S8 Mn4 94.2(9) . . ? C44 S8 Mn4 92.9(10) . . ? C1 O1 Mn2 125.5(18) . . ? C1 O1 Mn1 123.9(19) . . ? Mn2 O1 Mn1 99.5(9) . . ? C7 O2 Mn3 126.6(17) . . ? C7 O2 Mn2 126.3(17) . . ? Mn3 O2 Mn2 101.0(8) . . ? C13 O3 Mn3 124.7(18) . . ? C13 O3 Mn4 122.5(18) . . ? Mn3 O3 Mn4 98.3(9) . . ? C19 O4 Mn1 126.8(17) . . ? C19 O4 Mn4 124.8(18) . . ? Mn1 O4 Mn4 102.4(8) . . ? C25 O5 Mn1 125.1(17) . . ? C25 O5 Mn2 125.8(16) . . ? Mn1 O5 Mn2 104.9(8) . . ? C31 O6 Mn2 119.7(17) . . ? C31 O6 Mn3 121.2(17) . . ? Mn2 O6 Mn3 97.8(8) . . ? C37 O7 Mn3 126.9(18) . . ? C37 O7 Mn4 124.2(17) . . ? Mn3 O7 Mn4 105.3(9) . . ? C43 O8 Mn1 119.5(17) . . ? C43 O8 Mn4 116.5(16) . . ? Mn1 O8 Mn4 98.3(8) . . ? O1 C1 C2 125(3) . . ? O1 C1 C6 121(3) . . ? C2 C1 C6 114(3) . . ? C3 C2 C1 125(3) . . ? C3 C2 S1 119(2) . . ? C1 C2 S1 116(2) . . ? C2 C3 C4 120(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 119(3) . . ? C5 C4 C49 122(3) . . ? C3 C4 C49 118(3) . . ? C4 C5 C6 124(3) . . ? C4 C5 H5A 118.2 . . ? C6 C5 H5A 118.2 . . ? C5 C6 C1 119(3) . . ? C5 C6 S2 123(2) . . ? C1 C6 S2 118(2) . . ? O2 C7 C8 121(3) . . ? O2 C7 C12 123(2) . . ? C8 C7 C12 116(3) . . ? C7 C8 C9 120(3) . . ? C7 C8 S2 121(3) . . ? C9 C8 S2 118(2) . . ? C10 C9 C8 120(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 118(3) . . ? C9 C10 C55 118(3) . . ? C11 C10 C55 124(3) . . ? C12 C11 C10 121(3) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C7 125(3) . . ? C11 C12 S3 117(2) . . ? C7 C12 S3 118(2) . . ? O3 C13 C14 121(3) . . ? O3 C13 C18 122(3) . . ? C14 C13 C18 117(3) . . ? C13 C14 C15 120(3) . . ? C13 C14 S3 121(2) . . ? C15 C14 S3 119(2) . . ? C16 C15 C14 123(3) . . ? C16 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? C17 C16 C15 117(3) . . ? C17 C16 C61 121(3) . . ? C15 C16 C61 122(3) . . ? C16 C17 C18 123(3) . . ? C16 C17 H17A 118.7 . . ? C18 C17 H17A 118.7 . . ? C17 C18 C13 120(3) . . ? C17 C18 S4 120(2) . . ? C13 C18 S4 120(2) . . ? C24 C19 O4 120(3) . . ? C24 C19 C20 117(3) . . ? O4 C19 C20 123(3) . . ? C19 C20 C21 123(3) . . ? C19 C20 S4 119(2) . . ? C21 C20 S4 118(2) . . ? C22 C21 C20 120(3) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 116(3) . . ? C21 C22 C67 124(3) . . ? C23 C22 C67 119(3) . . ? C24 C23 C22 120(3) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C19 C24 C23 123(3) . . ? C19 C24 S1 121(3) . . ? C23 C24 S1 116(2) . . ? O5 C25 C30 124(3) . . ? O5 C25 C26 123(2) . . ? C30 C25 C26 112(3) . . ? C27 C26 C25 124(3) . . ? C27 C26 S5 119(2) . . ? C25 C26 S5 116(2) . . ? C26 C27 C28 120(3) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C27 C28 C29 119(3) . . ? C27 C28 C73 121(3) . . ? C29 C28 C73 120(3) . . ? C30 C29 C28 119(3) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? C29 C30 C25 125(3) . . ? C29 C30 S6 119(2) . . ? C25 C30 S6 116(2) . . ? O6 C31 C32 123(3) . . ? O6 C31 C36 122(2) . . ? C32 C31 C36 115(3) . . ? C31 C32 C33 121(3) . . ? C31 C32 S6 119(2) . . ? C33 C32 S6 120(2) . . ? C34 C33 C32 122(3) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C35 C34 C33 117(3) . . ? C35 C34 C79 119(3) . . ? C33 C34 C79 123(3) . . ? C34 C35 C36 124(3) . . ? C34 C35 H35A 117.9 . . ? C36 C35 H35A 117.9 . . ? C35 C36 C31 120(3) . . ? C35 C36 S7 122(2) . . ? C31 C36 S7 117(2) . . ? O7 C37 C38 121(2) . . ? O7 C37 C42 123(3) . . ? C38 C37 C42 116(2) . . ? C37 C38 C39 120(3) . . ? C37 C38 S7 119(2) . . ? C39 C38 S7 121(2) . . ? C40 C39 C38 126(3) . . ? C40 C39 H39A 117.2 . . ? C38 C39 H39A 117.2 . . ? C39 C40 C41 116(3) . . ? C39 C40 C85 122(3) . . ? C41 C40 C85 121(3) . . ? C40 C41 C42 120(3) . . ? C40 C41 H41A 120.2 . . ? C42 C41 H41A 120.2 . . ? C37 C42 C41 123(3) . . ? C37 C42 S8 119(2) . . ? C41 C42 S8 118(2) . . ? O8 C43 C44 125(3) . . ? O8 C43 C48 122(3) . . ? C44 C43 C48 113(3) . . ? C45 C44 C43 124(2) . . ? C45 C44 S8 119(2) . . ? C43 C44 S8 117(2) . . ? C44 C45 C46 121(2) . . ? C44 C45 H45A 119.4 . . ? C46 C45 H45A 119.3 . . ? C47 C46 C45 117(3) . . ? C47 C46 C91 122(3) . . ? C45 C46 C91 121(2) . . ? C48 C47 C46 123(3) . . ? C48 C47 H47A 118.6 . . ? C46 C47 H47A 118.6 . . ? C47 C48 C43 122(3) . . ? C47 C48 S5 120(2) . . ? C43 C48 S5 118(2) . . ? C54 C49 C50 119(3) . . ? C54 C49 C4 123(4) . . ? C50 C49 C4 118(3) . . ? C51 C50 C49 119(4) . . ? C51 C50 H50A 120.7 . . ? C49 C50 H50A 120.7 . . ? C52 C51 C50 119(4) . . ? C52 C51 H51A 120.4 . . ? C50 C51 H51A 120.4 . . ? C53 C52 C51 119(3) . . ? C53 C52 H52A 120.5 . . ? C51 C52 H52A 120.5 . . ? C52 C53 C54 121(4) . . ? C52 C53 H53A 119.3 . . ? C54 C53 H53A 119.3 . . ? C49 C54 C53 123(4) . . ? C49 C54 H54A 118.7 . . ? C53 C54 H54A 118.7 . . ? C56 C55 C60 111(4) . . ? C56 C55 C10 126(4) . . ? C60 C55 C10 122(4) . . ? C57 C56 C55 127(5) . . ? C57 C56 H56A 116.3 . . ? C55 C56 H56A 116.3 . . ? C58 C57 C56 120(7) . . ? C58 C57 H57A 120.2 . . ? C56 C57 H57A 120.2 . . ? C57 C58 C59 118(8) . . ? C57 C58 H58A 120.8 . . ? C59 C58 H58A 120.8 . . ? C60 C59 C58 123(7) . . ? C60 C59 H59A 118.6 . . ? C58 C59 H59A 118.6 . . ? C59 C60 C55 120(5) . . ? C59 C60 H60A 120.0 . . ? C55 C60 H60A 120.0 . . ? C66 C61 C62 116(4) . . ? C66 C61 C16 122(3) . . ? C62 C61 C16 122(3) . . ? C61 C62 C63 120(4) . . ? C61 C62 H62A 120.1 . . ? C63 C62 H62A 120.1 . . ? C64 C63 C62 124(4) . . ? C64 C63 H63A 118.2 . . ? C62 C63 H63A 118.2 . . ? C63 C64 C65 117(4) . . ? C63 C64 H64A 121.4 . . ? C65 C64 H64A 121.4 . . ? C66 C65 C64 121(3) . . ? C66 C65 H65A 119.4 . . ? C64 C65 H65A 119.4 . . ? C65 C66 C61 122(4) . . ? C65 C66 H66A 119.2 . . ? C61 C66 H66A 119.2 . . ? C72 C67 C68 115(4) . . ? C72 C67 C22 128(4) . . ? C68 C67 C22 117(4) . . ? C67 C68 C69 127(6) . . ? C67 C68 H68A 116.7 . . ? C69 C68 H68A 116.7 . . ? C68 C69 C70 110(5) . . ? C68 C69 H69A 125.1 . . ? C70 C69 H69A 125.1 . . ? C71 C70 C69 120(5) . . ? C71 C70 H70A 120.1 . . ? C69 C70 H70A 120.1 . . ? C70 C71 C72 119(5) . . ? C70 C71 H71A 120.5 . . ? C72 C71 H71A 120.5 . . ? C67 C72 C71 129(5) . . ? C67 C72 H72A 115.3 . . ? C71 C72 H72A 115.3 . . ? C74 C73 C78 120(4) . . ? C74 C73 C28 121(3) . . ? C78 C73 C28 119(3) . . ? C73 C74 C75 120(4) . . ? C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C76 C75 C74 120(4) . . ? C76 C75 H75A 119.9 . . ? C74 C75 H75A 119.9 . . ? C75 C76 C77 122(4) . . ? C75 C76 H76A 119.2 . . ? C77 C76 H76A 119.2 . . ? C76 C77 C78 122(4) . . ? C76 C77 H77A 118.9 . . ? C78 C77 H77A 118.9 . . ? C73 C78 C77 116(4) . . ? C73 C78 H78A 122.2 . . ? C77 C78 H78A 122.2 . . ? C80 C79 C34 129(4) . . ? C80 C79 C84 113(4) . . ? C34 C79 C84 117(4) . . ? C81 C80 C79 128(5) . . ? C81 C80 H80A 115.8 . . ? C79 C80 H80A 115.8 . . ? C82 C81 C80 121(7) . . ? C82 C81 H81A 119.3 . . ? C80 C81 H81A 119.3 . . ? C81 C82 C83 119(8) . . ? C81 C82 H82A 120.3 . . ? C83 C82 H82A 120.3 . . ? C82 C83 C84 124(8) . . ? C82 C83 H83A 118.0 . . ? C84 C83 H83A 118.0 . . ? C83 C84 C79 108(6) . . ? C83 C84 H84A 125.8 . . ? C79 C84 H84A 125.8 . . ? C90 C85 C86 116(4) . . ? C90 C85 C40 120(4) . . ? C86 C85 C40 124(3) . . ? C87 C86 C85 126(5) . . ? C87 C86 H86A 116.8 . . ? C85 C86 H86A 116.8 . . ? C88 C87 C86 116(5) . . ? C88 C87 H87A 122.1 . . ? C86 C87 H87A 122.1 . . ? C87 C88 C89 127(5) . . ? C87 C88 H88A 116.7 . . ? C89 C88 H88A 116.7 . . ? C88 C89 C90 111(5) . . ? C88 C89 H89A 124.6 . . ? C90 C89 H89A 124.6 . . ? C85 C90 C89 123(5) . . ? C85 C90 H90A 118.5 . . ? C89 C90 H90A 118.5 . . ? C96 C91 C46 125(3) . . ? C96 C91 C92 115(3) . . ? C46 C91 C92 119(3) . . ? C93 C92 C91 118(4) . . ? C93 C92 H92A 121.0 . . ? C91 C92 H92A 121.0 . . ? C94 C93 C92 121(4) . . ? C94 C93 H93A 119.6 . . ? C92 C93 H93A 119.6 . . ? C93 C94 C95 121(4) . . ? C93 C94 H94A 119.5 . . ? C95 C94 H94A 119.5 . . ? C96 C95 C94 116(3) . . ? C96 C95 H95A 121.8 . . ? C94 C95 H95A 121.8 . . ? C95 C96 C91 128(3) . . ? C95 C96 H96A 116.0 . . ? C91 C96 H96A 116.0 . . ? C5' C1' C9' 122(5) . . ? C5' C1' C8' 121(5) . . ? C9' C1' C8' 107(4) . . ? C1' C5' C3' 120(5) . . ? C1' C5' C2' 116(4) . . ? C3' C5' C2' 112(5) . . ? C6' C2' C5' 127(6) . . ? C6' C2' C7' 116(4) . . ? C5' C2' C7' 104(4) . . ? C2' C6' C10' 114(5) . . ? C2' C6' C22' 126(6) . . ? C10' C6' C22' 109(4) . . ? C1' C9' C10' 119(5) . . ? C1' C9' C21' 108(5) . . ? C10' C9' C21' 122(4) . . ? C9' C10' C6' 122(5) . . ? C9' C10' C16' 117(5) . . ? C6' C10' C16' 106(4) . . ? C26F C22' C18' 120(6) . . ? C26F C22' C6' 116(5) . . ? C18' C22' C6' 107(5) . . ? C29' C8' C4' 121(5) . . ? C29' C8' C1' 119(4) . . ? C4' C8' C1' 108(4) . . ? C25' C3' C5' 118(5) . . ? C25' C3' C11' 119(4) . . ? C5' C3' C11' 107(4) . . ? C3' C11' C7' 106(4) . . ? C3' C11' C12F 111(5) . . ? C7' C11' C12F 119(5) . . ? C14F C7' C2' 121(5) . . ? C14F C7' C11' 121(5) . . ? C2' C7' C11' 111(4) . . ? C21' C4' C8' 109(4) . . ? C21' C4' C13' 118(5) . . ? C8' C4' C13' 118(5) . . ? C24' C21' C4' 123(5) . . ? C24' C21' C9' 119(5) . . ? C4' C21' C9' 108(4) . . ? C21' C24' C27' 122(5) . . ? C21' C24' C23' 118(5) . . ? C27' C24' C23' 108(4) . . ? C28' C13' C19' 115(7) . . ? C28' C13' C4' 120(5) . . ? C19' C13' C4' 117(5) . . ? C22' C18' C28F 121(4) . . ? C22' C18' C16' 108(4) . . ? C28F C18' C16' 122(4) . . ? C10' C16' C18' 108(5) . . ? C10' C16' C27' 122(5) . . ? C18' C16' C27' 114(5) . . ? C24' C27' C16' 118(5) . . ? C24' C27' C17F 108(4) . . ? C16' C27' C17F 123(5) . . ? C17' C17F C23F 101(7) . . ? C17' C17F C27' 118(5) . . ? C23F C17F C27' 107(4) . . ? C8' C29' C30' 122(5) . . ? C8' C29' C25' 117(5) . . ? C30' C29' C25' 108(4) . . ? C3' C25' C15' 118(5) . . ? C3' C25' C29' 124(5) . . ? C15' C25' C29' 111(4) . . ? C20' C30' C29' 102(4) . . ? C20' C30' C19' 119(6) . . ? C29' C30' C19' 114(5) . . ? C18F C19' C13' 108(7) . . ? C18F C19' C30' 122(5) . . ? C13' C19' C30' 126(5) . . ? C17F C23F C24F 126(7) . . ? C17F C23F C23' 108(4) . . ? C24F C23F C23' 115(5) . . ? C28' C23' C24' 120(5) . . ? C28' C23' C23F 122(5) . . ? C24' C23' C23F 107(5) . . ? C13' C28' C27F 98(7) . . ? C13' C28' C23' 121(5) . . ? C27F C28' C23' 120(6) . . ? C21F C24F C23F 129(9) . . ? C21F C24F C16F 99(7) . . ? C23F C24F C16F 124(5) . . ? C17F C17' C28F 117(5) . . ? C17F C17' C4F 134(7) . . ? C28F C17' C4F 105(4) . . ? C17' C28F C18' 122(5) . . ? C17' C28F C19F 111(5) . . ? C18' C28F C19F 113(5) . . ? C13F C19F C30F 121(7) . . ? C13F C19F C28F 105(4) . . ? C30F C19F C28F 129(5) . . ? C7' C14F C26F 121(5) . . ? C7' C14F C15F 116(5) . . ? C26F C14F C15F 104(4) . . ? C19F C30F C26F 112(5) . . ? C19F C30F C29F 125(8) . . ? C26F C30F C29F 106(4) . . ? C22' C26F C30F 123(5) . . ? C22' C26F C14F 120(4) . . ? C30F C26F C14F 111(4) . . ? C10F C9F C1F 129(7) . . ? C10F C9F C21F 109(7) . . ? C1F C9F C21F 121(6) . . ? C24F C21F C4F 111(8) . . ? C24F C21F C9F 113(8) . . ? C4F C21F C9F 119(6) . . ? C21F C4F C17' 118(8) . . ? C21F C4F C13F 119(5) . . ? C17' C4F C13F 105(5) . . ? C19F C13F C8F 120(8) . . ? C19F C13F C4F 113(5) . . ? C8F C13F C4F 118(5) . . ? C9F C10F C6F 115(9) . . ? C9F C10F C16F 102(8) . . ? C6F C10F C16F 119(5) . . ? C10F C16F C24F 113(7) . . ? C10F C16F C27F 115(5) . . ? C24F C16F C27F 118(5) . . ? C28' C27F C18F 114(7) . . ? C28' C27F C16F 118(5) . . ? C18F C27F C16F 122(5) . . ? C19' C18F C22F 115(5) . . ? C19' C18F C27F 104(7) . . ? C22F C18F C27F 121(5) . . ? C18F C22F C6F 114(5) . . ? C18F C22F C26' 125(5) . . ? C6F C22F C26' 114(8) . . ? C10F C6F C2F 113(8) . . ? C10F C6F C22F 129(7) . . ? C2F C6F C22F 107(8) . . ? C12' C15' C20' 110(5) . . ? C12' C15' C25' 129(6) . . ? C20' C15' C25' 99(5) . . ? C15' C20' C30' 120(5) . . ? C15' C20' C26' 114(5) . . ? C30' C20' C26' 116(4) . . ? C14' C26' C22F 95(7) . . ? C14' C26' C20' 124(7) . . ? C22F C26' C20' 118(6) . . ? C11F C15F C29F 121(5) . . ? C11F C15F C14F 122(5) . . ? C29F C15F C14F 109(4) . . ? C25F C29F C30F 106(7) . . ? C25F C29F C15F 114(5) . . ? C30F C29F C15F 108(5) . . ? C26' C14' C7F 123(6) . . ? C26' C14' C2F 122(6) . . ? C7F C14' C2F 114(5) . . ? C20F C2F C14' 120(5) . . ? C20F C2F C6F 132(8) . . ? C14' C2F C6F 101(6) . . ? C14' C7F C3F 122(4) . . ? C14' C7F C12' 99(5) . . ? C3F C7F C12' 108.0 . . ? C5F C3F C11F 106(4) . . ? C5F C3F C7F 119(4) . . ? C11F C3F C7F 108.0 . . ? C3F C11F C12F 108.0 . . ? C3F C11F C15F 124(4) . . ? C12F C11F C15F 121(4) . . ? C11F C12F C12' 108.0 . . ? C11F C12F C11' 116(3) . . ? C12' C12F C11' 134(4) . . ? C15' C12' C12F 104(4) . . ? C15' C12' C7F 143(4) . . ? C12F C12' C7F 108.0 . . ? C3F C5F C20F 115(4) . . ? C3F C5F C25F 135(4) . . ? C20F C5F C25F 108.0 . . ? C29F C25F C8F 133(5) . . ? C29F C25F C5F 115(4) . . ? C8F C25F C5F 108.0 . . ? C13F C8F C25F 114(6) . . ? C13F C8F C1F 121(5) . . ? C25F C8F C1F 108.0 . . ? C9F C1F C20F 112(6) . . ? C9F C1F C8F 119(5) . . ? C20F C1F C8F 108.0 . . ? C2F C20F C5F 123(5) . . ? C2F C20F C1F 115(6) . . ? C5F C20F C1F 108.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.926 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.131 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.002 0.469 0.047 19905 6968 ' ' 2 0.000 0.000 0.104 20 10 ' ' 3 0.500 0.500 0.104 20 10 ' ' 4 0.250 0.250 0.354 20 5 ' ' 5 0.750 0.750 0.354 20 5 ' ' 6 0.000 0.500 0.604 20 10 ' ' 7 0.500 0.000 0.604 20 10 ' ' 8 0.250 0.750 0.854 20 5 ' ' 9 0.750 0.250 0.854 20 5 ' ' _platon_squeeze_details ; ; ###END data_compound_775186 _database_code_depnum_ccdc_archive 'CCDC 775186' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Mn4(C48H28O4S4)2)2 (C70)' _chemical_melting_point ? _chemical_formula_moiety 'C192 H112 Mn8 O16 S16, C70' _chemical_formula_sum 'C262 H112 Mn8 O16 S16' _chemical_formula_weight 4468.00 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_Int_Tables_number No.43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 57.682(2) _cell_length_b 30.0183(12) _cell_length_c 30.7680(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 53275(4) _cell_formula_units_Z 8 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used 9964 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 18144 _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9179 _exptl_absorpt_correction_T_max 0.9326 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94251 _diffrn_reflns_av_R_equivalents 0.1514 _diffrn_reflns_av_sigmaI/netI 0.1434 _diffrn_reflns_limit_h_min -67 _diffrn_reflns_limit_h_max 68 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 25.04 _reflns_number_total 23419 _reflns_number_gt 13728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. These atoms are as follows: C24, C88, and C55 > C60. The command 'dfix' was also used to model the C70 molecule. The restraint command lead to a relative high restraint number 302, but cannot be completely avoided. Suspect C-C bonds (especially in C70 molecule) are due to the weak high-angle diffractions and the disorders and these problems can't be solved by trials of refinement. The high Rint factor of compound might be due to the weak high-angle diffractions and the disorder of C70 and toluene molecules. Considering the large cell volume and large incorporated disordered toluene (the elcetron count to be 7364 within 20734 A3 void per cell), the present data is not good comparing to the ordinary ones and the resulted problems can not be completely solved by further refinement even with re-collected data. Those observations are familiar in calixarene-based compounds. ; _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^)+(0.1392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.35(3) _refine_ls_number_reflns 23419 _refine_ls_number_parameters 1257 _refine_ls_number_restraints 302 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2387 _refine_ls_wR_factor_gt 0.2176 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.965 _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 0.13290(2) 0.69783(4) 0.36927(4) 0.0330(3) Uani 1 1 d . . . Mn2 Mn 0.16337(2) 0.61211(4) 0.33271(5) 0.0338(3) Uani 1 1 d . . . Mn3 Mn 0.11666(2) 0.57140(4) 0.28524(5) 0.0324(3) Uani 1 1 d . . . Mn4 Mn 0.08614(2) 0.65658(4) 0.32265(5) 0.0341(3) Uani 1 1 d . . . S1 S 0.14698(4) 0.77657(7) 0.33636(8) 0.0354(5) Uani 1 1 d . . . S2 S 0.19753(4) 0.63484(8) 0.27748(8) 0.0373(6) Uani 1 1 d . . . S3 S 0.11940(4) 0.56945(7) 0.19698(8) 0.0349(6) Uani 1 1 d . . . S4 S 0.06814(4) 0.70949(7) 0.26051(8) 0.0381(6) Uani 1 1 d . . . S5 S 0.12994(4) 0.70370(7) 0.45505(7) 0.0303(5) Uani 1 1 d . . . S6 S 0.18073(4) 0.56063(7) 0.39636(8) 0.0365(6) Uani 1 1 d . . . S7 S 0.10337(4) 0.49218(7) 0.31653(8) 0.0367(6) Uani 1 1 d . . . S8 S 0.05196(4) 0.63405(7) 0.37757(8) 0.0360(6) Uani 1 1 d . . . O1 O 0.15637(10) 0.68086(18) 0.3170(2) 0.0359(14) Uani 1 1 d . . . O2 O 0.15150(10) 0.58863(18) 0.2714(2) 0.0332(14) Uani 1 1 d . . . O3 O 0.10340(10) 0.63562(18) 0.2640(2) 0.0372(15) Uani 1 1 d . . . O4 O 0.10580(10) 0.71670(18) 0.3267(2) 0.0353(14) Uani 1 1 d . . . O5 O 0.15333(9) 0.64422(17) 0.39076(18) 0.0267(13) Uani 1 1 d . . . O6 O 0.13633(10) 0.56263(17) 0.3450(2) 0.0350(14) Uani 1 1 d . . . O7 O 0.08778(9) 0.58673(17) 0.3232(2) 0.0305(13) Uani 1 1 d . . . O8 O 0.10245(9) 0.65714(17) 0.38562(18) 0.0284(13) Uani 1 1 d . . . C1 C 0.17153(16) 0.7093(3) 0.2985(3) 0.036(2) Uani 1 1 d . . . C2 C 0.16920(15) 0.7546(3) 0.3017(3) 0.031(2) Uani 1 1 d . . . C3 C 0.18367(16) 0.7832(3) 0.2818(3) 0.045(2) Uani 1 1 d . . . H3A H 0.1810 0.8143 0.2847 0.054 Uiso 1 1 calc R . . C4 C 0.20310(16) 0.7683(3) 0.2561(3) 0.039(2) Uani 1 1 d . . . C5 C 0.20610(18) 0.7231(4) 0.2558(3) 0.050(3) Uani 1 1 d . . . H5A H 0.2191 0.7116 0.2406 0.060 Uiso 1 1 calc R . . C6 C 0.19131(16) 0.6925(3) 0.2764(3) 0.038(2) Uani 1 1 d . . . C7 C 0.16078(17) 0.5984(3) 0.2334(3) 0.042(2) Uani 1 1 d . . . C8 C 0.18172(15) 0.6190(3) 0.2297(3) 0.039(2) Uani 1 1 d . . . C9 C 0.19204(16) 0.6272(4) 0.1889(3) 0.052(3) Uani 1 1 d . . . H9A H 0.2072 0.6397 0.1874 0.062 Uiso 1 1 calc R . . C10 C 0.18065(19) 0.6177(4) 0.1525(4) 0.068(3) Uani 1 1 d . . . C11 C 0.15833(18) 0.5995(4) 0.1545(3) 0.053(3) Uani 1 1 d . . . H11A H 0.1501 0.5939 0.1283 0.064 Uiso 1 1 calc R . . C12 C 0.14820(15) 0.5898(3) 0.1936(3) 0.037(2) Uani 1 1 d . . . C13 C 0.09624(14) 0.6447(3) 0.2233(3) 0.027(2) Uani 1 1 d . . . C14 C 0.10253(15) 0.6192(3) 0.1900(3) 0.032(2) Uani 1 1 d . . . C15 C 0.09515(16) 0.6299(3) 0.1451(3) 0.034(2) Uani 1 1 d . . . H15A H 0.1007 0.6127 0.1214 0.040 Uiso 1 1 calc R . . C16 C 0.08045(17) 0.6645(3) 0.1381(3) 0.040(2) Uani 1 1 d . . . C17 C 0.07321(15) 0.6887(3) 0.1739(3) 0.034(2) Uani 1 1 d . . . H17A H 0.0629 0.7129 0.1698 0.040 Uiso 1 1 calc R . . C18 C 0.08062(15) 0.6787(3) 0.2159(3) 0.031(2) Uani 1 1 d . . . C19 C 0.10652(17) 0.7494(3) 0.2980(3) 0.040(2) Uani 1 1 d . . . C20 C 0.08897(17) 0.7525(3) 0.2664(3) 0.038(2) Uani 1 1 d . . . C21 C 0.08867(17) 0.7881(3) 0.2377(3) 0.041(2) Uani 1 1 d . . . H21A H 0.0766 0.7901 0.2168 0.050 Uiso 1 1 calc R . . C22 C 0.10532(18) 0.8204(3) 0.2391(3) 0.043(2) Uani 1 1 d . . . C23 C 0.12253(16) 0.8173(3) 0.2713(3) 0.041(2) Uani 1 1 d . . . H23A H 0.1341 0.8397 0.2737 0.049 Uiso 1 1 calc R . . C24 C 0.12262(15) 0.7824(3) 0.2990(3) 0.031(2) Uani 1 1 d U . . C25 C 0.15338(15) 0.6279(3) 0.4288(3) 0.035(2) Uani 1 1 d . . . C26 C 0.14304(14) 0.6490(3) 0.4647(3) 0.028(2) Uani 1 1 d . . . C27 C 0.14420(17) 0.6335(3) 0.5057(3) 0.045(2) Uani 1 1 d . . . H27A H 0.1368 0.6499 0.5282 0.054 Uiso 1 1 calc R . . C28 C 0.15545(19) 0.5953(3) 0.5161(4) 0.053(3) Uani 1 1 d . . . C29 C 0.16624(18) 0.5706(3) 0.4812(3) 0.045(2) Uani 1 1 d . . . H29A H 0.1745 0.5439 0.4869 0.054 Uiso 1 1 calc R . . C30 C 0.16426(15) 0.5864(3) 0.4400(3) 0.037(2) Uani 1 1 d . . . C31 C 0.14250(17) 0.5240(3) 0.3587(3) 0.037(2) Uani 1 1 d . . . C32 C 0.16281(14) 0.5146(3) 0.3830(3) 0.036(2) Uani 1 1 d . . . C33 C 0.16811(18) 0.4710(3) 0.3962(3) 0.045(3) Uani 1 1 d . . . H33A H 0.1815 0.4664 0.4138 0.054 Uiso 1 1 calc R . . C34 C 0.15522(17) 0.4351(3) 0.3853(4) 0.046(3) Uani 1 1 d . . . C35 C 0.13568(18) 0.4426(3) 0.3646(4) 0.052(3) Uani 1 1 d . . . H35A H 0.1256 0.4179 0.3603 0.062 Uiso 1 1 calc R . . C36 C 0.12825(18) 0.4846(3) 0.3479(3) 0.042(2) Uani 1 1 d . . . C37 C 0.07860(15) 0.5610(3) 0.3528(3) 0.029(2) Uani 1 1 d . . . C38 C 0.08364(16) 0.5167(3) 0.3545(3) 0.036(2) Uani 1 1 d . . . C39 C 0.07144(16) 0.4877(3) 0.3839(3) 0.036(2) Uani 1 1 d . . . H39A H 0.0752 0.4569 0.3851 0.043 Uiso 1 1 calc R . . C40 C 0.05483(18) 0.5042(3) 0.4094(3) 0.042(2) Uani 1 1 d . . . C41 C 0.04921(16) 0.5482(3) 0.4092(3) 0.038(2) Uani 1 1 d . . . H41A H 0.0373 0.5594 0.4277 0.046 Uiso 1 1 calc R . . C42 C 0.06102(15) 0.5758(3) 0.3820(3) 0.035(2) Uani 1 1 d . . . C43 C 0.08992(14) 0.6692(2) 0.4204(3) 0.027(2) Uani 1 1 d . . . C44 C 0.06557(15) 0.6603(3) 0.4228(3) 0.033(2) Uani 1 1 d . . . C45 C 0.05244(16) 0.6736(3) 0.4561(3) 0.038(2) Uani 1 1 d . . . H45A H 0.0364 0.6665 0.4563 0.046 Uiso 1 1 calc R . . C46 C 0.06203(15) 0.6982(3) 0.4913(3) 0.033(2) Uani 1 1 d . . . C47 C 0.08504(15) 0.7065(3) 0.4883(3) 0.032(2) Uani 1 1 d . . . H47A H 0.0919 0.7240 0.5106 0.039 Uiso 1 1 calc R . . C48 C 0.09914(15) 0.6917(3) 0.4555(3) 0.032(2) Uani 1 1 d . . . C49 C 0.21695(17) 0.7986(3) 0.2318(4) 0.045(3) Uani 1 1 d . . . C50 C 0.22472(17) 0.8376(4) 0.2472(4) 0.052(3) Uani 1 1 d . . . H50A H 0.2211 0.8458 0.2762 0.062 Uiso 1 1 calc R . . C51 C 0.2381(2) 0.8668(4) 0.2214(5) 0.076(4) Uani 1 1 d . . . H51A H 0.2422 0.8950 0.2332 0.091 Uiso 1 1 calc R . . C52 C 0.2452(2) 0.8570(5) 0.1813(5) 0.078(4) Uani 1 1 d . . . H52A H 0.2542 0.8779 0.1655 0.093 Uiso 1 1 calc R . . C53 C 0.2397(3) 0.8159(5) 0.1626(5) 0.087(4) Uani 1 1 d . . . H53A H 0.2446 0.8072 0.1344 0.105 Uiso 1 1 calc R . . C54 C 0.2250(2) 0.7873(4) 0.1916(4) 0.064(3) Uani 1 1 d . . . H54A H 0.2210 0.7585 0.1811 0.077 Uiso 1 1 calc R . . C55 C 0.1907(2) 0.6285(5) 0.1079(5) 0.088(4) Uani 1 1 d DU . . C56 C 0.2062(3) 0.6682(6) 0.1055(6) 0.122(6) Uani 1 1 d DU . . H56A H 0.2079 0.6870 0.1302 0.146 Uiso 1 1 calc R . . C57 C 0.2192(4) 0.6788(10) 0.0642(8) 0.213(12) Uani 1 1 d DU . . H57A H 0.2287 0.7045 0.0613 0.256 Uiso 1 1 calc R . . C58 C 0.2161(4) 0.6459(9) 0.0286(9) 0.182(9) Uani 1 1 d DU . . H58A H 0.2253 0.6479 0.0031 0.218 Uiso 1 1 calc R . . C59 C 0.2004(4) 0.6137(8) 0.0324(8) 0.160(8) Uani 1 1 d DU . . H59A H 0.1972 0.5966 0.0071 0.192 Uiso 1 1 calc R . . C60 C 0.1878(3) 0.6022(6) 0.0718(6) 0.113(5) Uani 1 1 d DU . . H60A H 0.1778 0.5771 0.0726 0.135 Uiso 1 1 calc R . . C61 C 0.07187(19) 0.6754(3) 0.0949(3) 0.049(3) Uani 1 1 d . . . C62 C 0.0872(2) 0.6689(4) 0.0588(4) 0.073(4) Uani 1 1 d . . . H62A H 0.1027 0.6590 0.0635 0.088 Uiso 1 1 calc R . . C63 C 0.0787(2) 0.6780(4) 0.0139(4) 0.068(4) Uani 1 1 d . . . H63A H 0.0886 0.6749 -0.0106 0.081 Uiso 1 1 calc R . . C64 C 0.0566(3) 0.6905(5) 0.0095(4) 0.089(5) Uani 1 1 d . . . H64A H 0.0504 0.6951 -0.0187 0.107 Uiso 1 1 calc R . . C65 C 0.0426(2) 0.6969(4) 0.0458(5) 0.083(4) Uani 1 1 d . . . H65A H 0.0272 0.7074 0.0420 0.100 Uiso 1 1 calc R . . C66 C 0.05031(19) 0.6883(3) 0.0864(3) 0.051(3) Uani 1 1 d . . . H66A H 0.0398 0.6917 0.1100 0.061 Uiso 1 1 calc R . . C67 C 0.1052(2) 0.8593(4) 0.2083(4) 0.064(3) Uani 1 1 d . . . C68 C 0.1009(3) 0.8548(4) 0.1658(4) 0.084(4) Uani 1 1 d . . . H68A H 0.0994 0.8252 0.1552 0.101 Uiso 1 1 calc R . . C69 C 0.0982(3) 0.8906(6) 0.1340(6) 0.122(6) Uani 1 1 d . . . H69A H 0.0925 0.8868 0.1052 0.146 Uiso 1 1 calc R . . C70 C 0.1053(3) 0.9324(6) 0.1527(6) 0.110(5) Uani 1 1 d . . . H70A H 0.1063 0.9571 0.1335 0.132 Uiso 1 1 calc R . . C71 C 0.1109(3) 0.9402(6) 0.1952(7) 0.120(6) Uani 1 1 d . . . H71A H 0.1145 0.9693 0.2053 0.144 Uiso 1 1 calc R . . C72 C 0.1110(2) 0.9035(4) 0.2232(5) 0.089(5) Uani 1 1 d . . . H72A H 0.1149 0.9078 0.2529 0.107 Uiso 1 1 calc R . . C73 C 0.15799(17) 0.5808(3) 0.5606(3) 0.043(2) Uani 1 1 d . . . C74 C 0.16563(19) 0.6089(4) 0.5925(3) 0.051(3) Uani 1 1 d . . . H74A H 0.1694 0.6388 0.5854 0.061 Uiso 1 1 calc R . . C75 C 0.1679(2) 0.5946(4) 0.6352(4) 0.075(4) Uani 1 1 d . . . H75A H 0.1735 0.6155 0.6559 0.090 Uiso 1 1 calc R . . C76 C 0.1625(3) 0.5519(5) 0.6499(5) 0.085(4) Uani 1 1 d U . . H76A H 0.1633 0.5435 0.6796 0.102 Uiso 1 1 calc R . . C77 C 0.1562(3) 0.5235(5) 0.6180(5) 0.089(4) Uani 1 1 d U . . H77A H 0.1540 0.4932 0.6260 0.106 Uiso 1 1 calc R . . C78 C 0.1523(2) 0.5347(5) 0.5729(5) 0.091(4) Uani 1 1 d . . . H78A H 0.1464 0.5137 0.5526 0.109 Uiso 1 1 calc R . . C79 C 0.16106(19) 0.3919(4) 0.3989(4) 0.063(3) Uani 1 1 d . . . C80 C 0.1870(2) 0.3787(5) 0.4005(6) 0.096(5) Uani 1 1 d . . . H80A H 0.1991 0.3981 0.3914 0.116 Uiso 1 1 calc R . . C81 C 0.1912(3) 0.3357(5) 0.4167(6) 0.113(6) Uani 1 1 d . . . H81A H 0.2069 0.3282 0.4223 0.135 Uiso 1 1 calc R . . C82 C 0.1755(3) 0.3043(6) 0.4249(7) 0.123(7) Uani 1 1 d . . . H82A H 0.1801 0.2757 0.4349 0.148 Uiso 1 1 calc R . . C83 C 0.1511(3) 0.3152(5) 0.4183(7) 0.130(8) Uani 1 1 d . . . H83A H 0.1392 0.2935 0.4210 0.156 Uiso 1 1 calc R . . C84 C 0.1467(2) 0.3583(5) 0.4078(7) 0.120(7) Uani 1 1 d . . . H84A H 0.1307 0.3658 0.4067 0.143 Uiso 1 1 calc R . . C85 C 0.04044(17) 0.4715(3) 0.4364(3) 0.045(2) Uani 1 1 d . . . C86 C 0.0300(2) 0.4324(4) 0.4203(4) 0.061(3) Uani 1 1 d . . . H86A H 0.0322 0.4268 0.3902 0.074 Uiso 1 1 calc R . . C87 C 0.0182(3) 0.4040(5) 0.4406(5) 0.085(4) Uani 1 1 d . . . H87A H 0.0138 0.3767 0.4275 0.102 Uiso 1 1 calc R . . C88 C 0.0125(3) 0.4134(6) 0.4792(7) 0.107(5) Uani 1 1 d U . . H88A H 0.0037 0.3921 0.4949 0.128 Uiso 1 1 calc R . . C89 C 0.0187(3) 0.4554(7) 0.5014(7) 0.136(8) Uani 1 1 d . . . H89A H 0.0128 0.4623 0.5295 0.163 Uiso 1 1 calc R . . C90 C 0.0335(3) 0.4847(6) 0.4797(6) 0.118(6) Uani 1 1 d . . . H90A H 0.0387 0.5117 0.4926 0.141 Uiso 1 1 calc R . . C91 C 0.04732(15) 0.7164(3) 0.5262(3) 0.038(2) Uani 1 1 d . . . C92 C 0.0319(2) 0.6874(4) 0.5470(4) 0.072(3) Uani 1 1 d . . . H92A H 0.0319 0.6567 0.5398 0.086 Uiso 1 1 calc R . . C93 C 0.0163(2) 0.7040(4) 0.5788(5) 0.085(4) Uani 1 1 d . . . H93A H 0.0056 0.6845 0.5925 0.102 Uiso 1 1 calc R . . C94 C 0.0169(2) 0.7487(4) 0.5896(4) 0.063(3) Uani 1 1 d . . . H94A H 0.0065 0.7604 0.6106 0.075 Uiso 1 1 calc R . . C95 C 0.03242(17) 0.7752(4) 0.5702(4) 0.056(3) Uani 1 1 d . . . H95A H 0.0332 0.8057 0.5783 0.067 Uiso 1 1 calc R . . C96 C 0.04739(16) 0.7591(3) 0.5386(3) 0.047(2) Uani 1 1 d . . . H96A H 0.0580 0.7790 0.5254 0.057 Uiso 1 1 calc R . . C1F C 0.2014(5) 0.8286(8) 0.4932(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C2F C 0.2184(3) 0.8528(8) 0.5142(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C3F C 0.2340(2) 0.8788(6) 0.4899(4) 0.0863(9) Uiso 0.50 1 d PD A -1 C4F C 0.2317(3) 0.8800(8) 0.4429(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C5F C 0.2145(4) 0.8546(8) 0.4247(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C6F C 0.1991(4) 0.8291(6) 0.4483(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C7F C 0.1982(4) 0.7872(5) 0.5142(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C8F C 0.1917(6) 0.7483(5) 0.4919(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C9F C 0.1979(4) 0.7084(5) 0.5130(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C10F C 0.2138(5) 0.7076(6) 0.5487(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C11F C 0.2246(3) 0.7469(6) 0.5605(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C12F C 0.2145(4) 0.7865(6) 0.5487(10) 0.0863(9) Uiso 0.50 1 d PD A -1 C13F C 0.1933(5) 0.7110(6) 0.4205(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C14F C 0.2056(3) 0.7141(6) 0.3817(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C15F C 0.2138(4) 0.7518(5) 0.3629(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C16F C 0.1942(6) 0.7904(6) 0.4235(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C17F C 0.2056(3) 0.7896(6) 0.3826(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C18F C 0.1906(4) 0.7501(5) 0.4451(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C19F C 0.2275(3) 0.8250(6) 0.5470(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C20F C 0.2744(4) 0.7868(8) 0.3558(9) 0.0863(9) Uiso 0.50 1 d PD A -1 C21F C 0.2661(3) 0.8540(7) 0.5332(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C22F C 0.2587(3) 0.8791(7) 0.4970(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C23F C 0.2538(3) 0.8807(8) 0.4225(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C24F C 0.2708(3) 0.8800(7) 0.4561(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C25F C 0.2186(3) 0.8291(9) 0.3866(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C26F C 0.2574(3) 0.8552(8) 0.3853(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C27F C 0.2272(3) 0.6653(8) 0.5426(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C28F C 0.2513(3) 0.8245(7) 0.5557(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C29F C 0.2192(3) 0.6420(7) 0.5058(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C30F C 0.2014(4) 0.6694(6) 0.4867(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C31F C 0.2401(3) 0.8297(5) 0.3636(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C32F C 0.2792(5) 0.8322(11) 0.3808(9) 0.0863(9) Uiso 0.50 1 d PD A -1 C33F C 0.2953(4) 0.8321(7) 0.4125(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C34F C 0.2380(3) 0.7513(5) 0.3476(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C35F C 0.2511(3) 0.7907(7) 0.3468(14) 0.0863(9) Uiso 0.50 1 d PD A -1 C1' C 0.2867(3) 0.6642(6) 0.5215(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C2' C 0.2658(3) 0.6374(7) 0.5282(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C3' C 0.2576(2) 0.6153(6) 0.4913(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C4' C 0.2690(3) 0.6185(10) 0.4499(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C5' C 0.2894(3) 0.6428(8) 0.4466(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C6' C 0.2977(5) 0.6669(7) 0.4812(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C7' C 0.3059(5) 0.7455(4) 0.4928(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C8' C 0.3087(4) 0.7865(5) 0.4718(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C9' C 0.2843(6) 0.7832(7) 0.5479(9) 0.0863(9) Uiso 0.50 1 d PD A -1 C10' C 0.2617(3) 0.7826(6) 0.5661(9) 0.0863(9) Uiso 0.50 1 d PD A -1 C11' C 0.2471(5) 0.7461(10) 0.5752(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C12' C 0.2947(4) 0.7437(6) 0.5332(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C13' C 0.3067(6) 0.7886(6) 0.4259(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C14' C 0.2744(3) 0.7116(6) 0.3550(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C15' C 0.2873(4) 0.7499(6) 0.3656(10) 0.0863(9) Uiso 0.50 1 d PD A -1 C16' C 0.3042(4) 0.7493(6) 0.4002(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C17' C 0.3079(5) 0.7065(6) 0.4676(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C18' C 0.3066(5) 0.7086(6) 0.4226(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C19' C 0.2843(4) 0.7043(7) 0.5465(9) 0.0863(9) Uiso 0.50 1 d PD A -1 C20' C 0.2498(3) 0.6611(7) 0.5550(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C21' C 0.1985(4) 0.6705(7) 0.4424(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C22' C 0.2135(3) 0.6443(7) 0.4161(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C23' C 0.2335(3) 0.6161(7) 0.4794(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C24' C 0.2534(2) 0.6205(8) 0.4141(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C25' C 0.2308(3) 0.6171(8) 0.4332(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C26' C 0.2946(4) 0.6688(7) 0.4110(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C27' C 0.2564(3) 0.6482(8) 0.3781(7) 0.0863(9) Uiso 0.50 1 d PD A -1 C28' C 0.2858(4) 0.8250(6) 0.5259(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C29' C 0.2611(4) 0.7041(7) 0.5636(9) 0.0863(9) Uiso 0.50 1 d PD A -1 C30' C 0.2995(5) 0.8266(6) 0.4894(6) 0.0863(9) Uiso 0.50 1 d PD A -1 C31' C 0.2787(4) 0.6709(8) 0.3767(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C32' C 0.2390(3) 0.6769(7) 0.3606(8) 0.0863(9) Uiso 0.50 1 d PD A -1 C33' C 0.2179(4) 0.6751(7) 0.3830(11) 0.0863(9) Uiso 0.50 1 d PD A -1 C34' C 0.2913(4) 0.8544(7) 0.4532(5) 0.0863(9) Uiso 0.50 1 d PD A -1 C35' C 0.2503(3) 0.7125(7) 0.3455(13) 0.0863(9) Uiso 0.50 1 d PD A -1 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 0.0384(8) 0.0266(7) 0.0341(8) -0.0009(6) -0.0011(6) 0.0022(6) Mn2 0.0380(8) 0.0265(7) 0.0368(9) -0.0023(6) -0.0014(7) 0.0019(6) Mn3 0.0350(8) 0.0270(7) 0.0353(8) -0.0007(6) -0.0026(6) 0.0024(6) Mn4 0.0396(8) 0.0254(7) 0.0374(9) -0.0020(6) -0.0040(7) -0.0005(6) S1 0.0419(13) 0.0270(12) 0.0373(14) -0.0045(10) -0.0019(11) 0.0024(10) S2 0.0338(13) 0.0402(14) 0.0378(15) -0.0081(11) -0.0023(11) 0.0025(10) S3 0.0437(14) 0.0244(11) 0.0366(14) -0.0040(10) -0.0084(11) 0.0014(10) S4 0.0403(14) 0.0310(12) 0.0430(15) -0.0024(11) -0.0044(11) 0.0030(10) S5 0.0328(12) 0.0223(11) 0.0358(14) -0.0014(9) -0.0051(10) -0.0005(9) S6 0.0358(13) 0.0290(12) 0.0447(15) -0.0024(10) -0.0062(11) 0.0052(10) S7 0.0417(13) 0.0272(12) 0.0413(15) -0.0058(10) -0.0066(11) -0.0063(10) S8 0.0374(13) 0.0293(12) 0.0415(15) -0.0046(10) -0.0071(11) 0.0024(10) O1 0.044(4) 0.021(3) 0.042(4) -0.007(3) 0.006(3) -0.001(3) O2 0.039(3) 0.023(3) 0.038(4) 0.002(3) 0.003(3) 0.006(3) O3 0.044(4) 0.025(3) 0.043(4) 0.001(3) -0.008(3) 0.003(3) O4 0.036(3) 0.022(3) 0.048(4) 0.007(3) -0.013(3) 0.003(2) O5 0.037(3) 0.019(3) 0.023(3) 0.001(2) -0.002(3) 0.003(2) O6 0.040(3) 0.022(3) 0.043(4) -0.005(3) -0.007(3) -0.001(3) O7 0.029(3) 0.024(3) 0.038(4) -0.007(3) -0.003(3) -0.004(2) O8 0.033(3) 0.018(3) 0.034(4) 0.002(2) -0.004(3) -0.008(2) C1 0.032(5) 0.060(7) 0.016(5) 0.009(4) -0.001(4) 0.000(5) C2 0.035(5) 0.021(5) 0.038(6) -0.001(4) -0.002(4) -0.013(4) C3 0.047(6) 0.049(6) 0.040(6) 0.001(5) -0.011(5) -0.001(5) C4 0.040(5) 0.033(5) 0.044(6) -0.004(4) -0.011(5) -0.001(4) C5 0.044(6) 0.065(7) 0.041(6) -0.012(5) -0.004(5) 0.003(5) C6 0.042(5) 0.042(6) 0.028(5) -0.005(4) -0.011(4) -0.007(4) C7 0.042(6) 0.047(6) 0.036(6) -0.004(5) -0.009(5) 0.003(5) C8 0.027(5) 0.046(6) 0.044(6) -0.013(4) 0.007(4) 0.001(4) C9 0.028(5) 0.096(8) 0.031(6) -0.015(6) 0.000(4) -0.002(5) C10 0.052(7) 0.094(9) 0.059(8) -0.010(7) 0.007(6) -0.022(6) C11 0.057(7) 0.078(8) 0.025(5) -0.014(5) -0.002(5) 0.002(6) C12 0.033(5) 0.042(5) 0.038(6) -0.017(4) 0.003(4) -0.007(4) C13 0.023(4) 0.028(5) 0.030(5) 0.015(4) -0.004(4) -0.011(4) C14 0.034(5) 0.023(4) 0.039(6) 0.000(4) -0.001(4) 0.002(4) C15 0.046(5) 0.026(5) 0.029(5) -0.018(4) 0.007(4) -0.002(4) C16 0.063(6) 0.030(5) 0.025(5) -0.002(4) -0.008(5) -0.005(4) C17 0.042(5) 0.015(4) 0.044(6) -0.001(4) -0.008(4) -0.001(4) C18 0.032(5) 0.015(4) 0.046(6) -0.008(4) -0.003(4) -0.002(3) C19 0.052(6) 0.035(5) 0.031(6) -0.004(4) -0.004(5) 0.022(5) C20 0.057(6) 0.025(5) 0.032(6) 0.000(4) 0.000(5) 0.002(4) C21 0.053(6) 0.025(5) 0.046(6) -0.001(4) -0.017(5) 0.010(4) C22 0.061(6) 0.026(5) 0.041(6) 0.013(4) -0.005(5) -0.002(4) C23 0.038(5) 0.029(5) 0.056(7) -0.002(4) -0.010(5) 0.000(4) C24 0.032(4) 0.013(4) 0.047(5) -0.012(4) -0.006(4) 0.001(3) C25 0.035(5) 0.027(5) 0.042(6) -0.001(4) 0.006(4) -0.002(4) C26 0.023(4) 0.032(5) 0.030(5) -0.004(4) -0.014(4) 0.012(4) C27 0.043(6) 0.040(6) 0.052(7) -0.011(5) -0.001(5) 0.003(5) C28 0.053(7) 0.030(5) 0.074(9) 0.010(5) -0.009(6) -0.013(5) C29 0.069(7) 0.024(5) 0.041(6) -0.003(4) -0.002(5) 0.001(5) C30 0.031(5) 0.041(6) 0.038(6) -0.004(4) -0.012(4) 0.000(4) C31 0.059(6) 0.023(5) 0.029(5) -0.006(4) 0.004(5) 0.000(4) C32 0.024(5) 0.045(6) 0.039(6) -0.015(4) -0.007(4) 0.005(4) C33 0.057(6) 0.030(5) 0.047(7) 0.003(4) -0.020(5) 0.006(5) C34 0.045(6) 0.031(5) 0.061(7) 0.012(5) 0.004(5) 0.007(4) C35 0.053(7) 0.021(5) 0.081(8) 0.009(5) -0.003(6) 0.003(4) C36 0.055(6) 0.027(5) 0.044(6) -0.007(4) -0.002(5) -0.003(4) C37 0.033(5) 0.026(5) 0.028(5) -0.010(4) -0.005(4) -0.005(4) C38 0.032(5) 0.043(6) 0.034(6) 0.002(4) -0.012(4) -0.012(4) C39 0.046(6) 0.033(5) 0.028(5) 0.008(4) -0.009(4) -0.004(4) C40 0.055(6) 0.052(6) 0.019(5) -0.004(4) 0.000(5) -0.016(5) C41 0.043(5) 0.041(5) 0.030(5) -0.006(4) 0.011(4) -0.016(4) C42 0.031(5) 0.030(5) 0.043(6) -0.006(4) -0.009(4) 0.008(4) C43 0.027(5) 0.013(4) 0.042(6) 0.004(4) 0.012(4) 0.004(3) C44 0.035(5) 0.021(4) 0.043(6) 0.002(4) -0.005(4) 0.004(4) C45 0.036(5) 0.031(5) 0.047(6) 0.004(4) 0.002(5) -0.003(4) C46 0.035(5) 0.024(4) 0.041(5) 0.003(4) -0.008(4) -0.009(4) C47 0.040(5) 0.028(4) 0.029(5) -0.002(4) -0.003(4) 0.003(4) C48 0.041(5) 0.028(4) 0.027(5) -0.005(4) 0.003(4) 0.006(4) C49 0.038(6) 0.041(6) 0.057(7) 0.003(5) -0.003(5) -0.005(5) C50 0.049(6) 0.056(7) 0.050(7) 0.016(5) -0.001(5) 0.005(5) C51 0.067(8) 0.065(8) 0.095(11) 0.036(8) -0.010(8) -0.026(7) C52 0.047(7) 0.112(12) 0.074(10) 0.022(9) 0.011(7) -0.004(7) C53 0.100(11) 0.080(10) 0.082(11) 0.012(8) 0.002(9) -0.003(8) C54 0.061(7) 0.074(8) 0.058(8) -0.001(6) 0.021(6) -0.004(6) C55 0.088(7) 0.100(8) 0.076(7) 0.002(6) 0.006(6) -0.006(7) C56 0.120(9) 0.138(9) 0.106(9) -0.007(8) -0.003(8) -0.031(8) C57 0.218(15) 0.218(15) 0.205(15) -0.006(10) 0.005(10) -0.018(10) C58 0.178(12) 0.187(12) 0.180(12) -0.010(9) 0.019(9) -0.027(8) C59 0.163(11) 0.167(11) 0.149(11) -0.010(9) 0.003(9) -0.027(8) C60 0.117(9) 0.131(9) 0.090(8) -0.021(8) 0.007(7) -0.022(8) C61 0.060(7) 0.046(6) 0.042(6) -0.003(5) 0.007(5) -0.010(5) C62 0.070(8) 0.079(9) 0.071(10) 0.010(7) 0.000(7) 0.019(7) C63 0.068(8) 0.076(9) 0.060(8) 0.023(7) -0.004(7) 0.008(7) C64 0.113(12) 0.119(12) 0.035(7) 0.024(7) 0.013(8) 0.033(9) C65 0.069(8) 0.084(9) 0.097(12) 0.003(8) -0.039(8) 0.004(7) C66 0.057(7) 0.054(6) 0.042(6) 0.003(5) -0.007(5) 0.013(5) C67 0.081(8) 0.054(7) 0.057(8) 0.011(6) -0.019(6) -0.003(6) C68 0.136(13) 0.051(7) 0.066(9) 0.002(6) -0.020(9) 0.003(8) C69 0.124(14) 0.113(14) 0.128(16) 0.027(12) -0.017(12) -0.008(11) C70 0.156(16) 0.083(11) 0.090(13) 0.020(9) -0.023(12) -0.016(11) C71 0.148(17) 0.092(12) 0.121(16) 0.016(11) -0.021(13) -0.012(11) C72 0.096(10) 0.064(9) 0.109(12) 0.034(8) -0.027(9) -0.020(7) C73 0.048(6) 0.042(5) 0.038(6) -0.005(5) 0.000(5) 0.000(4) C74 0.065(7) 0.051(6) 0.036(6) 0.002(5) -0.003(5) 0.007(5) C75 0.110(11) 0.071(9) 0.043(8) -0.017(6) -0.005(7) 0.022(8) C76 0.119(12) 0.077(9) 0.059(9) 0.017(7) -0.028(8) -0.014(8) C77 0.096(10) 0.084(9) 0.085(11) 0.018(7) -0.009(8) 0.009(8) C78 0.089(10) 0.095(10) 0.088(11) 0.027(9) 0.003(8) 0.000(8) C79 0.047(6) 0.060(7) 0.083(9) -0.002(6) -0.021(6) 0.007(6) C80 0.070(9) 0.070(9) 0.149(14) 0.017(9) -0.019(9) 0.009(7) C81 0.122(13) 0.052(8) 0.164(17) 0.000(10) -0.024(12) 0.014(9) C82 0.118(14) 0.071(10) 0.18(2) 0.026(11) -0.026(13) 0.003(10) C83 0.100(12) 0.057(9) 0.23(2) 0.051(11) -0.046(14) -0.003(8) C84 0.043(7) 0.086(10) 0.23(2) 0.074(12) -0.051(10) -0.010(7) C85 0.049(6) 0.040(6) 0.048(7) 0.001(5) -0.001(5) 0.001(5) C86 0.066(8) 0.060(8) 0.059(8) 0.010(6) -0.004(6) -0.005(6) C87 0.094(11) 0.077(10) 0.084(11) -0.008(8) 0.011(9) -0.025(8) C88 0.106(9) 0.093(8) 0.121(9) 0.019(8) -0.002(8) -0.020(7) C89 0.136(16) 0.148(18) 0.124(16) 0.037(14) 0.071(13) 0.045(14) C90 0.127(15) 0.119(14) 0.107(14) 0.036(11) 0.035(12) 0.013(11) C91 0.027(5) 0.049(6) 0.039(6) -0.008(5) 0.002(4) -0.006(4) C92 0.081(9) 0.065(8) 0.070(9) -0.004(6) 0.014(7) 0.017(7) C93 0.077(9) 0.078(9) 0.100(11) 0.011(8) 0.034(8) -0.015(7) C94 0.074(8) 0.071(8) 0.044(7) -0.013(6) 0.024(6) 0.000(6) C95 0.047(6) 0.061(7) 0.059(7) -0.011(6) 0.001(6) -0.008(5) C96 0.038(5) 0.053(6) 0.050(6) -0.005(5) 0.005(5) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 2.101(5) . ? Mn1 O4 2.117(6) . ? Mn1 O1 2.164(6) . ? Mn1 O8 2.198(5) . ? Mn1 S5 2.650(3) . ? Mn1 S1 2.696(3) . ? Mn2 O5 2.111(6) . ? Mn2 O2 2.127(6) . ? Mn2 O1 2.158(6) . ? Mn2 O6 2.187(6) . ? Mn2 S6 2.688(3) . ? Mn2 S2 2.690(3) . ? Mn3 O7 2.087(6) . ? Mn3 O2 2.118(6) . ? Mn3 O3 2.175(6) . ? Mn3 O6 2.176(6) . ? Mn3 S7 2.677(3) . ? Mn3 S3 2.721(3) . ? Mn4 O7 2.099(5) . ? Mn4 O4 2.135(6) . ? Mn4 O8 2.154(6) . ? Mn4 O3 2.155(6) . ? Mn4 S8 2.683(3) . ? Mn4 S4 2.694(3) . ? S1 C2 1.793(9) . ? S1 C24 1.824(9) . ? S2 C6 1.769(10) . ? S2 C8 1.794(10) . ? S3 C12 1.773(9) . ? S3 C14 1.796(8) . ? S4 C20 1.773(10) . ? S4 C18 1.805(9) . ? S5 C48 1.813(9) . ? S5 C26 1.831(8) . ? S6 C32 1.774(9) . ? S6 C30 1.817(10) . ? S7 C36 1.745(10) . ? S7 C38 1.790(10) . ? S8 C44 1.782(9) . ? S8 C42 1.831(9) . ? O1 C1 1.349(11) . ? O2 C7 1.318(12) . ? O3 C13 1.346(10) . ? O4 C19 1.320(11) . ? O5 C25 1.270(10) . ? O6 C31 1.286(10) . ? O7 C37 1.305(10) . ? O8 C43 1.342(10) . ? C1 C2 1.368(12) . ? C1 C6 1.421(13) . ? C2 C3 1.346(12) . ? C3 C4 1.442(13) . ? C3 H3A 0.9500 . ? C4 C5 1.366(13) . ? C4 C49 1.424(14) . ? C5 C6 1.404(14) . ? C5 H5A 0.9500 . ? C7 C8 1.361(13) . ? C7 C12 1.447(13) . ? C8 C9 1.413(13) . ? C9 C10 1.330(14) . ? C9 H9A 0.9500 . ? C10 C11 1.399(14) . ? C10 C55 1.524(18) . ? C11 C12 1.369(13) . ? C11 H11A 0.9500 . ? C13 C14 1.329(12) . ? C13 C18 1.380(12) . ? C14 C15 1.480(13) . ? C15 C16 1.357(12) . ? C15 H15A 0.9500 . ? C16 C17 1.385(12) . ? C16 C61 1.455(14) . ? C17 C18 1.392(12) . ? C17 H17A 0.9500 . ? C19 C24 1.358(13) . ? C19 C20 1.408(13) . ? C20 C21 1.386(13) . ? C21 C22 1.365(13) . ? C21 H21A 0.9500 . ? C22 C23 1.407(13) . ? C22 C67 1.504(13) . ? C23 C24 1.348(13) . ? C23 H23A 0.9500 . ? C25 C26 1.405(12) . ? C25 C30 1.437(13) . ? C26 C27 1.346(13) . ? C27 C28 1.354(13) . ? C27 H27A 0.9500 . ? C28 C73 1.444(15) . ? C28 C29 1.448(15) . ? C29 C30 1.359(13) . ? C29 H29A 0.9500 . ? C31 C32 1.417(13) . ? C31 C36 1.478(12) . ? C32 C33 1.405(13) . ? C33 C34 1.350(13) . ? C33 H33A 0.9500 . ? C34 C35 1.315(14) . ? C34 C79 1.405(14) . ? C35 C36 1.426(13) . ? C35 H35A 0.9500 . ? C37 C38 1.363(12) . ? C37 C42 1.425(12) . ? C38 C39 1.439(13) . ? C39 C40 1.334(13) . ? C39 H39A 0.9500 . ? C40 C41 1.362(13) . ? C40 C85 1.531(13) . ? C41 C42 1.360(12) . ? C41 H41A 0.9500 . ? C43 C48 1.379(12) . ? C43 C44 1.432(11) . ? C44 C45 1.335(12) . ? C45 C46 1.423(12) . ? C45 H45A 0.9500 . ? C46 C47 1.354(12) . ? C46 C91 1.472(12) . ? C47 C48 1.372(12) . ? C47 H47A 0.9500 . ? C49 C50 1.340(14) . ? C49 C54 1.364(15) . ? C50 C51 1.411(15) . ? C50 H50A 0.9500 . ? C51 C52 1.332(18) . ? C51 H51A 0.9500 . ? C52 C53 1.397(19) . ? C52 H52A 0.9500 . ? C53 C54 1.500(18) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C55 C60 1.37(2) . ? C55 C56 1.49(2) . ? C56 C57 1.509(17) . ? C56 H56A 0.9500 . ? C57 C58 1.49(3) . ? C57 H57A 0.9500 . ? C58 C59 1.33(3) . ? C58 H58A 0.9500 . ? C59 C60 1.46(3) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? C61 C66 1.328(14) . ? C61 C62 1.434(16) . ? C62 C63 1.492(17) . ? C62 H62A 0.9500 . ? C63 C64 1.335(18) . ? C63 H63A 0.9500 . ? C64 C65 1.393(18) . ? C64 H64A 0.9500 . ? C65 C66 1.351(16) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C67 C68 1.338(17) . ? C67 C72 1.442(17) . ? C68 C69 1.46(2) . ? C68 H68A 0.9500 . ? C69 C70 1.44(2) . ? C69 H69A 0.9500 . ? C70 C71 1.37(2) . ? C70 H70A 0.9500 . ? C71 C72 1.40(2) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C73 C74 1.370(13) . ? C73 C78 1.471(17) . ? C74 C75 1.387(16) . ? C74 H74A 0.9500 . ? C75 C76 1.394(18) . ? C75 H75A 0.9500 . ? C76 C77 1.351(18) . ? C76 H76A 0.9500 . ? C77 C78 1.443(19) . ? C77 H77A 0.9500 . ? C78 H78A 0.9500 . ? C79 C84 1.336(16) . ? C79 C80 1.551(16) . ? C80 C81 1.404(19) . ? C80 H80A 0.9500 . ? C81 C82 1.33(2) . ? C81 H81A 0.9500 . ? C82 C83 1.46(2) . ? C82 H82A 0.9500 . ? C83 C84 1.359(18) . ? C83 H83A 0.9500 . ? C84 H84A 0.9500 . ? C85 C86 1.409(15) . ? C85 C90 1.45(2) . ? C86 C87 1.256(17) . ? C86 H86A 0.9500 . ? C87 C88 1.27(2) . ? C87 H87A 0.9500 . ? C88 C89 1.48(3) . ? C88 H88A 0.9500 . ? C89 C90 1.40(2) . ? C89 H89A 0.9500 . ? C90 H90A 0.9500 . ? C91 C96 1.337(13) . ? C91 C92 1.398(15) . ? C92 C93 1.418(17) . ? C92 H92A 0.9500 . ? C93 C94 1.385(16) . ? C93 H93A 0.9500 . ? C94 C95 1.337(15) . ? C94 H94A 0.9500 . ? C95 C96 1.388(14) . ? C95 H95A 0.9500 . ? C96 H96A 0.9500 . ? C1F C2F 1.379(17) . ? C1F C6F 1.386(13) . ? C1F C7F 1.414(17) . ? C2F C3F 1.408(11) . ? C2F C19F 1.412(13) . ? C3F C22F 1.437(11) . ? C3F C4F 1.455(13) . ? C4F C5F 1.373(13) . ? C4F C23F 1.418(13) . ? C5F C6F 1.380(17) . ? C5F C25F 1.419(17) . ? C6F C16F 1.419(17) . ? C7F C8F 1.406(13) . ? C7F C12F 1.420(17) . ? C8F C9F 1.408(13) . ? C8F C18F 1.440(13) . ? C9F C10F 1.432(13) . ? C9F C30F 1.436(12) . ? C10F C11F 1.383(17) . ? C10F C27F 1.499(17) . ? C11F C12F 1.373(13) . ? C11F C11' 1.373(19) . ? C12F C19F 1.379(17) . ? C13F C14F 1.393(17) . ? C13F C18F 1.409(13) . ? C13F C21' 1.421(16) . ? C14F C15F 1.353(13) . ? C14F C33' 1.370(16) . ? C15F C17F 1.371(13) . ? C15F C34F 1.473(13) . ? C16F C18F 1.395(13) . ? C16F C17F 1.419(16) . ? C17F C25F 1.411(17) . ? C19F C28F 1.399(11) . ? C20F C15' 1.367(17) . ? C20F C35F 1.373(18) . ? C20F C32F 1.59(3) . ? C21F C28F 1.410(13) . ? C21F C22F 1.412(11) . ? C21F C28' 1.445(17) . ? C22F C24F 1.442(13) . ? C23F C26F 1.391(13) . ? C23F C24F 1.425(13) . ? C24F C34' 1.411(13) . ? C25F C31F 1.423(13) . ? C26F C31F 1.427(16) . ? C26F C32F 1.440(18) . ? C27F C20' 1.364(17) . ? C27F C29F 1.410(13) . ? C28F C10' 1.431(16) . ? C29F C23' 1.393(13) . ? C29F C30F 1.442(13) . ? C30F C21' 1.375(13) . ? C31F C35F 1.431(18) . ? C32F C33F 1.345(17) . ? C33F C34' 1.440(13) . ? C33F C13' 1.519(17) . ? C34F C35' 1.364(13) . ? C34F C35F 1.407(14) . ? C1' C6' 1.395(13) . ? C1' C19' 1.438(14) . ? C1' C2' 1.464(13) . ? C2' C3' 1.398(13) . ? C2' C20' 1.427(13) . ? C3' C4' 1.436(13) . ? C3' C23' 1.441(13) . ? C4' C5' 1.389(13) . ? C4' C24' 1.425(13) . ? C5' C6' 1.373(17) . ? C5' C26' 1.378(17) . ? C6' C17' 1.392(17) . ? C7' C8' 1.398(12) . ? C7' C12' 1.404(13) . ? C7' C17' 1.411(13) . ? C8' C13' 1.420(13) . ? C8' C30' 1.424(13) . ? C9' C12' 1.404(17) . ? C9' C10' 1.42(3) . ? C9' C28' 1.427(18) . ? C10' C11' 1.411(19) . ? C11' C29' 1.54(4) . ? C12' C19' 1.385(17) . ? C13' C16' 1.427(17) . ? C14' C15' 1.406(13) . ? C14' C31' 1.417(18) . ? C14' C35' 1.422(18) . ? C15' C16' 1.445(17) . ? C16' C18' 1.412(13) . ? C17' C18' 1.387(17) . ? C18' C26' 1.427(17) . ? C19' C29' 1.439(18) . ? C20' C29' 1.468(18) . ? C21' C22' 1.423(17) . ? C22' C25' 1.391(13) . ? C22' C33' 1.399(16) . ? C23' C25' 1.431(13) . ? C24' C27' 1.395(13) . ? C24' C25' 1.433(13) . ? C26' C31' 1.398(13) . ? C27' C32' 1.430(18) . ? C27' C31' 1.453(17) . ? C28' C30' 1.377(13) . ? C30' C34' 1.470(13) . ? C32' C35' 1.335(16) . ? C32' C33' 1.400(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 O4 144.5(2) . . ? O5 Mn1 O1 72.7(2) . . ? O4 Mn1 O1 93.7(2) . . ? O5 Mn1 O8 87.2(2) . . ? O4 Mn1 O8 72.6(2) . . ? O1 Mn1 O8 122.6(2) . . ? O5 Mn1 S5 76.92(16) . . ? O4 Mn1 S5 123.45(18) . . ? O1 Mn1 S5 142.77(18) . . ? O8 Mn1 S5 75.97(16) . . ? O5 Mn1 S1 128.35(17) . . ? O4 Mn1 S1 75.84(16) . . ? O1 Mn1 S1 74.85(16) . . ? O8 Mn1 S1 144.47(16) . . ? S5 Mn1 S1 109.58(8) . . ? O5 Mn2 O2 144.4(2) . . ? O5 Mn2 O1 72.6(2) . . ? O2 Mn2 O1 93.3(2) . . ? O5 Mn2 O6 88.2(2) . . ? O2 Mn2 O6 72.5(2) . . ? O1 Mn2 O6 123.7(2) . . ? O5 Mn2 S6 75.42(16) . . ? O2 Mn2 S6 125.14(16) . . ? O1 Mn2 S6 141.52(18) . . ? O6 Mn2 S6 75.49(16) . . ? O5 Mn2 S2 128.30(17) . . ? O2 Mn2 S2 76.09(17) . . ? O1 Mn2 S2 75.69(17) . . ? O6 Mn2 S2 143.51(17) . . ? S6 Mn2 S2 109.46(9) . . ? O7 Mn3 O2 144.7(2) . . ? O7 Mn3 O3 72.1(2) . . ? O2 Mn3 O3 93.3(2) . . ? O7 Mn3 O6 88.3(2) . . ? O2 Mn3 O6 72.8(2) . . ? O3 Mn3 O6 123.0(2) . . ? O7 Mn3 S7 76.45(16) . . ? O2 Mn3 S7 124.12(16) . . ? O3 Mn3 S7 142.62(18) . . ? O6 Mn3 S7 74.82(15) . . ? O7 Mn3 S3 127.61(17) . . ? O2 Mn3 S3 75.49(18) . . ? O3 Mn3 S3 74.91(18) . . ? O6 Mn3 S3 144.13(17) . . ? S7 Mn3 S3 110.88(8) . . ? O7 Mn4 O4 145.1(2) . . ? O7 Mn4 O8 88.9(2) . . ? O4 Mn4 O8 73.1(2) . . ? O7 Mn4 O3 72.2(2) . . ? O4 Mn4 O3 92.9(2) . . ? O8 Mn4 O3 123.6(2) . . ? O7 Mn4 S8 77.05(17) . . ? O4 Mn4 S8 124.53(19) . . ? O8 Mn4 S8 75.90(16) . . ? O3 Mn4 S8 142.50(17) . . ? O7 Mn4 S4 127.77(18) . . ? O4 Mn4 S4 75.37(16) . . ? O8 Mn4 S4 143.33(15) . . ? O3 Mn4 S4 75.87(17) . . ? S8 Mn4 S4 108.21(8) . . ? C2 S1 C24 102.2(4) . . ? C2 S1 Mn1 96.7(3) . . ? C24 S1 Mn1 95.1(3) . . ? C6 S2 C8 98.1(4) . . ? C6 S2 Mn2 96.4(3) . . ? C8 S2 Mn2 94.5(3) . . ? C12 S3 C14 102.3(4) . . ? C12 S3 Mn3 96.1(3) . . ? C14 S3 Mn3 94.0(3) . . ? C20 S4 C18 100.4(4) . . ? C20 S4 Mn4 95.5(3) . . ? C18 S4 Mn4 94.8(3) . . ? C48 S5 C26 103.0(4) . . ? C48 S5 Mn1 93.3(3) . . ? C26 S5 Mn1 94.3(3) . . ? C32 S6 C30 101.4(4) . . ? C32 S6 Mn2 93.6(3) . . ? C30 S6 Mn2 95.7(3) . . ? C36 S7 C38 102.4(4) . . ? C36 S7 Mn3 94.6(3) . . ? C38 S7 Mn3 93.0(3) . . ? C44 S8 C42 103.8(4) . . ? C44 S8 Mn4 93.3(3) . . ? C42 S8 Mn4 94.5(3) . . ? C1 O1 Mn2 125.4(5) . . ? C1 O1 Mn1 124.8(5) . . ? Mn2 O1 Mn1 100.1(2) . . ? C7 O2 Mn3 128.1(6) . . ? C7 O2 Mn2 125.6(6) . . ? Mn3 O2 Mn2 102.0(3) . . ? C13 O3 Mn4 125.3(5) . . ? C13 O3 Mn3 124.5(5) . . ? Mn4 O3 Mn3 99.8(3) . . ? C19 O4 Mn1 126.1(6) . . ? C19 O4 Mn4 127.4(6) . . ? Mn1 O4 Mn4 101.7(2) . . ? C25 O5 Mn1 125.9(5) . . ? C25 O5 Mn2 127.2(5) . . ? Mn1 O5 Mn2 103.7(2) . . ? C31 O6 Mn3 122.1(5) . . ? C31 O6 Mn2 118.2(6) . . ? Mn3 O6 Mn2 98.3(2) . . ? C37 O7 Mn3 125.7(5) . . ? C37 O7 Mn4 125.3(5) . . ? Mn3 O7 Mn4 104.6(3) . . ? C43 O8 Mn4 119.0(5) . . ? C43 O8 Mn1 117.6(5) . . ? Mn4 O8 Mn1 98.5(2) . . ? O1 C1 C2 122.3(8) . . ? O1 C1 C6 119.9(9) . . ? C2 C1 C6 117.7(8) . . ? C3 C2 C1 122.7(9) . . ? C3 C2 S1 118.7(7) . . ? C1 C2 S1 118.6(6) . . ? C2 C3 C4 122.2(9) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C5 C4 C49 124.1(9) . . ? C5 C4 C3 114.2(9) . . ? C49 C4 C3 121.6(9) . . ? C4 C5 C6 124.6(10) . . ? C4 C5 H5A 117.7 . . ? C6 C5 H5A 117.7 . . ? C5 C6 C1 118.2(9) . . ? C5 C6 S2 121.7(8) . . ? C1 C6 S2 120.1(7) . . ? O2 C7 C8 122.3(9) . . ? O2 C7 C12 120.5(8) . . ? C8 C7 C12 117.1(9) . . ? C7 C8 C9 121.9(9) . . ? C7 C8 S2 120.2(8) . . ? C9 C8 S2 117.9(7) . . ? C10 C9 C8 120.2(9) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 120.1(11) . . ? C9 C10 C55 121.7(10) . . ? C11 C10 C55 118.1(11) . . ? C12 C11 C10 121.0(10) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C7 119.5(8) . . ? C11 C12 S3 121.7(7) . . ? C7 C12 S3 118.8(7) . . ? C14 C13 O3 121.1(8) . . ? C14 C13 C18 118.4(8) . . ? O3 C13 C18 120.3(8) . . ? C13 C14 C15 121.1(7) . . ? C13 C14 S3 122.3(7) . . ? C15 C14 S3 116.6(6) . . ? C16 C15 C14 119.6(8) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C15 C16 C17 117.5(8) . . ? C15 C16 C61 122.0(8) . . ? C17 C16 C61 120.4(9) . . ? C16 C17 C18 122.1(8) . . ? C16 C17 H17A 118.9 . . ? C18 C17 H17A 118.9 . . ? C13 C18 C17 120.9(8) . . ? C13 C18 S4 120.9(7) . . ? C17 C18 S4 118.2(6) . . ? O4 C19 C24 123.4(9) . . ? O4 C19 C20 119.2(9) . . ? C24 C19 C20 117.3(9) . . ? C21 C20 C19 120.0(9) . . ? C21 C20 S4 119.2(8) . . ? C19 C20 S4 120.7(7) . . ? C22 C21 C20 121.3(9) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C23 118.0(8) . . ? C21 C22 C67 122.0(9) . . ? C23 C22 C67 119.9(9) . . ? C24 C23 C22 120.0(8) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C19 123.3(9) . . ? C23 C24 S1 118.4(7) . . ? C19 C24 S1 118.0(7) . . ? O5 C25 C26 123.3(8) . . ? O5 C25 C30 123.7(8) . . ? C26 C25 C30 112.9(8) . . ? C27 C26 C25 123.9(8) . . ? C27 C26 S5 118.9(7) . . ? C25 C26 S5 116.9(7) . . ? C26 C27 C28 122.6(10) . . ? C26 C27 H27A 118.7 . . ? C28 C27 H27A 118.7 . . ? C27 C28 C73 122.0(11) . . ? C27 C28 C29 117.7(10) . . ? C73 C28 C29 120.3(9) . . ? C30 C29 C28 118.5(9) . . ? C30 C29 H29A 120.8 . . ? C28 C29 H29A 120.8 . . ? C29 C30 C25 124.2(9) . . ? C29 C30 S6 119.8(7) . . ? C25 C30 S6 114.9(7) . . ? O6 C31 C32 125.5(8) . . ? O6 C31 C36 119.6(9) . . ? C32 C31 C36 114.8(8) . . ? C33 C32 C31 121.1(8) . . ? C33 C32 S6 122.1(7) . . ? C31 C32 S6 116.7(7) . . ? C34 C33 C32 123.4(9) . . ? C34 C33 H33A 118.3 . . ? C32 C33 H33A 118.3 . . ? C35 C34 C33 117.2(9) . . ? C35 C34 C79 120.5(9) . . ? C33 C34 C79 122.0(10) . . ? C34 C35 C36 125.7(9) . . ? C34 C35 H35A 117.2 . . ? C36 C35 H35A 117.2 . . ? C35 C36 C31 117.3(9) . . ? C35 C36 S7 124.2(7) . . ? C31 C36 S7 118.5(7) . . ? O7 C37 C38 121.1(8) . . ? O7 C37 C42 123.0(8) . . ? C38 C37 C42 115.5(8) . . ? C37 C38 C39 120.7(9) . . ? C37 C38 S7 120.8(7) . . ? C39 C38 S7 118.2(7) . . ? C40 C39 C38 119.7(9) . . ? C40 C39 H39A 120.2 . . ? C38 C39 H39A 120.2 . . ? C39 C40 C41 122.0(9) . . ? C39 C40 C85 118.1(9) . . ? C41 C40 C85 119.7(9) . . ? C42 C41 C40 118.3(9) . . ? C42 C41 H41A 120.9 . . ? C40 C41 H41A 120.9 . . ? C41 C42 C37 123.8(8) . . ? C41 C42 S8 119.0(7) . . ? C37 C42 S8 116.9(7) . . ? O8 C43 C48 123.3(7) . . ? O8 C43 C44 121.3(8) . . ? C48 C43 C44 115.4(8) . . ? C45 C44 C43 122.7(8) . . ? C45 C44 S8 118.8(7) . . ? C43 C44 S8 118.3(7) . . ? C44 C45 C46 121.3(8) . . ? C44 C45 H45A 119.4 . . ? C46 C45 H45A 119.4 . . ? C47 C46 C45 115.1(8) . . ? C47 C46 C91 123.1(8) . . ? C45 C46 C91 121.5(8) . . ? C46 C47 C48 124.9(8) . . ? C46 C47 H47A 117.6 . . ? C48 C47 H47A 117.6 . . ? C47 C48 C43 120.4(8) . . ? C47 C48 S5 121.4(7) . . ? C43 C48 S5 118.0(6) . . ? C50 C49 C54 115.1(10) . . ? C50 C49 C4 124.2(10) . . ? C54 C49 C4 120.5(10) . . ? C49 C50 C51 121.8(12) . . ? C49 C50 H50A 119.1 . . ? C51 C50 H50A 119.1 . . ? C52 C51 C50 123.4(13) . . ? C52 C51 H51A 118.3 . . ? C50 C51 H51A 118.3 . . ? C51 C52 C53 120.4(13) . . ? C51 C52 H52A 119.8 . . ? C53 C52 H52A 119.8 . . ? C52 C53 C54 112.9(13) . . ? C52 C53 H53A 123.6 . . ? C54 C53 H53A 123.6 . . ? C49 C54 C53 126.1(12) . . ? C49 C54 H54A 117.0 . . ? C53 C54 H54A 117.0 . . ? C60 C55 C56 119.5(15) . . ? C60 C55 C10 124.0(14) . . ? C56 C55 C10 116.2(13) . . ? C55 C56 C57 120.5(19) . . ? C55 C56 H56A 119.8 . . ? C57 C56 H56A 119.8 . . ? C58 C57 C56 115(2) . . ? C58 C57 H57A 122.6 . . ? C56 C57 H57A 122.6 . . ? C59 C58 C57 120(3) . . ? C59 C58 H58A 119.9 . . ? C57 C58 H58A 119.9 . . ? C58 C59 C60 126(3) . . ? C58 C59 H59A 117.1 . . ? C60 C59 H59A 117.1 . . ? C55 C60 C59 118.5(18) . . ? C55 C60 H60A 120.7 . . ? C59 C60 H60A 120.7 . . ? C66 C61 C62 117.8(10) . . ? C66 C61 C16 124.3(10) . . ? C62 C61 C16 117.8(10) . . ? C61 C62 C63 119.2(11) . . ? C61 C62 H62A 120.4 . . ? C63 C62 H62A 120.4 . . ? C64 C63 C62 117.4(12) . . ? C64 C63 H63A 121.3 . . ? C62 C63 H63A 121.3 . . ? C63 C64 C65 120.9(13) . . ? C63 C64 H64A 119.6 . . ? C65 C64 H64A 119.6 . . ? C66 C65 C64 121.5(12) . . ? C66 C65 H65A 119.2 . . ? C64 C65 H65A 119.2 . . ? C61 C66 C65 123.2(12) . . ? C61 C66 H66A 118.4 . . ? C65 C66 H66A 118.4 . . ? C68 C67 C72 116.6(11) . . ? C68 C67 C22 122.5(11) . . ? C72 C67 C22 120.8(11) . . ? C67 C68 C69 126.9(14) . . ? C67 C68 H68A 116.6 . . ? C69 C68 H68A 116.6 . . ? C70 C69 C68 109.9(16) . . ? C70 C69 H69A 125.0 . . ? C68 C69 H69A 125.0 . . ? C71 C70 C69 126.9(17) . . ? C71 C70 H70A 116.6 . . ? C69 C70 H70A 116.6 . . ? C70 C71 C72 117.0(17) . . ? C70 C71 H71A 121.5 . . ? C72 C71 H71A 121.5 . . ? C71 C72 C67 121.8(15) . . ? C71 C72 H72A 119.1 . . ? C67 C72 H72A 119.1 . . ? C74 C73 C28 121.7(9) . . ? C74 C73 C78 117.8(10) . . ? C28 C73 C78 120.5(10) . . ? C73 C74 C75 121.2(11) . . ? C73 C74 H74A 119.4 . . ? C75 C74 H74A 119.4 . . ? C74 C75 C76 124.8(12) . . ? C74 C75 H75A 117.6 . . ? C76 C75 H75A 117.6 . . ? C77 C76 C75 113.9(13) . . ? C77 C76 H76A 123.1 . . ? C75 C76 H76A 123.1 . . ? C76 C77 C78 126.4(14) . . ? C76 C77 H77A 116.8 . . ? C78 C77 H77A 116.8 . . ? C77 C78 C73 115.6(14) . . ? C77 C78 H78A 122.2 . . ? C73 C78 H78A 122.2 . . ? C84 C79 C34 127.6(10) . . ? C84 C79 C80 113.7(11) . . ? C34 C79 C80 118.5(11) . . ? C81 C80 C79 114.4(14) . . ? C81 C80 H80A 122.8 . . ? C79 C80 H80A 122.8 . . ? C82 C81 C80 126.9(17) . . ? C82 C81 H81A 116.5 . . ? C80 C81 H81A 116.5 . . ? C81 C82 C83 118.2(15) . . ? C81 C82 H82A 120.9 . . ? C83 C82 H82A 120.9 . . ? C84 C83 C82 115.4(14) . . ? C84 C83 H83A 122.3 . . ? C82 C83 H83A 122.3 . . ? C79 C84 C83 130.6(13) . . ? C79 C84 H84A 114.7 . . ? C83 C84 H84A 114.7 . . ? C86 C85 C90 115.8(12) . . ? C86 C85 C40 125.0(10) . . ? C90 C85 C40 118.4(11) . . ? C87 C86 C85 128.3(14) . . ? C87 C86 H86A 115.9 . . ? C85 C86 H86A 115.9 . . ? C86 C87 C88 117.2(15) . . ? C86 C87 H87A 121.4 . . ? C88 C87 H87A 121.4 . . ? C87 C88 C89 124.2(17) . . ? C87 C88 H88A 117.9 . . ? C89 C88 H88A 117.9 . . ? C90 C89 C88 117.5(18) . . ? C90 C89 H89A 121.2 . . ? C88 C89 H89A 121.2 . . ? C89 C90 C85 116.0(18) . . ? C89 C90 H90A 122.0 . . ? C85 C90 H90A 122.0 . . ? C96 C91 C92 117.8(9) . . ? C96 C91 C46 124.2(8) . . ? C92 C91 C46 118.0(9) . . ? C91 C92 C93 120.1(11) . . ? C91 C92 H92A 120.0 . . ? C93 C92 H92A 120.0 . . ? C94 C93 C92 119.4(11) . . ? C94 C93 H93A 120.3 . . ? C92 C93 H93A 120.3 . . ? C95 C94 C93 119.1(11) . . ? C95 C94 H94A 120.5 . . ? C93 C94 H94A 120.5 . . ? C94 C95 C96 121.4(10) . . ? C94 C95 H95A 119.3 . . ? C96 C95 H95A 119.3 . . ? C91 C96 C95 122.2(10) . . ? C91 C96 H96A 118.9 . . ? C95 C96 H96A 118.9 . . ? C2F C1F C6F 122.1(15) . . ? C2F C1F C7F 110.0(19) . . ? C6F C1F C7F 116.8(16) . . ? C1F C2F C3F 119.8(16) . . ? C1F C2F C19F 106.8(19) . . ? C3F C2F C19F 117.8(14) . . ? C2F C3F C22F 123.9(11) . . ? C2F C3F C4F 118.8(13) . . ? C22F C3F C4F 104.1(12) . . ? C5F C4F C23F 118.5(15) . . ? C5F C4F C3F 117.3(14) . . ? C23F C4F C3F 110.8(13) . . ? C4F C5F C6F 124.0(16) . . ? C4F C5F C25F 120.9(16) . . ? C6F C5F C25F 104.3(18) . . ? C5F C6F C1F 117.9(14) . . ? C5F C6F C16F 107.2(19) . . ? C1F C6F C16F 123.2(14) . . ? C8F C7F C1F 122.9(15) . . ? C8F C7F C12F 121.9(16) . . ? C1F C7F C12F 105.4(18) . . ? C7F C8F C9F 114.5(14) . . ? C7F C8F C18F 117.8(14) . . ? C9F C8F C18F 120.4(15) . . ? C8F C9F C10F 122.0(14) . . ? C8F C9F C30F 117.8(15) . . ? C10F C9F C30F 109.2(13) . . ? C11F C10F C9F 118.6(17) . . ? C11F C10F C27F 122(2) . . ? C9F C10F C27F 104.4(12) . . ? C12F C11F C11' 120.2(18) . . ? C12F C11F C10F 118.5(15) . . ? C11' C11F C10F 120(2) . . ? C11F C12F C19F 120.3(14) . . ? C11F C12F C7F 119.6(16) . . ? C19F C12F C7F 109(2) . . ? C14F C13F C18F 117.4(15) . . ? C14F C13F C21' 111.0(19) . . ? C18F C13F C21' 118.8(14) . . ? C15F C14F C33' 123.2(16) . . ? C15F C14F C13F 126.9(17) . . ? C33' C14F C13F 100.4(18) . . ? C14F C15F C17F 112.5(14) . . ? C14F C15F C34F 117.3(15) . . ? C17F C15F C34F 118.5(14) . . ? C18F C16F C17F 118.5(15) . . ? C18F C16F C6F 118.8(16) . . ? C17F C16F C6F 114(2) . . ? C15F C17F C25F 123.3(16) . . ? C15F C17F C16F 124.5(16) . . ? C25F C17F C16F 99.0(18) . . ? C16F C18F C13F 116.7(13) . . ? C16F C18F C8F 120.3(14) . . ? C13F C18F C8F 120.0(12) . . ? C12F C19F C28F 121.2(15) . . ? C12F C19F C2F 108.5(19) . . ? C28F C19F C2F 120.7(12) . . ? C15' C20F C35F 130(3) . . ? C15' C20F C32F 119(2) . . ? C35F C20F C32F 101.2(16) . . ? C28F C21F C22F 122.5(13) . . ? C28F C21F C28' 100.0(18) . . ? C22F C21F C28' 116.0(15) . . ? C21F C22F C3F 114.7(12) . . ? C21F C22F C24F 123.4(14) . . ? C3F C22F C24F 110.3(13) . . ? C26F C23F C4F 119.4(13) . . ? C26F C23F C24F 118.9(15) . . ? C4F C23F C24F 107.4(13) . . ? C34' C24F C23F 122.7(13) . . ? C34' C24F C22F 116.8(13) . . ? C23F C24F C22F 107.4(13) . . ? C17F C25F C5F 115.7(18) . . ? C17F C25F C31F 115.6(15) . . ? C5F C25F C31F 123.3(13) . . ? C23F C26F C31F 125.0(15) . . ? C23F C26F C32F 118.4(15) . . ? C31F C26F C32F 108.0(18) . . ? C20' C27F C29F 119.5(14) . . ? C20' C27F C10F 122(2) . . ? C29F C27F C10F 110.6(14) . . ? C19F C28F C21F 119.6(11) . . ? C19F C28F C10' 117.6(15) . . ? C21F C28F C10' 114.0(18) . . ? C23' C29F C27F 123.6(15) . . ? C23' C29F C30F 120.2(15) . . ? C27F C29F C30F 106.1(14) . . ? C21' C30F C9F 121.6(13) . . ? C21' C30F C29F 120.2(15) . . ? C9F C30F C29F 109.6(13) . . ? C25F C31F C26F 112.6(15) . . ? C25F C31F C35F 123.9(16) . . ? C26F C31F C35F 107.2(16) . . ? C33F C32F C26F 122.2(16) . . ? C33F C32F C20F 118(2) . . ? C26F C32F C20F 107.9(19) . . ? C32F C33F C34' 121.2(16) . . ? C32F C33F C13' 120(2) . . ? C34' C33F C13' 103.4(12) . . ? C35' C34F C35F 115.9(14) . . ? C35' C34F C15F 121.1(13) . . ? C35F C34F C15F 120.5(14) . . ? C20F C35F C34F 117(2) . . ? C20F C35F C31F 115.7(18) . . ? C34F C35F C31F 116.2(17) . . ? C6' C1' C19' 118.2(15) . . ? C6' C1' C2' 122.2(15) . . ? C19' C1' C2' 107.7(13) . . ? C3' C2' C20' 119.2(15) . . ? C3' C2' C1' 115.0(14) . . ? C20' C2' C1' 109.9(13) . . ? C2' C3' C4' 122.4(13) . . ? C2' C3' C23' 121.7(13) . . ? C4' C3' C23' 102.5(12) . . ? C5' C4' C24' 117.2(15) . . ? C5' C4' C3' 119.2(15) . . ? C24' C4' C3' 113.5(14) . . ? C6' C5' C26' 104.0(19) . . ? C6' C5' C4' 121.0(17) . . ? C26' C5' C4' 122.5(16) . . ? C5' C6' C17' 111(2) . . ? C5' C6' C1' 120.0(14) . . ? C17' C6' C1' 120.6(15) . . ? C8' C7' C12' 119.9(13) . . ? C8' C7' C17' 117.8(12) . . ? C12' C7' C17' 119.5(14) . . ? C7' C8' C13' 119.3(15) . . ? C7' C8' C30' 121.7(15) . . ? C13' C8' C30' 108.0(14) . . ? C12' C9' C10' 120(2) . . ? C12' C9' C28' 124.4(16) . . ? C10' C9' C28' 105(2) . . ? C11' C10' C9' 130(2) . . ? C11' C10' C28F 118.5(16) . . ? C9' C10' C28F 106.6(18) . . ? C11F C11' C10' 119(2) . . ? C11F C11' C29' 116(2) . . ? C10' C11' C29' 106(2) . . ? C19' C12' C7' 119.7(16) . . ? C19' C12' C9' 116.3(19) . . ? C7' C12' C9' 116.6(16) . . ? C8' C13' C16' 121.4(15) . . ? C8' C13' C33F 110.2(14) . . ? C16' C13' C33F 121(2) . . ? C15' C14' C31' 120.3(14) . . ? C15' C14' C35' 123.2(16) . . ? C31' C14' C35' 106(2) . . ? C20F C15' C14' 108.9(17) . . ? C20F C15' C16' 123(2) . . ? C14' C15' C16' 121.2(15) . . ? C18' C16' C13' 115.9(14) . . ? C18' C16' C15' 116.0(15) . . ? C13' C16' C15' 118(2) . . ? C18' C17' C6' 108.5(19) . . ? C18' C17' C7' 120.5(16) . . ? C6' C17' C7' 120.6(16) . . ? C17' C18' C16' 122.1(16) . . ? C17' C18' C26' 104(2) . . ? C16' C18' C26' 123.6(13) . . ? C12' C19' C1' 121.0(15) . . ? C12' C19' C29' 121(2) . . ? C1' C19' C29' 106.4(15) . . ? C27F C20' C2' 120.1(16) . . ? C27F C20' C29' 113(2) . . ? C2' C20' C29' 104.9(13) . . ? C30F C21' C13F 121.1(16) . . ? C30F C21' C22' 118.4(14) . . ? C13F C21' C22' 109.3(18) . . ? C25' C22' C33' 122.1(14) . . ? C25' C22' C21' 123.1(15) . . ? C33' C22' C21' 99.1(19) . . ? C29F C23' C25' 120.2(13) . . ? C29F C23' C3' 115.5(15) . . ? C25' C23' C3' 110.9(13) . . ? C27' C24' C4' 124.1(14) . . ? C27' C24' C25' 118.8(14) . . ? C4' C24' C25' 104.8(13) . . ? C22' C25' C23' 117.7(15) . . ? C22' C25' C24' 117.2(15) . . ? C23' C25' C24' 108.1(13) . . ? C5' C26' C31' 118.9(15) . . ? C5' C26' C18' 112(2) . . ? C31' C26' C18' 118.2(16) . . ? C24' C27' C32' 124.7(15) . . ? C24' C27' C31' 114.4(15) . . ? C32' C27' C31' 109.1(19) . . ? C30' C28' C9' 116.9(14) . . ? C30' C28' C21F 123.9(12) . . ? C9' C28' C21F 114.1(19) . . ? C19' C29' C20' 110.5(16) . . ? C19' C29' C11' 124.6(19) . . ? C20' C29' C11' 122.1(18) . . ? C28' C30' C8' 119.7(16) . . ? C28' C30' C34' 116.9(16) . . ? C8' C30' C34' 108.3(13) . . ? C26' C31' C14' 120.5(16) . . ? C26' C31' C27' 122.4(16) . . ? C14' C31' C27' 105(2) . . ? C35' C32' C33' 128.9(19) . . ? C35' C32' C27' 105.7(19) . . ? C33' C32' C27' 113.7(16) . . ? C14F C33' C22' 119.5(19) . . ? C14F C33' C32' 113.6(14) . . ? C22' C33' C32' 122.8(17) . . ? C24F C34' C33F 116.2(14) . . ? C24F C34' C30' 122.1(15) . . ? C33F C34' C30' 110.1(13) . . ? C32' C35' C34F 114.3(16) . . ? C32' C35' C14' 113(2) . . ? C34F C35' C14' 121.0(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.820 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.159 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.056 0.836 0.016 20470 7272 ' ' 2 0.000 0.500 0.204 33 14 ' ' 3 0.500 0.000 0.204 33 14 ' ' 4 0.250 0.750 0.454 33 9 ' ' 5 0.750 0.250 0.454 33 9 ' ' 6 0.000 0.000 0.704 33 14 ' ' 7 0.500 0.500 0.704 33 14 ' ' 8 0.250 0.250 0.954 33 9 ' ' 9 0.750 0.750 0.954 33 9 ' ' _platon_squeeze_details ; ; ###END data_compound_775187 _database_code_depnum_ccdc_archive 'CCDC 775187' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Mn4(C48H28O4S4)2) (C60)2' _chemical_melting_point ? _chemical_formula_moiety 'C96 H56 Mn4 O8 S8, 2(C60)' _chemical_formula_sum 'C216 H56 Mn4 O8 S8' _chemical_formula_weight 3254.85 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number No.15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.470(2) _cell_length_b 14.4254(9) _cell_length_c 37.212(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.3000(10) _cell_angle_gamma 90.00 _cell_volume 17966.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 9253 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6576 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9350 _exptl_absorpt_correction_T_max 0.9507 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70547 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.06 _reflns_number_total 15913 _reflns_number_gt 10247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. These atoms include C39 > C42, C75, C77, C100. The restraint command leads to a 42 restraints which cannot be completely avoided. The high Rint factor for this compound might be due to the weak high-angle diffractions and the disorder of toluene molecules and phenyl groups. Considering the large cell volume and some incorporated disordered toluenes (the elcetron counts being 6352.4 within 17966.4 A^3^ per cell), the present data is not so good compared with the ordinary ones so that the resulted problems can not be completely solved by further refinements even with some re-collected data. These problems are common for the calixarene-based compounds due to the big molecules of calixarenes and their flexibility. ; _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^)+(0.1193P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15913 _refine_ls_number_parameters 1053 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1718 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.69183(5) 0.2500 0.02046(18) Uani 1 2 d S . . Mn2 Mn -0.067360(15) 0.52809(4) 0.232844(13) 0.02100(15) Uani 1 1 d . . . Mn3 Mn 0.0000 0.36445(5) 0.2500 0.02150(19) Uani 1 2 d S . . S1 S 0.01800(2) 0.79599(6) 0.19085(2) 0.0220(2) Uani 1 1 d . . . S2 S -0.09605(2) 0.52734(6) 0.16584(2) 0.0243(2) Uani 1 1 d . . . S3 S 0.01884(2) 0.26063(6) 0.19068(2) 0.0234(2) Uani 1 1 d . . . S4 S 0.13070(2) 0.52921(6) 0.22350(2) 0.0213(2) Uani 1 1 d . . . O1 O -0.03914(7) 0.64426(17) 0.20928(6) 0.0263(6) Uani 1 1 d . . . O2 O -0.02776(7) 0.43439(17) 0.20506(6) 0.0274(6) Uani 1 1 d . . . O3 O 0.05735(7) 0.41100(17) 0.23386(6) 0.0272(6) Uani 1 1 d . . . O4 O 0.04952(7) 0.62177(17) 0.22474(6) 0.0266(6) Uani 1 1 d . . . C1 C -0.04012(9) 0.6663(2) 0.17496(8) 0.0205(7) Uani 1 1 d . . . C2 C -0.01583(9) 0.7369(2) 0.16111(8) 0.0208(7) Uani 1 1 d . . . C3 C -0.01879(10) 0.7654(2) 0.12572(9) 0.0256(8) Uani 1 1 d . . . H3A H -0.0024 0.8146 0.1174 0.031 Uiso 1 1 calc R . . C4 C -0.04544(11) 0.7227(3) 0.10211(9) 0.0296(8) Uani 1 1 d . B . C5 C -0.06927(11) 0.6511(3) 0.11512(10) 0.0319(9) Uani 1 1 d . . . H5A H -0.0878 0.6213 0.0995 0.038 Uiso 1 1 calc R . . C6 C -0.06630(10) 0.6225(2) 0.15089(9) 0.0230(8) Uani 1 1 d . . . C7 C -0.03607(10) 0.3976(2) 0.17375(8) 0.0212(7) Uani 1 1 d . . . C8 C -0.06644(10) 0.4321(2) 0.15094(9) 0.0231(8) Uani 1 1 d . . . C9 C -0.07375(11) 0.3944(3) 0.11731(9) 0.0269(8) Uani 1 1 d . . . H9A H -0.0939 0.4209 0.1024 0.032 Uiso 1 1 calc R . . C10 C -0.05215(11) 0.3184(3) 0.10483(9) 0.0308(9) Uani 1 1 d . . . C11 C -0.02306(10) 0.2803(3) 0.12747(9) 0.0265(8) Uani 1 1 d . . . H11A H -0.0081 0.2282 0.1196 0.032 Uiso 1 1 calc R . . C12 C -0.01567(9) 0.3173(2) 0.16126(9) 0.0230(8) Uani 1 1 d . . . C13 C 0.07760(9) 0.3912(2) 0.20496(8) 0.0210(7) Uani 1 1 d . . . C14 C 0.06440(10) 0.3204(2) 0.18135(9) 0.0235(8) Uani 1 1 d . . . C15 C 0.08672(10) 0.2941(3) 0.15190(9) 0.0280(8) Uani 1 1 d . . . H15A H 0.0769 0.2471 0.1363 0.034 Uiso 1 1 calc R . . C16 C 0.12374(11) 0.3359(3) 0.14476(9) 0.0298(9) Uani 1 1 d . . . C17 C 0.13662(10) 0.4062(3) 0.16759(9) 0.0274(8) Uani 1 1 d . . . H17A H 0.1615 0.4356 0.1633 0.033 Uiso 1 1 calc R . . C18 C 0.11380(10) 0.4342(2) 0.19649(9) 0.0213(7) Uani 1 1 d . . . C19 C 0.07461(9) 0.6589(2) 0.20217(8) 0.0204(7) Uani 1 1 d . . . C20 C 0.11363(9) 0.6253(2) 0.19692(8) 0.0216(7) Uani 1 1 d . . . C21 C 0.13929(10) 0.6632(3) 0.17141(9) 0.0250(8) Uani 1 1 d . . . H21A H 0.1653 0.6381 0.1686 0.030 Uiso 1 1 calc R . . C22 C 0.12733(10) 0.7373(3) 0.14999(9) 0.0272(8) Uani 1 1 d . . . C23 C 0.08931(10) 0.7750(3) 0.15583(9) 0.0249(8) Uani 1 1 d . . . H23A H 0.0808 0.8267 0.1420 0.030 Uiso 1 1 calc R . . C24 C 0.06396(10) 0.7383(2) 0.18137(8) 0.0222(7) Uani 1 1 d . . . C25 C -0.04917(13) 0.7541(3) 0.06420(10) 0.0412(10) Uani 1 1 d . . . C28 C -0.0537(2) 0.8102(5) -0.00679(15) 0.0896(14) Uani 1 1 d . . . H28A H -0.0553 0.8259 -0.0315 0.107 Uiso 1 1 calc R A 1 C26 C -0.0852(5) 0.7911(9) 0.0533(3) 0.0896(14) Uani 0.543(6) 1 d P B 1 H26A H -0.1077 0.7936 0.0687 0.107 Uiso 0.543(6) 1 calc PR B 1 C27 C -0.0863(5) 0.8266(9) 0.0161(3) 0.0896(14) Uani 0.543(6) 1 d P B 1 H27A H -0.1089 0.8602 0.0076 0.107 Uiso 0.543(6) 1 calc PR B 1 C29 C -0.0212(5) 0.7731(9) 0.0064(3) 0.0896(14) Uani 0.543(6) 1 d P B 1 H29A H 0.0010 0.7620 -0.0089 0.107 Uiso 0.543(6) 1 calc PR B 1 C30 C -0.0188(5) 0.7501(9) 0.0421(3) 0.0896(14) Uani 0.543(6) 1 d P B 1 H30A H 0.0063 0.7302 0.0514 0.107 Uiso 0.543(6) 1 calc PR B 1 C26' C -0.0630(5) 0.8343(11) 0.0531(3) 0.0896(14) Uani 0.457(6) 1 d P B 2 H26B H -0.0737 0.8756 0.0704 0.107 Uiso 0.457(6) 1 calc PR B 2 C27' C -0.0627(5) 0.8620(12) 0.0170(3) 0.0896(14) Uani 0.457(6) 1 d P B 2 H27B H -0.0698 0.9240 0.0113 0.107 Uiso 0.457(6) 1 calc PR B 2 C29' C -0.0374(5) 0.7203(11) -0.0016(3) 0.0896(14) Uani 0.457(6) 1 d P B 2 H29B H -0.0292 0.6816 -0.0209 0.107 Uiso 0.457(6) 1 calc PR B 2 C30' C -0.0344(5) 0.6939(11) 0.0350(3) 0.0896(14) Uani 0.457(6) 1 d P B 2 H30B H -0.0226 0.6359 0.0410 0.107 Uiso 0.457(6) 1 calc PR B 2 C31 C -0.06012(13) 0.2778(3) 0.06870(10) 0.0401(10) Uani 1 1 d . . . C32 C -0.07234(17) 0.3327(4) 0.03983(12) 0.0678(16) Uani 1 1 d . . . H32A H -0.0756 0.3975 0.0434 0.081 Uiso 1 1 calc R . . C33 C -0.0799(2) 0.2955(5) 0.00608(14) 0.105(3) Uani 1 1 d . . . H33A H -0.0880 0.3340 -0.0133 0.126 Uiso 1 1 calc R . . C34 C -0.0752(2) 0.2006(5) 0.00136(14) 0.104(3) Uani 1 1 d . . . H34A H -0.0805 0.1738 -0.0215 0.125 Uiso 1 1 calc R . . C35 C -0.06314(18) 0.1462(4) 0.02875(13) 0.0806(19) Uani 1 1 d . . . H35A H -0.0599 0.0816 0.0250 0.097 Uiso 1 1 calc R . . C36 C -0.05538(14) 0.1834(3) 0.06237(11) 0.0523(12) Uani 1 1 d . . . H36A H -0.0467 0.1440 0.0813 0.063 Uiso 1 1 calc R . . C37 C 0.14791(13) 0.3058(3) 0.11336(12) 0.0499(12) Uani 1 1 d . . . C38 C 0.13188(17) 0.2913(4) 0.07998(11) 0.0633(15) Uani 1 1 d . . . H38A H 0.1039 0.2993 0.0769 0.076 Uiso 1 1 calc R . . C39 C 0.1542(2) 0.2656(5) 0.05054(17) 0.093(2) Uani 1 1 d U . . H39A H 0.1419 0.2559 0.0278 0.112 Uiso 1 1 calc R . . C40 C 0.1945(3) 0.2544(6) 0.0551(2) 0.123(3) Uani 1 1 d U . . H40A H 0.2105 0.2392 0.0349 0.147 Uiso 1 1 calc R . . C41 C 0.2125(2) 0.2647(6) 0.0884(2) 0.116(2) Uani 1 1 d U . . H41A H 0.2403 0.2532 0.0913 0.139 Uiso 1 1 calc R . . C42 C 0.18913(17) 0.2922(5) 0.11781(17) 0.0870(19) Uani 1 1 d U . . H42A H 0.2013 0.3017 0.1407 0.104 Uiso 1 1 calc R . . C43 C 0.15415(11) 0.7755(3) 0.12235(10) 0.0332(9) Uani 1 1 d . . . C44 C 0.19383(12) 0.7957(3) 0.12995(12) 0.0451(11) Uani 1 1 d . . . H44A H 0.2039 0.7842 0.1534 0.054 Uiso 1 1 calc R . . C45 C 0.21922(14) 0.8324(4) 0.10409(15) 0.0773(19) Uani 1 1 d . . . H45A H 0.2463 0.8460 0.1099 0.093 Uiso 1 1 calc R . . C46 C 0.20448(15) 0.8489(5) 0.06973(16) 0.091(2) Uani 1 1 d . . . H46A H 0.2213 0.8745 0.0518 0.109 Uiso 1 1 calc R . . C47 C 0.16489(16) 0.8277(5) 0.06164(13) 0.081(2) Uani 1 1 d . . . H47A H 0.1549 0.8370 0.0380 0.098 Uiso 1 1 calc R . . C48 C 0.14001(13) 0.7931(4) 0.08801(11) 0.0533(13) Uani 1 1 d . . . H48A H 0.1128 0.7813 0.0824 0.064 Uiso 1 1 calc R . . C49 C 0.3391(3) 0.4228(6) 0.12338(15) 0.099(2) Uani 1 1 d . . . C50 C 0.3765(2) 0.4794(6) 0.12170(15) 0.085(2) Uani 1 1 d . . . C51 C 0.3750(3) 0.5688(6) 0.12082(15) 0.090(2) Uani 1 1 d . . . C52 C 0.3398(3) 0.6208(7) 0.12184(18) 0.110(3) Uani 1 1 d . . . C53 C 0.3028(2) 0.5727(6) 0.12256(14) 0.078(2) Uani 1 1 d . . . C54 C 0.3020(2) 0.4724(5) 0.12356(14) 0.077(2) Uani 1 1 d . . . C55 C 0.27024(18) 0.4435(4) 0.14686(16) 0.0701(17) Uani 1 1 d . . . C56 C 0.27601(16) 0.3662(4) 0.16948(16) 0.0677(16) Uani 1 1 d . . . C57 C 0.31440(17) 0.3172(4) 0.16784(17) 0.0651(15) Uani 1 1 d . . . C58 C 0.3432(3) 0.3464(5) 0.1459(2) 0.103(2) Uani 1 1 d . . . C59 C 0.24992(15) 0.5258(5) 0.16160(17) 0.0670(16) Uani 1 1 d . . . C60 C 0.23741(14) 0.5272(5) 0.19624(19) 0.0722(17) Uani 1 1 d . . . C61 C 0.24296(12) 0.4455(4) 0.21875(16) 0.0586(14) Uani 1 1 d . . . C62 C 0.26264(15) 0.3665(4) 0.20429(15) 0.0665(16) Uani 1 1 d . . . C63 C 0.29109(15) 0.3198(4) 0.22921(16) 0.0587(14) Uani 1 1 d . . . C64 C 0.3243(2) 0.2870(4) 0.2055(2) 0.088(2) Uani 1 1 d . . . C65 C 0.3604(2) 0.2881(4) 0.2168(2) 0.091(2) Uani 1 1 d . . . C66 C 0.39245(17) 0.3178(3) 0.1934(2) 0.0720(18) Uani 1 1 d . . . C67 C 0.38683(18) 0.3503(5) 0.15869(17) 0.0693(16) Uani 1 1 d . . . C68 C 0.4062(3) 0.4260(6) 0.1459(2) 0.099(2) Uani 1 1 d . . . C69 C 0.4061(3) 0.6224(6) 0.1442(2) 0.102(3) Uani 1 1 d . . . C70 C 0.38765(19) 0.6989(4) 0.15535(16) 0.0660(15) Uani 1 1 d . . . C71 C 0.3433(3) 0.7000(6) 0.1422(2) 0.102(3) Uani 1 1 d . . . C72 C 0.31529(17) 0.7340(4) 0.16400(18) 0.0676(16) Uani 1 1 d . . . C73 C 0.27638(19) 0.6858(5) 0.1663(2) 0.089(2) Uani 1 1 d . . . C74 C 0.2704(2) 0.6083(5) 0.14595(18) 0.084(2) Uani 1 1 d . . . C75 C 0.3241(2) 0.7676(4) 0.2012(2) 0.098(2) Uani 1 1 d U . . C76 C 0.29218(17) 0.7392(4) 0.2254(2) 0.0704(17) Uani 1 1 d . . . C77 C 0.26247(17) 0.6872(5) 0.20182(18) 0.0799(19) Uani 1 1 d U . . C78 C 0.24287(13) 0.6108(4) 0.21730(16) 0.0624(15) Uani 1 1 d . . . C79 C 0.36846(17) 0.3220(4) 0.25338(19) 0.0655(16) Uani 1 1 d . . . C80 C 0.40780(19) 0.3718(5) 0.2506(2) 0.088(2) Uani 1 1 d . . . C81 C 0.41359(18) 0.4487(4) 0.27121(17) 0.0718(18) Uani 1 1 d . . . C82 C 0.3801(2) 0.4826(5) 0.29510(14) 0.0739(19) Uani 1 1 d . . . C83 C 0.38096(19) 0.5842(5) 0.29377(14) 0.0760(19) Uani 1 1 d . . . C84 C 0.3456(3) 0.6327(6) 0.29417(15) 0.090(2) Uani 1 1 d . . . C85 C 0.3413(3) 0.7086(5) 0.2725(2) 0.098(2) Uani 1 1 d . . . C86 C 0.44057(12) 0.6089(4) 0.19875(16) 0.0565(14) Uani 1 1 d . . . C87 C 0.44638(13) 0.5282(4) 0.22111(19) 0.0692(17) Uani 1 1 d . . . C88 C 0.44026(13) 0.4455(4) 0.19979(17) 0.0578(14) Uani 1 1 d . . . C89 C 0.43111(19) 0.4714(6) 0.1640(2) 0.092(2) Uani 1 1 d . . . C90 C 0.42192(16) 0.3687(4) 0.21570(15) 0.0654(16) Uani 1 1 d . . . C91 C 0.41384(17) 0.6129(4) 0.27024(15) 0.0617(15) Uani 1 1 d . . . C92 C 0.40752(15) 0.6902(4) 0.24841(15) 0.0632(15) Uani 1 1 d . . . C93 C 0.36941(16) 0.7386(4) 0.25020(16) 0.0592(14) Uani 1 1 d . . . C94 C 0.42165(15) 0.6872(4) 0.21340(15) 0.0630(15) Uani 1 1 d . . . C95 C 0.2966(2) 0.7062(5) 0.25870(19) 0.0739(17) Uani 1 1 d . . . C96 C 0.3447(3) 0.4345(7) 0.29610(18) 0.103(3) Uani 1 1 d . . . C97 C 0.39212(15) 0.7353(3) 0.18793(17) 0.0603(15) Uani 1 1 d . . . C98 C 0.43342(14) 0.5301(4) 0.25564(17) 0.0636(16) Uani 1 1 d . . . C99 C 0.43069(19) 0.5807(6) 0.1634(2) 0.0813(19) Uani 1 1 d . . . C100 C 0.3598(2) 0.7681(4) 0.2120(2) 0.090(2) Uani 1 1 d U . . C101 C 0.25278(17) 0.5869(6) 0.2533(2) 0.085(2) Uani 1 1 d . . . C102 C 0.2783(3) 0.6328(7) 0.2723(2) 0.102(2) Uani 1 1 d . . . C103 C 0.3074(2) 0.5782(6) 0.29614(14) 0.086(2) Uani 1 1 d . . . C104 C 0.3087(3) 0.4868(6) 0.29711(15) 0.089(2) Uani 1 1 d . . . C105 C 0.2785(3) 0.4334(8) 0.2739(2) 0.111(3) Uani 1 1 d . . . C106 C 0.25279(18) 0.4730(6) 0.2544(2) 0.085(2) Uani 1 1 d . . . C107 C 0.2961(2) 0.3553(5) 0.26149(17) 0.0700(16) Uani 1 1 d . . . C108 C 0.3404(3) 0.3557(6) 0.2757(2) 0.107(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0165(4) 0.0229(4) 0.0220(4) 0.000 0.0001(3) 0.000 Mn2 0.0196(3) 0.0212(3) 0.0222(3) -0.0008(2) -0.0007(2) -0.0003(2) Mn3 0.0172(4) 0.0239(4) 0.0234(4) 0.000 -0.0004(3) 0.000 S1 0.0179(4) 0.0205(5) 0.0276(4) -0.0012(4) -0.0018(3) 0.0015(4) S2 0.0187(4) 0.0265(5) 0.0278(4) -0.0007(4) -0.0035(3) -0.0011(4) S3 0.0199(4) 0.0217(5) 0.0285(5) 0.0006(4) -0.0009(3) -0.0011(4) S4 0.0168(4) 0.0215(5) 0.0255(4) 0.0007(4) -0.0022(3) 0.0007(4) O1 0.0268(13) 0.0304(15) 0.0217(12) 0.0052(10) -0.0047(10) -0.0046(11) O2 0.0261(13) 0.0312(15) 0.0249(12) -0.0040(11) -0.0046(10) 0.0052(11) O3 0.0218(12) 0.0281(15) 0.0316(13) -0.0069(11) 0.0054(10) -0.0024(11) O4 0.0230(12) 0.0292(15) 0.0275(13) 0.0097(11) 0.0052(10) 0.0068(11) C1 0.0204(17) 0.0173(19) 0.0237(17) 0.0030(14) -0.0021(14) 0.0059(14) C2 0.0188(17) 0.0203(19) 0.0234(17) -0.0020(14) -0.0030(13) 0.0047(15) C3 0.0303(19) 0.0162(19) 0.0302(19) 0.0029(15) 0.0037(15) 0.0034(16) C4 0.035(2) 0.026(2) 0.0274(19) 0.0040(16) -0.0071(16) 0.0010(17) C5 0.035(2) 0.027(2) 0.034(2) 0.0020(17) -0.0096(16) 0.0017(18) C6 0.0221(18) 0.0195(19) 0.0273(18) 0.0034(15) -0.0043(14) 0.0038(15) C7 0.0223(17) 0.024(2) 0.0175(16) 0.0006(14) 0.0014(13) -0.0042(15) C8 0.0210(17) 0.0225(19) 0.0258(18) 0.0009(15) 0.0024(14) -0.0002(15) C9 0.0307(19) 0.026(2) 0.0238(18) 0.0023(15) -0.0041(15) -0.0048(16) C10 0.037(2) 0.030(2) 0.0255(19) -0.0005(16) -0.0020(16) -0.0060(18) C11 0.031(2) 0.020(2) 0.0277(19) -0.0026(15) -0.0009(15) -0.0026(16) C12 0.0160(17) 0.025(2) 0.0278(18) 0.0042(15) -0.0009(14) -0.0036(15) C13 0.0188(17) 0.0204(19) 0.0240(17) 0.0013(14) 0.0015(14) 0.0028(14) C14 0.0173(17) 0.023(2) 0.0302(18) 0.0003(15) -0.0007(14) 0.0005(15) C15 0.0276(19) 0.026(2) 0.0301(19) -0.0057(16) 0.0009(15) 0.0027(16) C16 0.029(2) 0.033(2) 0.0275(19) -0.0074(16) 0.0074(15) -0.0012(17) C17 0.0213(18) 0.026(2) 0.035(2) -0.0022(16) 0.0038(15) -0.0021(16) C18 0.0204(17) 0.0168(18) 0.0267(18) -0.0001(14) -0.0032(14) -0.0015(14) C19 0.0203(17) 0.0215(19) 0.0193(16) -0.0014(14) -0.0022(13) -0.0012(15) C20 0.0193(17) 0.0219(19) 0.0236(17) -0.0002(14) -0.0013(13) 0.0007(15) C21 0.0216(18) 0.027(2) 0.0260(18) -0.0015(15) 0.0006(14) 0.0018(16) C22 0.0286(19) 0.031(2) 0.0219(17) 0.0050(16) 0.0002(14) 0.0019(17) C23 0.0258(19) 0.024(2) 0.0253(18) 0.0034(15) -0.0025(14) -0.0006(16) C24 0.0227(17) 0.0204(19) 0.0235(17) -0.0020(14) -0.0004(14) 0.0000(15) C25 0.057(3) 0.037(3) 0.030(2) 0.0033(19) -0.0153(19) -0.007(2) C28 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C26 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C27 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C29 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C30 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C26' 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C27' 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C29' 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C30' 0.149(4) 0.080(3) 0.0398(16) 0.0112(19) -0.014(2) 0.002(3) C31 0.050(3) 0.043(3) 0.027(2) -0.0066(18) -0.0055(18) 0.006(2) C32 0.103(4) 0.058(4) 0.042(3) -0.002(2) -0.020(3) 0.027(3) C33 0.169(7) 0.106(6) 0.040(3) -0.031(3) -0.041(4) 0.075(5) C34 0.164(7) 0.109(6) 0.038(3) -0.032(3) -0.044(4) 0.058(5) C35 0.114(5) 0.073(4) 0.055(3) -0.033(3) -0.027(3) 0.034(4) C36 0.068(3) 0.054(3) 0.035(2) -0.014(2) -0.011(2) 0.012(3) C37 0.046(3) 0.048(3) 0.056(3) -0.026(2) 0.023(2) -0.016(2) C38 0.082(4) 0.070(4) 0.038(2) -0.018(2) 0.017(2) -0.019(3) C39 0.102(4) 0.104(4) 0.075(3) -0.030(3) 0.020(3) -0.018(3) C40 0.120(4) 0.138(5) 0.110(4) -0.051(4) 0.036(4) -0.022(4) C41 0.075(3) 0.145(5) 0.127(4) -0.049(4) 0.033(3) -0.019(3) C42 0.069(3) 0.101(4) 0.092(3) -0.051(3) 0.028(3) -0.016(3) C43 0.029(2) 0.037(2) 0.033(2) 0.0110(18) 0.0076(16) 0.0068(18) C44 0.031(2) 0.052(3) 0.052(3) 0.027(2) 0.0071(19) 0.005(2) C45 0.035(3) 0.099(5) 0.097(4) 0.051(4) 0.018(3) 0.010(3) C46 0.046(3) 0.131(6) 0.096(4) 0.078(4) 0.036(3) 0.024(3) C47 0.063(3) 0.132(6) 0.050(3) 0.050(3) 0.023(3) 0.029(4) C48 0.040(2) 0.080(4) 0.040(2) 0.023(2) 0.007(2) 0.007(2) C49 0.149(7) 0.109(6) 0.038(3) -0.039(4) 0.003(4) 0.010(6) C50 0.096(5) 0.115(6) 0.044(3) -0.020(4) 0.023(3) 0.027(5) C51 0.129(7) 0.100(6) 0.041(3) 0.009(4) 0.039(4) -0.021(6) C52 0.137(7) 0.144(8) 0.048(4) 0.053(5) 0.020(4) 0.033(7) C53 0.074(4) 0.119(6) 0.040(3) 0.037(4) -0.026(3) -0.028(4) C54 0.081(4) 0.110(6) 0.039(3) -0.037(3) -0.026(3) 0.028(4) C55 0.069(4) 0.070(4) 0.070(4) -0.004(3) -0.049(3) -0.018(3) C56 0.056(3) 0.068(4) 0.079(4) -0.018(3) -0.018(3) -0.027(3) C57 0.070(4) 0.045(3) 0.081(4) -0.032(3) 0.007(3) -0.021(3) C58 0.161(8) 0.076(5) 0.072(4) -0.052(4) 0.002(5) 0.002(5) C59 0.040(3) 0.081(5) 0.080(4) 0.003(4) -0.029(3) 0.004(3) C60 0.022(2) 0.091(5) 0.104(5) -0.011(4) -0.016(3) 0.001(3) C61 0.016(2) 0.074(4) 0.085(4) 0.009(3) 0.002(2) -0.020(2) C62 0.048(3) 0.073(4) 0.078(4) -0.013(3) 0.008(3) -0.048(3) C63 0.046(3) 0.038(3) 0.092(4) 0.011(3) 0.013(3) -0.022(2) C64 0.083(5) 0.023(3) 0.158(7) 0.001(3) -0.021(5) -0.015(3) C65 0.107(6) 0.019(3) 0.147(7) 0.003(3) -0.012(5) 0.007(3) C66 0.058(3) 0.018(3) 0.140(6) -0.006(3) 0.035(4) 0.011(2) C67 0.064(4) 0.063(4) 0.081(4) -0.039(4) 0.005(3) 0.021(3) C68 0.096(6) 0.092(6) 0.109(6) -0.032(5) 0.064(5) 0.027(5) C69 0.114(7) 0.093(6) 0.101(6) 0.020(5) 0.060(5) -0.037(6) C70 0.079(4) 0.056(4) 0.063(4) 0.024(3) 0.011(3) -0.018(3) C71 0.162(8) 0.076(5) 0.066(4) 0.054(4) 0.003(5) -0.004(5) C72 0.062(4) 0.052(4) 0.089(4) 0.045(3) 0.000(3) 0.015(3) C73 0.072(4) 0.088(5) 0.108(5) 0.028(4) -0.027(4) 0.037(4) C74 0.092(5) 0.070(5) 0.089(4) 0.010(4) -0.068(4) 0.023(4) C75 0.103(5) 0.030(3) 0.161(6) 0.018(4) -0.013(5) 0.019(3) C76 0.062(4) 0.032(3) 0.118(5) 0.003(3) 0.033(4) 0.026(3) C77 0.056(3) 0.084(4) 0.100(4) 0.027(4) 0.010(3) 0.054(3) C78 0.024(2) 0.077(4) 0.086(4) 0.003(3) 0.009(2) 0.022(3) C79 0.061(4) 0.043(3) 0.093(4) 0.038(3) -0.006(3) 0.002(3) C80 0.080(4) 0.067(4) 0.117(5) 0.023(4) -0.041(4) 0.040(4) C81 0.074(4) 0.049(4) 0.092(4) 0.003(3) -0.056(4) 0.016(3) C82 0.080(4) 0.103(5) 0.038(3) 0.029(3) -0.029(3) -0.025(4) C83 0.084(4) 0.095(5) 0.049(3) -0.038(3) -0.035(3) 0.037(4) C84 0.136(7) 0.095(6) 0.040(3) -0.035(3) 0.005(4) 0.005(5) C85 0.137(7) 0.076(5) 0.080(5) -0.058(4) -0.005(5) 0.012(5) C86 0.021(2) 0.050(3) 0.098(4) 0.001(3) 0.016(2) -0.011(2) C87 0.017(2) 0.079(5) 0.111(5) 0.001(4) -0.009(3) 0.001(3) C88 0.026(2) 0.053(4) 0.095(4) -0.005(3) 0.007(3) 0.021(2) C89 0.051(4) 0.119(7) 0.106(6) -0.040(5) 0.044(4) -0.009(4) C90 0.060(3) 0.065(4) 0.071(4) 0.011(3) 0.006(3) 0.044(3) C91 0.066(3) 0.048(3) 0.071(3) -0.008(3) -0.044(3) -0.011(3) C92 0.053(3) 0.050(3) 0.086(4) -0.023(3) -0.015(3) -0.019(3) C93 0.059(3) 0.036(3) 0.083(4) -0.026(3) 0.007(3) -0.010(3) C94 0.047(3) 0.059(4) 0.083(4) -0.014(3) 0.010(3) -0.042(3) C95 0.076(4) 0.056(4) 0.089(5) -0.032(4) 0.009(4) 0.030(3) C96 0.133(7) 0.125(7) 0.052(4) 0.047(4) 0.005(4) 0.019(6) C97 0.058(3) 0.020(2) 0.103(4) 0.011(3) 0.029(3) -0.010(2) C98 0.030(2) 0.064(4) 0.097(4) 0.010(3) -0.031(3) -0.002(3) C99 0.059(4) 0.094(6) 0.092(5) 0.008(4) 0.040(4) -0.013(4) C100 0.091(4) 0.018(3) 0.160(6) -0.001(3) 0.003(4) -0.006(3) C101 0.042(3) 0.110(6) 0.103(5) -0.032(5) 0.040(3) -0.001(4) C102 0.097(6) 0.107(7) 0.104(6) -0.037(5) 0.052(5) 0.033(5) C103 0.114(6) 0.111(6) 0.035(3) -0.005(4) 0.028(3) 0.034(5) C104 0.125(7) 0.102(6) 0.041(3) 0.014(4) 0.022(4) -0.030(5) C105 0.090(6) 0.162(9) 0.082(5) 0.034(6) 0.047(5) -0.037(6) C106 0.039(3) 0.126(7) 0.089(5) 0.011(5) 0.025(3) -0.016(4) C107 0.080(4) 0.062(4) 0.068(4) 0.024(3) 0.011(3) -0.023(3) C108 0.183(10) 0.070(5) 0.068(4) 0.040(4) -0.014(5) -0.018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.112(2) . ? Mn1 O1 2.113(2) 2 ? Mn1 O4 2.161(2) . ? Mn1 O4 2.161(2) 2 ? Mn1 S1 2.7348(9) 2 ? Mn1 S1 2.7349(9) . ? Mn2 O1 2.116(2) . ? Mn2 O3 2.120(2) 2 ? Mn2 O4 2.160(2) 2 ? Mn2 O2 2.160(2) . ? Mn2 S2 2.6671(10) . ? Mn2 S4 2.6777(10) 2 ? Mn3 O3 2.123(2) 2 ? Mn3 O3 2.123(2) . ? Mn3 O2 2.159(2) 2 ? Mn3 O2 2.159(2) . ? Mn3 S3 2.7436(10) 2 ? Mn3 S3 2.7436(10) . ? S1 C24 1.786(3) . ? S1 C2 1.795(3) . ? S2 C8 1.784(4) . ? S2 C6 1.787(4) . ? S3 C12 1.786(3) . ? S3 C14 1.788(3) . ? S4 C18 1.790(3) . ? S4 C20 1.794(3) . ? S4 Mn2 2.6776(10) 2 ? O1 C1 1.316(4) . ? O2 C7 1.309(4) . ? O3 C13 1.306(4) . ? O3 Mn2 2.120(2) 2 ? O4 C19 1.306(4) . ? O4 Mn2 2.160(2) 2 ? C1 C6 1.400(4) . ? C1 C2 1.403(5) . ? C2 C3 1.382(5) . ? C3 C4 1.392(5) . ? C3 H3A 0.9500 . ? C4 C5 1.394(5) . ? C4 C25 1.486(5) . ? C5 C6 1.396(5) . ? C5 H5A 0.9500 . ? C7 C8 1.411(4) . ? C7 C12 1.423(5) . ? C8 C9 1.385(5) . ? C9 C10 1.394(5) . ? C9 H9A 0.9500 . ? C10 C11 1.397(5) . ? C10 C31 1.489(5) . ? C11 C12 1.387(5) . ? C11 H11A 0.9500 . ? C13 C18 1.399(5) . ? C13 C14 1.416(5) . ? C14 C15 1.383(5) . ? C15 C16 1.405(5) . ? C15 H15A 0.9500 . ? C16 C17 1.390(5) . ? C16 C37 1.489(5) . ? C17 C18 1.383(5) . ? C17 H17A 0.9500 . ? C19 C20 1.408(4) . ? C19 C24 1.426(5) . ? C20 C21 1.395(4) . ? C21 C22 1.391(5) . ? C21 H21A 0.9500 . ? C22 C23 1.402(5) . ? C22 C43 1.475(5) . ? C23 C24 1.383(5) . ? C23 H23A 0.9500 . ? C25 C26' 1.312(16) . ? C25 C30 1.312(14) . ? C25 C26 1.377(14) . ? C25 C30' 1.477(15) . ? C28 C27' 1.199(15) . ? C28 C29 1.306(14) . ? C28 C27 1.409(15) . ? C28 C29' 1.419(16) . ? C28 H28A 0.9500 . ? C26 C27 1.478(14) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C29 C30 1.373(13) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C26' C27' 1.399(16) . ? C26' H26B 0.9500 . ? C27' H27B 0.9500 . ? C29' C30' 1.420(15) . ? C29' H29B 0.9500 . ? C30' H30B 0.9500 . ? C31 C36 1.391(6) . ? C31 C32 1.395(6) . ? C32 C33 1.388(7) . ? C32 H32A 0.9500 . ? C33 C34 1.389(9) . ? C33 H33A 0.9500 . ? C34 C35 1.346(8) . ? C34 H34A 0.9500 . ? C35 C36 1.384(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.367(6) . ? C37 C42 1.402(7) . ? C38 C39 1.380(7) . ? C38 H38A 0.9500 . ? C39 C40 1.368(9) . ? C39 H39A 0.9500 . ? C40 C41 1.383(10) . ? C40 H40A 0.9500 . ? C41 C42 1.406(8) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C48 1.384(5) . ? C43 C44 1.387(5) . ? C44 C45 1.392(6) . ? C44 H44A 0.9500 . ? C45 C46 1.389(7) . ? C45 H45A 0.9500 . ? C46 C47 1.391(8) . ? C46 H46A 0.9500 . ? C47 C48 1.383(6) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C58 1.392(10) . ? C49 C54 1.435(9) . ? C49 C50 1.495(11) . ? C50 C51 1.291(10) . ? C50 C68 1.544(11) . ? C51 C52 1.399(10) . ? C51 C69 1.558(11) . ? C52 C71 1.375(10) . ? C52 C53 1.418(10) . ? C53 C54 1.448(9) . ? C53 C74 1.486(9) . ? C54 C55 1.437(9) . ? C55 C56 1.410(8) . ? C55 C59 1.476(8) . ? C56 C62 1.373(7) . ? C56 C57 1.468(8) . ? C57 C58 1.333(9) . ? C57 C64 1.502(9) . ? C58 C67 1.535(10) . ? C59 C60 1.357(8) . ? C59 C74 1.493(9) . ? C60 C78 1.450(8) . ? C60 C61 1.457(8) . ? C61 C106 1.421(9) . ? C61 C62 1.423(8) . ? C62 C63 1.487(8) . ? C63 C107 1.316(8) . ? C63 C64 1.499(8) . ? C64 C65 1.278(8) . ? C65 C66 1.452(8) . ? C65 C79 1.470(9) . ? C66 C67 1.385(8) . ? C66 C90 1.481(8) . ? C67 C68 1.357(9) . ? C68 C89 1.255(10) . ? C69 C99 1.243(10) . ? C69 C70 1.331(10) . ? C70 C97 1.329(8) . ? C70 C71 1.560(10) . ? C71 C72 1.338(9) . ? C72 C73 1.479(9) . ? C72 C75 1.494(10) . ? C73 C74 1.365(9) . ? C73 C77 1.403(9) . ? C75 C100 1.260(9) . ? C75 C76 1.458(9) . ? C76 C95 1.336(8) . ? C76 C77 1.520(9) . ? C77 C78 1.407(8) . ? C78 C101 1.422(9) . ? C79 C108 1.348(10) . ? C79 C80 1.503(8) . ? C80 C81 1.362(8) . ? C80 C90 1.385(8) . ? C81 C98 1.470(8) . ? C81 C82 1.515(9) . ? C82 C96 1.373(10) . ? C82 C83 1.467(9) . ? C83 C84 1.374(9) . ? C83 C91 1.470(8) . ? C84 C85 1.367(10) . ? C84 C103 1.502(10) . ? C85 C93 1.331(9) . ? C85 C95 1.579(9) . ? C86 C94 1.407(7) . ? C86 C99 1.415(9) . ? C86 C87 1.444(8) . ? C87 C98 1.359(8) . ? C87 C88 1.446(8) . ? C88 C90 1.400(8) . ? C88 C89 1.414(9) . ? C89 C99 1.576(10) . ? C91 C92 1.395(7) . ? C91 C98 1.468(8) . ? C92 C94 1.389(7) . ? C92 C93 1.456(7) . ? C93 C100 1.515(9) . ? C94 C97 1.532(8) . ? C95 C102 1.324(10) . ? C96 C108 1.374(11) . ? C96 C104 1.422(11) . ? C97 C100 1.486(8) . ? C101 C102 1.289(9) . ? C101 C106 1.644(10) . ? C102 C103 1.532(10) . ? C103 C104 1.320(10) . ? C104 C105 1.534(11) . ? C105 C106 1.261(10) . ? C105 C107 1.354(10) . ? C107 C108 1.570(10) . ? 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 O1 142.09(14) . 2 ? O1 Mn1 O4 90.59(9) . . ? O1 Mn1 O4 71.69(8) 2 . ? O1 Mn1 O4 71.70(8) . 2 ? O1 Mn1 O4 90.59(9) 2 2 ? O4 Mn1 O4 124.23(13) . 2 ? O1 Mn1 S1 128.12(7) . 2 ? O1 Mn1 S1 74.90(6) 2 2 ? O4 Mn1 S1 141.25(6) . 2 ? O4 Mn1 S1 74.58(6) 2 2 ? O1 Mn1 S1 74.90(6) . . ? O1 Mn1 S1 128.12(7) 2 . ? O4 Mn1 S1 74.58(6) . . ? O4 Mn1 S1 141.25(6) 2 . ? S1 Mn1 S1 113.34(4) 2 . ? O1 Mn2 O3 143.47(9) . 2 ? O1 Mn2 O4 71.64(9) . 2 ? O3 Mn2 O4 91.67(10) 2 2 ? O1 Mn2 O2 91.20(10) . . ? O3 Mn2 O2 71.69(9) 2 . ? O4 Mn2 O2 124.99(9) 2 . ? O1 Mn2 S2 77.00(6) . . ? O3 Mn2 S2 126.73(7) 2 . ? O4 Mn2 S2 141.49(7) 2 . ? O2 Mn2 S2 76.64(6) . . ? O1 Mn2 S4 127.09(7) . 2 ? O3 Mn2 S4 76.91(6) 2 2 ? O4 Mn2 S4 76.67(6) 2 2 ? O2 Mn2 S4 141.61(7) . 2 ? S2 Mn2 S4 106.55(3) . 2 ? O3 Mn3 O3 143.13(14) 2 . ? O3 Mn3 O2 91.10(9) 2 2 ? O3 Mn3 O2 71.65(9) . 2 ? O3 Mn3 O2 71.65(9) 2 . ? O3 Mn3 O2 91.10(9) . . ? O2 Mn3 O2 124.28(14) 2 . ? O3 Mn3 S3 74.52(7) 2 2 ? O3 Mn3 S3 127.74(7) . 2 ? O2 Mn3 S3 74.44(6) 2 2 ? O2 Mn3 S3 141.11(7) . 2 ? O3 Mn3 S3 127.74(7) 2 . ? O3 Mn3 S3 74.52(7) . . ? O2 Mn3 S3 141.12(7) 2 . ? O2 Mn3 S3 74.44(6) . . ? S3 Mn3 S3 113.83(5) 2 . ? C24 S1 C2 101.44(15) . . ? C24 S1 Mn1 95.54(11) . . ? C2 S1 Mn1 95.42(11) . . ? C8 S2 C6 100.60(16) . . ? C8 S2 Mn2 95.49(11) . . ? C6 S2 Mn2 95.14(11) . . ? C12 S3 C14 102.10(16) . . ? C12 S3 Mn3 95.31(12) . . ? C14 S3 Mn3 95.32(11) . . ? C18 S4 C20 100.55(15) . . ? C18 S4 Mn2 95.00(11) . 2 ? C20 S4 Mn2 95.06(11) . 2 ? C1 O1 Mn1 129.0(2) . . ? C1 O1 Mn2 125.8(2) . . ? Mn1 O1 Mn2 103.68(9) . . ? C7 O2 Mn3 126.0(2) . . ? C7 O2 Mn2 123.5(2) . . ? Mn3 O2 Mn2 100.63(9) . . ? C13 O3 Mn2 125.1(2) . 2 ? C13 O3 Mn3 129.6(2) . . ? Mn2 O3 Mn3 103.11(10) 2 . ? C19 O4 Mn2 123.4(2) . 2 ? C19 O4 Mn1 125.8(2) . . ? Mn2 O4 Mn1 100.62(9) 2 . ? O1 C1 C6 121.6(3) . . ? O1 C1 C2 121.4(3) . . ? C6 C1 C2 117.0(3) . . ? C3 C2 C1 121.8(3) . . ? C3 C2 S1 119.2(3) . . ? C1 C2 S1 118.9(2) . . ? C2 C3 C4 120.8(3) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C3 C4 C5 118.3(3) . . ? C3 C4 C25 121.0(3) . . ? C5 C4 C25 120.7(3) . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 121.2(3) . . ? C5 C6 S2 119.1(3) . . ? C1 C6 S2 119.7(2) . . ? O2 C7 C8 122.7(3) . . ? O2 C7 C12 121.4(3) . . ? C8 C7 C12 115.8(3) . . ? C9 C8 C7 121.9(3) . . ? C9 C8 S2 119.2(3) . . ? C7 C8 S2 119.0(3) . . ? C8 C9 C10 121.4(3) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C9 C10 C11 118.0(3) . . ? C9 C10 C31 121.3(3) . . ? C11 C10 C31 120.7(4) . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C7 121.7(3) . . ? C11 C12 S3 119.4(3) . . ? C7 C12 S3 118.8(2) . . ? O3 C13 C18 122.8(3) . . ? O3 C13 C14 120.5(3) . . ? C18 C13 C14 116.6(3) . . ? C15 C14 C13 121.5(3) . . ? C15 C14 S3 119.1(3) . . ? C13 C14 S3 119.4(2) . . ? C14 C15 C16 120.8(3) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C17 C16 C15 117.9(3) . . ? C17 C16 C37 121.6(3) . . ? C15 C16 C37 120.4(3) . . ? C18 C17 C16 121.2(3) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C13 121.9(3) . . ? C17 C18 S4 119.1(3) . . ? C13 C18 S4 119.0(3) . . ? O4 C19 C20 123.2(3) . . ? O4 C19 C24 121.3(3) . . ? C20 C19 C24 115.5(3) . . ? C21 C20 C19 122.3(3) . . ? C21 C20 S4 118.9(2) . . ? C19 C20 S4 118.9(2) . . ? C22 C21 C20 121.0(3) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C21 C22 C23 117.9(3) . . ? C21 C22 C43 120.8(3) . . ? C23 C22 C43 121.3(3) . . ? C24 C23 C22 121.3(3) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? C23 C24 C19 121.9(3) . . ? C23 C24 S1 119.3(3) . . ? C19 C24 S1 118.7(2) . . ? C26' C25 C30 96.5(9) . . ? C26' C25 C26 42.2(7) . . ? C30 C25 C26 120.9(8) . . ? C26' C25 C30' 113.9(8) . . ? C30 C25 C30' 41.5(7) . . ? C26 C25 C30' 107.9(8) . . ? C26' C25 C4 126.6(7) . . ? C30 C25 C4 121.3(6) . . ? C26 C25 C4 117.8(6) . . ? C30' C25 C4 119.5(6) . . ? C27' C28 C29 100.9(10) . . ? C27' C28 C27 41.5(8) . . ? C29 C28 C27 119.3(8) . . ? C27' C28 C29' 124.6(10) . . ? C29 C28 C29' 41.9(7) . . ? C27 C28 C29' 111.8(9) . . ? C27' C28 H28A 123.7 . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C29' C28 H28A 111.7 . . ? C25 C26 C27 115.4(12) . . ? C25 C26 H26A 122.3 . . ? C27 C26 H26A 122.3 . . ? C28 C27 C26 119.4(12) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C28 C29 C30 120.5(13) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C25 C30 C29 123.6(13) . . ? C25 C30 H30A 118.2 . . ? C29 C30 H30A 118.2 . . ? C25 C26' C27' 123.4(14) . . ? C25 C26' H26B 118.3 . . ? C27' C26' H26B 118.3 . . ? C28 C27' C26' 122.2(14) . . ? C28 C27' H27B 118.9 . . ? C26' C27' H27B 118.9 . . ? C28 C29' C30' 113.6(12) . . ? C28 C29' H29B 123.2 . . ? C30' C29' H29B 123.2 . . ? C29' C30' C25 121.8(13) . . ? C29' C30' H30B 119.1 . . ? C25 C30' H30B 119.1 . . ? C36 C31 C32 117.3(4) . . ? C36 C31 C10 121.2(4) . . ? C32 C31 C10 121.5(4) . . ? C33 C32 C31 121.9(5) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 118.4(5) . . ? C32 C33 H33A 120.8 . . ? C34 C33 H33A 120.8 . . ? C35 C34 C33 120.8(5) . . ? C35 C34 H34A 119.6 . . ? C33 C34 H34A 119.6 . . ? C34 C35 C36 120.8(6) . . ? C34 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C35 C36 C31 120.7(5) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? C38 C37 C42 117.9(4) . . ? C38 C37 C16 123.0(4) . . ? C42 C37 C16 119.1(4) . . ? C37 C38 C39 123.4(6) . . ? C37 C38 H38A 118.3 . . ? C39 C38 H38A 118.3 . . ? C40 C39 C38 118.1(6) . . ? C40 C39 H39A 120.9 . . ? C38 C39 H39A 120.9 . . ? C39 C40 C41 121.4(7) . . ? C39 C40 H40A 119.3 . . ? C41 C40 H40A 119.3 . . ? C40 C41 C42 119.2(7) . . ? C40 C41 H41A 120.4 . . ? C42 C41 H41A 120.4 . . ? C37 C42 C41 119.9(6) . . ? C37 C42 H42A 120.1 . . ? C41 C42 H42A 120.1 . . ? C48 C43 C44 118.2(4) . . ? C48 C43 C22 120.4(3) . . ? C44 C43 C22 121.5(3) . . ? C43 C44 C45 121.8(4) . . ? C43 C44 H44A 119.1 . . ? C45 C44 H44A 119.1 . . ? C46 C45 C44 119.1(5) . . ? C46 C45 H45A 120.5 . . ? C44 C45 H45A 120.5 . . ? C45 C46 C47 119.7(4) . . ? C45 C46 H46A 120.2 . . ? C47 C46 H46A 120.2 . . ? C48 C47 C46 120.1(5) . . ? C48 C47 H47A 119.9 . . ? C46 C47 H47A 119.9 . . ? C47 C48 C43 121.1(4) . . ? C47 C48 H48A 119.4 . . ? C43 C48 H48A 119.4 . . ? C58 C49 C54 118.3(8) . . ? C58 C49 C50 112.3(8) . . ? C54 C49 C50 116.9(8) . . ? C51 C50 C49 121.0(7) . . ? C51 C50 C68 122.5(8) . . ? C49 C50 C68 103.8(7) . . ? C50 C51 C52 124.5(8) . . ? C50 C51 C69 117.2(8) . . ? C52 C51 C69 106.2(8) . . ? C71 C52 C51 112.9(9) . . ? C71 C52 C53 118.0(8) . . ? C51 C52 C53 118.3(9) . . ? C52 C53 C54 120.4(7) . . ? C52 C53 C74 118.8(7) . . ? C54 C53 C74 108.4(5) . . ? C49 C54 C55 120.1(7) . . ? C49 C54 C53 118.8(7) . . ? C55 C54 C53 108.7(5) . . ? C56 C55 C54 119.4(6) . . ? C56 C55 C59 118.5(6) . . ? C54 C55 C59 109.5(5) . . ? C62 C56 C55 121.1(6) . . ? C62 C56 C57 109.3(5) . . ? C55 C56 C57 118.2(6) . . ? C58 C57 C56 120.6(7) . . ? C58 C57 C64 120.4(6) . . ? C56 C57 C64 106.8(5) . . ? C57 C58 C49 123.4(8) . . ? C57 C58 C67 120.8(7) . . ? C49 C58 C67 104.3(8) . . ? C60 C59 C55 120.6(6) . . ? C60 C59 C74 120.2(6) . . ? C55 C59 C74 106.4(6) . . ? C59 C60 C78 119.1(6) . . ? C59 C60 C61 119.7(6) . . ? C78 C60 C61 110.3(6) . . ? C106 C61 C62 118.1(6) . . ? C106 C61 C60 109.8(6) . . ? C62 C61 C60 119.2(5) . . ? C56 C62 C61 120.9(6) . . ? C56 C62 C63 112.1(5) . . ? C61 C62 C63 115.0(5) . . ? C107 C63 C62 118.2(6) . . ? C107 C63 C64 124.6(6) . . ? C62 C63 C64 104.5(5) . . ? C65 C64 C63 120.3(7) . . ? C65 C64 C57 120.5(7) . . ? C63 C64 C57 107.3(5) . . ? C64 C65 C66 120.4(7) . . ? C64 C65 C79 118.6(7) . . ? C66 C65 C79 109.0(6) . . ? C67 C66 C65 124.3(6) . . ? C67 C66 C90 116.2(5) . . ? C65 C66 C90 107.5(6) . . ? C68 C67 C66 122.5(7) . . ? C68 C67 C58 112.2(7) . . ? C66 C67 C58 113.6(6) . . ? C89 C68 C67 123.3(9) . . ? C89 C68 C50 118.5(8) . . ? C67 C68 C50 107.4(8) . . ? C99 C69 C70 122.0(9) . . ? C99 C69 C51 121.2(8) . . ? C70 C69 C51 106.1(8) . . ? C97 C70 C69 124.2(7) . . ? C97 C70 C71 112.7(6) . . ? C69 C70 C71 110.6(7) . . ? C72 C71 C52 125.4(8) . . ? C72 C71 C70 118.8(7) . . ? C52 C71 C70 104.2(8) . . ? C71 C72 C73 118.9(7) . . ? C71 C72 C75 123.1(6) . . ? C73 C72 C75 105.5(6) . . ? C74 C73 C77 119.1(7) . . ? C74 C73 C72 118.6(7) . . ? C77 C73 C72 110.2(7) . . ? C73 C74 C53 120.2(7) . . ? C73 C74 C59 120.1(7) . . ? C53 C74 C59 106.9(6) . . ? C100 C75 C76 120.0(8) . . ? C100 C75 C72 118.7(8) . . ? C76 C75 C72 109.8(6) . . ? C95 C76 C75 126.5(7) . . ? C95 C76 C77 115.4(6) . . ? C75 C76 C77 105.2(6) . . ? C73 C77 C78 122.2(7) . . ? C73 C77 C76 109.3(6) . . ? C78 C77 C76 117.1(5) . . ? C77 C78 C101 118.0(6) . . ? C77 C78 C60 119.2(6) . . ? C101 C78 C60 109.6(6) . . ? C108 C79 C65 124.4(6) . . ? C108 C79 C80 118.9(7) . . ? C65 C79 C80 104.6(6) . . ? C81 C80 C90 120.4(7) . . ? C81 C80 C79 118.2(7) . . ? C90 C80 C79 110.6(6) . . ? C80 C81 C98 119.5(7) . . ? C80 C81 C82 119.3(6) . . ? C98 C81 C82 108.1(5) . . ? C96 C82 C83 121.5(7) . . ? C96 C82 C81 119.6(7) . . ? C83 C82 C81 106.7(5) . . ? C84 C83 C82 119.4(7) . . ? C84 C83 C91 120.6(7) . . ? C82 C83 C91 108.5(5) . . ? C85 C84 C83 119.4(8) . . ? C85 C84 C103 111.1(7) . . ? C83 C84 C103 117.8(7) . . ? C93 C85 C84 123.7(8) . . ? C93 C85 C95 118.4(7) . . ? C84 C85 C95 105.8(8) . . ? C94 C86 C99 119.2(6) . . ? C94 C86 C87 118.9(5) . . ? C99 C86 C87 109.5(6) . . ? C98 C87 C86 119.1(6) . . ? C98 C87 C88 119.4(6) . . ? C86 C87 C88 109.3(6) . . ? C90 C88 C89 120.9(6) . . ? C90 C88 C87 118.8(6) . . ? C89 C88 C87 109.1(6) . . ? C68 C89 C88 120.5(8) . . ? C68 C89 C99 120.5(8) . . ? C88 C89 C99 106.3(6) . . ? C80 C90 C88 121.6(6) . . ? C80 C90 C66 108.2(6) . . ? C88 C90 C66 116.6(5) . . ? C92 C91 C98 120.1(5) . . ? C92 C91 C83 117.5(5) . . ? C98 C91 C83 109.1(5) . . ? C94 C92 C91 118.0(5) . . ? C94 C92 C93 111.1(5) . . ? C91 C92 C93 119.1(5) . . ? C85 C93 C92 119.7(6) . . ? C85 C93 C100 121.9(6) . . ? C92 C93 C100 105.9(5) . . ? C92 C94 C86 123.0(6) . . ? C92 C94 C97 110.2(5) . . ? C86 C94 C97 114.5(5) . . ? C102 C95 C76 126.1(7) . . ? C102 C95 C85 109.4(7) . . ? C76 C95 C85 113.3(7) . . ? C82 C96 C108 119.4(9) . . ? C82 C96 C104 117.6(9) . . ? C108 C96 C104 111.5(9) . . ? C70 C97 C100 126.7(6) . . ? C70 C97 C94 117.0(5) . . ? C100 C97 C94 103.9(5) . . ? C87 C98 C91 120.8(5) . . ? C87 C98 C81 120.2(6) . . ? C91 C98 C81 107.5(5) . . ? C69 C99 C86 123.0(8) . . ? C69 C99 C89 120.0(8) . . ? C86 C99 C89 105.8(6) . . ? C75 C100 C97 119.8(8) . . ? C75 C100 C93 119.7(7) . . ? C97 C100 C93 109.0(6) . . ? C102 C101 C78 122.8(8) . . ? C102 C101 C106 120.0(7) . . ? C78 C101 C106 105.4(6) . . ? C101 C102 C95 120.6(8) . . ? C101 C102 C103 118.1(8) . . ? C95 C102 C103 109.8(8) . . ? C104 C103 C84 119.7(7) . . ? C104 C103 C102 123.3(8) . . ? C84 C103 C102 104.0(7) . . ? C103 C104 C96 123.9(8) . . ? C103 C104 C105 117.7(8) . . ? C96 C104 C105 105.9(8) . . ? C106 C105 C107 118.5(9) . . ? C106 C105 C104 122.9(10) . . ? C107 C105 C104 108.8(8) . . ? C105 C106 C61 124.5(8) . . ? C105 C106 C101 117.8(8) . . ? C61 C106 C101 104.9(6) . . ? C63 C107 C105 125.5(7) . . ? C63 C107 C108 115.2(7) . . ? C105 C107 C108 107.1(7) . . ? C79 C108 C96 124.5(9) . . ? C79 C108 C107 116.8(7) . . ? C96 C108 C107 106.6(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.235 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.157 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.006 -0.035 0.000 3069 1462 ' ' 2 -0.045 0.053 0.500 3069 1468 ' ' 3 0.158 0.028 0.291 23 1 ' ' 4 0.158 0.972 0.791 23 1 ' ' 5 0.341 0.528 0.209 23 1 ' ' 6 0.341 0.472 0.709 23 1 ' ' 7 0.658 0.528 0.291 23 1 ' ' 8 0.658 0.472 0.791 23 1 ' ' 9 0.841 0.028 0.209 23 1 ' ' 10 0.841 0.972 0.709 23 1 ' ' _platon_squeeze_details ; ; ###END