# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Srinivasan Natarajan' _publ_contact_author_email snatarajan@sscu.iisc.ernet.in _publ_author_name S.Natarajan ######END####### data_Compound(2) _database_code_depnum_ccdc_archive 'CCDC 834723' #TrackingRef '- all compounds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Manganese Sulfonyldibenzoate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H52 K2 Mn5 O38 S6' _chemical_formula_weight 2214.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7407(3) _cell_length_b 12.7787(3) _cell_length_c 15.9960(4) _cell_angle_alpha 86.701(2) _cell_angle_beta 72.142(2) _cell_angle_gamma 60.438(3) _cell_volume 2142.27(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1115 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 0.909 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47793 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8409 _reflns_number_gt 6828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0419P)^2^+0.6508P] 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 8409 _refine_ls_number_parameters 610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.5000 0.0000 0.02062(12) Uani 1 2 d S . . Mn2 Mn -0.14550(3) 0.75564(3) 0.29065(2) 0.01992(9) Uani 1 1 d . . . Mn3 Mn -0.04292(3) 0.73886(3) 0.08735(2) 0.01993(9) Uani 1 1 d . . . K1 K -0.92634(6) 0.62388(6) 0.41794(4) 0.04052(16) Uani 1 1 d . . . S1 S 0.22053(6) 0.79725(6) -0.47701(4) 0.02871(15) Uani 1 1 d . . . S2 S -0.61947(5) 0.49817(5) 0.19097(4) 0.02204(13) Uani 1 1 d . . . S3 S 0.42604(6) 0.98036(5) 0.20096(5) 0.02914(15) Uani 1 1 d . . . O1 O 0.04336(17) 0.60527(16) -0.09109(11) 0.0338(4) Uani 1 1 d . . . O2 O -0.16861(14) 0.66168(14) 0.08744(11) 0.0237(4) Uani 1 1 d . . . O3 O 0.07789(15) 1.54119(14) 0.09370(11) 0.0249(4) Uani 1 1 d . . . O4 O 0.80924(16) 0.72578(16) -0.57942(11) 0.0314(4) Uani 1 1 d . . . O5 O -0.26596(19) -0.06313(16) 0.28080(15) 0.0448(5) Uani 1 1 d . . . O6 O -0.24323(16) 0.70077(16) 0.23418(12) 0.0328(4) Uani 1 1 d . . . O7 O -0.00611(16) 0.79846(16) 0.29791(12) 0.0327(4) Uani 1 1 d . . . O8 O 0.01420(16) 1.57446(15) 0.24065(12) 0.0321(4) Uani 1 1 d . . . O9 O -0.20241(18) -0.09446(17) 0.13390(15) 0.0462(5) Uani 1 1 d . . . O10 O 0.0273(2) 0.77069(19) -0.03957(12) 0.0490(6) Uani 1 1 d . . . O11 O 0.05386(18) 0.77825(17) 0.15101(13) 0.0391(5) Uani 1 1 d . . . O12 O 0.8329(2) 0.5670(2) -0.50712(16) 0.0589(6) Uani 1 1 d . . . O13 O 0.14689(17) 0.92344(18) -0.48512(12) 0.0423(5) Uani 1 1 d . . . O14 O 0.22468(18) 0.70986(19) -0.53295(12) 0.0406(5) Uani 1 1 d . . . O15 O -0.65228(17) 0.51572(16) 0.11107(12) 0.0330(4) Uani 1 1 d . . . O16 O -0.71910(15) 0.54796(15) 0.27493(12) 0.0318(4) Uani 1 1 d . . . O17 O 0.44961(19) 0.97227(17) 0.28384(14) 0.0431(5) Uani 1 1 d . . . O18 O 0.53029(16) 0.92663(16) 0.12034(14) 0.0433(5) Uani 1 1 d . . . O19 O -1.1128(3) 0.8402(2) 0.52361(17) 0.0765(8) Uani 1 1 d . . . C1 C 0.0518(2) 0.6989(2) -0.10164(16) 0.0274(6) Uani 1 1 d . . . C2 C 0.0936(2) 0.7252(2) -0.19469(16) 0.0267(5) Uani 1 1 d . . . C3 C 0.1052(3) 0.8276(2) -0.21212(17) 0.0351(6) Uani 1 1 d . . . H3 H 0.0877 0.8804 -0.1656 0.042 Uiso 1 1 calc R . . C4 C 0.1427(3) 0.8511(2) -0.29820(17) 0.0340(6) Uani 1 1 d . . . H4 H 0.1504 0.9195 -0.3103 0.041 Uiso 1 1 calc R . . C5 C 0.1685(2) 0.7712(2) -0.36614(15) 0.0256(5) Uani 1 1 d . . . C6 C 0.1566(3) 0.6698(3) -0.34999(17) 0.0342(6) Uani 1 1 d . . . H6 H 0.1730 0.6177 -0.3965 0.041 Uiso 1 1 calc R . . C7 C 0.1200(3) 0.6469(2) -0.26390(17) 0.0328(6) Uani 1 1 d . . . H7 H 0.1129 0.5781 -0.2522 0.039 Uiso 1 1 calc R . . C8 C 0.3796(2) 0.7611(2) -0.49446(15) 0.0261(5) Uani 1 1 d . . . C9 C 0.4211(2) 0.8408(2) -0.52841(17) 0.0320(6) Uani 1 1 d . . . H9 H 0.3650 0.9164 -0.5408 0.038 Uiso 1 1 calc R . . C10 C 0.5475(2) 0.8067(2) -0.54384(17) 0.0319(6) Uani 1 1 d . . . H10 H 0.5764 0.8596 -0.5675 0.038 Uiso 1 1 calc R . . C11 C 0.6314(2) 0.6953(2) -0.52461(15) 0.0258(5) Uani 1 1 d . . . C12 C 0.5878(2) 0.6157(2) -0.49059(17) 0.0303(6) Uani 1 1 d . . . H12 H 0.6437 0.5401 -0.4782 0.036 Uiso 1 1 calc R . . C13 C 0.4620(2) 0.6486(2) -0.47515(17) 0.0314(6) Uani 1 1 d . . . H13 H 0.4329 0.5957 -0.4520 0.038 Uiso 1 1 calc R . . C14 C 0.7688(2) 0.6580(2) -0.53780(16) 0.0303(6) Uani 1 1 d . . . C15 C -0.2438(2) 0.6658(2) 0.16329(16) 0.0224(5) Uani 1 1 d . . . C16 C -0.3391(2) 0.6264(2) 0.16913(15) 0.0217(5) Uani 1 1 d . . . C17 C -0.3361(2) 0.5711(2) 0.09550(16) 0.0273(5) Uani 1 1 d . . . H17 H -0.2749 0.5587 0.0413 0.033 Uiso 1 1 calc R . . C18 C -0.4239(2) 0.5342(2) 0.10238(16) 0.0269(5) Uani 1 1 d . . . H18 H -0.4224 0.4977 0.0530 0.032 Uiso 1 1 calc R . . C19 C -0.5135(2) 0.5525(2) 0.18334(15) 0.0214(5) Uani 1 1 d . . . C20 C -0.5183(2) 0.6074(2) 0.25752(16) 0.0285(6) Uani 1 1 d . . . H20 H -0.5794 0.6194 0.3117 0.034 Uiso 1 1 calc R . . C21 C -0.4304(2) 0.6441(2) 0.24955(16) 0.0293(6) Uani 1 1 d . . . H21 H -0.4326 0.6811 0.2990 0.035 Uiso 1 1 calc R . . C22 C -0.5242(2) 0.3414(2) 0.19452(15) 0.0219(5) Uani 1 1 d . . . C23 C -0.4451(3) 0.2657(2) 0.11692(18) 0.0382(7) Uani 1 1 d . . . H23 H -0.4461 0.2951 0.0625 0.046 Uiso 1 1 calc R . . C24 C -0.3642(3) 0.1451(2) 0.12182(19) 0.0403(7) Uani 1 1 d . . . H24 H -0.3103 0.0929 0.0700 0.048 Uiso 1 1 calc R . . C25 C -0.3625(2) 0.1012(2) 0.20220(18) 0.0282(6) Uani 1 1 d . . . C26 C -0.4452(3) 0.1775(2) 0.27907(18) 0.0369(7) Uani 1 1 d . . . H26 H -0.4462 0.1476 0.3335 0.044 Uiso 1 1 calc R . . C27 C -0.5267(3) 0.2984(2) 0.27541(17) 0.0352(6) Uani 1 1 d . . . H27 H -0.5826 0.3500 0.3271 0.042 Uiso 1 1 calc R . . C28 C -0.2706(2) -0.0290(2) 0.2063(2) 0.0349(6) Uani 1 1 d . . . C29 C 0.0612(2) 0.8024(2) 0.22302(18) 0.0271(6) Uani 1 1 d . . . C30 C 0.1557(2) 0.8428(2) 0.21772(16) 0.0232(5) Uani 1 1 d . . . C31 C 0.1545(2) 0.8904(2) 0.29386(17) 0.0299(6) Uani 1 1 d . . . H31 H 0.0973 0.8953 0.3482 0.036 Uiso 1 1 calc R . . C32 C 0.2386(2) 0.9307(2) 0.28870(17) 0.0317(6) Uani 1 1 d . . . H32 H 0.2381 0.9632 0.3395 0.038 Uiso 1 1 calc R . . C33 C 0.3231(2) 0.9224(2) 0.20785(17) 0.0248(5) Uani 1 1 d . . . C34 C 0.3271(3) 0.8729(3) 0.13183(18) 0.0353(6) Uani 1 1 d . . . H34 H 0.3858 0.8664 0.0777 0.042 Uiso 1 1 calc R . . C35 C 0.2424(3) 0.8332(3) 0.13750(17) 0.0349(6) Uani 1 1 d . . . H35 H 0.2438 0.7997 0.0868 0.042 Uiso 1 1 calc R . . C36 C 0.3287(2) 1.1353(2) 0.19110(17) 0.0253(5) Uani 1 1 d . . . C37 C 0.2519(3) 1.2165(2) 0.26632(18) 0.0348(6) Uani 1 1 d . . . H37 H 0.2537 1.1909 0.3217 0.042 Uiso 1 1 calc R . . C38 C 0.1721(3) 1.3365(2) 0.25852(18) 0.0335(6) Uani 1 1 d . . . H38 H 0.1199 1.3917 0.3090 0.040 Uiso 1 1 calc R . . C39 C 0.1693(2) 1.3751(2) 0.17582(16) 0.0232(5) Uani 1 1 d . . . C40 C 0.2458(2) 1.2919(2) 0.10142(17) 0.0304(6) Uani 1 1 d . . . H40 H 0.2433 1.3169 0.0460 0.036 Uiso 1 1 calc R . . C41 C 0.3264(2) 1.1713(2) 0.10842(18) 0.0324(6) Uani 1 1 d . . . H41 H 0.3780 1.1157 0.0581 0.039 Uiso 1 1 calc R . . C42 C 0.0807(2) 1.5060(2) 0.17021(16) 0.0236(5) 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 0.0244(3) 0.0186(3) 0.0192(3) 0.0028(2) -0.0041(2) -0.0127(2) Mn2 0.01998(18) 0.0215(2) 0.02000(19) 0.00460(15) -0.00748(15) -0.01128(15) Mn3 0.02303(19) 0.01950(19) 0.01792(18) 0.00204(14) -0.00606(15) -0.01140(15) K1 0.0305(3) 0.0430(4) 0.0395(4) 0.0123(3) -0.0118(3) -0.0126(3) S1 0.0255(3) 0.0404(4) 0.0201(3) 0.0094(3) -0.0059(2) -0.0178(3) S2 0.0173(3) 0.0187(3) 0.0299(3) 0.0034(2) -0.0074(2) -0.0090(2) S3 0.0226(3) 0.0203(3) 0.0509(4) 0.0138(3) -0.0185(3) -0.0127(3) O1 0.0394(10) 0.0351(11) 0.0324(10) 0.0163(8) -0.0094(8) -0.0252(9) O2 0.0169(8) 0.0227(9) 0.0282(9) 0.0003(7) -0.0027(7) -0.0098(7) O3 0.0254(9) 0.0216(9) 0.0313(9) 0.0075(7) -0.0153(7) -0.0114(7) O4 0.0327(10) 0.0435(11) 0.0250(9) 0.0089(8) -0.0078(8) -0.0254(9) O5 0.0482(12) 0.0256(10) 0.0649(14) 0.0118(10) -0.0355(11) -0.0125(9) O6 0.0310(10) 0.0433(11) 0.0325(10) -0.0009(8) -0.0117(8) -0.0233(9) O7 0.0262(9) 0.0357(11) 0.0408(11) 0.0045(8) -0.0073(8) -0.0209(8) O8 0.0281(9) 0.0218(9) 0.0347(10) 0.0009(8) -0.0060(8) -0.0061(8) O9 0.0337(11) 0.0233(10) 0.0684(15) -0.0032(10) -0.0134(11) -0.0056(9) O10 0.0846(16) 0.0503(13) 0.0201(10) 0.0056(9) -0.0064(10) -0.0456(12) O11 0.0470(11) 0.0444(12) 0.0471(12) 0.0090(9) -0.0275(10) -0.0315(10) O12 0.0380(12) 0.0594(14) 0.0862(17) 0.0449(13) -0.0325(12) -0.0259(11) O13 0.0314(10) 0.0464(12) 0.0382(11) 0.0208(9) -0.0100(9) -0.0139(9) O14 0.0440(11) 0.0644(14) 0.0255(10) 0.0043(9) -0.0114(9) -0.0356(11) O15 0.0363(10) 0.0326(10) 0.0413(11) 0.0112(8) -0.0242(9) -0.0193(8) O16 0.0199(8) 0.0263(9) 0.0395(11) -0.0031(8) 0.0022(8) -0.0107(7) O17 0.0504(12) 0.0373(11) 0.0699(14) 0.0285(10) -0.0454(11) -0.0298(10) O18 0.0214(9) 0.0261(10) 0.0720(15) 0.0080(10) -0.0047(9) -0.0105(8) O19 0.101(2) 0.0600(16) 0.0590(16) -0.0046(13) -0.0096(15) -0.0415(15) C1 0.0245(12) 0.0341(15) 0.0223(13) 0.0087(11) -0.0055(10) -0.0155(11) C2 0.0273(13) 0.0281(13) 0.0239(13) 0.0062(11) -0.0046(10) -0.0157(11) C3 0.0513(17) 0.0346(15) 0.0220(13) 0.0030(11) -0.0054(12) -0.0269(14) C4 0.0476(16) 0.0327(15) 0.0264(14) 0.0083(12) -0.0073(12) -0.0267(13) C5 0.0238(12) 0.0315(14) 0.0208(12) 0.0070(11) -0.0045(10) -0.0153(11) C6 0.0406(15) 0.0410(16) 0.0231(13) -0.0004(12) -0.0029(12) -0.0256(13) C7 0.0417(15) 0.0303(15) 0.0293(14) 0.0063(12) -0.0052(12) -0.0239(13) C8 0.0242(12) 0.0324(14) 0.0199(12) 0.0042(10) -0.0040(10) -0.0146(11) C9 0.0291(13) 0.0334(15) 0.0297(14) 0.0130(12) -0.0087(11) -0.0142(12) C10 0.0307(14) 0.0347(15) 0.0322(14) 0.0127(12) -0.0067(11) -0.0205(12) C11 0.0250(12) 0.0313(14) 0.0205(12) 0.0053(10) -0.0046(10) -0.0155(11) C12 0.0301(13) 0.0267(14) 0.0326(14) 0.0090(11) -0.0097(11) -0.0140(11) C13 0.0325(14) 0.0305(14) 0.0345(15) 0.0083(12) -0.0079(12) -0.0203(12) C14 0.0284(13) 0.0391(16) 0.0241(13) 0.0081(12) -0.0067(11) -0.0188(12) C15 0.0182(11) 0.0165(12) 0.0295(13) 0.0019(10) -0.0092(10) -0.0056(9) C16 0.0182(11) 0.0193(12) 0.0249(12) 0.0016(10) -0.0063(10) -0.0078(10) C17 0.0250(12) 0.0340(14) 0.0225(13) 0.0008(11) -0.0025(10) -0.0172(11) C18 0.0301(13) 0.0341(14) 0.0225(13) 0.0005(11) -0.0062(10) -0.0214(12) C19 0.0173(11) 0.0196(12) 0.0280(13) 0.0040(10) -0.0076(10) -0.0097(10) C20 0.0257(13) 0.0348(15) 0.0234(13) -0.0032(11) 0.0008(10) -0.0183(11) C21 0.0312(13) 0.0357(15) 0.0249(13) -0.0044(11) -0.0052(11) -0.0210(12) C22 0.0190(11) 0.0185(12) 0.0263(13) 0.0008(10) -0.0060(10) -0.0085(10) C23 0.0476(17) 0.0276(15) 0.0266(14) 0.0033(12) -0.0068(13) -0.0124(13) C24 0.0428(16) 0.0263(15) 0.0323(15) -0.0057(12) -0.0032(13) -0.0073(13) C25 0.0236(12) 0.0196(13) 0.0428(16) 0.0024(11) -0.0140(12) -0.0098(10) C26 0.0443(16) 0.0260(14) 0.0307(15) 0.0067(12) -0.0148(13) -0.0093(12) C27 0.0384(15) 0.0251(14) 0.0268(14) 0.0007(11) -0.0078(12) -0.0063(12) C28 0.0252(13) 0.0230(14) 0.061(2) 0.0031(14) -0.0205(14) -0.0110(11) C29 0.0248(13) 0.0195(12) 0.0415(16) 0.0074(11) -0.0180(12) -0.0106(10) C30 0.0223(12) 0.0210(12) 0.0294(13) 0.0049(10) -0.0097(10) -0.0125(10) C31 0.0322(14) 0.0402(16) 0.0248(13) 0.0070(11) -0.0078(11) -0.0247(12) C32 0.0371(14) 0.0419(16) 0.0283(14) 0.0056(12) -0.0138(12) -0.0268(13) C33 0.0218(12) 0.0195(12) 0.0369(14) 0.0086(11) -0.0138(11) -0.0113(10) C34 0.0357(15) 0.0444(17) 0.0300(14) 0.0011(12) -0.0014(12) -0.0281(13) C35 0.0424(15) 0.0448(17) 0.0269(14) -0.0009(12) -0.0083(12) -0.0297(14) C36 0.0228(12) 0.0199(12) 0.0385(15) 0.0086(11) -0.0130(11) -0.0132(10) C37 0.0451(16) 0.0289(15) 0.0318(15) 0.0110(12) -0.0199(13) -0.0159(13) C38 0.0405(15) 0.0266(14) 0.0293(14) 0.0034(11) -0.0135(12) -0.0127(12) C39 0.0216(12) 0.0211(12) 0.0312(13) 0.0071(10) -0.0118(10) -0.0122(10) C40 0.0337(14) 0.0241(13) 0.0276(14) 0.0076(11) -0.0101(11) -0.0106(11) C41 0.0295(13) 0.0227(13) 0.0316(14) 0.0017(11) -0.0028(11) -0.0071(11) C42 0.0197(11) 0.0216(13) 0.0333(14) 0.0070(11) -0.0105(11) -0.0123(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.0620(17) . ? Mn1 O1 2.0620(17) 2_565 ? Mn1 O2 2.2249(15) . ? Mn1 O2 2.2249(15) 2_565 ? Mn1 O3 2.2421(15) 2_575 ? Mn1 O3 2.2421(15) 1_545 ? Mn1 Mn3 3.1533(3) 2_565 ? Mn1 Mn3 3.1533(3) . ? Mn2 O4 2.0465(17) 1_456 ? Mn2 O5 2.0839(18) 1_565 ? Mn2 O6 2.1172(16) . ? Mn2 O7 2.1353(17) . ? Mn2 O8 2.1695(17) 1_545 ? Mn2 Mn3 3.0866(5) . ? Mn2 K1 3.6373(7) 1_655 ? Mn3 O9 2.0504(18) 1_565 ? Mn3 O10 2.0587(19) . ? Mn3 O11 2.0621(17) . ? Mn3 O3 2.2339(16) 1_545 ? Mn3 O2 2.2570(16) . ? K1 O16 2.6776(18) . ? K1 O12 2.679(2) 2_565 ? K1 O19 2.781(3) . ? K1 O7 2.8569(19) 1_455 ? K1 O4 2.9389(18) 1_356 ? K1 O14 2.9393(19) 1_456 ? K1 O8 3.3182(19) 1_445 ? K1 O12 3.349(2) 1_356 ? K1 C14 3.530(3) 1_356 ? K1 Mn2 3.6373(7) 1_455 ? K1 K1 4.7249(13) 2_366 ? S1 O13 1.434(2) . ? S1 O14 1.4415(19) . ? S1 C5 1.767(2) . ? S1 C8 1.773(2) . ? S2 O15 1.4356(17) . ? S2 O16 1.4407(18) . ? S2 C22 1.766(2) . ? S2 C19 1.771(2) . ? S3 O18 1.432(2) . ? S3 O17 1.434(2) . ? S3 C33 1.772(2) . ? S3 C36 1.773(2) . ? O1 C1 1.251(3) . ? O2 C15 1.280(3) . ? O3 C42 1.284(3) . ? O3 Mn3 2.2339(16) 1_565 ? O3 Mn1 2.2421(15) 1_565 ? O4 C14 1.275(3) . ? O4 Mn2 2.0465(17) 1_654 ? O4 K1 2.9389(18) 1_754 ? O5 C28 1.254(3) . ? O5 Mn2 2.0839(18) 1_545 ? O6 C15 1.246(3) . ? O7 C29 1.257(3) . ? O7 K1 2.8569(19) 1_655 ? O8 C42 1.245(3) . ? O8 Mn2 2.1695(17) 1_565 ? O8 K1 3.3182(19) 1_665 ? O9 C28 1.254(3) . ? O9 Mn3 2.0504(18) 1_545 ? O10 C1 1.248(3) . ? O11 C29 1.252(3) . ? O12 C14 1.226(3) . ? O12 K1 2.679(2) 2_565 ? O12 K1 3.349(2) 1_754 ? O14 K1 2.9393(19) 1_654 ? C1 C2 1.498(3) . ? C2 C7 1.382(3) . ? C2 C3 1.392(4) . ? C3 C4 1.380(4) . ? C4 C5 1.381(3) . ? C5 C6 1.379(4) . ? C6 C7 1.376(4) . ? C8 C9 1.380(4) . ? C8 C13 1.387(3) . ? C9 C10 1.386(4) . ? C10 C11 1.384(3) . ? C11 C12 1.395(3) . ? C11 C14 1.516(3) . ? C12 C13 1.382(3) . ? C14 K1 3.530(3) 1_754 ? C15 C16 1.503(3) . ? C16 C21 1.384(3) . ? C16 C17 1.390(3) . ? C17 C18 1.387(3) . ? C18 C19 1.378(3) . ? C19 C20 1.383(3) . ? C20 C21 1.384(3) . ? C22 C27 1.374(3) . ? C22 C23 1.379(3) . ? C23 C24 1.383(4) . ? C24 C25 1.375(4) . ? C25 C26 1.379(4) . ? C25 C28 1.502(3) . ? C26 C27 1.382(3) . ? C29 C30 1.505(3) . ? C30 C35 1.377(4) . ? C30 C31 1.386(3) . ? C31 C32 1.380(3) . ? C32 C33 1.375(4) . ? C33 C34 1.378(3) . ? C34 C35 1.382(4) . ? C36 C37 1.379(4) . ? C36 C41 1.379(4) . ? C37 C38 1.386(4) . ? C38 C39 1.389(3) . ? C39 C40 1.382(3) . ? C39 C42 1.503(3) . ? C40 C41 1.390(3) . ? 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 180.0(0) . 2_565 ? O1 Mn1 O2 92.20(7) . . ? O1 Mn1 O2 87.80(7) 2_565 . ? O1 Mn1 O2 87.80(7) . 2_565 ? O1 Mn1 O2 92.20(7) 2_565 2_565 ? O2 Mn1 O2 180.0 . 2_565 ? O1 Mn1 O3 86.99(7) . 2_575 ? O1 Mn1 O3 93.01(7) 2_565 2_575 ? O2 Mn1 O3 103.50(6) . 2_575 ? O2 Mn1 O3 76.50(6) 2_565 2_575 ? O1 Mn1 O3 93.01(7) . 1_545 ? O1 Mn1 O3 86.99(7) 2_565 1_545 ? O2 Mn1 O3 76.50(6) . 1_545 ? O2 Mn1 O3 103.50(6) 2_565 1_545 ? O3 Mn1 O3 180.0(0) 2_575 1_545 ? O1 Mn1 Mn3 113.29(5) . 2_565 ? O1 Mn1 Mn3 66.71(5) 2_565 2_565 ? O2 Mn1 Mn3 134.30(4) . 2_565 ? O2 Mn1 Mn3 45.70(4) 2_565 2_565 ? O3 Mn1 Mn3 45.10(4) 2_575 2_565 ? O3 Mn1 Mn3 134.90(4) 1_545 2_565 ? O1 Mn1 Mn3 66.71(5) . . ? O1 Mn1 Mn3 113.29(5) 2_565 . ? O2 Mn1 Mn3 45.70(4) . . ? O2 Mn1 Mn3 134.30(4) 2_565 . ? O3 Mn1 Mn3 134.90(4) 2_575 . ? O3 Mn1 Mn3 45.10(4) 1_545 . ? Mn3 Mn1 Mn3 180.0(0) 2_565 . ? O4 Mn2 O5 108.68(8) 1_456 1_565 ? O4 Mn2 O6 105.47(7) 1_456 . ? O5 Mn2 O6 91.18(7) 1_565 . ? O4 Mn2 O7 94.03(7) 1_456 . ? O5 Mn2 O7 89.89(7) 1_565 . ? O6 Mn2 O7 158.98(7) . . ? O4 Mn2 O8 96.43(7) 1_456 1_545 ? O5 Mn2 O8 154.72(8) 1_565 1_545 ? O6 Mn2 O8 84.69(7) . 1_545 ? O7 Mn2 O8 85.41(7) . 1_545 ? O4 Mn2 Mn3 167.28(5) 1_456 . ? O5 Mn2 Mn3 83.73(6) 1_565 . ? O6 Mn2 Mn3 70.68(5) . . ? O7 Mn2 Mn3 88.59(5) . . ? O8 Mn2 Mn3 71.34(5) 1_545 . ? O4 Mn2 K1 53.85(5) 1_456 1_655 ? O5 Mn2 K1 129.75(6) 1_565 1_655 ? O6 Mn2 K1 136.79(5) . 1_655 ? O7 Mn2 K1 51.70(5) . 1_655 ? O8 Mn2 K1 63.97(5) 1_545 1_655 ? Mn3 Mn2 K1 120.338(15) . 1_655 ? O9 Mn3 O10 99.46(9) 1_565 . ? O9 Mn3 O11 91.23(8) 1_565 . ? O10 Mn3 O11 101.03(8) . . ? O9 Mn3 O3 153.25(8) 1_565 1_545 ? O10 Mn3 O3 106.36(8) . 1_545 ? O11 Mn3 O3 90.62(7) . 1_545 ? O9 Mn3 O2 89.36(7) 1_565 . ? O10 Mn3 O2 108.60(7) . . ? O11 Mn3 O2 149.85(7) . . ? O3 Mn3 O2 76.02(6) 1_545 . ? O9 Mn3 Mn2 71.31(6) 1_565 . ? O10 Mn3 Mn2 163.59(6) . . ? O11 Mn3 Mn2 66.46(6) . . ? O3 Mn3 Mn2 85.08(4) 1_545 . ? O2 Mn3 Mn2 85.30(4) . . ? O9 Mn3 Mn1 131.98(6) 1_565 . ? O10 Mn3 Mn1 86.06(6) . . ? O11 Mn3 Mn1 134.81(6) . . ? O3 Mn3 Mn1 45.32(4) 1_545 . ? O2 Mn3 Mn1 44.87(4) . . ? Mn2 Mn3 Mn1 110.259(13) . . ? O16 K1 O12 97.53(7) . 2_565 ? O16 K1 O19 137.68(7) . . ? O12 K1 O19 114.66(8) 2_565 . ? O16 K1 O7 75.55(5) . 1_455 ? O12 K1 O7 170.52(7) 2_565 1_455 ? O19 K1 O7 74.54(7) . 1_455 ? O16 K1 O4 126.88(5) . 1_356 ? O12 K1 O4 117.73(6) 2_565 1_356 ? O19 K1 O4 61.42(7) . 1_356 ? O7 K1 O4 63.71(5) 1_455 1_356 ? O16 K1 O14 76.59(5) . 1_456 ? O12 K1 O14 88.78(6) 2_565 1_456 ? O19 K1 O14 77.38(7) . 1_456 ? O7 K1 O14 95.77(5) 1_455 1_456 ? O4 K1 O14 137.16(6) 1_356 1_456 ? O16 K1 O8 69.47(5) . 1_445 ? O12 K1 O8 115.91(7) 2_565 1_445 ? O19 K1 O8 114.80(7) . 1_445 ? O7 K1 O8 55.83(5) 1_455 1_445 ? O4 K1 O8 59.98(5) 1_356 1_445 ? O14 K1 O8 139.84(5) 1_456 1_445 ? O16 K1 O12 136.12(6) . 1_356 ? O12 K1 O12 77.35(6) 2_565 1_356 ? O19 K1 O12 79.91(7) . 1_356 ? O7 K1 O12 102.99(5) 1_455 1_356 ? O4 K1 O12 40.50(5) 1_356 1_356 ? O14 K1 O12 145.36(6) 1_456 1_356 ? O8 K1 O12 73.94(5) 1_445 1_356 ? O16 K1 C14 134.89(6) . 1_356 ? O12 K1 C14 97.59(7) 2_565 1_356 ? O19 K1 C14 69.44(8) . 1_356 ? O7 K1 C14 83.31(6) 1_455 1_356 ? O4 K1 C14 20.19(5) 1_356 1_356 ? O14 K1 C14 145.85(6) 1_456 1_356 ? O8 K1 C14 65.68(5) 1_445 1_356 ? O12 K1 C14 20.31(5) 1_356 1_356 ? O16 K1 Mn2 93.63(4) . 1_455 ? O12 K1 Mn2 140.56(5) 2_565 1_455 ? O19 K1 Mn2 78.94(6) . 1_455 ? O7 K1 Mn2 35.91(3) 1_455 1_455 ? O4 K1 Mn2 34.22(3) 1_356 1_455 ? O14 K1 Mn2 130.65(4) 1_456 1_455 ? O8 K1 Mn2 35.98(3) 1_445 1_455 ? O12 K1 Mn2 68.61(4) 1_356 1_455 ? C14 K1 Mn2 50.61(4) 1_356 1_455 ? O16 K1 K1 125.82(5) . 2_366 ? O12 K1 K1 43.75(5) 2_565 2_366 ? O19 K1 K1 96.46(6) . 2_366 ? O7 K1 K1 135.94(4) 1_455 2_366 ? O4 K1 K1 74.03(4) 1_356 2_366 ? O14 K1 K1 124.82(4) 1_456 2_366 ? O8 K1 K1 92.97(4) 1_445 2_366 ? O12 K1 K1 33.60(3) 1_356 2_366 ? C14 K1 K1 53.85(4) 1_356 2_366 ? Mn2 K1 K1 100.34(2) 1_455 2_366 ? O13 S1 O14 118.77(12) . . ? O13 S1 C5 109.25(11) . . ? O14 S1 C5 107.83(12) . . ? O13 S1 C8 108.51(12) . . ? O14 S1 C8 107.65(11) . . ? C5 S1 C8 103.82(11) . . ? O15 S2 O16 119.51(11) . . ? O15 S2 C22 108.79(11) . . ? O16 S2 C22 107.82(11) . . ? O15 S2 C19 108.65(11) . . ? O16 S2 C19 108.14(11) . . ? C22 S2 C19 102.63(11) . . ? O18 S3 O17 120.20(12) . . ? O18 S3 C33 108.44(12) . . ? O17 S3 C33 108.21(12) . . ? O18 S3 C36 108.36(12) . . ? O17 S3 C36 108.25(12) . . ? C33 S3 C36 101.83(11) . . ? C1 O1 Mn1 145.39(17) . . ? C15 O2 Mn1 128.42(15) . . ? C15 O2 Mn3 115.53(14) . . ? Mn1 O2 Mn3 89.42(5) . . ? C42 O3 Mn3 117.59(15) . 1_565 ? C42 O3 Mn1 128.91(15) . 1_565 ? Mn3 O3 Mn1 89.58(5) 1_565 1_565 ? C14 O4 Mn2 133.36(16) . 1_654 ? C14 O4 K1 107.07(15) . 1_754 ? Mn2 O4 K1 91.93(6) 1_654 1_754 ? C28 O5 Mn2 119.62(18) . 1_545 ? C15 O6 Mn2 143.80(17) . . ? C29 O7 Mn2 112.54(15) . . ? C29 O7 K1 127.15(15) . 1_655 ? Mn2 O7 K1 92.39(6) . 1_655 ? C42 O8 Mn2 140.52(16) . 1_565 ? C42 O8 K1 134.18(14) . 1_665 ? Mn2 O8 K1 80.05(5) 1_565 1_665 ? C28 O9 Mn3 138.14(19) . 1_545 ? C1 O10 Mn3 117.76(17) . . ? C29 O11 Mn3 147.28(19) . . ? C14 O12 K1 168.13(19) . 2_565 ? C14 O12 K1 88.21(16) . 1_754 ? K1 O12 K1 102.65(6) 2_565 1_754 ? S1 O14 K1 145.26(11) . 1_654 ? S2 O16 K1 168.91(11) . . ? O10 C1 O1 123.8(2) . . ? O10 C1 C2 118.8(2) . . ? O1 C1 C2 117.3(2) . . ? C7 C2 C3 119.8(2) . . ? C7 C2 C1 119.3(2) . . ? C3 C2 C1 120.9(2) . . ? C4 C3 C2 120.2(2) . . ? C3 C4 C5 118.9(2) . . ? C6 C5 C4 121.7(2) . . ? C6 C5 S1 118.60(19) . . ? C4 C5 S1 119.70(19) . . ? C7 C6 C5 119.0(2) . . ? C6 C7 C2 120.5(2) . . ? C9 C8 C13 121.0(2) . . ? C9 C8 S1 121.17(19) . . ? C13 C8 S1 117.80(19) . . ? C8 C9 C10 119.0(2) . . ? C11 C10 C9 121.0(2) . . ? C10 C11 C12 119.1(2) . . ? C10 C11 C14 121.9(2) . . ? C12 C11 C14 118.9(2) . . ? C13 C12 C11 120.4(2) . . ? C12 C13 C8 119.4(2) . . ? O12 C14 O4 124.2(2) . . ? O12 C14 C11 118.9(2) . . ? O4 C14 C11 116.9(2) . . ? O12 C14 K1 71.48(15) . 1_754 ? O4 C14 K1 52.73(12) . 1_754 ? C11 C14 K1 169.46(18) . 1_754 ? O6 C15 O2 123.7(2) . . ? O6 C15 C16 117.0(2) . . ? O2 C15 C16 119.3(2) . . ? C21 C16 C17 119.3(2) . . ? C21 C16 C15 119.5(2) . . ? C17 C16 C15 121.2(2) . . ? C18 C17 C16 120.4(2) . . ? C19 C18 C17 119.1(2) . . ? C18 C19 C20 121.6(2) . . ? C18 C19 S2 117.93(18) . . ? C20 C19 S2 120.47(18) . . ? C19 C20 C21 118.7(2) . . ? C20 C21 C16 121.0(2) . . ? C27 C22 C23 121.3(2) . . ? C27 C22 S2 118.80(18) . . ? C23 C22 S2 119.83(19) . . ? C22 C23 C24 118.6(2) . . ? C25 C24 C23 120.9(2) . . ? C24 C25 C26 119.6(2) . . ? C24 C25 C28 120.2(2) . . ? C26 C25 C28 120.2(2) . . ? C25 C26 C27 120.2(2) . . ? C22 C27 C26 119.3(2) . . ? O5 C28 O9 125.3(2) . . ? O5 C28 C25 118.1(3) . . ? O9 C28 C25 116.7(3) . . ? O11 C29 O7 124.9(2) . . ? O11 C29 C30 116.4(2) . . ? O7 C29 C30 118.7(2) . . ? C35 C30 C31 120.1(2) . . ? C35 C30 C29 120.2(2) . . ? C31 C30 C29 119.7(2) . . ? C32 C31 C30 119.8(2) . . ? C33 C32 C31 119.4(2) . . ? C32 C33 C34 121.5(2) . . ? C32 C33 S3 119.20(19) . . ? C34 C33 S3 119.3(2) . . ? C33 C34 C35 118.8(2) . . ? C30 C35 C34 120.5(2) . . ? C37 C36 C41 121.1(2) . . ? C37 C36 S3 119.52(19) . . ? C41 C36 S3 119.26(19) . . ? C36 C37 C38 119.4(2) . . ? C37 C38 C39 120.5(2) . . ? C40 C39 C38 119.2(2) . . ? C40 C39 C42 121.9(2) . . ? C38 C39 C42 118.9(2) . . ? C39 C40 C41 120.8(2) . . ? C36 C41 C40 119.0(2) . . ? O8 C42 O3 123.6(2) . . ? O8 C42 C39 117.7(2) . . ? O3 C42 C39 118.7(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.515 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.065 ######END####### data_Compound(3) _database_code_depnum_ccdc_archive 'CCDC 834724' #TrackingRef '- all compounds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Manganese Sulfonyldibenzoate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H48 Cs2 Mn5 O36 S6' _chemical_formula_weight 2366.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5500(6) _cell_length_b 12.9301(6) _cell_length_c 16.1279(7) _cell_angle_alpha 106.080(4) _cell_angle_beta 93.353(4) _cell_angle_gamma 118.627(5) _cell_volume 2149.86(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1171 _exptl_absorpt_coefficient_mu 1.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 0.836 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16812 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8429 _reflns_number_gt 5712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0529P)^2^+1.4702P] 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 8429 _refine_ls_number_parameters 601 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.5000 1.0000 0.0233(3) Uani 1 2 d S . . Mn2 Mn -0.20059(8) 0.54498(9) 1.08793(5) 0.0221(2) Uani 1 1 d . . . Mn3 Mn -1.11414(8) -0.34744(9) 0.29086(5) 0.0232(2) Uani 1 1 d . . . Cs1 Cs -0.21030(5) 0.44983(5) 0.43779(3) 0.05122(17) Uani 1 1 d . . . S1 S -0.54245(17) 0.28127(17) 0.52723(10) 0.0378(4) Uani 1 1 d . . . S2 S 0.60968(14) 1.12146(15) 1.19048(10) 0.0263(3) Uani 1 1 d . . . S3 S -0.09369(15) 0.91996(16) 0.79675(12) 0.0348(4) Uani 1 1 d . . . O1 O -0.1471(4) 0.4570(4) 0.9042(3) 0.0352(11) Uani 1 1 d . . . O2 O 0.0023(4) 0.6666(4) 1.0892(2) 0.0268(9) Uani 1 1 d . . . O3 O 0.1215(4) 0.5765(4) 0.9097(2) 0.0271(9) Uani 1 1 d . . . O4 O 0.7903(5) 0.7041(5) 1.1371(3) 0.0461(13) Uani 1 1 d . . . O5 O -0.2960(4) 0.4760(5) 0.9589(3) 0.0449(13) Uani 1 1 d . . . O6 O -0.6546(4) 0.5563(4) 0.8591(3) 0.0372(11) Uani 1 1 d . . . O7 O -1.0389(4) -0.3009(4) 0.4203(2) 0.0337(11) Uani 1 1 d . . . O8 O 0.0933(4) 0.5082(4) 0.7635(3) 0.0345(11) Uani 1 1 d . . . O9 O 0.0392(4) 0.7452(4) 1.2363(3) 0.0329(10) Uani 1 1 d . . . O10 O 0.8295(5) 0.7779(5) 1.2845(3) 0.0454(13) Uani 1 1 d . . . O11 O -0.7016(4) 0.4837(4) 0.7126(3) 0.0367(11) Uani 1 1 d . . . O12 O -0.8988(6) -0.3216(5) 0.4910(4) 0.078(2) Uani 1 1 d . . . O13 O -0.4606(5) 0.2817(5) 0.4689(3) 0.0570(15) Uani 1 1 d . . . O14 O -0.6025(5) 0.3513(5) 0.5253(3) 0.0539(15) Uani 1 1 d . . . O15 O -0.0423(4) 1.0281(4) 0.8764(3) 0.0488(13) Uani 1 1 d . . . O16 O -0.0818(4) 0.9362(5) 0.7133(3) 0.0485(13) Uani 1 1 d . . . O17 O 0.6582(4) 1.2243(4) 1.2737(3) 0.0380(11) Uani 1 1 d . . . O18 O 0.6211(4) 1.1482(4) 1.1099(3) 0.0375(11) Uani 1 1 d . . . C1 C -0.2514(6) 0.4515(6) 0.8975(4) 0.0281(14) Uani 1 1 d . . . C2 C -0.3233(6) 0.4076(6) 0.8036(4) 0.0259(14) Uani 1 1 d . . . C3 C -0.2748(6) 0.3814(7) 0.7322(4) 0.0360(16) Uani 1 1 d . . . H3 H -0.1974 0.3883 0.7408 0.043 Uiso 1 1 calc R . . C4 C -0.3407(6) 0.3446(6) 0.6476(4) 0.0359(16) Uani 1 1 d . . . H4 H -0.3075 0.3282 0.5989 0.043 Uiso 1 1 calc R . . C5 C -0.4553(6) 0.3326(6) 0.6365(4) 0.0303(15) Uani 1 1 d . . . C6 C -0.5086(6) 0.3558(7) 0.7068(4) 0.0346(16) Uani 1 1 d . . . H6 H -0.5874 0.3456 0.6976 0.042 Uiso 1 1 calc R . . C7 C -0.4399(6) 0.3950(7) 0.7922(4) 0.0361(16) Uani 1 1 d . . . H7 H -0.4722 0.4125 0.8411 0.043 Uiso 1 1 calc R . . C8 C -0.6560(6) 0.1245(6) 0.5073(4) 0.0311(15) Uani 1 1 d . . . C9 C -0.6211(6) 0.0419(6) 0.5189(4) 0.0361(16) Uani 1 1 d . . . H9 H -0.5372 0.0703 0.5375 0.043 Uiso 1 1 calc R . . C10 C -0.7079(6) -0.0796(7) 0.5036(4) 0.0376(17) Uani 1 1 d . . . H10 H -0.6826 -0.1332 0.5127 0.045 Uiso 1 1 calc R . . C11 C -0.8342(6) -0.1262(6) 0.4744(4) 0.0304(14) Uani 1 1 d . . . C12 C -0.8683(6) -0.0421(7) 0.4620(4) 0.0352(16) Uani 1 1 d . . . H12 H -0.9519 -0.0710 0.4418 0.042 Uiso 1 1 calc R . . C13 C -0.7818(7) 0.0811(6) 0.4789(4) 0.0368(16) Uani 1 1 d . . . H13 H -0.8066 0.1358 0.4715 0.044 Uiso 1 1 calc R . . C14 C -0.9291(7) -0.2577(7) 0.4619(4) 0.0345(16) Uani 1 1 d . . . C15 C 0.0908(5) 0.5775(6) 0.8337(4) 0.0250(13) Uani 1 1 d . . . C16 C 0.0492(6) 0.6667(6) 0.8266(4) 0.0288(14) Uani 1 1 d . . . C17 C 0.0221(6) 0.6724(7) 0.7440(4) 0.0360(16) Uani 1 1 d . . . H17 H 0.0296 0.6213 0.6941 0.043 Uiso 1 1 calc R . . C18 C -0.0164(6) 0.7547(7) 0.7355(4) 0.0372(17) Uani 1 1 d . . . H18 H -0.0305 0.7622 0.6808 0.045 Uiso 1 1 calc R . . C19 C -0.0328(6) 0.8232(6) 0.8082(4) 0.0298(14) Uani 1 1 d . . . C20 C -0.0067(6) 0.8194(7) 0.8914(4) 0.0376(17) Uani 1 1 d . . . H20 H -0.0166 0.8691 0.9407 0.045 Uiso 1 1 calc R . . C21 C 0.0338(6) 0.7408(6) 0.8995(4) 0.0318(15) Uani 1 1 d . . . H21 H 0.0515 0.7370 0.9550 0.038 Uiso 1 1 calc R . . C22 C -0.2529(6) 0.8210(6) 0.7926(4) 0.0290(14) Uani 1 1 d . . . C23 C -0.3314(6) 0.7309(7) 0.7119(4) 0.0354(16) Uani 1 1 d . . . H23 H -0.3022 0.7266 0.6601 0.042 Uiso 1 1 calc R . . C24 C -0.4535(6) 0.6479(6) 0.7102(4) 0.0299(14) Uani 1 1 d . . . H24 H -0.5076 0.5884 0.6565 0.036 Uiso 1 1 calc R . . C25 C -0.4962(6) 0.6521(6) 0.7871(4) 0.0298(14) Uani 1 1 d . . . C26 C -0.4159(6) 0.7441(6) 0.8668(4) 0.0330(15) Uani 1 1 d . . . H26 H -0.4451 0.7489 0.9186 0.040 Uiso 1 1 calc R . . C27 C -0.2953(6) 0.8269(7) 0.8702(4) 0.0386(17) Uani 1 1 d . . . H27 H -0.2419 0.8869 0.9239 0.046 Uiso 1 1 calc R . . C28 C -0.6284(6) 0.5579(6) 0.7864(4) 0.0286(14) Uani 1 1 d . . . C29 C 0.0745(6) 0.7443(6) 1.1657(4) 0.0255(13) Uani 1 1 d . . . C30 C 0.2078(5) 0.8398(6) 1.1716(4) 0.0239(13) Uani 1 1 d . . . C31 C 0.2800(6) 0.9343(6) 1.2506(4) 0.0335(15) Uani 1 1 d . . . H31 H 0.2457 0.9390 1.3001 0.040 Uiso 1 1 calc R . . C32 C 0.4020(6) 1.0221(6) 1.2580(4) 0.0320(15) Uani 1 1 d . . . H32 H 0.4506 1.0851 1.3121 0.038 Uiso 1 1 calc R . . C33 C 0.4513(5) 1.0154(5) 1.1835(3) 0.0213(12) Uani 1 1 d . . . C34 C 0.3802(6) 0.9218(6) 1.1030(4) 0.0300(14) Uani 1 1 d . . . H34 H 0.4142 0.9179 1.0533 0.036 Uiso 1 1 calc R . . C35 C 0.2578(6) 0.8340(6) 1.0972(4) 0.0302(14) Uani 1 1 d . . . H35 H 0.2089 0.7709 1.0432 0.036 Uiso 1 1 calc R . . C36 C 0.6777(6) 1.0311(6) 1.1953(4) 0.0281(14) Uani 1 1 d . . . C37 C 0.7204(7) 1.0334(7) 1.2769(4) 0.0383(17) Uani 1 1 d . . . H37 H 0.7216 1.0887 1.3286 0.046 Uiso 1 1 calc R . . C38 C 0.7614(7) 0.9525(7) 1.2810(4) 0.0396(18) Uani 1 1 d . . . H38 H 0.7897 0.9530 1.3358 0.047 Uiso 1 1 calc R . . C39 C 0.7606(6) 0.8712(6) 1.2042(4) 0.0300(14) Uani 1 1 d . . . C40 C 0.7215(7) 0.8729(7) 1.1244(4) 0.0395(17) Uani 1 1 d . . . H40 H 0.7223 0.8188 1.0729 0.047 Uiso 1 1 calc R . . C41 C 0.6801(7) 0.9539(7) 1.1179(4) 0.0398(18) Uani 1 1 d . . . H41 H 0.6550 0.9556 1.0631 0.048 Uiso 1 1 calc R . . C42 C 0.7973(6) 0.7797(6) 1.2107(5) 0.0396(17) 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 0.0173(6) 0.0276(8) 0.0259(6) 0.0083(5) 0.0034(5) 0.0129(6) Mn2 0.0191(5) 0.0251(5) 0.0226(4) 0.0077(4) 0.0036(4) 0.0121(4) Mn3 0.0189(5) 0.0235(5) 0.0264(4) 0.0100(4) 0.0035(4) 0.0098(4) Cs1 0.0404(3) 0.0420(3) 0.0556(3) 0.0281(2) 0.0018(2) 0.0049(2) S1 0.0340(10) 0.0321(10) 0.0261(8) 0.0126(7) -0.0024(7) 0.0011(8) S2 0.0181(7) 0.0224(8) 0.0387(8) 0.0133(7) 0.0058(7) 0.0094(7) S3 0.0181(8) 0.0289(10) 0.0644(11) 0.0267(9) 0.0089(8) 0.0119(8) O1 0.022(2) 0.039(3) 0.039(2) 0.014(2) -0.005(2) 0.013(2) O2 0.020(2) 0.024(2) 0.033(2) 0.0089(19) 0.0036(19) 0.010(2) O3 0.024(2) 0.025(2) 0.036(2) 0.0143(19) 0.0064(19) 0.014(2) O4 0.039(3) 0.030(3) 0.072(3) 0.012(3) 0.009(3) 0.022(3) O5 0.033(3) 0.076(4) 0.030(2) 0.011(2) 0.004(2) 0.035(3) O6 0.025(2) 0.042(3) 0.044(3) 0.024(2) 0.015(2) 0.012(2) O7 0.024(2) 0.030(3) 0.028(2) 0.0096(19) -0.0011(19) 0.001(2) O8 0.038(3) 0.032(3) 0.040(2) 0.010(2) 0.008(2) 0.025(2) O9 0.025(2) 0.031(3) 0.034(2) 0.014(2) 0.013(2) 0.006(2) O10 0.051(3) 0.050(3) 0.063(3) 0.036(3) 0.024(3) 0.037(3) O11 0.021(2) 0.033(3) 0.045(3) 0.010(2) 0.006(2) 0.008(2) O12 0.051(4) 0.048(4) 0.114(5) 0.051(4) -0.023(4) 0.002(3) O13 0.042(3) 0.056(4) 0.031(2) 0.016(2) 0.003(2) -0.005(3) O14 0.062(4) 0.033(3) 0.049(3) 0.018(2) -0.016(3) 0.013(3) O15 0.027(3) 0.025(3) 0.090(4) 0.018(3) 0.005(3) 0.013(2) O16 0.030(3) 0.059(4) 0.080(3) 0.054(3) 0.021(3) 0.023(3) O17 0.024(2) 0.028(3) 0.052(3) 0.007(2) 0.002(2) 0.010(2) O18 0.032(3) 0.040(3) 0.055(3) 0.032(2) 0.019(2) 0.020(2) C1 0.025(3) 0.024(3) 0.025(3) 0.009(3) -0.004(3) 0.005(3) C2 0.023(3) 0.028(4) 0.026(3) 0.012(3) 0.000(3) 0.012(3) C3 0.021(3) 0.046(4) 0.035(3) 0.007(3) 0.002(3) 0.017(3) C4 0.031(4) 0.038(4) 0.032(3) 0.010(3) 0.007(3) 0.014(4) C5 0.026(3) 0.023(4) 0.026(3) 0.008(3) -0.002(3) 0.003(3) C6 0.028(4) 0.047(4) 0.028(3) 0.011(3) 0.001(3) 0.020(4) C7 0.031(4) 0.050(5) 0.023(3) 0.008(3) 0.001(3) 0.022(4) C8 0.024(3) 0.033(4) 0.021(3) 0.007(3) 0.000(3) 0.005(3) C9 0.020(3) 0.036(4) 0.043(4) 0.010(3) -0.001(3) 0.011(3) C10 0.031(4) 0.033(4) 0.046(4) 0.010(3) -0.004(3) 0.017(3) C11 0.029(3) 0.024(4) 0.026(3) 0.007(3) 0.001(3) 0.006(3) C12 0.022(3) 0.041(4) 0.033(3) 0.012(3) -0.005(3) 0.011(3) C13 0.038(4) 0.028(4) 0.038(3) 0.011(3) -0.005(3) 0.014(3) C14 0.036(4) 0.034(4) 0.026(3) 0.008(3) -0.001(3) 0.015(4) C15 0.017(3) 0.025(3) 0.036(3) 0.016(3) 0.008(3) 0.010(3) C16 0.020(3) 0.030(4) 0.047(4) 0.024(3) 0.014(3) 0.014(3) C17 0.037(4) 0.046(5) 0.041(4) 0.024(3) 0.019(3) 0.027(4) C18 0.038(4) 0.049(5) 0.045(4) 0.026(3) 0.015(3) 0.031(4) C19 0.017(3) 0.030(4) 0.050(4) 0.022(3) 0.006(3) 0.013(3) C20 0.039(4) 0.040(4) 0.042(4) 0.014(3) 0.007(3) 0.027(4) C21 0.035(4) 0.032(4) 0.031(3) 0.011(3) 0.000(3) 0.021(3) C22 0.018(3) 0.027(4) 0.048(4) 0.020(3) 0.009(3) 0.012(3) C23 0.028(4) 0.048(5) 0.037(3) 0.026(3) 0.016(3) 0.018(4) C24 0.022(3) 0.032(4) 0.030(3) 0.013(3) 0.006(3) 0.009(3) C25 0.018(3) 0.028(4) 0.043(4) 0.016(3) 0.000(3) 0.010(3) C26 0.024(3) 0.039(4) 0.030(3) 0.013(3) 0.008(3) 0.012(3) C27 0.020(3) 0.039(4) 0.039(4) 0.009(3) -0.005(3) 0.006(3) C28 0.022(3) 0.024(4) 0.045(4) 0.018(3) 0.008(3) 0.013(3) C29 0.021(3) 0.018(3) 0.037(3) 0.011(3) 0.003(3) 0.010(3) C30 0.020(3) 0.018(3) 0.031(3) 0.009(3) 0.005(3) 0.007(3) C31 0.025(3) 0.035(4) 0.039(4) 0.014(3) 0.012(3) 0.014(3) C32 0.025(3) 0.029(4) 0.032(3) 0.003(3) 0.000(3) 0.011(3) C33 0.021(3) 0.020(3) 0.027(3) 0.010(2) 0.004(3) 0.013(3) C34 0.025(3) 0.030(4) 0.033(3) 0.015(3) 0.015(3) 0.010(3) C35 0.023(3) 0.031(4) 0.029(3) 0.009(3) 0.006(3) 0.009(3) C36 0.023(3) 0.020(3) 0.038(3) 0.006(3) 0.003(3) 0.010(3) C37 0.055(5) 0.046(5) 0.030(3) 0.014(3) 0.014(3) 0.036(4) C38 0.053(5) 0.044(5) 0.037(3) 0.017(3) 0.006(3) 0.035(4) C39 0.024(3) 0.031(4) 0.041(3) 0.018(3) 0.011(3) 0.015(3) C40 0.048(5) 0.040(4) 0.040(4) 0.011(3) 0.013(3) 0.031(4) C41 0.051(5) 0.051(5) 0.034(3) 0.013(3) 0.005(3) 0.039(4) C42 0.029(4) 0.025(4) 0.071(5) 0.021(4) 0.021(4) 0.016(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 2.077(4) 2_567 ? Mn1 O1 2.077(4) . ? Mn1 O2 2.220(4) 2_567 ? Mn1 O2 2.220(4) . ? Mn1 O3 2.244(4) . ? Mn1 O3 2.244(4) 2_567 ? Mn1 Mn2 3.1703(9) 2_567 ? Mn1 Mn2 3.1703(9) . ? Mn2 O4 2.051(5) 1_455 ? Mn2 O5 2.053(4) . ? Mn2 O6 2.067(5) 2_467 ? Mn2 O3 2.230(4) 2_567 ? Mn2 O2 2.258(4) . ? Mn2 Mn3 3.0725(11) 1_666 ? Mn3 O7 2.035(4) . ? Mn3 O10 2.078(4) 1_344 ? Mn3 O11 2.117(5) 2_356 ? Mn3 O9 2.118(4) 1_444 ? Mn3 O8 2.167(4) 2_456 ? Mn3 Mn2 3.0725(11) 1_444 ? Mn3 Cs1 3.8324(10) 1_445 ? Cs1 O17 2.973(4) 1_444 ? Cs1 O12 2.998(5) 2_456 ? Cs1 O7 3.004(4) 1_665 ? Cs1 O13 3.014(5) . ? Cs1 O11 3.097(4) 2_466 ? Cs1 O12 3.448(6) 1_665 ? Cs1 C14 3.626(7) 1_665 ? Cs1 O8 3.709(4) 2_566 ? Cs1 Mn3 3.8324(10) 1_665 ? Cs1 Cs1 4.9326(10) 2_566 ? S1 O13 1.432(5) . ? S1 O14 1.434(5) . ? S1 C8 1.749(7) . ? S1 C5 1.781(6) . ? S2 O18 1.433(4) . ? S2 O17 1.442(4) . ? S2 C36 1.759(6) . ? S2 C33 1.766(6) . ? S3 O16 1.424(5) . ? S3 O15 1.437(5) . ? S3 C22 1.767(6) . ? S3 C19 1.792(6) . ? O1 C1 1.273(7) . ? O2 C29 1.290(7) . ? O3 C15 1.270(6) . ? O3 Mn2 2.230(4) 2_567 ? O4 C42 1.278(8) . ? O4 Mn2 2.051(4) 1_655 ? O5 C1 1.206(7) . ? O6 C28 1.238(7) . ? O6 Mn2 2.067(5) 2_467 ? O7 C14 1.269(7) . ? O7 Cs1 3.004(4) 1_445 ? O8 C15 1.246(7) . ? O8 Mn3 2.167(4) 2_456 ? O8 Cs1 3.709(4) 2_566 ? O9 C29 1.245(7) . ? O9 Mn3 2.118(4) 1_666 ? O10 C42 1.246(8) . ? O10 Mn3 2.078(4) 1_766 ? O11 C28 1.256(7) . ? O11 Mn3 2.117(5) 2_356 ? O11 Cs1 3.097(4) 2_466 ? O12 C14 1.243(8) . ? O12 Cs1 2.998(5) 2_456 ? O12 Cs1 3.448(6) 1_445 ? O17 Cs1 2.973(4) 1_666 ? C1 C2 1.517(7) . ? C2 C3 1.369(8) . ? C2 C7 1.387(8) . ? C3 C4 1.379(8) . ? C4 C5 1.367(9) . ? C5 C6 1.384(9) . ? C6 C7 1.397(8) . ? C8 C9 1.385(9) . ? C8 C13 1.393(9) . ? C9 C10 1.353(9) . ? C10 C11 1.392(9) . ? C11 C12 1.400(9) . ? C11 C14 1.479(9) . ? C12 C13 1.363(9) . ? C14 Cs1 3.626(7) 1_445 ? C15 C16 1.503(8) . ? C16 C21 1.385(8) . ? C16 C17 1.386(8) . ? C17 C18 1.397(8) . ? C18 C19 1.353(9) . ? C19 C20 1.383(8) . ? C20 C21 1.368(8) . ? C22 C27 1.384(9) . ? C22 C23 1.391(9) . ? C23 C24 1.379(9) . ? C24 C25 1.378(8) . ? C25 C26 1.391(8) . ? C25 C28 1.513(9) . ? C26 C27 1.358(9) . ? C29 C30 1.507(8) . ? C30 C31 1.370(8) . ? C30 C35 1.387(8) . ? C31 C32 1.373(9) . ? C32 C33 1.384(8) . ? C33 C34 1.381(8) . ? C34 C35 1.382(9) . ? C36 C41 1.378(8) . ? C36 C37 1.379(8) . ? C37 C38 1.383(8) . ? C38 C39 1.382(9) . ? C39 C40 1.360(8) . ? C39 C42 1.485(8) . ? C40 C41 1.397(8) . ? 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 180.0(0) 2_567 . ? O1 Mn1 O2 93.24(15) 2_567 2_567 ? O1 Mn1 O2 86.76(15) . 2_567 ? O1 Mn1 O2 86.76(15) 2_567 . ? O1 Mn1 O2 93.24(15) . . ? O2 Mn1 O2 180.0(0) 2_567 . ? O1 Mn1 O3 94.24(16) 2_567 . ? O1 Mn1 O3 85.76(16) . . ? O2 Mn1 O3 76.56(15) 2_567 . ? O2 Mn1 O3 103.44(15) . . ? O1 Mn1 O3 85.76(16) 2_567 2_567 ? O1 Mn1 O3 94.24(16) . 2_567 ? O2 Mn1 O3 103.44(15) 2_567 2_567 ? O2 Mn1 O3 76.56(15) . 2_567 ? O3 Mn1 O3 180.0(0) . 2_567 ? O1 Mn1 Mn2 68.91(12) 2_567 2_567 ? O1 Mn1 Mn2 111.09(12) . 2_567 ? O2 Mn1 Mn2 45.41(11) 2_567 2_567 ? O2 Mn1 Mn2 134.59(11) . 2_567 ? O3 Mn1 Mn2 44.71(9) . 2_567 ? O3 Mn1 Mn2 135.29(9) 2_567 2_567 ? O1 Mn1 Mn2 111.09(12) 2_567 . ? O1 Mn1 Mn2 68.91(12) . . ? O2 Mn1 Mn2 134.59(11) 2_567 . ? O2 Mn1 Mn2 45.41(11) . . ? O3 Mn1 Mn2 135.29(9) . . ? O3 Mn1 Mn2 44.71(9) 2_567 . ? Mn2 Mn1 Mn2 180.0(0) 2_567 . ? O4 Mn2 O5 100.9(2) 1_455 . ? O4 Mn2 O6 92.7(2) 1_455 2_467 ? O5 Mn2 O6 99.07(19) . 2_467 ? O4 Mn2 O3 153.71(17) 1_455 2_567 ? O5 Mn2 O3 104.09(17) . 2_567 ? O6 Mn2 O3 91.48(17) 2_467 2_567 ? O4 Mn2 O2 89.23(18) 1_455 . ? O5 Mn2 O2 106.02(18) . . ? O6 Mn2 O2 154.00(15) 2_467 . ? O3 Mn2 O2 76.08(15) 2_567 . ? O4 Mn2 Mn3 70.15(14) 1_455 1_666 ? O5 Mn2 Mn3 165.85(13) . 1_666 ? O6 Mn2 Mn3 71.18(12) 2_467 1_666 ? O3 Mn2 Mn3 86.76(10) 2_567 1_666 ? O2 Mn2 Mn3 85.20(10) . 1_666 ? O4 Mn2 Mn1 131.54(15) 1_455 . ? O5 Mn2 Mn1 83.64(13) . . ? O6 Mn2 Mn1 134.67(13) 2_467 . ? O3 Mn2 Mn1 45.06(11) 2_567 . ? O2 Mn2 Mn1 44.45(10) . . ? Mn3 Mn2 Mn1 110.51(3) 1_666 . ? O7 Mn3 O10 107.37(19) . 1_344 ? O7 Mn3 O11 97.74(17) . 2_356 ? O10 Mn3 O11 90.75(19) 1_344 2_356 ? O7 Mn3 O9 105.18(17) . 1_444 ? O10 Mn3 O9 90.18(18) 1_344 1_444 ? O11 Mn3 O9 155.64(17) 2_356 1_444 ? O7 Mn3 O8 97.89(16) . 2_456 ? O10 Mn3 O8 154.70(18) 1_344 2_456 ? O11 Mn3 O8 84.41(17) 2_356 2_456 ? O9 Mn3 O8 84.41(17) 1_444 2_456 ? O7 Mn3 Mn2 166.88(13) . 1_444 ? O10 Mn3 Mn2 85.46(14) 1_344 1_444 ? O11 Mn3 Mn2 84.54(12) 2_356 1_444 ? O9 Mn3 Mn2 71.27(11) 1_444 1_444 ? O8 Mn3 Mn2 69.38(11) 2_456 1_444 ? O7 Mn3 Cs1 51.05(13) . 1_445 ? O10 Mn3 Cs1 125.59(14) 1_344 1_445 ? O11 Mn3 Cs1 53.83(12) 2_356 1_445 ? O9 Mn3 Cs1 139.71(12) 1_444 1_445 ? O8 Mn3 Cs1 70.21(12) 2_456 1_445 ? Mn2 Mn3 Cs1 123.57(3) 1_444 1_445 ? O17 Cs1 O12 88.88(15) 1_444 2_456 ? O17 Cs1 O7 118.12(12) 1_444 1_665 ? O12 Cs1 O7 119.29(14) 2_456 1_665 ? O17 Cs1 O13 74.05(13) 1_444 . ? O12 Cs1 O13 90.62(16) 2_456 . ? O7 Cs1 O13 146.41(14) 1_665 . ? O17 Cs1 O11 70.08(12) 1_444 2_466 ? O12 Cs1 O11 153.14(16) 2_456 2_466 ? O7 Cs1 O11 61.67(11) 1_665 2_466 ? O13 Cs1 O11 99.00(12) . 2_466 ? O17 Cs1 O12 125.81(15) 1_444 1_665 ? O12 Cs1 O12 80.38(15) 2_456 1_665 ? O7 Cs1 O12 39.17(11) 1_665 1_665 ? O13 Cs1 O12 157.54(14) . 1_665 ? O11 Cs1 O12 98.18(12) 2_466 1_665 ? O17 Cs1 C14 125.72(13) 1_444 1_665 ? O12 Cs1 C14 100.40(15) 2_456 1_665 ? O7 Cs1 C14 19.28(11) 1_665 1_665 ? O13 Cs1 C14 157.08(15) . 1_665 ? O11 Cs1 C14 80.11(13) 2_466 1_665 ? O12 Cs1 C14 20.03(12) 1_665 1_665 ? O17 Cs1 O8 64.45(11) 1_444 2_566 ? O12 Cs1 O8 107.32(15) 2_456 2_566 ? O7 Cs1 O8 55.14(10) 1_665 2_566 ? O13 Cs1 O8 133.82(11) . 2_566 ? O11 Cs1 O8 49.02(10) 2_466 2_566 ? O12 Cs1 O8 68.64(13) 1_665 2_566 ? C14 Cs1 O8 61.72(12) 1_665 2_566 ? O17 Cs1 Mn3 88.20(9) 1_444 1_665 ? O12 Cs1 Mn3 134.06(13) 2_456 1_665 ? O7 Cs1 Mn3 31.79(7) 1_665 1_665 ? O13 Cs1 Mn3 132.04(10) . 1_665 ? O11 Cs1 Mn3 33.50(8) 2_466 1_665 ? O12 Cs1 Mn3 64.87(9) 1_665 1_665 ? C14 Cs1 Mn3 48.02(9) 1_665 1_665 ? O8 Cs1 Mn3 33.34(6) 2_566 1_665 ? O17 Cs1 Cs1 113.40(8) 1_444 2_566 ? O12 Cs1 Cs1 43.57(11) 2_456 2_566 ? O7 Cs1 Cs1 75.84(8) 1_665 2_566 ? O13 Cs1 Cs1 130.74(10) . 2_566 ? O11 Cs1 Cs1 129.91(8) 2_466 2_566 ? O12 Cs1 Cs1 36.81(8) 1_665 2_566 ? C14 Cs1 Cs1 56.84(10) 1_665 2_566 ? O8 Cs1 Cs1 85.77(6) 2_566 2_566 ? Mn3 Cs1 Cs1 97.23(2) 1_665 2_566 ? O13 S1 O14 118.7(3) . . ? O13 S1 C8 107.6(3) . . ? O14 S1 C8 109.1(3) . . ? O13 S1 C5 106.8(3) . . ? O14 S1 C5 109.9(3) . . ? C8 S1 C5 103.7(3) . . ? O18 S2 O17 119.1(3) . . ? O18 S2 C36 108.7(3) . . ? O17 S2 C36 108.3(3) . . ? O18 S2 C33 108.9(3) . . ? O17 S2 C33 108.5(3) . . ? C36 S2 C33 102.0(3) . . ? O16 S3 O15 119.8(3) . . ? O16 S3 C22 108.9(3) . . ? O15 S3 C22 108.3(3) . . ? O16 S3 C19 108.3(3) . . ? O15 S3 C19 108.9(3) . . ? C22 S3 C19 101.0(3) . . ? C1 O1 Mn1 140.3(4) . . ? C29 O2 Mn1 129.0(3) . . ? C29 O2 Mn2 116.0(4) . . ? Mn1 O2 Mn2 90.13(15) . . ? C15 O3 Mn2 115.2(4) . 2_567 ? C15 O3 Mn1 129.2(4) . . ? Mn2 O3 Mn1 90.24(14) 2_567 . ? C42 O4 Mn2 140.4(5) . 1_655 ? C1 O5 Mn2 121.7(4) . . ? C28 O6 Mn2 140.4(4) . 2_467 ? C14 O7 Mn3 132.6(4) . . ? C14 O7 Cs1 109.3(4) . 1_445 ? Mn3 O7 Cs1 97.16(15) . 1_445 ? C15 O8 Mn3 143.0(4) . 2_456 ? C15 O8 Cs1 135.9(4) . 2_566 ? Mn3 O8 Cs1 76.44(12) 2_456 2_566 ? C29 O9 Mn3 143.6(4) . 1_666 ? C42 O10 Mn3 118.9(4) . 1_766 ? C28 O11 Mn3 118.8(4) . 2_356 ? C28 O11 Cs1 127.8(4) . 2_466 ? Mn3 O11 Cs1 92.68(14) 2_356 2_466 ? C14 O12 Cs1 172.2(5) . 2_456 ? C14 O12 Cs1 88.1(4) . 1_445 ? Cs1 O12 Cs1 99.62(15) 2_456 1_445 ? S1 O13 Cs1 142.0(3) . . ? S2 O17 Cs1 172.5(3) . 1_666 ? O5 C1 O1 125.1(5) . . ? O5 C1 C2 119.4(6) . . ? O1 C1 C2 115.5(6) . . ? C3 C2 C7 120.9(5) . . ? C3 C2 C1 121.2(5) . . ? C7 C2 C1 118.0(6) . . ? C2 C3 C4 120.1(6) . . ? C5 C4 C3 118.9(6) . . ? C4 C5 C6 122.7(5) . . ? C4 C5 S1 119.1(5) . . ? C6 C5 S1 118.2(5) . . ? C5 C6 C7 117.7(6) . . ? C2 C7 C6 119.7(6) . . ? C9 C8 C13 119.3(6) . . ? C9 C8 S1 120.0(5) . . ? C13 C8 S1 120.7(5) . . ? C10 C9 C8 120.6(6) . . ? C9 C10 C11 121.5(6) . . ? C10 C11 C12 117.4(6) . . ? C10 C11 C14 121.2(6) . . ? C12 C11 C14 121.4(6) . . ? C13 C12 C11 121.6(6) . . ? C12 C13 C8 119.6(6) . . ? O12 C14 O7 122.6(7) . . ? O12 C14 C11 119.6(6) . . ? O7 C14 C11 117.8(6) . . ? O12 C14 Cs1 71.9(4) . 1_445 ? O7 C14 Cs1 51.4(3) . 1_445 ? C11 C14 Cs1 166.3(4) . 1_445 ? O8 C15 O3 123.6(5) . . ? O8 C15 C16 117.4(5) . . ? O3 C15 C16 119.0(5) . . ? C21 C16 C17 119.0(5) . . ? C21 C16 C15 122.1(5) . . ? C17 C16 C15 118.9(6) . . ? C16 C17 C18 120.1(6) . . ? C19 C18 C17 118.8(6) . . ? C18 C19 C20 122.3(6) . . ? C18 C19 S3 119.3(5) . . ? C20 C19 S3 118.4(5) . . ? C21 C20 C19 118.4(6) . . ? C20 C21 C16 121.3(6) . . ? C27 C22 C23 121.0(6) . . ? C27 C22 S3 119.9(5) . . ? C23 C22 S3 118.9(5) . . ? C24 C23 C22 118.6(6) . . ? C25 C24 C23 120.8(6) . . ? C24 C25 C26 119.3(6) . . ? C24 C25 C28 121.1(6) . . ? C26 C25 C28 119.6(6) . . ? C27 C26 C25 121.0(6) . . ? C26 C27 C22 119.3(6) . . ? O6 C28 O11 124.9(6) . . ? O6 C28 C25 117.2(6) . . ? O11 C28 C25 117.8(6) . . ? O9 C29 O2 123.0(6) . . ? O9 C29 C30 117.4(5) . . ? O2 C29 C30 119.5(5) . . ? C31 C30 C35 119.6(6) . . ? C31 C30 C29 120.0(6) . . ? C35 C30 C29 120.4(5) . . ? C30 C31 C32 121.2(6) . . ? C31 C32 C33 118.9(6) . . ? C34 C33 C32 121.0(6) . . ? C34 C33 S2 118.2(5) . . ? C32 C33 S2 120.7(5) . . ? C33 C34 C35 119.2(6) . . ? C34 C35 C30 120.2(6) . . ? C41 C36 C37 121.4(6) . . ? C41 C36 S2 119.7(5) . . ? C37 C36 S2 118.8(5) . . ? C36 C37 C38 119.3(6) . . ? C39 C38 C37 120.3(6) . . ? C40 C39 C38 119.5(6) . . ? C40 C39 C42 121.5(6) . . ? C38 C39 C42 119.0(6) . . ? C39 C40 C41 121.7(6) . . ? C36 C41 C40 117.8(6) . . ? O10 C42 O4 124.0(6) . . ? O10 C42 C39 120.1(6) . . ? O4 C42 C39 115.9(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.790 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.120 ######END####### data_Compound(4) _database_code_depnum_ccdc_archive 'CCDC 834725' #TrackingRef '- all compounds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Manganese Sulfonyldibenzoate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H60 Mn5 N2 O38 S6' _chemical_formula_weight 2172.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7609(6) _cell_length_b 12.7682(6) _cell_length_c 16.0315(7) _cell_angle_alpha 87.646(4) _cell_angle_beta 72.508(4) _cell_angle_gamma 60.477(5) _cell_volume 2149.71(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1099 _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.823 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16202 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8362 _reflns_number_gt 6027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 1990)' _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. DFIX and DANG restarints were adopted to fix the hydrogens on the Nitrogen and in order to model the ammonium ion properly. ; _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^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8362 _refine_ls_number_parameters 626 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.5000 0.5000 0.02226(16) Uani 1 2 d S . . Mn2 Mn 0.54319(4) 0.25865(4) 0.41249(3) 0.02169(12) Uani 1 1 d . . . Mn3 Mn 0.64718(4) 0.23515(4) 0.21056(3) 0.02183(12) Uani 1 1 d . . . S1 S 0.07756(8) 0.01329(7) 0.29621(7) 0.0345(2) Uani 1 1 d . . . S2 S 1.11891(7) 0.49597(7) 0.31185(5) 0.02393(18) Uani 1 1 d . . . S3 S 1.28124(8) 0.20477(8) -0.02632(5) 0.0328(2) Uani 1 1 d . . . O1 O 1.4551(2) 0.3979(2) -0.40787(15) 0.0357(6) Uani 1 1 d . . . O2 O 0.66855(19) 0.33565(18) 0.41330(14) 0.0257(5) Uani 1 1 d . . . O3 O 0.42344(19) -0.54353(17) 0.40585(14) 0.0251(5) Uani 1 1 d . . . O4 O 0.7013(2) 1.0898(2) 0.36850(18) 0.0476(7) Uani 1 1 d . . . O5 O 0.4459(2) 0.2185(2) 0.34992(16) 0.0418(6) Uani 1 1 d . . . O6 O 1.4707(3) 0.2325(2) -0.46029(15) 0.0509(7) Uani 1 1 d . . . O7 O 0.7055(2) 0.2545(2) 0.08018(14) 0.0344(6) Uani 1 1 d . . . O8 O 0.7669(2) 1.0544(2) 0.22227(18) 0.0460(7) Uani 1 1 d . . . O9 O 0.7446(2) 0.2915(2) 0.26709(14) 0.0342(6) Uani 1 1 d . . . O10 O 0.5085(2) 0.1931(2) 0.20341(16) 0.0385(6) Uani 1 1 d . . . O11 O 0.4892(2) -0.58126(19) 0.25953(15) 0.0332(5) Uani 1 1 d . . . O12 O 0.6670(3) 0.4214(3) 0.0190(2) 0.0688(9) Uani 1 1 d . . . O13 O 0.0561(2) 0.0189(2) 0.21300(18) 0.0491(7) Uani 1 1 d . . . O14 O -0.0280(2) 0.0691(2) 0.37623(18) 0.0498(7) Uani 1 1 d . . . O15 O 1.1503(2) 0.48014(19) 0.39187(15) 0.0349(6) Uani 1 1 d . . . O16 O 1.2192(2) 0.44357(19) 0.22877(15) 0.0337(5) Uani 1 1 d . . . O17 O 1.2735(2) 0.2941(2) 0.03058(14) 0.0454(7) Uani 1 1 d . . . O18 O 1.3587(2) 0.0789(2) -0.01978(16) 0.0473(7) Uani 1 1 d . . . O19 O 1.3922(4) -0.1522(3) 0.0208(2) 0.0965(12) Uani 1 1 d . . . N1 N 0.4311(3) 0.3846(3) 0.0765(2) 0.0411(8) Uani 1 1 d D . . C1 C 0.4404(3) 0.1910(3) 0.2778(2) 0.0305(8) Uani 1 1 d . . . C2 C 0.3453(3) 0.1525(3) 0.2821(2) 0.0246(7) Uani 1 1 d . . . C3 C 0.3451(3) 0.1061(3) 0.2058(2) 0.0349(8) Uani 1 1 d . . . H3 H 0.4011 0.1023 0.1515 0.042 Uiso 1 1 calc R . . C4 C 0.2618(3) 0.0653(3) 0.2102(2) 0.0357(9) Uani 1 1 d . . . H4 H 0.2619 0.0332 0.1592 0.043 Uiso 1 1 calc R . . C5 C 0.1791(3) 0.0725(3) 0.2902(2) 0.0281(8) Uani 1 1 d . . . C6 C 0.1753(3) 0.1214(3) 0.3670(2) 0.0371(9) Uani 1 1 d . . . H6 H 0.1170 0.1277 0.4209 0.044 Uiso 1 1 calc R . . C7 C 0.2599(3) 0.1604(3) 0.3620(2) 0.0367(9) Uani 1 1 d . . . H7 H 0.2594 0.1927 0.4132 0.044 Uiso 1 1 calc R . . C8 C 0.1751(3) -0.1413(3) 0.3069(2) 0.0287(8) Uani 1 1 d . . . C9 C 0.2525(3) -0.2238(3) 0.2321(2) 0.0371(9) Uani 1 1 d . . . H9 H 0.2514 -0.1996 0.1767 0.045 Uiso 1 1 calc R . . C10 C 0.3323(3) -0.3437(3) 0.2404(2) 0.0361(8) Uani 1 1 d . . . H10 H 0.3852 -0.4000 0.1901 0.043 Uiso 1 1 calc R . . C11 C 0.3339(3) -0.3802(3) 0.3227(2) 0.0224(7) Uani 1 1 d . . . C12 C 0.2560(3) -0.2946(3) 0.3963(2) 0.0325(8) Uani 1 1 d . . . H12 H 0.2574 -0.3178 0.4518 0.039 Uiso 1 1 calc R . . C13 C 0.1756(3) -0.1749(3) 0.3890(2) 0.0362(8) Uani 1 1 d . . . H13 H 0.1229 -0.1182 0.4391 0.043 Uiso 1 1 calc R . . C14 C 0.4218(3) -0.5108(3) 0.3292(2) 0.0249(7) Uani 1 1 d . . . C15 C 0.7443(3) 0.3289(3) 0.3373(2) 0.0258(7) Uani 1 1 d . . . C16 C 0.8393(3) 0.3684(3) 0.3318(2) 0.0223(7) Uani 1 1 d . . . C17 C 0.8354(3) 0.4257(3) 0.4053(2) 0.0290(7) Uani 1 1 d . . . H17 H 0.7738 0.4395 0.4593 0.035 Uiso 1 1 calc R . . C18 C 0.9228(3) 0.4622(3) 0.3986(2) 0.0306(8) Uani 1 1 d . . . H18 H 0.9204 0.5001 0.4480 0.037 Uiso 1 1 calc R . . C19 C 1.0131(3) 0.4424(3) 0.3187(2) 0.0231(7) Uani 1 1 d . . . C20 C 1.0193(3) 0.3851(3) 0.2443(2) 0.0300(8) Uani 1 1 d . . . H20 H 1.0811 0.3712 0.1904 0.036 Uiso 1 1 calc R . . C21 C 0.9308(3) 0.3488(3) 0.2523(2) 0.0297(8) Uani 1 1 d . . . H21 H 0.9334 0.3105 0.2030 0.036 Uiso 1 1 calc R . . C22 C 1.0241(3) 0.6524(3) 0.3082(2) 0.0234(7) Uani 1 1 d . . . C23 C 0.9462(4) 0.7302(3) 0.3849(2) 0.0408(9) Uani 1 1 d . . . H23 H 0.9481 0.7022 0.4392 0.049 Uiso 1 1 calc R . . C24 C 0.8650(4) 0.8505(3) 0.3807(2) 0.0439(9) Uani 1 1 d . . . H24 H 0.8110 0.9035 0.4325 0.053 Uiso 1 1 calc R . . C25 C 0.8633(3) 0.8926(3) 0.3003(2) 0.0281(7) Uani 1 1 d . . . C26 C 0.9454(3) 0.8141(3) 0.2240(2) 0.0401(9) Uani 1 1 d . . . H26 H 0.9464 0.8423 0.1695 0.048 Uiso 1 1 calc R . . C27 C 1.0261(3) 0.6938(3) 0.2282(2) 0.0374(8) Uani 1 1 d . . . H27 H 1.0819 0.6409 0.1766 0.045 Uiso 1 1 calc R . . C28 C 0.7708(3) 1.0230(3) 0.2964(3) 0.0353(9) Uani 1 1 d . . . C29 C 0.7398(3) 0.3270(3) 0.0418(2) 0.0333(8) Uani 1 1 d . . . C30 C 0.8753(3) 0.2942(3) 0.0247(2) 0.0263(7) Uani 1 1 d . . . C31 C 0.9628(3) 0.1835(3) 0.0412(2) 0.0340(8) Uani 1 1 d . . . H31 H 0.9372 0.1287 0.0641 0.041 Uiso 1 1 calc R . . C32 C 1.0874(3) 0.1531(3) 0.0242(2) 0.0338(8) Uani 1 1 d . . . H32 H 1.1460 0.0777 0.0346 0.041 Uiso 1 1 calc R . . C33 C 1.1245(3) 0.2357(3) -0.0084(2) 0.0275(7) Uani 1 1 d . . . C34 C 1.0378(3) 0.3476(3) -0.0247(2) 0.0344(8) Uani 1 1 d . . . H34 H 1.0635 0.4027 -0.0467 0.041 Uiso 1 1 calc R . . C35 C 0.9134(3) 0.3772(3) -0.0083(2) 0.0311(8) Uani 1 1 d . . . H35 H 0.8550 0.4522 -0.0192 0.037 Uiso 1 1 calc R . . C36 C 1.3314(3) 0.2316(3) -0.1362(2) 0.0274(7) Uani 1 1 d . . . C37 C 1.3416(3) 0.3337(3) -0.1506(2) 0.0362(8) Uani 1 1 d . . . H37 H 1.3250 0.3858 -0.1035 0.043 Uiso 1 1 calc R . . C38 C 1.3769(3) 0.3574(3) -0.2362(2) 0.0351(8) Uani 1 1 d . . . H38 H 1.3818 0.4274 -0.2466 0.042 Uiso 1 1 calc R . . C39 C 1.4050(3) 0.2787(3) -0.3063(2) 0.0265(7) Uani 1 1 d . . . C40 C 1.3944(3) 0.1763(3) -0.2900(2) 0.0370(9) Uani 1 1 d . . . H40 H 1.4124 0.1233 -0.3370 0.044 Uiso 1 1 calc R . . C41 C 1.3579(3) 0.1521(3) -0.2054(2) 0.0353(8) Uani 1 1 d . . . H41 H 1.3510 0.0833 -0.1948 0.042 Uiso 1 1 calc R . . C42 C 1.4463(3) 0.3043(3) -0.3979(2) 0.0294(7) Uani 1 1 d . . . H1A H 0.383(4) 0.456(3) 0.047(3) 0.117(19) Uiso 1 1 d D . . H1B H 0.516(3) 0.374(5) 0.075(4) 0.18(3) Uiso 1 1 d D . . H1C H 0.381(4) 0.390(4) 0.1398(15) 0.14(2) Uiso 1 1 d D . . H1D H 0.461(3) 0.306(2) 0.044(2) 0.059(12) Uiso 1 1 d 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 0.0279(4) 0.0198(3) 0.0212(4) 0.0039(3) -0.0060(3) -0.0148(3) Mn2 0.0259(3) 0.0205(2) 0.0197(3) 0.00197(19) -0.0064(2) -0.0129(2) Mn3 0.0229(3) 0.0229(3) 0.0220(3) 0.0050(2) -0.0083(2) -0.0128(2) S1 0.0276(5) 0.0234(4) 0.0624(7) 0.0167(4) -0.0236(5) -0.0157(4) S2 0.0193(4) 0.0215(4) 0.0317(5) 0.0038(3) -0.0075(4) -0.0112(3) S3 0.0289(5) 0.0505(6) 0.0227(5) 0.0118(4) -0.0082(4) -0.0232(4) O1 0.0428(15) 0.0358(14) 0.0357(14) 0.0167(11) -0.0108(12) -0.0270(12) O2 0.0210(12) 0.0238(12) 0.0304(13) 0.0017(10) -0.0039(10) -0.0123(10) O3 0.0290(13) 0.0205(11) 0.0322(13) 0.0094(10) -0.0171(11) -0.0135(10) O4 0.0337(16) 0.0244(13) 0.071(2) -0.0040(13) -0.0134(15) -0.0061(12) O5 0.0505(17) 0.0427(15) 0.0521(17) 0.0079(13) -0.0298(14) -0.0308(13) O6 0.086(2) 0.0527(17) 0.0231(14) 0.0060(13) -0.0077(14) -0.0475(17) O7 0.0388(15) 0.0512(15) 0.0240(13) 0.0098(11) -0.0086(11) -0.0316(13) O8 0.0505(18) 0.0280(14) 0.0649(19) 0.0106(13) -0.0350(16) -0.0150(12) O9 0.0345(14) 0.0429(14) 0.0338(14) -0.0018(11) -0.0125(12) -0.0245(12) O10 0.0331(15) 0.0407(15) 0.0486(17) 0.0044(12) -0.0094(13) -0.0255(12) O11 0.0318(14) 0.0232(12) 0.0345(14) -0.0002(11) -0.0077(12) -0.0080(10) O12 0.0399(18) 0.067(2) 0.108(3) 0.0496(19) -0.0355(19) -0.0289(16) O13 0.0595(18) 0.0400(15) 0.083(2) 0.0340(14) -0.0555(17) -0.0344(14) O14 0.0223(14) 0.0289(14) 0.086(2) 0.0115(14) -0.0062(14) -0.0110(11) O15 0.0363(15) 0.0356(13) 0.0439(15) 0.0128(11) -0.0250(13) -0.0201(12) O16 0.0243(13) 0.0278(12) 0.0408(15) -0.0012(11) 0.0022(11) -0.0139(10) O17 0.0534(18) 0.0771(19) 0.0223(13) 0.0013(13) -0.0083(13) -0.0466(16) O18 0.0323(15) 0.0579(17) 0.0434(16) 0.0266(13) -0.0111(13) -0.0188(13) O19 0.126(3) 0.070(2) 0.074(2) -0.0018(19) -0.013(2) -0.045(2) N1 0.0339(19) 0.049(2) 0.043(2) 0.0108(17) -0.0152(17) -0.0209(17) C1 0.030(2) 0.0231(17) 0.044(2) 0.0076(16) -0.0180(18) -0.0140(15) C2 0.0238(18) 0.0228(16) 0.0307(19) 0.0054(14) -0.0101(15) -0.0137(14) C3 0.035(2) 0.046(2) 0.034(2) 0.0081(17) -0.0126(17) -0.0276(18) C4 0.046(2) 0.042(2) 0.033(2) 0.0067(17) -0.0167(19) -0.0303(19) C5 0.0290(19) 0.0210(16) 0.044(2) 0.0124(15) -0.0186(17) -0.0165(15) C6 0.042(2) 0.042(2) 0.034(2) 0.0047(17) -0.0068(18) -0.0298(19) C7 0.044(2) 0.048(2) 0.026(2) -0.0008(17) -0.0094(18) -0.0302(19) C8 0.0254(19) 0.0244(17) 0.045(2) 0.0114(16) -0.0159(17) -0.0164(15) C9 0.050(2) 0.0305(19) 0.033(2) 0.0140(16) -0.0221(19) -0.0176(18) C10 0.045(2) 0.0277(19) 0.033(2) 0.0027(16) -0.0138(18) -0.0157(17) C11 0.0232(17) 0.0197(16) 0.0296(19) 0.0054(14) -0.0120(15) -0.0128(14) C12 0.033(2) 0.0272(18) 0.029(2) 0.0083(15) -0.0077(17) -0.0103(16) C13 0.037(2) 0.0258(18) 0.033(2) 0.0036(16) -0.0061(17) -0.0098(16) C14 0.0213(17) 0.0223(17) 0.038(2) 0.0066(15) -0.0131(16) -0.0142(14) C15 0.0233(18) 0.0163(16) 0.037(2) 0.0037(14) -0.0103(16) -0.0091(14) C16 0.0212(17) 0.0222(16) 0.0240(18) 0.0037(13) -0.0075(14) -0.0113(14) C17 0.0282(19) 0.0355(19) 0.0246(18) 0.0026(15) -0.0038(15) -0.0195(16) C18 0.034(2) 0.041(2) 0.0254(19) -0.0004(15) -0.0069(16) -0.0264(17) C19 0.0207(17) 0.0215(16) 0.0289(19) 0.0059(14) -0.0091(15) -0.0115(14) C20 0.0295(19) 0.0336(19) 0.0256(19) -0.0024(15) 0.0009(15) -0.0200(16) C21 0.031(2) 0.0367(19) 0.0254(19) -0.0052(15) -0.0072(16) -0.0203(16) C22 0.0216(17) 0.0181(16) 0.0321(19) 0.0014(14) -0.0090(15) -0.0109(14) C23 0.053(3) 0.0297(19) 0.026(2) 0.0053(16) -0.0094(19) -0.0125(18) C24 0.050(3) 0.0255(19) 0.033(2) -0.0051(16) -0.0060(19) -0.0059(17) C25 0.0262(19) 0.0210(16) 0.042(2) 0.0058(15) -0.0158(17) -0.0129(15) C26 0.050(2) 0.032(2) 0.032(2) 0.0121(17) -0.0168(19) -0.0144(18) C27 0.041(2) 0.0272(19) 0.025(2) 0.0021(15) -0.0041(17) -0.0066(16) C28 0.032(2) 0.0244(18) 0.057(3) 0.0071(18) -0.024(2) -0.0143(16) C29 0.027(2) 0.041(2) 0.030(2) 0.0080(17) -0.0070(16) -0.0175(17) C30 0.0272(19) 0.0332(18) 0.0188(17) 0.0038(14) -0.0037(15) -0.0176(15) C31 0.034(2) 0.037(2) 0.035(2) 0.0150(16) -0.0099(17) -0.0229(17) C32 0.031(2) 0.035(2) 0.035(2) 0.0159(16) -0.0114(17) -0.0158(17) C33 0.0246(18) 0.0361(19) 0.0226(18) 0.0041(15) -0.0050(15) -0.0172(16) C34 0.035(2) 0.0297(19) 0.041(2) 0.0067(16) -0.0065(18) -0.0216(17) C35 0.030(2) 0.0317(19) 0.028(2) 0.0045(15) -0.0063(16) -0.0148(16) C36 0.0249(18) 0.040(2) 0.0191(18) 0.0070(15) -0.0035(15) -0.0199(16) C37 0.042(2) 0.042(2) 0.027(2) -0.0003(16) -0.0051(17) -0.0263(18) C38 0.046(2) 0.0331(19) 0.030(2) 0.0047(16) -0.0049(18) -0.0269(18) C39 0.0285(19) 0.0298(18) 0.0225(18) 0.0063(14) -0.0051(15) -0.0175(15) C40 0.058(3) 0.040(2) 0.0214(19) 0.0052(16) -0.0085(18) -0.032(2) C41 0.050(2) 0.034(2) 0.030(2) 0.0103(16) -0.0103(18) -0.0294(19) C42 0.0283(19) 0.0336(19) 0.0259(19) 0.0076(16) -0.0075(16) -0.0163(16) _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 2.068(2) 1_456 ? Mn1 O1 2.068(2) 2_765 ? Mn1 O2 2.226(2) 2_666 ? Mn1 O2 2.226(2) . ? Mn1 O3 2.2432(18) 2_656 ? Mn1 O3 2.2433(18) 1_565 ? Mn1 Mn2 3.1598(4) 2_666 ? Mn1 Mn2 3.1598(4) . ? Mn2 O4 2.049(2) 1_545 ? Mn2 O5 2.057(2) . ? Mn2 O6 2.059(2) 1_456 ? Mn2 O3 2.236(2) 1_565 ? Mn2 O2 2.2560(18) . ? Mn2 Mn3 3.0718(7) . ? Mn3 O7 2.046(2) . ? Mn3 O8 2.087(2) 1_545 ? Mn3 O9 2.1200(19) . ? Mn3 O10 2.121(2) . ? Mn3 O11 2.172(2) 1_565 ? S1 O13 1.433(2) . ? S1 O14 1.435(3) . ? S1 C5 1.773(3) . ? S1 C8 1.776(3) . ? S2 O15 1.434(2) . ? S2 O16 1.437(2) . ? S2 C22 1.763(3) . ? S2 C19 1.766(3) . ? S3 O18 1.433(3) . ? S3 O17 1.436(2) . ? S3 C36 1.767(3) . ? S3 C33 1.768(3) . ? O1 C42 1.254(3) . ? O1 Mn1 2.068(2) 1_654 ? O2 C15 1.283(4) . ? O3 C14 1.284(3) . ? O3 Mn2 2.236(2) 1_545 ? O3 Mn1 2.2433(18) 1_545 ? O4 C28 1.252(4) . ? O4 Mn2 2.049(2) 1_565 ? O5 C1 1.253(4) . ? O6 C42 1.242(4) . ? O6 Mn2 2.059(2) 1_654 ? O7 C29 1.272(4) . ? O8 C28 1.246(4) . ? O8 Mn3 2.087(2) 1_565 ? O9 C15 1.239(3) . ? O10 C1 1.256(4) . ? O11 C14 1.241(4) . ? O11 Mn3 2.172(2) 1_545 ? O12 C29 1.231(4) . ? C1 C2 1.502(4) . ? C2 C7 1.379(4) . ? C2 C3 1.382(4) . ? C3 C4 1.379(4) . ? C4 C5 1.366(4) . ? C5 C6 1.380(4) . ? C6 C7 1.377(4) . ? C8 C13 1.368(4) . ? C8 C9 1.375(5) . ? C9 C10 1.387(4) . ? C10 C11 1.385(4) . ? C11 C12 1.380(4) . ? C11 C14 1.504(4) . ? C12 C13 1.383(4) . ? C15 C16 1.506(4) . ? C16 C21 1.376(4) . ? C16 C17 1.388(4) . ? C17 C18 1.382(4) . ? C18 C19 1.374(4) . ? C19 C20 1.386(4) . ? C20 C21 1.390(4) . ? C22 C27 1.364(4) . ? C22 C23 1.371(4) . ? C23 C24 1.378(5) . ? C24 C25 1.379(4) . ? C25 C26 1.376(5) . ? C25 C28 1.506(4) . ? C26 C27 1.378(4) . ? C29 C30 1.501(4) . ? C30 C31 1.380(4) . ? C30 C35 1.396(4) . ? C31 C32 1.376(4) . ? C32 C33 1.382(4) . ? C33 C34 1.386(4) . ? C34 C35 1.377(4) . ? C36 C37 1.376(4) . ? C36 C41 1.379(4) . ? C37 C38 1.381(4) . ? C38 C39 1.378(4) . ? C39 C40 1.387(4) . ? C39 C42 1.486(4) . ? C40 C41 1.371(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O1 180.0(0) 1_456 2_765 ? O1 Mn1 O2 87.55(8) 1_456 2_666 ? O1 Mn1 O2 92.45(8) 2_765 2_666 ? O1 Mn1 O2 92.45(8) 1_456 . ? O1 Mn1 O2 87.55(8) 2_765 . ? O2 Mn1 O2 180.0(0) 2_666 . ? O1 Mn1 O3 86.44(8) 1_456 2_656 ? O1 Mn1 O3 93.56(8) 2_765 2_656 ? O2 Mn1 O3 76.35(7) 2_666 2_656 ? O2 Mn1 O3 103.65(7) . 2_656 ? O1 Mn1 O3 93.56(8) 1_456 1_565 ? O1 Mn1 O3 86.44(8) 2_765 1_565 ? O2 Mn1 O3 103.65(7) 2_666 1_565 ? O2 Mn1 O3 76.35(7) . 1_565 ? O3 Mn1 O3 180.0(0) 2_656 1_565 ? O1 Mn1 Mn2 112.67(6) 1_456 2_666 ? O1 Mn1 Mn2 67.33(6) 2_765 2_666 ? O2 Mn1 Mn2 45.56(5) 2_666 2_666 ? O2 Mn1 Mn2 134.44(5) . 2_666 ? O3 Mn1 Mn2 45.03(5) 2_656 2_666 ? O3 Mn1 Mn2 134.97(5) 1_565 2_666 ? O1 Mn1 Mn2 67.33(6) 1_456 . ? O1 Mn1 Mn2 112.67(6) 2_765 . ? O2 Mn1 Mn2 134.44(5) 2_666 . ? O2 Mn1 Mn2 45.56(5) . . ? O3 Mn1 Mn2 134.97(5) 2_656 . ? O3 Mn1 Mn2 45.03(5) 1_565 . ? Mn2 Mn1 Mn2 180.0 2_666 . ? O4 Mn2 O5 91.70(10) 1_545 . ? O4 Mn2 O6 99.17(11) 1_545 1_456 ? O5 Mn2 O6 100.88(10) . 1_456 ? O4 Mn2 O3 154.17(10) 1_545 1_565 ? O5 Mn2 O3 90.64(8) . 1_565 ? O6 Mn2 O3 105.63(10) 1_456 1_565 ? O4 Mn2 O2 89.80(8) 1_545 . ? O5 Mn2 O2 150.48(9) . . ? O6 Mn2 O2 107.98(8) 1_456 . ? O3 Mn2 O2 75.91(7) 1_565 . ? O4 Mn2 Mn3 71.95(8) 1_545 . ? O5 Mn2 Mn3 66.79(7) . . ? O6 Mn2 Mn3 163.92(6) 1_456 . ? O3 Mn2 Mn3 85.43(6) 1_565 . ? O2 Mn2 Mn3 85.78(6) . . ? O4 Mn2 Mn1 132.11(6) 1_545 . ? O5 Mn2 Mn1 134.60(7) . . ? O6 Mn2 Mn1 85.24(6) 1_456 . ? O3 Mn2 Mn1 45.23(5) 1_565 . ? O2 Mn2 Mn1 44.79(5) . . ? Mn3 Mn2 Mn1 110.708(16) . . ? O7 Mn3 O8 106.36(10) . 1_545 ? O7 Mn3 O9 103.45(8) . . ? O8 Mn3 O9 90.73(9) 1_545 . ? O7 Mn3 O10 96.48(9) . . ? O8 Mn3 O10 90.31(9) 1_545 . ? O9 Mn3 O10 158.88(9) . . ? O7 Mn3 O11 99.05(9) . 1_565 ? O8 Mn3 O11 154.57(10) 1_545 1_565 ? O9 Mn3 O11 84.17(8) . 1_565 ? O10 Mn3 O11 85.88(9) . 1_565 ? O7 Mn3 Mn2 168.83(7) . . ? O8 Mn3 Mn2 83.46(8) 1_545 . ? O9 Mn3 Mn2 70.55(6) . . ? O10 Mn3 Mn2 88.62(7) . . ? O11 Mn3 Mn2 71.33(6) 1_565 . ? O13 S1 O14 120.26(16) . . ? O13 S1 C5 107.96(14) . . ? O14 S1 C5 108.35(15) . . ? O13 S1 C8 108.46(15) . . ? O14 S1 C8 108.38(15) . . ? C5 S1 C8 101.89(14) . . ? O15 S2 O16 119.41(14) . . ? O15 S2 C22 108.86(13) . . ? O16 S2 C22 108.25(14) . . ? O15 S2 C19 108.62(13) . . ? O16 S2 C19 108.01(13) . . ? C22 S2 C19 102.34(14) . . ? O18 S3 O17 118.71(15) . . ? O18 S3 C36 109.11(16) . . ? O17 S3 C36 107.86(14) . . ? O18 S3 C33 108.39(14) . . ? O17 S3 C33 107.50(15) . . ? C36 S3 C33 104.34(14) . . ? C42 O1 Mn1 144.4(2) . 1_654 ? C15 O2 Mn1 128.60(19) . . ? C15 O2 Mn2 114.81(17) . . ? Mn1 O2 Mn2 89.65(7) . . ? C14 O3 Mn2 117.23(19) . 1_545 ? C14 O3 Mn1 129.19(17) . 1_545 ? Mn2 O3 Mn1 89.74(7) 1_545 1_545 ? C28 O4 Mn2 137.4(2) . 1_565 ? C1 O5 Mn2 146.5(2) . . ? C42 O6 Mn2 119.2(2) . 1_654 ? C29 O7 Mn3 131.8(2) . . ? C28 O8 Mn3 119.9(2) . 1_565 ? C15 O9 Mn3 143.9(2) . . ? C1 O10 Mn3 112.9(2) . . ? C14 O11 Mn3 140.8(2) . 1_545 ? O5 C1 O10 124.8(3) . . ? O5 C1 C2 116.8(3) . . ? O10 C1 C2 118.4(3) . . ? C7 C2 C3 119.6(3) . . ? C7 C2 C1 120.4(3) . . ? C3 C2 C1 119.9(3) . . ? C4 C3 C2 119.9(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 121.7(3) . . ? C4 C5 S1 119.3(2) . . ? C6 C5 S1 119.0(3) . . ? C7 C6 C5 118.3(3) . . ? C6 C7 C2 120.9(3) . . ? C13 C8 C9 121.4(3) . . ? C13 C8 S1 119.5(3) . . ? C9 C8 S1 119.1(3) . . ? C8 C9 C10 119.1(3) . . ? C11 C10 C9 120.7(3) . . ? C12 C11 C10 118.6(3) . . ? C12 C11 C14 122.1(3) . . ? C10 C11 C14 119.3(3) . . ? C11 C12 C13 121.3(3) . . ? C8 C13 C12 118.9(3) . . ? O11 C14 O3 123.5(3) . . ? O11 C14 C11 117.7(3) . . ? O3 C14 C11 118.8(3) . . ? O9 C15 O2 124.0(3) . . ? O9 C15 C16 117.3(3) . . ? O2 C15 C16 118.8(3) . . ? C21 C16 C17 119.3(3) . . ? C21 C16 C15 119.5(3) . . ? C17 C16 C15 121.2(3) . . ? C18 C17 C16 120.2(3) . . ? C19 C18 C17 119.7(3) . . ? C18 C19 C20 121.2(3) . . ? C18 C19 S2 118.3(2) . . ? C20 C19 S2 120.4(2) . . ? C19 C20 C21 118.3(3) . . ? C16 C21 C20 121.3(3) . . ? C27 C22 C23 120.8(3) . . ? C27 C22 S2 119.1(2) . . ? C23 C22 S2 120.1(2) . . ? C22 C23 C24 119.3(3) . . ? C23 C24 C25 120.5(3) . . ? C26 C25 C24 119.3(3) . . ? C26 C25 C28 120.6(3) . . ? C24 C25 C28 120.1(3) . . ? C25 C26 C27 120.2(3) . . ? C22 C27 C26 119.9(3) . . ? O8 C28 O4 125.6(3) . . ? O8 C28 C25 117.5(3) . . ? O4 C28 C25 116.9(3) . . ? O12 C29 O7 122.9(3) . . ? O12 C29 C30 119.6(3) . . ? O7 C29 C30 117.5(3) . . ? C31 C30 C35 119.5(3) . . ? C31 C30 C29 121.2(3) . . ? C35 C30 C29 119.3(3) . . ? C32 C31 C30 121.0(3) . . ? C31 C32 C33 119.3(3) . . ? C32 C33 C34 120.5(3) . . ? C32 C33 S3 121.3(3) . . ? C34 C33 S3 118.1(2) . . ? C35 C34 C33 120.0(3) . . ? C34 C35 C30 119.8(3) . . ? C37 C36 C41 121.4(3) . . ? C37 C36 S3 118.5(2) . . ? C41 C36 S3 120.1(2) . . ? C36 C37 C38 118.9(3) . . ? C39 C38 C37 120.7(3) . . ? C38 C39 C40 119.2(3) . . ? C38 C39 C42 119.8(3) . . ? C40 C39 C42 121.0(3) . . ? C41 C40 C39 120.8(3) . . ? C40 C41 C36 118.9(3) . . ? O6 C42 O1 123.6(3) . . ? O6 C42 C39 118.9(3) . . ? O1 C42 C39 117.6(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.458 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.074 ######END####### data_Compound(1) _database_code_depnum_ccdc_archive 'CCDC 864134' #TrackingRef '- all compounds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Manganese Sulfonyldibenzoate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H59 Mn5 O40.50 S6' _chemical_formula_weight 2183.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.700(5) _cell_length_b 12.714(5) _cell_length_c 15.990(5) _cell_angle_alpha 72.773(5) _cell_angle_beta 88.047(5) _cell_angle_gamma 60.583(5) _cell_volume 2128.8(14) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1099 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_T_max 0.891 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48370 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.63 _reflns_number_total 9581 _reflns_number_gt 7433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0384P)^2^+3.6886P] 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 9581 _refine_ls_number_parameters 611 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.0000 1.0000 0.0000 0.01211(13) Uani 1 2 d S . . Mn2 Mn 0.26714(4) 0.85600(4) 0.28847(3) 0.01188(10) Uani 1 1 d . . . Mn3 Mn 0.24269(4) 0.95817(4) 0.08716(3) 0.01133(10) Uani 1 1 d . . . S1 S 0.00872(6) 0.37761(6) 0.18809(5) 0.01243(14) Uani 1 1 d . . . S2 S 0.29598(7) 0.21433(7) 0.52467(5) 0.01739(15) Uani 1 1 d . . . S3 S 0.48598(6) 1.42919(7) 0.20126(6) 0.02118(17) Uani 1 1 d . . . O1 O 0.09913(17) 0.04591(18) 0.90520(13) 0.0172(4) Uani 1 1 d . . . O2 O 0.16532(16) 0.83306(17) 0.08544(13) 0.0146(4) Uani 1 1 d . . . O3 O 1.04459(17) 1.07761(17) 0.09331(13) 0.0140(4) Uani 1 1 d . . . O4 O 0.25391(19) 0.78813(19) 0.41946(13) 0.0191(4) Uani 1 1 d . . . O5 O -0.55095(18) 0.7400(2) 0.27476(14) 0.0222(5) Uani 1 1 d . . . O6 O 0.21235(18) 0.75641(19) 0.23209(13) 0.0191(4) Uani 1 1 d . . . O7 O 0.30821(18) 0.99404(18) 0.30086(14) 0.0188(4) Uani 1 1 d . . . O8 O 1.08190(17) 1.01227(19) 0.24057(13) 0.0177(4) Uani 1 1 d . . . O9 O -0.58698(17) 0.79842(19) 0.12780(14) 0.0211(5) Uani 1 1 d . . . O10 O 0.26557(19) 0.0332(2) 0.95946(13) 0.0231(5) Uani 1 1 d . . . O11 O 0.28460(18) 1.0512(2) 0.15423(14) 0.0209(5) Uani 1 1 d . . . O12 O 0.0795(2) 0.8318(2) 0.47463(16) 0.0298(5) Uani 1 1 d . . . H12A H 0.0726 0.9025 0.4616 0.045 Uiso 1 1 calc R . . O13 O 0.02412(17) 0.34509(18) 0.10813(13) 0.0170(4) Uani 1 1 d . . . O14 O 0.06201(17) 0.27755(18) 0.27193(13) 0.0175(4) Uani 1 1 d . . . O15 O 0.2051(2) 0.2231(2) 0.46717(14) 0.0252(5) Uani 1 1 d . . . O16 O 0.4229(2) 0.13542(19) 0.51847(14) 0.0248(5) Uani 1 1 d . . . O17 O 0.48128(19) 1.4530(2) 0.28405(17) 0.0301(6) Uani 1 1 d . . . O18 O 0.42942(19) 1.53324(19) 0.12060(16) 0.0285(5) Uani 1 1 d . . . O19 O 0.1103(3) 0.0686(2) 0.42351(19) 0.0437(7) Uani 1 1 d . . . O20 O 0.6517(2) 0.1152(3) 0.48058(17) 0.0400(6) Uani 1 1 d . . . O21 O 0.0000 1.0000 0.5000 0.0051(9) Uiso 0.50 2 d SP . . C1 C 0.1737(2) 0.7564(3) 0.16165(19) 0.0145(6) Uani 1 1 d . . . C2 C 0.1345(2) 0.6607(2) 0.16706(18) 0.0126(5) Uani 1 1 d . . . C3 C 0.0744(2) 0.6655(3) 0.09322(18) 0.0147(6) Uani 1 1 d . . . H3 H 0.0585 0.7283 0.0394 0.018 Uiso 1 1 calc R . . C4 C 0.0385(2) 0.5768(3) 0.10008(18) 0.0149(6) Uani 1 1 d . . . H4 H -0.0011 0.5793 0.0511 0.018 Uiso 1 1 calc R . . C5 C 0.0625(2) 0.4841(2) 0.18110(18) 0.0128(5) Uani 1 1 d . . . C6 C 0.1214(2) 0.4780(3) 0.25519(19) 0.0154(6) Uani 1 1 d . . . H6 H 0.1364 0.4156 0.3090 0.018 Uiso 1 1 calc R . . C7 C 0.1575(3) 0.5672(3) 0.24742(19) 0.0164(6) Uani 1 1 d . . . H7 H 0.1975 0.5641 0.2965 0.020 Uiso 1 1 calc R . . C8 C -0.1485(2) 0.4734(3) 0.19121(18) 0.0129(5) Uani 1 1 d . . . C9 C -0.2273(3) 0.5476(3) 0.11305(19) 0.0194(6) Uani 1 1 d . . . H9 H -0.1995 0.5421 0.0591 0.023 Uiso 1 1 calc R . . C10 C -0.3487(3) 0.6306(3) 0.1168(2) 0.0203(6) Uani 1 1 d . . . H10 H -0.4032 0.6814 0.0650 0.024 Uiso 1 1 calc R . . C11 C -0.3891(2) 0.6378(3) 0.19791(19) 0.0149(6) Uani 1 1 d . . . C12 C -0.3098(3) 0.5607(3) 0.2753(2) 0.0221(7) Uani 1 1 d . . . H12 H -0.3378 0.5646 0.3294 0.026 Uiso 1 1 calc R . . C13 C -0.1886(3) 0.4778(3) 0.2725(2) 0.0218(7) Uani 1 1 d . . . H13 H -0.1347 0.4256 0.3245 0.026 Uiso 1 1 calc R . . C14 C -0.5197(2) 0.7322(3) 0.2006(2) 0.0174(6) Uani 1 1 d . . . C15 C 0.1771(3) 0.7575(3) 0.45502(19) 0.0178(6) Uani 1 1 d . . . C16 C 0.2089(3) 0.6207(3) 0.47309(18) 0.0143(6) Uani 1 1 d . . . C17 C 0.1248(3) 0.5836(3) 0.50625(18) 0.0162(6) Uani 1 1 d . . . H17 H 0.0497 0.6427 0.5169 0.019 Uiso 1 1 calc R . . C18 C 0.1537(3) 0.4588(3) 0.52310(19) 0.0167(6) Uani 1 1 d . . . H18 H 0.0982 0.4334 0.5452 0.020 Uiso 1 1 calc R . . C19 C 0.2661(3) 0.3715(3) 0.50683(18) 0.0152(6) Uani 1 1 d . . . C20 C 0.3511(3) 0.4061(3) 0.47483(19) 0.0191(6) Uani 1 1 d . . . H20 H 0.4265 0.3463 0.4650 0.023 Uiso 1 1 calc R . . C21 C 0.3212(3) 0.5320(3) 0.45762(19) 0.0180(6) Uani 1 1 d . . . H21 H 0.3770 0.5571 0.4356 0.022 Uiso 1 1 calc R . . C22 C 0.2685(3) 0.1655(3) 0.63446(18) 0.0165(6) Uani 1 1 d . . . C23 C 0.1647(3) 0.1563(3) 0.6483(2) 0.0195(6) Uani 1 1 d . . . H23 H 0.1122 0.1732 0.6008 0.023 Uiso 1 1 calc R . . C24 C 0.1404(3) 0.1217(3) 0.73377(19) 0.0184(6) Uani 1 1 d . . . H24 H 0.0706 0.1160 0.7441 0.022 Uiso 1 1 calc R . . C25 C 0.2200(2) 0.0953(3) 0.80463(19) 0.0156(6) Uani 1 1 d . . . C26 C 0.3242(3) 0.1051(3) 0.78935(19) 0.0186(6) Uani 1 1 d . . . H26 H 0.3771 0.0878 0.8367 0.022 Uiso 1 1 calc R . . C27 C 0.3489(3) 0.1407(3) 0.70385(19) 0.0174(6) Uani 1 1 d . . . H27 H 0.4179 0.1477 0.6931 0.021 Uiso 1 1 calc R . . C28 C 0.1931(3) 0.0560(3) 0.89646(19) 0.0164(6) Uani 1 1 d . . . C29 C 0.3102(2) 1.0611(3) 0.22553(19) 0.0155(6) Uani 1 1 d . . . C30 C 0.3484(2) 1.1571(3) 0.22013(19) 0.0141(6) Uani 1 1 d . . . C31 C 0.4002(3) 1.1558(3) 0.29578(19) 0.0171(6) Uani 1 1 d . . . H31 H 0.4077 1.0978 0.3502 0.020 Uiso 1 1 calc R . . C32 C 0.4406(3) 1.2402(3) 0.2905(2) 0.0182(6) Uani 1 1 d . . . H32 H 0.4759 1.2392 0.3409 0.022 Uiso 1 1 calc R . . C33 C 0.4276(2) 1.3266(3) 0.2087(2) 0.0161(6) Uani 1 1 d . . . C34 C 0.3750(3) 1.3297(3) 0.1328(2) 0.0190(6) Uani 1 1 d . . . H34 H 0.3662 1.3887 0.0786 0.023 Uiso 1 1 calc R . . C35 C 0.3358(3) 1.2439(3) 0.13865(19) 0.0180(6) Uani 1 1 d . . . H35 H 0.3011 1.2444 0.0882 0.022 Uiso 1 1 calc R . . C36 C 0.6412(3) 1.3311(3) 0.1909(2) 0.0194(6) Uani 1 1 d . . . C37 C 0.7254(3) 1.2547(3) 0.2669(2) 0.0301(8) Uani 1 1 d . . . H37 H 0.7018 1.2577 0.3222 0.036 Uiso 1 1 calc R . . C38 C 0.8452(3) 1.1739(3) 0.2585(2) 0.0289(8) Uani 1 1 d . . . H38 H 0.9026 1.1222 0.3087 0.035 Uiso 1 1 calc R . . C39 C 0.8802(2) 1.1696(3) 0.1756(2) 0.0164(6) Uani 1 1 d . . . C40 C 0.7939(3) 1.2444(3) 0.1010(2) 0.0199(6) Uani 1 1 d . . . H40 H 0.8168 1.2398 0.0457 0.024 Uiso 1 1 calc R . . C41 C 0.6736(3) 1.3260(3) 0.1083(2) 0.0212(6) Uani 1 1 d . . . H41 H 0.6157 1.3766 0.0583 0.025 Uiso 1 1 calc R . . C42 C 1.0118(2) 1.0798(3) 0.16990(19) 0.0144(6) 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 0.0085(3) 0.0121(3) 0.0154(3) -0.0034(2) 0.0012(2) -0.0055(2) Mn2 0.0107(2) 0.0112(2) 0.0145(2) -0.00498(16) 0.00297(15) -0.00569(16) Mn3 0.0087(2) 0.0117(2) 0.0136(2) -0.00423(16) 0.00137(15) -0.00505(16) S1 0.0093(3) 0.0094(3) 0.0177(3) -0.0048(3) 0.0013(2) -0.0039(2) S2 0.0250(4) 0.0135(3) 0.0140(3) -0.0044(3) 0.0045(3) -0.0100(3) S3 0.0115(3) 0.0151(4) 0.0436(5) -0.0166(3) 0.0105(3) -0.0079(3) O1 0.0147(10) 0.0173(10) 0.0204(11) -0.0041(8) 0.0057(8) -0.0100(8) O2 0.0104(9) 0.0114(9) 0.0207(11) -0.0041(8) 0.0017(8) -0.0052(8) O3 0.0115(9) 0.0127(9) 0.0200(10) -0.0074(8) 0.0038(8) -0.0065(8) O4 0.0244(11) 0.0198(11) 0.0180(11) -0.0030(9) 0.0036(8) -0.0166(9) O5 0.0127(10) 0.0253(12) 0.0312(12) -0.0179(10) 0.0060(9) -0.0068(9) O6 0.0227(11) 0.0187(11) 0.0203(11) -0.0082(9) 0.0014(8) -0.0123(9) O7 0.0191(11) 0.0131(10) 0.0250(11) -0.0040(9) 0.0016(8) -0.0097(8) O8 0.0112(10) 0.0179(10) 0.0212(11) -0.0062(9) 0.0017(8) -0.0052(8) O9 0.0114(10) 0.0159(10) 0.0310(12) -0.0079(9) 0.0001(9) -0.0027(8) O10 0.0210(11) 0.0370(13) 0.0154(11) -0.0041(9) 0.0022(8) -0.0198(10) O11 0.0192(11) 0.0229(11) 0.0271(12) -0.0144(9) 0.0042(9) -0.0119(9) O12 0.0292(13) 0.0179(11) 0.0473(15) -0.0155(11) 0.0156(11) -0.0134(10) O13 0.0159(10) 0.0181(10) 0.0223(11) -0.0116(9) 0.0050(8) -0.0097(8) O14 0.0139(10) 0.0118(10) 0.0219(11) -0.0014(8) 0.0002(8) -0.0048(8) O15 0.0417(14) 0.0270(12) 0.0154(11) -0.0057(9) 0.0019(9) -0.0241(11) O16 0.0291(12) 0.0165(11) 0.0235(12) -0.0071(9) 0.0111(9) -0.0077(9) O17 0.0194(11) 0.0343(13) 0.0568(16) -0.0358(12) 0.0178(11) -0.0173(10) O18 0.0164(11) 0.0135(11) 0.0535(16) -0.0081(10) 0.0104(10) -0.0078(9) O19 0.0514(17) 0.0342(15) 0.0533(18) -0.0199(13) 0.0226(14) -0.0248(13) O20 0.0325(14) 0.0508(17) 0.0355(15) -0.0126(13) 0.0011(11) -0.0207(12) C1 0.0071(13) 0.0099(13) 0.0236(16) -0.0058(11) 0.0025(11) -0.0019(10) C2 0.0085(12) 0.0109(13) 0.0193(14) -0.0067(11) 0.0027(10) -0.0046(10) C3 0.0142(14) 0.0144(14) 0.0143(14) -0.0036(11) 0.0019(10) -0.0069(11) C4 0.0146(14) 0.0151(14) 0.0149(14) -0.0049(11) 0.0009(10) -0.0074(11) C5 0.0089(13) 0.0089(13) 0.0200(14) -0.0052(11) 0.0011(10) -0.0037(10) C6 0.0136(13) 0.0112(13) 0.0169(14) -0.0014(11) -0.0001(11) -0.0045(11) C7 0.0143(14) 0.0168(14) 0.0194(15) -0.0067(12) -0.0008(11) -0.0081(11) C8 0.0076(12) 0.0115(13) 0.0196(14) -0.0064(11) 0.0013(10) -0.0041(10) C9 0.0150(14) 0.0213(15) 0.0173(15) -0.0070(12) 0.0027(11) -0.0053(12) C10 0.0112(14) 0.0204(15) 0.0218(16) -0.0046(13) -0.0031(11) -0.0033(12) C11 0.0102(13) 0.0102(13) 0.0259(16) -0.0083(12) 0.0028(11) -0.0049(11) C12 0.0183(15) 0.0243(16) 0.0203(16) -0.0100(13) 0.0041(12) -0.0069(13) C13 0.0149(15) 0.0222(16) 0.0183(15) -0.0049(13) -0.0013(11) -0.0027(12) C14 0.0103(13) 0.0150(14) 0.0323(17) -0.0137(13) 0.0031(12) -0.0068(11) C15 0.0220(15) 0.0159(14) 0.0149(14) -0.0033(12) 0.0014(11) -0.0100(12) C16 0.0185(14) 0.0136(14) 0.0108(13) -0.0018(11) 0.0013(10) -0.0093(11) C17 0.0146(14) 0.0163(14) 0.0163(14) -0.0049(11) 0.0026(11) -0.0070(11) C18 0.0163(14) 0.0174(14) 0.0176(15) -0.0034(12) 0.0024(11) -0.0104(12) C19 0.0205(15) 0.0137(14) 0.0105(13) -0.0026(11) -0.0006(11) -0.0086(11) C20 0.0169(14) 0.0181(15) 0.0188(15) -0.0059(12) 0.0045(11) -0.0063(12) C21 0.0189(15) 0.0183(15) 0.0194(15) -0.0054(12) 0.0054(11) -0.0117(12) C22 0.0218(15) 0.0114(13) 0.0151(14) -0.0045(11) 0.0039(11) -0.0075(11) C23 0.0200(15) 0.0206(15) 0.0181(15) -0.0023(12) -0.0011(11) -0.0123(12) C24 0.0152(14) 0.0192(15) 0.0232(16) -0.0050(12) 0.0034(11) -0.0115(12) C25 0.0147(14) 0.0122(13) 0.0182(15) -0.0037(11) 0.0033(11) -0.0063(11) C26 0.0165(14) 0.0225(15) 0.0182(15) -0.0064(12) 0.0027(11) -0.0110(12) C27 0.0134(14) 0.0197(15) 0.0206(15) -0.0067(12) 0.0048(11) -0.0094(12) C28 0.0156(14) 0.0134(14) 0.0174(15) -0.0047(11) 0.0037(11) -0.0055(11) C29 0.0093(13) 0.0123(13) 0.0257(16) -0.0088(12) 0.0033(11) -0.0047(11) C30 0.0107(13) 0.0123(13) 0.0202(15) -0.0062(11) 0.0032(10) -0.0061(11) C31 0.0178(14) 0.0157(14) 0.0180(15) -0.0054(12) 0.0026(11) -0.0087(12) C32 0.0171(14) 0.0191(15) 0.0212(15) -0.0100(12) 0.0008(11) -0.0092(12) C33 0.0097(13) 0.0126(13) 0.0277(16) -0.0090(12) 0.0055(11) -0.0058(11) C34 0.0197(15) 0.0160(14) 0.0211(15) -0.0034(12) 0.0041(12) -0.0104(12) C35 0.0186(15) 0.0209(15) 0.0173(15) -0.0055(12) 0.0005(11) -0.0122(12) C36 0.0125(14) 0.0150(14) 0.0384(18) -0.0157(13) 0.0081(12) -0.0090(11) C37 0.0155(15) 0.047(2) 0.0324(19) -0.0282(17) 0.0080(13) -0.0106(15) C38 0.0126(15) 0.044(2) 0.0310(18) -0.0224(16) 0.0023(13) -0.0087(14) C39 0.0098(13) 0.0156(14) 0.0298(16) -0.0133(12) 0.0059(11) -0.0074(11) C40 0.0166(15) 0.0164(15) 0.0238(16) -0.0054(12) 0.0070(12) -0.0071(12) C41 0.0135(14) 0.0163(15) 0.0276(17) -0.0018(13) 0.0031(12) -0.0058(12) C42 0.0123(13) 0.0118(13) 0.0260(16) -0.0110(12) 0.0062(11) -0.0085(11) _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 2.0715(19) 2_566 ? Mn1 O1 2.0715(19) 1_564 ? Mn1 O2 2.2091(19) 2_575 ? Mn1 O2 2.2091(19) . ? Mn1 O3 2.236(2) 2_675 ? Mn1 O3 2.236(2) 1_455 ? Mn1 Mn3 3.1573(12) 2_575 ? Mn1 Mn3 3.1573(12) . ? Mn2 O4 2.051(2) . ? Mn2 O5 2.091(2) 1_655 ? Mn2 O6 2.118(2) . ? Mn2 O7 2.122(2) . ? Mn2 O8 2.168(2) 1_455 ? Mn2 Mn3 3.0563(11) . ? Mn3 O9 2.056(2) 1_655 ? Mn3 O11 2.059(2) . ? Mn3 O10 2.059(2) 1_564 ? Mn3 O3 2.228(2) 1_455 ? Mn3 O2 2.249(2) . ? S1 O13 1.435(2) . ? S1 O14 1.442(2) . ? S1 C8 1.764(3) . ? S1 C5 1.768(3) . ? S2 O15 1.440(2) . ? S2 O16 1.441(2) . ? S2 C22 1.765(3) . ? S2 C19 1.773(3) . ? S3 O18 1.431(2) . ? S3 O17 1.436(2) . ? S3 C33 1.767(3) . ? S3 C36 1.775(3) . ? O1 C28 1.260(3) . ? O1 Mn1 2.0715(19) 1_546 ? O2 C1 1.284(3) . ? O3 C42 1.284(3) . ? O3 Mn3 2.228(2) 1_655 ? O3 Mn1 2.236(2) 1_655 ? O4 C15 1.277(3) . ? O5 C14 1.254(4) . ? O5 Mn2 2.091(2) 1_455 ? O6 C1 1.244(3) . ? O7 C29 1.261(3) . ? O8 C42 1.245(3) . ? O8 Mn2 2.168(2) 1_655 ? O9 C14 1.255(4) . ? O9 Mn3 2.056(2) 1_455 ? O10 C28 1.255(4) . ? O10 Mn3 2.059(2) 1_546 ? O11 C29 1.254(3) . ? O12 C15 1.235(4) . ? C1 C2 1.506(4) . ? C2 C7 1.389(4) . ? C2 C3 1.397(4) . ? C3 C4 1.386(4) . ? C4 C5 1.389(4) . ? C5 C6 1.385(4) . ? C6 C7 1.391(4) . ? C8 C9 1.383(4) . ? C8 C13 1.386(4) . ? C9 C10 1.389(4) . ? C10 C11 1.390(4) . ? C11 C12 1.380(4) . ? C11 C14 1.504(4) . ? C12 C13 1.383(4) . ? C15 C16 1.514(4) . ? C16 C21 1.389(4) . ? C16 C17 1.398(4) . ? C17 C18 1.380(4) . ? C18 C19 1.389(4) . ? C19 C20 1.384(4) . ? C20 C21 1.390(4) . ? C22 C23 1.384(4) . ? C22 C27 1.388(4) . ? C23 C24 1.380(4) . ? C24 C25 1.392(4) . ? C25 C26 1.395(4) . ? C25 C28 1.491(4) . ? C26 C27 1.384(4) . ? C29 C30 1.498(4) . ? C30 C31 1.389(4) . ? C30 C35 1.389(4) . ? C31 C32 1.381(4) . ? C32 C33 1.390(4) . ? C33 C34 1.386(4) . ? C34 C35 1.385(4) . ? C36 C41 1.381(4) . ? C36 C37 1.390(5) . ? C37 C38 1.386(4) . ? C38 C39 1.393(4) . ? C39 C40 1.386(4) . ? C39 C42 1.510(4) . ? C40 C41 1.389(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O1 180.0(0) 2_566 1_564 ? O1 Mn1 O2 92.98(8) 2_566 2_575 ? O1 Mn1 O2 87.02(8) 1_564 2_575 ? O1 Mn1 O2 87.02(8) 2_566 . ? O1 Mn1 O2 92.98(8) 1_564 . ? O2 Mn1 O2 180.0 2_575 . ? O1 Mn1 O3 94.34(8) 2_566 2_675 ? O1 Mn1 O3 85.66(8) 1_564 2_675 ? O2 Mn1 O3 76.48(7) 2_575 2_675 ? O2 Mn1 O3 103.52(7) . 2_675 ? O1 Mn1 O3 85.66(8) 2_566 1_455 ? O1 Mn1 O3 94.34(8) 1_564 1_455 ? O2 Mn1 O3 103.52(7) 2_575 1_455 ? O2 Mn1 O3 76.48(7) . 1_455 ? O3 Mn1 O3 180.0(0) 2_675 1_455 ? O1 Mn1 Mn3 68.55(6) 2_566 2_575 ? O1 Mn1 Mn3 111.45(6) 1_564 2_575 ? O2 Mn1 Mn3 45.43(5) 2_575 2_575 ? O2 Mn1 Mn3 134.57(5) . 2_575 ? O3 Mn1 Mn3 44.88(5) 2_675 2_575 ? O3 Mn1 Mn3 135.12(5) 1_455 2_575 ? O1 Mn1 Mn3 111.45(6) 2_566 . ? O1 Mn1 Mn3 68.55(6) 1_564 . ? O2 Mn1 Mn3 134.57(5) 2_575 . ? O2 Mn1 Mn3 45.43(5) . . ? O3 Mn1 Mn3 135.12(5) 2_675 . ? O3 Mn1 Mn3 44.88(5) 1_455 . ? Mn3 Mn1 Mn3 180.0 2_575 . ? O4 Mn2 O5 105.21(9) . 1_655 ? O4 Mn2 O6 101.67(8) . . ? O5 Mn2 O6 90.83(9) 1_655 . ? O4 Mn2 O7 96.32(8) . . ? O5 Mn2 O7 90.03(8) 1_655 . ? O6 Mn2 O7 161.09(8) . . ? O4 Mn2 O8 100.70(8) . 1_455 ? O5 Mn2 O8 154.08(8) 1_655 1_455 ? O6 Mn2 O8 84.46(8) . 1_455 ? O7 Mn2 O8 86.53(8) . 1_455 ? O4 Mn2 Mn3 169.38(6) . . ? O5 Mn2 Mn3 82.43(6) 1_655 . ? O6 Mn2 Mn3 70.42(6) . . ? O7 Mn2 Mn3 90.98(6) . . ? O8 Mn2 Mn3 71.97(5) 1_455 . ? O9 Mn3 O11 92.10(9) 1_655 . ? O9 Mn3 O10 98.75(9) 1_655 1_564 ? O11 Mn3 O10 102.64(9) . 1_564 ? O9 Mn3 O3 155.13(8) 1_655 1_455 ? O11 Mn3 O3 90.94(8) . 1_455 ? O10 Mn3 O3 104.64(8) 1_564 1_455 ? O9 Mn3 O2 89.20(8) 1_655 . ? O11 Mn3 O2 149.03(8) . . ? O10 Mn3 O2 107.73(8) 1_564 . ? O3 Mn3 O2 75.83(7) 1_455 . ? O9 Mn3 Mn2 73.64(6) 1_655 . ? O11 Mn3 Mn2 64.53(6) . . ? O10 Mn3 Mn2 164.20(6) 1_564 . ? O3 Mn3 Mn2 85.50(5) 1_455 . ? O2 Mn3 Mn2 86.31(5) . . ? O9 Mn3 Mn1 130.83(7) 1_655 . ? O11 Mn3 Mn1 135.22(6) . . ? O10 Mn3 Mn1 84.92(6) 1_564 . ? O3 Mn3 Mn1 45.08(5) 1_455 . ? O2 Mn3 Mn1 44.40(5) . . ? Mn2 Mn3 Mn1 110.607(19) . . ? O13 S1 O14 119.46(12) . . ? O13 S1 C8 108.78(12) . . ? O14 S1 C8 108.48(12) . . ? O13 S1 C5 108.89(12) . . ? O14 S1 C5 107.78(13) . . ? C8 S1 C5 102.05(13) . . ? O15 S2 O16 118.85(14) . . ? O15 S2 C22 107.83(14) . . ? O16 S2 C22 109.28(13) . . ? O15 S2 C19 107.35(13) . . ? O16 S2 C19 108.41(13) . . ? C22 S2 C19 104.14(13) . . ? O18 S3 O17 120.28(14) . . ? O18 S3 C33 108.29(14) . . ? O17 S3 C33 108.39(14) . . ? O18 S3 C36 108.42(14) . . ? O17 S3 C36 108.25(14) . . ? C33 S3 C36 101.61(13) . . ? C28 O1 Mn1 142.14(19) . 1_546 ? C1 O2 Mn1 128.67(17) . . ? C1 O2 Mn3 114.35(18) . . ? Mn1 O2 Mn3 90.17(8) . . ? C42 O3 Mn3 117.29(17) . 1_655 ? C42 O3 Mn1 128.76(17) . 1_655 ? Mn3 O3 Mn1 90.03(7) 1_655 1_655 ? C15 O4 Mn2 129.79(19) . . ? C14 O5 Mn2 121.04(19) . 1_455 ? C1 O6 Mn2 143.81(19) . . ? C29 O7 Mn2 110.00(18) . . ? C42 O8 Mn2 139.76(18) . 1_655 ? C14 O9 Mn3 134.58(19) . 1_455 ? C28 O10 Mn3 119.44(19) . 1_546 ? C29 O11 Mn3 150.1(2) . . ? O6 C1 O2 123.9(3) . . ? O6 C1 C2 117.5(2) . . ? O2 C1 C2 118.7(3) . . ? C7 C2 C3 119.8(3) . . ? C7 C2 C1 119.0(2) . . ? C3 C2 C1 121.2(2) . . ? C4 C3 C2 120.0(3) . . ? C3 C4 C5 119.1(3) . . ? C6 C5 C4 121.7(3) . . ? C6 C5 S1 120.6(2) . . ? C4 C5 S1 117.6(2) . . ? C5 C6 C7 118.6(3) . . ? C2 C7 C6 120.6(3) . . ? C9 C8 C13 121.6(3) . . ? C9 C8 S1 119.7(2) . . ? C13 C8 S1 118.6(2) . . ? C8 C9 C10 118.6(3) . . ? C9 C10 C11 120.1(3) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 C14 120.2(3) . . ? C10 C11 C14 119.4(3) . . ? C11 C12 C13 120.1(3) . . ? C12 C13 C8 119.1(3) . . ? O5 C14 O9 125.8(3) . . ? O5 C14 C11 117.4(3) . . ? O9 C14 C11 116.7(3) . . ? O12 C15 O4 124.5(3) . . ? O12 C15 C16 118.6(3) . . ? O4 C15 C16 116.9(2) . . ? C21 C16 C17 120.0(3) . . ? C21 C16 C15 120.5(2) . . ? C17 C16 C15 119.6(2) . . ? C18 C17 C16 119.8(3) . . ? C17 C18 C19 119.5(3) . . ? C20 C19 C18 121.6(3) . . ? C20 C19 S2 120.6(2) . . ? C18 C19 S2 117.8(2) . . ? C19 C20 C21 118.6(3) . . ? C16 C21 C20 120.6(3) . . ? C23 C22 C27 122.0(3) . . ? C23 C22 S2 118.4(2) . . ? C27 C22 S2 119.6(2) . . ? C24 C23 C22 118.9(3) . . ? C23 C24 C25 120.3(3) . . ? C24 C25 C26 120.0(3) . . ? C24 C25 C28 119.3(3) . . ? C26 C25 C28 120.7(3) . . ? C27 C26 C25 120.2(3) . . ? C26 C27 C22 118.6(3) . . ? O10 C28 O1 124.5(3) . . ? O10 C28 C25 118.4(3) . . ? O1 C28 C25 117.1(3) . . ? O11 C29 O7 124.2(3) . . ? O11 C29 C30 117.4(3) . . ? O7 C29 C30 118.4(3) . . ? C31 C30 C35 120.4(3) . . ? C31 C30 C29 120.0(3) . . ? C35 C30 C29 119.6(3) . . ? C32 C31 C30 120.2(3) . . ? C31 C32 C33 118.9(3) . . ? C34 C33 C32 121.5(3) . . ? C34 C33 S3 119.6(2) . . ? C32 C33 S3 118.8(2) . . ? C35 C34 C33 119.1(3) . . ? C34 C35 C30 119.9(3) . . ? C41 C36 C37 121.6(3) . . ? C41 C36 S3 119.2(2) . . ? C37 C36 S3 119.0(2) . . ? C38 C37 C36 118.7(3) . . ? C37 C38 C39 120.5(3) . . ? C40 C39 C38 119.7(3) . . ? C40 C39 C42 121.7(3) . . ? C38 C39 C42 118.5(3) . . ? C39 C40 C41 120.4(3) . . ? C36 C41 C40 119.0(3) . . ? O8 C42 O3 124.1(2) . . ? O8 C42 C39 117.4(2) . . ? O3 C42 C39 118.6(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.427 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.087