# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _journal_name_full CrystEngComm _journal_coden_cambridge ? _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jian Zhang' _publ_contact_author_email zhj@fjirsm.ac.cn loop_ _publ_author_name 'Jian Zhang' 'Yan-Xi Tan' 'Yan-Ping He' 'Ying Zhang' 'Yan-Jun Zheng' data_1_CCDC_934687 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 Mn2 N3 O11 S2' _chemical_formula_weight 705.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4155(6) _cell_length_b 9.9399(4) _cell_length_c 15.3997(8) _cell_angle_alpha 82.238(7) _cell_angle_beta 86.946(7) _cell_angle_gamma 88.633(8) _cell_volume 1425.81(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4325 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 12228 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.1362 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.42 _reflns_number_total 6400 _reflns_number_gt 3271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6400 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1467 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 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 0.46329(7) 0.28618(7) 0.26264(5) 0.0239(2) Uani 1 1 d . . . Mn2 Mn 0.06270(7) 0.30354(7) 0.24542(5) 0.0233(2) Uani 1 1 d . . . S1 S -0.32074(13) 0.54346(15) 0.45425(9) 0.0353(4) Uani 1 1 d . . . S2 S 0.15332(12) 0.79948(12) 0.22760(9) 0.0284(3) Uani 1 1 d . . . O1 O 0.0394(4) 0.3131(4) 0.1032(2) 0.0369(9) Uani 1 1 d . . . O2 O 0.5567(4) 0.2595(4) 0.1326(2) 0.0444(11) Uani 1 1 d . . . O3 O -0.3514(3) 0.6839(4) 0.6140(2) 0.0377(10) Uani 1 1 d . . . O4 O 0.2860(3) 1.1693(3) 0.2264(2) 0.0304(8) Uani 1 1 d . . . O5 O 0.5821(4) 0.1073(4) 0.3270(3) 0.0415(10) Uani 1 1 d . . . O6 O 0.1432(4) 0.5048(3) 0.2212(2) 0.0366(10) Uani 1 1 d . . . O7 O -0.1545(3) 0.3451(4) 0.2700(2) 0.0315(9) Uani 1 1 d . . . O8 O 0.3783(4) 0.4714(3) 0.1953(2) 0.0330(9) Uani 1 1 d . . . O9 O 0.0711(3) 1.0821(3) 0.2473(2) 0.0311(8) Uani 1 1 d . . . O10 O -0.1192(3) 0.7222(4) 0.6209(2) 0.0310(8) Uani 1 1 d . . . O11 O -0.3770(3) 0.4061(4) 0.3023(2) 0.0354(9) Uani 1 1 d . . . C10 C 0.6713(10) 0.1434(10) 0.0192(7) 0.111(3) Uiso 1 1 d . . . H10A H 0.5829 0.1131 -0.0007 0.134 Uiso 1 1 calc R . . H10B H 0.7021 0.2226 -0.0207 0.134 Uiso 1 1 calc R . . C11 C 0.0808(6) 0.3421(6) -0.0559(4) 0.0445(15) Uani 1 1 d . . . H11A H 0.0043 0.4076 -0.0686 0.053 Uiso 1 1 calc R . . H11B H 0.0509 0.2538 -0.0674 0.053 Uiso 1 1 calc R . . N3 N 0.6003(5) 0.1728(6) 0.4625(3) 0.0520(14) Uani 1 1 d . . . H3A H 0.5308 0.2305 0.4570 0.062 Uiso 1 1 calc R . . C1 C 0.7988(10) 0.0545(9) 0.5139(6) 0.103(4) Uani 1 1 d . . . H1B H 0.8891 0.1007 0.5088 0.124 Uiso 1 1 calc R . . H1C H 0.8053 -0.0242 0.5583 0.124 Uiso 1 1 calc R . . C2 C 0.7669(8) 0.0098(7) 0.4260(5) 0.072(2) Uani 1 1 d . . . H2B H 0.8466 0.0262 0.3836 0.086 Uiso 1 1 calc R . . H2C H 0.7429 -0.0855 0.4326 0.086 Uiso 1 1 calc R . . C3 C 0.8442(7) 0.0271(7) 0.1087(5) 0.060(2) Uani 1 1 d . . . H3B H 0.8484 -0.0658 0.1375 0.073 Uiso 1 1 calc R . . H3C H 0.9384 0.0657 0.1041 0.073 Uiso 1 1 calc R . . C4 C 0.6788(7) 0.1507(9) 0.5408(5) 0.082(3) Uani 1 1 d . . . H4A H 0.6208 0.1084 0.5905 0.098 Uiso 1 1 calc R . . H4B H 0.7162 0.2349 0.5548 0.098 Uiso 1 1 calc R . . C5 C 0.7774(9) 0.0374(8) 0.0187(5) 0.081(3) Uani 1 1 d . . . H5A H 0.8487 0.0600 -0.0284 0.097 Uiso 1 1 calc R . . H5B H 0.7345 -0.0478 0.0113 0.097 Uiso 1 1 calc R . . C6 C 0.2151(9) 0.3850(10) -0.1098(5) 0.087(3) Uani 1 1 d . . . H6A H 0.2403 0.3200 -0.1500 0.104 Uiso 1 1 calc R . . H6B H 0.2007 0.4733 -0.1439 0.104 Uiso 1 1 calc R . . C7 C 0.6401(6) 0.1002(6) 0.3999(4) 0.0391(14) Uani 1 1 d . . . C8 C 0.3288(7) 0.3912(8) -0.0495(4) 0.066(2) Uani 1 1 d . . . H8A H 0.4018 0.3228 -0.0573 0.080 Uiso 1 1 calc R . . H8B H 0.3719 0.4800 -0.0585 0.080 Uiso 1 1 calc R . . C9 C 0.1226(6) 0.3367(5) 0.0381(4) 0.0338(12) Uani 1 1 d . . . N1 N 0.7393(5) 0.1104(6) 0.1529(4) 0.0671(19) Uani 1 1 d . . . H1A H 0.7401 0.1121 0.2086 0.080 Uiso 1 1 calc R . . N2 N 0.2576(5) 0.3652(6) 0.0372(3) 0.0501(14) Uani 1 1 d . . . H2A H 0.3012 0.3684 0.0846 0.060 Uiso 1 1 calc R . . C12 C 0.6482(6) 0.1793(6) 0.1078(4) 0.0386(14) Uani 1 1 d . . . C13 C -0.1988(4) 0.5050(5) 0.3719(3) 0.0232(10) Uani 1 1 d . . . C14 C 0.4035(5) 0.8910(5) 0.2249(4) 0.0305(12) Uani 1 1 d . . . H14A H 0.4792 0.9492 0.2258 0.037 Uiso 1 1 calc R . . C15 C -0.1949(5) 0.6314(5) 0.4992(3) 0.0256(11) Uani 1 1 d . . . C16 C 0.2962(5) 0.6889(5) 0.2186(3) 0.0255(11) Uani 1 1 d . . . C17 C -0.2444(5) 0.4100(5) 0.3112(3) 0.0249(11) Uani 1 1 d . . . C18 C 0.2632(5) 0.9319(5) 0.2291(3) 0.0246(10) Uani 1 1 d . . . C19 C -0.2233(5) 0.6839(5) 0.5846(3) 0.0278(11) Uani 1 1 d . . . C20 C -0.0724(5) 0.6367(5) 0.4493(3) 0.0338(13) Uani 1 1 d . . . H20A H 0.0061 0.6848 0.4614 0.041 Uiso 1 1 calc R . . C21 C 0.4197(5) 0.7554(5) 0.2191(4) 0.0315(12) Uani 1 1 d . . . H21A H 0.5083 0.7125 0.2159 0.038 Uiso 1 1 calc R . . C22 C 0.2700(5) 0.5422(5) 0.2126(3) 0.0227(10) Uani 1 1 d . . . C23 C 0.2046(6) 1.0700(5) 0.2352(3) 0.0288(11) Uani 1 1 d . . . C24 C -0.0737(5) 0.5636(5) 0.3777(3) 0.0326(13) Uani 1 1 d . . . H24A H 0.0039 0.5566 0.3385 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0226(4) 0.0246(4) 0.0259(4) -0.0082(3) -0.0013(3) 0.0008(3) Mn2 0.0246(4) 0.0199(4) 0.0262(4) -0.0067(3) -0.0001(3) -0.0010(3) S1 0.0219(6) 0.0519(10) 0.0358(8) -0.0205(7) 0.0057(5) -0.0083(6) S2 0.0241(6) 0.0183(7) 0.0438(8) -0.0076(6) -0.0019(5) 0.0003(5) O1 0.039(2) 0.042(2) 0.030(2) -0.0069(19) -0.0021(16) 0.0014(17) O2 0.034(2) 0.065(3) 0.035(2) -0.011(2) -0.0008(17) 0.020(2) O3 0.0200(17) 0.063(3) 0.034(2) -0.021(2) 0.0021(15) 0.0039(17) O4 0.035(2) 0.0172(18) 0.041(2) -0.0100(16) -0.0049(15) -0.0066(15) O5 0.059(3) 0.032(2) 0.033(2) -0.0002(18) -0.0085(18) 0.0037(18) O6 0.043(2) 0.0197(19) 0.047(2) -0.0095(18) 0.0157(17) -0.0143(16) O7 0.0248(18) 0.038(2) 0.035(2) -0.0174(18) -0.0002(15) -0.0019(15) O8 0.039(2) 0.0175(19) 0.043(2) -0.0058(17) 0.0014(16) -0.0013(15) O9 0.0224(18) 0.026(2) 0.047(2) -0.0103(17) -0.0036(15) 0.0060(14) O10 0.0250(18) 0.037(2) 0.033(2) -0.0131(17) -0.0064(14) 0.0043(15) O11 0.0146(16) 0.045(2) 0.050(2) -0.018(2) -0.0063(15) 0.0009(15) C11 0.051(4) 0.047(4) 0.038(4) -0.013(3) -0.011(3) 0.016(3) N3 0.062(4) 0.066(4) 0.028(3) -0.007(3) -0.007(2) 0.005(3) C1 0.107(7) 0.084(6) 0.130(9) -0.032(6) -0.090(6) 0.052(6) C2 0.072(5) 0.052(5) 0.086(6) 0.017(4) -0.023(4) 0.010(4) C3 0.043(4) 0.065(5) 0.080(6) -0.038(4) -0.009(3) 0.019(3) C4 0.060(5) 0.141(8) 0.040(4) 0.013(5) -0.026(3) -0.013(5) C5 0.102(6) 0.073(6) 0.073(6) -0.036(5) -0.008(5) 0.046(5) C6 0.099(7) 0.132(8) 0.026(4) 0.003(5) 0.005(4) -0.016(6) C7 0.031(3) 0.037(3) 0.046(4) 0.004(3) -0.004(2) 0.000(2) C8 0.061(5) 0.094(6) 0.039(4) 0.001(4) 0.014(3) -0.007(4) C9 0.051(3) 0.023(3) 0.029(3) -0.006(2) -0.002(2) -0.001(2) N1 0.049(3) 0.111(5) 0.050(4) -0.044(4) -0.020(3) 0.043(3) N2 0.030(3) 0.088(4) 0.033(3) -0.012(3) -0.004(2) 0.006(3) C12 0.056(4) 0.033(3) 0.028(3) -0.012(3) 0.009(3) -0.003(3) C13 0.015(2) 0.028(3) 0.027(3) -0.008(2) 0.0012(18) 0.0053(19) C14 0.023(2) 0.023(3) 0.047(3) -0.010(3) -0.002(2) -0.001(2) C15 0.022(2) 0.029(3) 0.027(3) -0.011(2) 0.0006(19) 0.003(2) C16 0.022(2) 0.026(3) 0.027(3) -0.003(2) 0.0027(19) 0.004(2) C17 0.019(2) 0.031(3) 0.024(3) -0.004(2) 0.0004(18) -0.002(2) C18 0.028(2) 0.019(3) 0.028(3) -0.005(2) -0.0031(19) -0.004(2) C19 0.033(3) 0.026(3) 0.024(3) -0.003(2) -0.001(2) 0.002(2) C20 0.029(3) 0.041(3) 0.034(3) -0.015(3) 0.003(2) -0.014(2) C21 0.029(3) 0.024(3) 0.042(3) -0.011(2) 0.001(2) -0.002(2) C22 0.020(2) 0.019(3) 0.029(3) -0.006(2) -0.0009(18) 0.0064(19) C23 0.049(3) 0.022(3) 0.017(3) -0.003(2) -0.005(2) -0.004(2) C24 0.036(3) 0.034(3) 0.030(3) -0.015(3) 0.011(2) -0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O11 2.106(3) 1_655 ? Mn1 O8 2.146(4) . ? Mn1 O3 2.176(3) 2_566 ? Mn1 O2 2.190(4) . ? Mn1 O4 2.194(3) 1_545 ? Mn1 O5 2.224(4) . ? Mn2 O7 2.101(3) . ? Mn2 O10 2.134(4) 2_566 ? Mn2 O6 2.135(3) . ? Mn2 O9 2.197(3) 1_545 ? Mn2 O1 2.201(4) . ? Mn2 O4 2.488(3) 1_545 ? S1 C15 1.717(5) . ? S1 C13 1.740(4) . ? S2 C18 1.697(5) . ? S2 C16 1.729(5) . ? O1 C9 1.240(6) . ? O2 C12 1.240(6) . ? O3 C19 1.266(5) . ? O3 Mn1 2.176(3) 2_566 ? O4 C23 1.253(6) . ? O4 Mn1 2.194(3) 1_565 ? O4 Mn2 2.488(3) 1_565 ? O5 C7 1.266(7) . ? O6 C22 1.254(5) . ? O7 C17 1.251(5) . ? O8 C22 1.262(5) . ? O9 C23 1.266(6) . ? O9 Mn2 2.197(3) 1_565 ? O10 C19 1.245(6) . ? O10 Mn2 2.134(4) 2_566 ? O11 C17 1.265(5) . ? O11 Mn1 2.106(3) 1_455 ? C10 C5 1.435(11) . ? C10 C12 1.461(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C9 1.513(7) . ? C11 C6 1.513(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N3 C7 1.315(7) . ? N3 C4 1.436(7) . ? N3 H3A 0.8600 . ? C1 C2 1.528(10) . ? C1 C4 1.539(10) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C7 1.516(8) . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 N1 1.472(7) . ? C3 C5 1.541(9) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C8 1.462(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 N2 1.456(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.308(7) . ? N1 C12 1.263(8) . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? C13 C24 1.339(6) . ? C13 C17 1.501(6) . ? C14 C21 1.366(6) . ? C14 C18 1.373(6) . ? C14 H14A 0.9300 . ? C15 C20 1.350(6) . ? C15 C19 1.489(6) . ? C16 C21 1.351(6) . ? C16 C22 1.501(6) . ? C18 C23 1.480(7) . ? C20 C24 1.400(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C24 H24A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Mn1 O8 86.47(14) 1_655 . ? O11 Mn1 O3 85.48(13) 1_655 2_566 ? O8 Mn1 O3 92.74(14) . 2_566 ? O11 Mn1 O2 98.43(14) 1_655 . ? O8 Mn1 O2 83.85(14) . . ? O3 Mn1 O2 174.62(13) 2_566 . ? O11 Mn1 O4 175.97(12) 1_655 1_545 ? O8 Mn1 O4 91.65(13) . 1_545 ? O3 Mn1 O4 91.06(13) 2_566 1_545 ? O2 Mn1 O4 84.90(14) . 1_545 ? O11 Mn1 O5 86.77(14) 1_655 . ? O8 Mn1 O5 171.68(14) . . ? O3 Mn1 O5 91.55(15) 2_566 . ? O2 Mn1 O5 92.36(14) . . ? O4 Mn1 O5 95.39(14) 1_545 . ? O7 Mn2 O10 96.53(13) . 2_566 ? O7 Mn2 O6 100.51(14) . . ? O10 Mn2 O6 92.67(14) 2_566 . ? O7 Mn2 O9 103.31(13) . 1_545 ? O10 Mn2 O9 89.60(14) 2_566 1_545 ? O6 Mn2 O9 155.64(13) . 1_545 ? O7 Mn2 O1 92.85(13) . . ? O10 Mn2 O1 170.26(13) 2_566 . ? O6 Mn2 O1 88.17(14) . . ? O9 Mn2 O1 85.69(14) 1_545 . ? O7 Mn2 O4 159.12(13) . 1_545 ? O10 Mn2 O4 82.54(12) 2_566 1_545 ? O6 Mn2 O4 100.37(12) . 1_545 ? O9 Mn2 O4 55.90(11) 1_545 1_545 ? O1 Mn2 O4 87.76(12) . 1_545 ? C15 S1 C13 91.2(2) . . ? C18 S2 C16 91.5(2) . . ? C9 O1 Mn2 133.8(4) . . ? C12 O2 Mn1 132.4(4) . . ? C19 O3 Mn1 136.3(3) . 2_566 ? C23 O4 Mn1 154.2(4) . 1_565 ? C23 O4 Mn2 84.2(3) . 1_565 ? Mn1 O4 Mn2 108.05(12) 1_565 1_565 ? C7 O5 Mn1 125.6(3) . . ? C22 O6 Mn2 128.8(3) . . ? C17 O7 Mn2 146.1(3) . . ? C22 O8 Mn1 131.4(3) . . ? C23 O9 Mn2 97.2(3) . 1_565 ? C19 O10 Mn2 132.1(3) . 2_566 ? C17 O11 Mn1 142.7(3) . 1_455 ? C5 C10 C12 109.8(8) . . ? C5 C10 H10A 109.7 . . ? C12 C10 H10A 109.7 . . ? C5 C10 H10B 109.7 . . ? C12 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C9 C11 C6 104.0(5) . . ? C9 C11 H11A 110.9 . . ? C6 C11 H11A 110.9 . . ? C9 C11 H11B 110.9 . . ? C6 C11 H11B 110.9 . . ? H11A C11 H11B 109.0 . . ? C7 N3 C4 116.6(6) . . ? C7 N3 H3A 121.7 . . ? C4 N3 H3A 121.7 . . ? C2 C1 C4 109.0(6) . . ? C2 C1 H1B 109.9 . . ? C4 C1 H1B 109.9 . . ? C2 C1 H1C 109.9 . . ? C4 C1 H1C 109.9 . . ? H1B C1 H1C 108.3 . . ? C7 C2 C1 101.5(6) . . ? C7 C2 H2B 111.5 . . ? C1 C2 H2B 111.5 . . ? C7 C2 H2C 111.5 . . ? C1 C2 H2C 111.5 . . ? H2B C2 H2C 109.3 . . ? N1 C3 C5 98.9(5) . . ? N1 C3 H3B 112.0 . . ? C5 C3 H3B 112.0 . . ? N1 C3 H3C 112.0 . . ? C5 C3 H3C 112.0 . . ? H3B C3 H3C 109.7 . . ? N3 C4 C1 101.4(6) . . ? N3 C4 H4A 111.5 . . ? C1 C4 H4A 111.5 . . ? N3 C4 H4B 111.5 . . ? C1 C4 H4B 111.5 . . ? H4A C4 H4B 109.3 . . ? C10 C5 C3 105.4(6) . . ? C10 C5 H5A 110.7 . . ? C3 C5 H5A 110.7 . . ? C10 C5 H5B 110.7 . . ? C3 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C8 C6 C11 108.0(6) . . ? C8 C6 H6A 110.1 . . ? C11 C6 H6A 110.1 . . ? C8 C6 H6B 110.1 . . ? C11 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? O5 C7 N3 124.5(5) . . ? O5 C7 C2 124.8(6) . . ? N3 C7 C2 110.7(6) . . ? N2 C8 C6 104.2(5) . . ? N2 C8 H8A 110.9 . . ? C6 C8 H8A 110.9 . . ? N2 C8 H8B 110.9 . . ? C6 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? O1 C9 N2 127.2(5) . . ? O1 C9 C11 124.5(5) . . ? N2 C9 C11 108.3(5) . . ? C12 N1 C3 118.8(6) . . ? C12 N1 H1A 120.6 . . ? C3 N1 H1A 120.6 . . ? C9 N2 C8 115.3(5) . . ? C9 N2 H2A 122.4 . . ? C8 N2 H2A 122.4 . . ? O2 C12 N1 128.0(5) . . ? O2 C12 C10 126.6(7) . . ? N1 C12 C10 105.5(6) . . ? C24 C13 C17 131.0(4) . . ? C24 C13 S1 111.2(3) . . ? C17 C13 S1 117.7(3) . . ? C21 C14 C18 112.6(4) . . ? C21 C14 H14A 123.7 . . ? C18 C14 H14A 123.7 . . ? C20 C15 C19 127.8(4) . . ? C20 C15 S1 110.6(4) . . ? C19 C15 S1 121.5(3) . . ? C21 C16 C22 130.3(4) . . ? C21 C16 S2 110.2(4) . . ? C22 C16 S2 119.5(3) . . ? O7 C17 O11 123.6(4) . . ? O7 C17 C13 120.8(4) . . ? O11 C17 C13 115.5(4) . . ? C14 C18 C23 128.1(4) . . ? C14 C18 S2 111.3(3) . . ? C23 C18 S2 120.6(4) . . ? O10 C19 O3 126.2(4) . . ? O10 C19 C15 117.3(4) . . ? O3 C19 C15 116.5(4) . . ? C15 C20 C24 114.2(4) . . ? C15 C20 H20A 122.9 . . ? C24 C20 H20A 122.9 . . ? C16 C21 C14 114.4(5) . . ? C16 C21 H21A 122.8 . . ? C14 C21 H21A 122.8 . . ? O6 C22 O8 127.1(4) . . ? O6 C22 C16 116.9(4) . . ? O8 C22 C16 115.9(4) . . ? O4 C23 O9 122.7(5) . . ? O4 C23 C18 120.0(5) . . ? O9 C23 C18 117.3(4) . . ? C13 C24 C20 112.6(4) . . ? C13 C24 H24A 123.7 . . ? C20 C24 H24A 123.7 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.139 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.146 #end data_2_CCDC_934688 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H27 Mn3 N3 O15 S3' _chemical_formula_weight 930.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.4733(12) _cell_length_b 10.6596(6) _cell_length_c 21.7791(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.688(5) _cell_angle_gamma 90.00 _cell_volume 3820.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11827 _cell_measurement_theta_min 2.1265 _cell_measurement_theta_max 27.4778 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.211 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 28075 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.43 _reflns_number_total 8656 _reflns_number_gt 7172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8656 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1795 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 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 0.26134(4) 0.30605(6) -0.13458(3) 0.02195(18) Uani 1 1 d . . . Mn2 Mn 0.24741(4) 0.26517(6) 0.02553(3) 0.02176(18) Uani 1 1 d . . . Mn3 Mn 0.22672(4) 0.07881(6) 0.18757(3) 0.02095(17) Uani 1 1 d . . . S1 S 0.49356(8) 0.44511(13) 0.14572(5) 0.0378(3) Uani 1 1 d . . . S2 S -0.00783(7) 0.36916(13) 0.19653(5) 0.0346(3) Uani 1 1 d . . . S3 S 0.22711(8) 0.71832(11) 0.04261(5) 0.0314(3) Uani 1 1 d . . . O1 O 0.3419(2) 0.3265(4) 0.09011(17) 0.0445(9) Uani 1 1 d . . . O2 O 0.3145(3) 0.2144(5) 0.1730(2) 0.0627(13) Uani 1 1 d . . . O3 O 0.2203(3) 0.4544(3) 0.00691(17) 0.0434(9) Uani 1 1 d . . . O4 O 0.2727(2) 1.0756(3) 0.03906(17) 0.0394(9) Uani 1 1 d . . . O5 O 0.2895(2) 0.1240(4) -0.17248(17) 0.0428(9) Uani 1 1 d . . . O6 O 0.6394(2) 0.6057(3) 0.17596(16) 0.0373(8) Uani 1 1 d . . . O7 O -0.1630(2) 0.6485(4) 0.19722(15) 0.0357(8) Uani 1 1 d . . . O8 O 0.2231(2) 0.9556(3) 0.11307(15) 0.0408(9) Uani 1 1 d . . . O9 O -0.1357(2) 0.4893(4) 0.26131(15) 0.0407(9) Uani 1 1 d . . . O10 O 0.1361(2) 0.2194(4) 0.16943(16) 0.0400(9) Uani 1 1 d . . . O11 O 0.1323(2) 0.2539(3) 0.06795(15) 0.0337(8) Uani 1 1 d . . . O12 O 0.2434(2) 0.4822(3) -0.09259(16) 0.0413(9) Uani 1 1 d . . . O13 O 0.6865(2) 0.4860(4) 0.25482(18) 0.0498(10) Uani 1 1 d . . . O14 O 0.34023(19) 0.2589(3) -0.05025(14) 0.0313(7) Uani 1 1 d . . . O15 O 0.17933(19) 0.2083(3) -0.06757(14) 0.0311(7) Uani 1 1 d . . . C5 C 0.4652(4) 0.1959(10) -0.0940(3) 0.084(3) Uani 1 1 d . . . H5A H 0.4622 0.2552 -0.1278 0.101 Uiso 1 1 calc R . . H5B H 0.4471 0.1148 -0.1096 0.101 Uiso 1 1 calc R . . N2 N 0.2168(3) 0.0655(5) -0.2592(2) 0.0537(13) Uani 1 1 d . . . H2A H 0.1846 0.1291 -0.2607 0.064 Uiso 1 1 calc R . . N3 N 0.0520(3) 0.1600(6) -0.0393(2) 0.0506(13) Uani 1 1 d . . . H3A H 0.0575 0.1881 -0.0024 0.061 Uiso 1 1 calc R . . C1 C 0.5453(8) 0.2208(14) -0.0042(6) 0.143(5) Uiso 1 1 d . . . H1B H 0.5813 0.2906 0.0058 0.171 Uiso 1 1 calc R . . H1C H 0.5605 0.1502 0.0220 0.171 Uiso 1 1 calc R . . C2 C 0.5482(7) 0.1866(12) -0.0696(5) 0.114(4) Uiso 1 1 d . . . H2B H 0.5831 0.2438 -0.0909 0.137 Uiso 1 1 calc R . . H2C H 0.5686 0.1019 -0.0741 0.137 Uiso 1 1 calc R . . C3 C 0.0046(6) 0.0297(10) -0.1203(5) 0.098(3) Uiso 1 1 d . . . H3B H 0.0141 -0.0570 -0.1086 0.117 Uiso 1 1 calc R . . H3C H -0.0348 0.0322 -0.1548 0.117 Uiso 1 1 calc R . . C4 C 0.2701(6) -0.1283(11) -0.2788(5) 0.112(3) Uiso 1 1 d . . . H4A H 0.3074 -0.1530 -0.3098 0.134 Uiso 1 1 calc R . . H4B H 0.2410 -0.2023 -0.2661 0.134 Uiso 1 1 calc R . . N1 N 0.4594(6) 0.2564(9) 0.0031(5) 0.120(3) Uiso 1 1 d . . . H1A H 0.4415 0.2868 0.0365 0.144 Uiso 1 1 calc R . . C6 C 0.0829(4) 0.0929(8) -0.1363(3) 0.069(2) Uani 1 1 d . . . H6A H 0.0734 0.1520 -0.1698 0.082 Uiso 1 1 calc R . . H6B H 0.1226 0.0315 -0.1483 0.082 Uiso 1 1 calc R . . C7 C 0.4133(3) 0.2365(7) -0.0469(2) 0.0483(15) Uani 1 1 d . . . C8 C -0.0249(4) 0.1071(10) -0.0657(4) 0.089(3) Uani 1 1 d . . . H8A H -0.0623 0.1727 -0.0795 0.106 Uiso 1 1 calc R . . H8B H -0.0511 0.0541 -0.0362 0.106 Uiso 1 1 calc R . . C9 C 0.3160(5) -0.0718(6) -0.2248(3) 0.068(2) Uani 1 1 d . . . H9A H 0.3726 -0.0591 -0.2336 0.082 Uiso 1 1 calc R . . H9B H 0.3132 -0.1252 -0.1889 0.082 Uiso 1 1 calc R . . C10 C 0.4658(4) 0.2887(6) 0.2298(3) 0.0522(17) Uani 1 1 d . . . H10A H 0.4413 0.2277 0.2532 0.063 Uiso 1 1 calc R . . C11 C 0.2120(6) -0.0335(8) -0.3045(3) 0.082(3) Uani 1 1 d . . . H11A H 0.2281 -0.0036 -0.3442 0.098 Uiso 1 1 calc R . . H11B H 0.1574 -0.0676 -0.3088 0.098 Uiso 1 1 calc R . . C12 C -0.0458(4) 0.5284(6) 0.1129(2) 0.0455(14) Uani 1 1 d . . . H12A H -0.0702 0.5951 0.0915 0.055 Uiso 1 1 calc R . . C13 C 0.2509(3) 0.8706(5) -0.0457(2) 0.0376(11) Uani 1 1 d . . . H13A H 0.2597 0.9435 -0.0679 0.045 Uiso 1 1 calc R . . C14 C 0.4333(3) 0.3306(5) 0.1755(2) 0.0360(11) Uani 1 1 d . . . C15 C 0.5402(4) 0.3458(6) 0.2477(3) 0.0535(17) Uani 1 1 d . . . H15A H 0.5702 0.3261 0.2836 0.064 Uiso 1 1 calc R . . C16 C 0.0144(3) 0.4522(6) 0.0887(2) 0.0406(13) Uani 1 1 d . . . H16A H 0.0331 0.4616 0.0493 0.049 Uiso 1 1 calc R . . C17 C 0.1115(3) 0.1599(5) -0.0783(2) 0.0329(10) Uani 1 1 d . . . C18 C 0.3571(3) 0.2879(5) 0.1437(2) 0.0345(11) Uani 1 1 d . . . C19 C 0.0422(3) 0.3632(5) 0.1289(2) 0.0305(10) Uani 1 1 d . . . C20 C 0.2744(4) 0.0513(5) -0.2149(2) 0.0385(11) Uani 1 1 d . . . C21 C 0.2461(4) 0.7491(5) -0.0724(2) 0.0419(13) Uani 1 1 d . . . H21A H 0.2507 0.7335 -0.1141 0.050 Uiso 1 1 calc R . . C22 C 0.2454(3) 0.9752(4) 0.0592(2) 0.0281(9) Uani 1 1 d . . . C23 C 0.6360(3) 0.5152(5) 0.2124(2) 0.0307(10) Uani 1 1 d . . . C24 C 0.5629(3) 0.4328(5) 0.2065(2) 0.0310(10) Uani 1 1 d . . . C25 C 0.2341(3) 0.6581(4) -0.0299(2) 0.0290(10) Uani 1 1 d . . . C26 C -0.1257(3) 0.5472(5) 0.2122(2) 0.0305(10) Uani 1 1 d . . . C27 C 0.1086(3) 0.2714(4) 0.12172(19) 0.0257(9) Uani 1 1 d . . . C28 C 0.2410(3) 0.8681(4) 0.0166(2) 0.0278(9) Uani 1 1 d . . . C29 C 0.2319(3) 0.5196(4) -0.0392(2) 0.0309(10) Uani 1 1 d . . . C30 C -0.0650(3) 0.4946(5) 0.1711(2) 0.0313(10) 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 0.0236(3) 0.0231(3) 0.0189(3) -0.0017(2) -0.0014(2) 0.0003(2) Mn2 0.0249(4) 0.0200(3) 0.0201(3) -0.0007(2) -0.0012(2) -0.0016(2) Mn3 0.0199(3) 0.0230(3) 0.0197(3) 0.0004(2) -0.0019(2) -0.0001(2) S1 0.0371(7) 0.0473(8) 0.0278(6) 0.0080(5) -0.0095(5) -0.0195(6) S2 0.0378(7) 0.0443(7) 0.0223(5) 0.0070(5) 0.0069(4) 0.0182(5) S3 0.0492(7) 0.0216(5) 0.0237(5) -0.0013(4) 0.0039(5) -0.0006(5) O1 0.044(2) 0.049(2) 0.0395(19) -0.0003(18) -0.0143(16) -0.0156(18) O2 0.054(3) 0.079(3) 0.055(3) 0.001(2) -0.003(2) -0.043(2) O3 0.070(3) 0.0231(17) 0.0380(19) 0.0003(16) 0.0089(18) 0.0025(17) O4 0.057(2) 0.0161(16) 0.045(2) -0.0027(15) 0.0006(17) 0.0025(14) O5 0.050(2) 0.037(2) 0.0416(19) -0.0122(17) 0.0017(16) 0.0073(17) O6 0.0323(19) 0.038(2) 0.0424(19) -0.0006(17) 0.0040(15) -0.0101(15) O7 0.0292(17) 0.046(2) 0.0306(16) -0.0095(16) -0.0070(13) 0.0182(15) O8 0.063(2) 0.0327(19) 0.0267(16) -0.0075(15) 0.0076(16) -0.0045(17) O9 0.042(2) 0.051(2) 0.0298(17) -0.0036(17) 0.0064(14) 0.0183(17) O10 0.047(2) 0.043(2) 0.0298(17) 0.0051(16) -0.0013(15) 0.0243(17) O11 0.0335(19) 0.041(2) 0.0267(16) -0.0031(15) 0.0075(13) 0.0074(15) O12 0.065(2) 0.0260(18) 0.0324(17) -0.0094(15) -0.0003(16) 0.0056(17) O13 0.042(2) 0.056(3) 0.049(2) 0.002(2) -0.0231(17) -0.0170(19) O14 0.0240(17) 0.043(2) 0.0268(16) 0.0050(14) -0.0007(12) 0.0028(14) O15 0.0290(17) 0.042(2) 0.0224(15) -0.0043(14) -0.0023(12) -0.0085(14) C5 0.042(4) 0.154(9) 0.057(4) 0.009(5) 0.003(3) 0.021(5) N2 0.072(4) 0.039(3) 0.049(3) -0.003(2) -0.014(3) 0.009(2) N3 0.034(2) 0.080(4) 0.038(2) -0.002(2) -0.0005(19) -0.009(2) C6 0.057(4) 0.119(7) 0.030(3) -0.018(3) 0.001(3) -0.042(4) C7 0.025(3) 0.087(5) 0.033(3) 0.006(3) -0.005(2) 0.002(3) C8 0.043(4) 0.156(9) 0.066(5) 0.014(5) -0.004(3) -0.040(5) C9 0.109(6) 0.040(4) 0.056(4) -0.012(3) -0.002(4) 0.030(4) C10 0.050(3) 0.068(4) 0.038(3) 0.018(3) -0.009(2) -0.034(3) C11 0.130(7) 0.060(5) 0.052(4) -0.019(4) -0.027(4) 0.004(5) C12 0.059(3) 0.049(3) 0.029(2) 0.012(2) 0.007(2) 0.029(3) C13 0.062(3) 0.022(2) 0.029(2) 0.002(2) 0.007(2) 0.000(2) C14 0.033(3) 0.041(3) 0.033(2) 0.000(2) -0.0009(19) -0.018(2) C15 0.055(4) 0.066(4) 0.037(3) 0.023(3) -0.018(2) -0.031(3) C16 0.044(3) 0.057(3) 0.022(2) 0.012(2) 0.011(2) 0.023(3) C17 0.026(2) 0.042(3) 0.031(2) 0.001(2) -0.0051(18) -0.005(2) C18 0.029(2) 0.039(3) 0.036(2) -0.007(2) -0.0009(19) -0.013(2) C19 0.028(2) 0.038(3) 0.026(2) 0.000(2) 0.0005(17) 0.0110(19) C20 0.054(3) 0.031(3) 0.032(2) 0.002(2) 0.007(2) 0.001(2) C21 0.079(4) 0.027(3) 0.020(2) -0.0052(19) 0.006(2) 0.004(2) C22 0.028(2) 0.024(2) 0.031(2) -0.0024(19) -0.0043(17) 0.0014(18) C23 0.026(2) 0.037(3) 0.030(2) -0.011(2) 0.0033(17) -0.0086(19) C24 0.031(2) 0.036(3) 0.026(2) -0.0012(19) -0.0036(18) -0.0093(19) C25 0.039(3) 0.022(2) 0.026(2) -0.0045(18) -0.0035(18) 0.0001(18) C26 0.030(2) 0.037(3) 0.024(2) -0.0052(19) -0.0037(17) 0.0076(19) C27 0.026(2) 0.027(2) 0.023(2) -0.0011(18) -0.0005(16) 0.0032(17) C28 0.036(2) 0.018(2) 0.029(2) -0.0005(18) 0.0038(18) 0.0006(17) C29 0.038(3) 0.021(2) 0.033(2) -0.0033(19) -0.0036(19) 0.0024(18) C30 0.031(2) 0.039(3) 0.024(2) 0.000(2) 0.0009(17) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O12 2.116(3) . ? Mn1 O6 2.123(3) 3_665 ? Mn1 O7 2.125(3) 3_565 ? Mn1 O5 2.167(4) . ? Mn1 O14 2.256(3) . ? Mn1 O15 2.286(3) . ? Mn2 O4 2.081(3) 1_545 ? Mn2 O3 2.101(4) . ? Mn2 O1 2.150(3) . ? Mn2 O11 2.152(3) . ? Mn2 O14 2.303(3) . ? Mn2 O15 2.350(3) . ? Mn3 O2 2.079(4) . ? Mn3 O8 2.086(3) 1_545 ? Mn3 O13 2.104(3) 2_645 ? Mn3 O9 2.135(3) 2_545 ? Mn3 O10 2.139(3) . ? S1 C24 1.713(5) . ? S1 C14 1.719(5) . ? S2 C30 1.712(5) . ? S2 C19 1.722(5) . ? S3 C28 1.713(5) . ? S3 C25 1.714(4) . ? O1 C18 1.252(6) . ? O2 C18 1.247(6) . ? O3 C29 1.243(6) . ? O4 C22 1.249(6) . ? O4 Mn2 2.081(3) 1_565 ? O5 C20 1.222(6) . ? O6 C23 1.252(6) . ? O6 Mn1 2.123(3) 3_665 ? O7 C26 1.276(6) . ? O7 Mn1 2.125(3) 3_565 ? O8 C22 1.263(6) . ? O8 Mn3 2.086(3) 1_565 ? O9 C26 1.252(6) . ? O9 Mn3 2.135(3) 2 ? O10 C27 1.244(5) . ? O11 C27 1.265(5) . ? O12 C29 1.253(6) . ? O13 C23 1.253(6) . ? O13 Mn3 2.104(3) 2_655 ? O14 C7 1.225(6) . ? O15 C17 1.242(5) . ? C5 C7 1.434(9) . ? C5 C2 1.447(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N2 C20 1.330(7) . ? N2 C11 1.444(8) . ? N2 H2A 0.8600 . ? N3 C17 1.327(7) . ? N3 C8 1.478(8) . ? N3 H3A 0.8600 . ? C1 C2 1.475(16) . ? C1 N1 1.480(15) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C6 1.509(11) . ? C3 C8 1.546(13) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C11 1.483(12) . ? C4 C9 1.495(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N1 C7 1.315(11) . ? N1 H1A 0.8600 . ? C6 C17 1.509(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C20 1.501(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C14 1.351(7) . ? C10 C15 1.407(7) . ? C10 H10A 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C30 1.370(6) . ? C12 C16 1.404(7) . ? C12 H12A 0.9300 . ? C13 C28 1.374(6) . ? C13 C21 1.420(7) . ? C13 H13A 0.9300 . ? C14 C18 1.476(6) . ? C15 C24 1.354(7) . ? C15 H15A 0.9300 . ? C16 C19 1.357(7) . ? C16 H16A 0.9300 . ? C19 C27 1.481(6) . ? C21 C25 1.361(7) . ? C21 H21A 0.9300 . ? C22 C28 1.471(6) . ? C23 C24 1.491(6) . ? C25 C29 1.490(6) . ? C26 C30 1.483(6) . ? 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 O12 Mn1 O6 85.18(15) . 3_665 ? O12 Mn1 O7 87.54(14) . 3_565 ? O6 Mn1 O7 101.85(14) 3_665 3_565 ? O12 Mn1 O5 174.92(15) . . ? O6 Mn1 O5 93.02(15) 3_665 . ? O7 Mn1 O5 97.47(14) 3_565 . ? O12 Mn1 O14 86.13(14) . . ? O6 Mn1 O14 91.06(13) 3_665 . ? O7 Mn1 O14 165.08(13) 3_565 . ? O5 Mn1 O14 89.17(14) . . ? O12 Mn1 O15 91.72(14) . . ? O6 Mn1 O15 164.32(13) 3_665 . ? O7 Mn1 O15 93.34(13) 3_565 . ? O5 Mn1 O15 88.76(14) . . ? O14 Mn1 O15 73.38(12) . . ? O4 Mn2 O3 176.94(15) 1_545 . ? O4 Mn2 O1 93.91(15) 1_545 . ? O3 Mn2 O1 88.60(16) . . ? O4 Mn2 O11 93.42(14) 1_545 . ? O3 Mn2 O11 87.30(14) . . ? O1 Mn2 O11 111.21(14) . . ? O4 Mn2 O14 86.45(14) 1_545 . ? O3 Mn2 O14 91.82(13) . . ? O1 Mn2 O14 89.59(14) . . ? O11 Mn2 O14 159.14(13) . . ? O4 Mn2 O15 87.48(14) 1_545 . ? O3 Mn2 O15 89.57(14) . . ? O1 Mn2 O15 160.79(14) . . ? O11 Mn2 O15 87.79(12) . . ? O14 Mn2 O15 71.35(11) . . ? O2 Mn3 O8 108.25(17) . 1_545 ? O2 Mn3 O13 87.72(19) . 2_645 ? O8 Mn3 O13 99.30(16) 1_545 2_645 ? O2 Mn3 O9 154.30(17) . 2_545 ? O8 Mn3 O9 97.44(14) 1_545 2_545 ? O13 Mn3 O9 87.32(16) 2_645 2_545 ? O2 Mn3 O10 88.23(19) . . ? O8 Mn3 O10 107.65(15) 1_545 . ? O13 Mn3 O10 152.64(15) 2_645 . ? O9 Mn3 O10 84.71(15) 2_545 . ? C24 S1 C14 91.7(2) . . ? C30 S2 C19 91.8(2) . . ? C28 S3 C25 91.6(2) . . ? C18 O1 Mn2 128.1(3) . . ? C18 O2 Mn3 158.0(4) . . ? C29 O3 Mn2 130.8(3) . . ? C22 O4 Mn2 144.0(3) . 1_565 ? C20 O5 Mn1 144.7(4) . . ? C23 O6 Mn1 132.0(3) . 3_665 ? C26 O7 Mn1 134.4(3) . 3_565 ? C22 O8 Mn3 128.3(3) . 1_565 ? C26 O9 Mn3 110.4(3) . 2 ? C27 O10 Mn3 133.6(3) . . ? C27 O11 Mn2 134.8(3) . . ? C29 O12 Mn1 135.6(3) . . ? C23 O13 Mn3 137.1(4) . 2_655 ? C7 O14 Mn1 128.2(3) . . ? C7 O14 Mn2 130.2(3) . . ? Mn1 O14 Mn2 101.57(13) . . ? C17 O15 Mn1 128.5(3) . . ? C17 O15 Mn2 131.1(3) . . ? Mn1 O15 Mn2 99.25(12) . . ? C7 C5 C2 110.1(7) . . ? C7 C5 H5A 109.6 . . ? C2 C5 H5A 109.6 . . ? C7 C5 H5B 109.6 . . ? C2 C5 H5B 109.6 . . ? H5A C5 H5B 108.2 . . ? C20 N2 C11 115.3(6) . . ? C20 N2 H2A 122.4 . . ? C11 N2 H2A 122.4 . . ? C17 N3 C8 113.4(5) . . ? C17 N3 H3A 123.3 . . ? C8 N3 H3A 123.3 . . ? C2 C1 N1 104.0(11) . . ? C2 C1 H1B 111.0 . . ? N1 C1 H1B 111.0 . . ? C2 C1 H1C 110.9 . . ? N1 C1 H1C 111.0 . . ? H1B C1 H1C 109.0 . . ? C5 C2 C1 105.3(10) . . ? C5 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? C5 C2 H2C 110.7 . . ? C1 C2 H2C 110.7 . . ? H2B C2 H2C 108.8 . . ? C6 C3 C8 104.1(7) . . ? C6 C3 H3B 110.9 . . ? C8 C3 H3B 110.9 . . ? C6 C3 H3C 110.9 . . ? C8 C3 H3C 110.9 . . ? H3B C3 H3C 109.0 . . ? C11 C4 C9 108.4(8) . . ? C11 C4 H4A 110.0 . . ? C9 C4 H4A 110.0 . . ? C11 C4 H4B 110.0 . . ? C9 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C7 N1 C1 112.8(10) . . ? C7 N1 H1A 123.6 . . ? C1 N1 H1A 123.6 . . ? C3 C6 C17 104.8(5) . . ? C3 C6 H6A 110.8 . . ? C17 C6 H6A 110.8 . . ? C3 C6 H6B 110.8 . . ? C17 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? O14 C7 N1 123.1(7) . . ? O14 C7 C5 129.2(5) . . ? N1 C7 C5 107.5(7) . . ? N3 C8 C3 102.0(6) . . ? N3 C8 H8A 111.4 . . ? C3 C8 H8A 111.4 . . ? N3 C8 H8B 111.4 . . ? C3 C8 H8B 111.4 . . ? H8A C8 H8B 109.2 . . ? C4 C9 C20 104.3(7) . . ? C4 C9 H9A 110.9 . . ? C20 C9 H9A 110.9 . . ? C4 C9 H9B 110.9 . . ? C20 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? C14 C10 C15 113.8(5) . . ? C14 C10 H10A 123.1 . . ? C15 C10 H10A 123.1 . . ? N2 C11 C4 103.1(7) . . ? N2 C11 H11A 111.1 . . ? C4 C11 H11A 111.1 . . ? N2 C11 H11B 111.1 . . ? C4 C11 H11B 111.1 . . ? H11A C11 H11B 109.1 . . ? C30 C12 C16 113.2(4) . . ? C30 C12 H12A 123.4 . . ? C16 C12 H12A 123.4 . . ? C28 C13 C21 112.3(4) . . ? C28 C13 H13A 123.8 . . ? C21 C13 H13A 123.8 . . ? C10 C14 C18 127.0(5) . . ? C10 C14 S1 110.7(4) . . ? C18 C14 S1 122.3(4) . . ? C24 C15 C10 112.2(5) . . ? C24 C15 H15A 123.9 . . ? C10 C15 H15A 123.9 . . ? C19 C16 C12 112.6(4) . . ? C19 C16 H16A 123.7 . . ? C12 C16 H16A 123.7 . . ? O15 C17 N3 124.4(5) . . ? O15 C17 C6 126.7(5) . . ? N3 C17 C6 108.9(4) . . ? O2 C18 O1 126.1(5) . . ? O2 C18 C14 116.2(5) . . ? O1 C18 C14 117.7(4) . . ? C16 C19 C27 128.5(4) . . ? C16 C19 S2 111.5(3) . . ? C27 C19 S2 120.0(3) . . ? O5 C20 N2 126.1(5) . . ? O5 C20 C9 125.8(6) . . ? N2 C20 C9 108.1(5) . . ? C25 C21 C13 112.3(4) . . ? C25 C21 H21A 123.9 . . ? C13 C21 H21A 123.9 . . ? O4 C22 O8 126.4(4) . . ? O4 C22 C28 116.8(4) . . ? O8 C22 C28 116.8(4) . . ? O6 C23 O13 127.6(4) . . ? O6 C23 C24 117.4(4) . . ? O13 C23 C24 115.0(4) . . ? C15 C24 C23 126.4(5) . . ? C15 C24 S1 111.6(4) . . ? C23 C24 S1 121.9(4) . . ? C21 C25 C29 128.1(4) . . ? C21 C25 S3 112.2(4) . . ? C29 C25 S3 119.6(3) . . ? O9 C26 O7 123.7(4) . . ? O9 C26 C30 116.6(4) . . ? O7 C26 C30 119.7(4) . . ? O10 C27 O11 126.2(4) . . ? O10 C27 C19 116.6(4) . . ? O11 C27 C19 117.2(4) . . ? C13 C28 C22 127.1(4) . . ? C13 C28 S3 111.6(4) . . ? C22 C28 S3 121.2(3) . . ? O3 C29 O12 127.4(4) . . ? O3 C29 C25 116.7(4) . . ? O12 C29 C25 115.9(4) . . ? C12 C30 C26 130.6(4) . . ? C12 C30 S2 110.9(4) . . ? C26 C30 S2 118.5(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.327 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.244 #end data_3_CCDC_934689 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H11 Mn N O5 S' _chemical_formula_weight 312.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.857(9) _cell_length_b 18.273(13) _cell_length_c 11.496(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.20(2) _cell_angle_gamma 90.00 _cell_volume 2459(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3585 _cell_measurement_theta_min 2.0633 _cell_measurement_theta_max 25.0473 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.255 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5289 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.06 _reflns_number_total 2160 _reflns_number_gt 1733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1443P)^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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.016(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2160 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.2340 _refine_ls_wR_factor_gt 0.1539 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.008 _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 0.23040(7) 0.2500 0.0202(5) Uani 1 2 d S . . Mn2 Mn 0.2500 0.2500 0.0000 0.0202(5) Uani 1 2 d S . . S1 S 0.26796(14) 0.00343(9) 0.31886(14) 0.0347(6) Uani 1 1 d . . . O5 O 0.2192(3) 0.1872(2) 0.1473(3) 0.0276(10) Uani 1 1 d . . . O4 O 0.2262(4) -0.1497(2) 0.3988(4) 0.0340(11) Uani 1 1 d . . . O3 O 0.3725(3) 0.1495(2) 0.2718(4) 0.0343(11) Uani 1 1 d . . . O2 O 0.1137(3) -0.1817(2) 0.2328(4) 0.0330(11) Uani 1 1 d . . . O1 O 0.5600(3) 0.2237(2) 0.4479(3) 0.0271(10) Uani 1 1 d . . . C10 C 0.2755(5) 0.1406(3) 0.2099(5) 0.0245(13) Uani 1 1 d . . . C9 C 0.1715(4) -0.1376(3) 0.2989(5) 0.0231(13) Uani 1 1 d . . . C8 C 0.1406(6) 0.0388(4) 0.1297(7) 0.0460(18) Uani 1 1 d . . . H8A H 0.1049 0.0650 0.0647 0.055 Uiso 1 1 calc R . . C7 C 0.2232(5) 0.0668(3) 0.2113(5) 0.0268(13) Uani 1 1 d . . . C6 C 0.1753(4) -0.0616(3) 0.2513(5) 0.0247(13) Uani 1 1 d . . . C5 C 0.1140(6) -0.0343(4) 0.1527(6) 0.0424(17) Uani 1 1 d . . . H5A H 0.0590 -0.0613 0.1039 0.051 Uiso 1 1 calc R . . C4 C 0.5002(6) 0.1890(5) 0.5119(6) 0.053(2) Uani 1 1 d . . . C3 C 0.5070(7) 0.1053(5) 0.5139(7) 0.065(3) Uani 1 1 d . . . H3A H 0.4323 0.0853 0.5150 0.097 Uiso 1 1 calc R . . H3B H 0.5577 0.0897 0.5831 0.097 Uiso 1 1 calc R . . H3C H 0.5353 0.0884 0.4450 0.097 Uiso 1 1 calc R . . C2 C 0.4311(7) 0.3009(6) 0.5701(8) 0.065(2) Uani 1 1 d . . . H2A H 0.4594 0.3181 0.5013 0.098 Uiso 1 1 calc R . . H2B H 0.4776 0.3202 0.6393 0.098 Uiso 1 1 calc R . . H2C H 0.3536 0.3170 0.5676 0.098 Uiso 1 1 calc R . . N1 N 0.4351(5) 0.2207(6) 0.5734(6) 0.071(3) Uani 1 1 d . . . C1 C 0.3626(9) 0.1826(7) 0.6457(9) 0.085(3) Uiso 1 1 d . . . H1A H 0.4087 0.1505 0.6997 0.127 Uiso 1 1 calc R . . H1B H 0.3058 0.1546 0.5957 0.127 Uiso 1 1 calc R . . H1C H 0.3257 0.2178 0.6890 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0186(7) 0.0143(8) 0.0270(8) 0.000 0.0015(5) 0.000 Mn2 0.0220(7) 0.0142(8) 0.0239(8) 0.0012(5) 0.0018(5) 0.0012(4) S1 0.0404(10) 0.0189(10) 0.0384(10) 0.0091(7) -0.0130(7) -0.0099(6) O5 0.031(2) 0.020(2) 0.032(2) 0.0097(18) 0.0034(17) 0.0004(17) O4 0.046(3) 0.018(2) 0.035(2) 0.0035(19) -0.002(2) -0.0057(18) O3 0.030(2) 0.024(3) 0.044(3) 0.0095(19) -0.0071(19) -0.0098(18) O2 0.036(2) 0.020(2) 0.042(2) 0.0017(19) 0.0050(19) -0.0106(18) O1 0.024(2) 0.034(3) 0.025(2) 0.0015(18) 0.0049(16) -0.0084(17) C10 0.027(3) 0.022(3) 0.024(3) 0.004(2) 0.006(2) -0.002(2) C9 0.024(3) 0.014(3) 0.032(3) -0.001(2) 0.007(2) -0.001(2) C8 0.045(4) 0.026(4) 0.059(4) 0.012(3) -0.016(3) -0.006(3) C7 0.026(3) 0.020(3) 0.033(3) 0.005(3) -0.001(2) -0.002(2) C6 0.023(3) 0.016(3) 0.033(3) 0.002(2) -0.002(2) -0.006(2) C5 0.049(4) 0.030(4) 0.041(4) 0.003(3) -0.014(3) -0.017(3) C4 0.034(4) 0.088(7) 0.032(4) 0.018(4) -0.009(3) -0.021(4) C3 0.062(5) 0.051(5) 0.069(5) 0.028(4) -0.029(4) -0.026(4) C2 0.055(5) 0.071(7) 0.073(6) -0.006(5) 0.023(4) 0.007(4) N1 0.030(3) 0.136(9) 0.049(4) 0.012(4) 0.017(3) -0.007(4) _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 O2 2.126(4) 4 ? Mn1 O2 2.126(4) 3 ? Mn1 O3 2.158(4) . ? Mn1 O3 2.158(4) 2_655 ? Mn1 O1 2.276(4) 2_655 ? Mn1 O1 2.276(4) . ? Mn2 O5 2.125(4) . ? Mn2 O5 2.125(4) 7 ? Mn2 O4 2.165(4) 6 ? Mn2 O4 2.165(4) 4 ? Mn2 O1 2.288(4) 8_455 ? Mn2 O1 2.288(4) 2_655 ? S1 C7 1.715(6) . ? S1 C6 1.717(6) . ? O5 C10 1.239(7) . ? O4 C9 1.245(7) . ? O4 Mn2 2.165(4) 4_545 ? O3 C10 1.263(7) . ? O2 C9 1.238(7) . ? O2 Mn1 2.126(4) 3_445 ? O1 C4 1.270(8) . ? O1 Mn2 2.288(4) 2_655 ? C10 C7 1.485(8) . ? C9 C6 1.496(8) . ? C8 C7 1.345(9) . ? C8 C5 1.408(10) . ? C8 H8A 0.9300 . ? C6 C5 1.341(9) . ? C5 H5A 0.9300 . ? C4 N1 1.268(11) . ? C4 C3 1.531(14) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C2 N1 1.467(14) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? N1 C1 1.464(13) . ? C1 H1A 0.9603 . ? C1 H1B 0.9603 . ? C1 H1C 0.9603 . ? 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 O2 Mn1 O2 81.9(2) 4 3 ? O2 Mn1 O3 92.31(18) 4 . ? O2 Mn1 O3 174.17(17) 3 . ? O2 Mn1 O3 174.17(17) 4 2_655 ? O2 Mn1 O3 92.31(18) 3 2_655 ? O3 Mn1 O3 93.5(2) . 2_655 ? O2 Mn1 O1 91.84(15) 4 2_655 ? O2 Mn1 O1 92.81(16) 3 2_655 ? O3 Mn1 O1 88.10(16) . 2_655 ? O3 Mn1 O1 87.68(15) 2_655 2_655 ? O2 Mn1 O1 92.81(16) 4 . ? O2 Mn1 O1 91.84(15) 3 . ? O3 Mn1 O1 87.68(15) . . ? O3 Mn1 O1 88.10(16) 2_655 . ? O1 Mn1 O1 173.8(2) 2_655 . ? O5 Mn2 O5 180.00(18) . 7 ? O5 Mn2 O4 86.96(17) . 6 ? O5 Mn2 O4 93.04(17) 7 6 ? O5 Mn2 O4 93.04(17) . 4 ? O5 Mn2 O4 86.96(17) 7 4 ? O4 Mn2 O4 180.00(12) 6 4 ? O5 Mn2 O1 91.97(14) . 8_455 ? O5 Mn2 O1 88.03(14) 7 8_455 ? O4 Mn2 O1 89.95(15) 6 8_455 ? O4 Mn2 O1 90.05(15) 4 8_455 ? O5 Mn2 O1 88.03(14) . 2_655 ? O5 Mn2 O1 91.97(14) 7 2_655 ? O4 Mn2 O1 90.05(15) 6 2_655 ? O4 Mn2 O1 89.95(15) 4 2_655 ? O1 Mn2 O1 180.0 8_455 2_655 ? C7 S1 C6 92.2(3) . . ? C10 O5 Mn2 133.5(4) . . ? C9 O4 Mn2 130.5(4) . 4_545 ? C10 O3 Mn1 127.9(4) . . ? C9 O2 Mn1 137.1(4) . 3_445 ? C4 O1 Mn1 119.5(4) . . ? C4 O1 Mn2 124.8(4) . 2_655 ? Mn1 O1 Mn2 112.81(15) . 2_655 ? O5 C10 O3 126.6(6) . . ? O5 C10 C7 116.3(5) . . ? O3 C10 C7 117.0(5) . . ? O2 C9 O4 127.3(5) . . ? O2 C9 C6 115.2(5) . . ? O4 C9 C6 117.5(5) . . ? C7 C8 C5 113.0(6) . . ? C7 C8 H8A 123.5 . . ? C5 C8 H8A 123.5 . . ? C8 C7 C10 126.6(5) . . ? C8 C7 S1 110.6(5) . . ? C10 C7 S1 122.7(4) . . ? C5 C6 C9 127.6(5) . . ? C5 C6 S1 110.3(5) . . ? C9 C6 S1 122.0(4) . . ? C6 C5 C8 113.8(6) . . ? C6 C5 H5A 123.1 . . ? C8 C5 H5A 123.1 . . ? N1 C4 O1 122.7(9) . . ? N1 C4 C3 118.9(8) . . ? O1 C4 C3 118.4(8) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C2 H2A 109.4 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 N1 C1 124.4(10) . . ? C4 N1 C2 117.6(7) . . ? C1 N1 C2 118.1(8) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.4 . . ? N1 C1 H1C 109.4 . . ? H1A C1 H1C 109.4 . . ? H1B C1 H1C 109.4 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.260 _refine_diff_density_min -1.493 _refine_diff_density_rms 0.389 #end data_4_CCDC_934690 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H7 Mn2 O10 S2' _chemical_formula_weight 509.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/nmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 22.7772(16) _cell_length_b 22.7772(16) _cell_length_c 12.8156(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6648.7(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14944 _cell_measurement_theta_min 2.0308 _cell_measurement_theta_max 23.2791 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5589 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14522 _diffrn_reflns_av_R_equivalents 0.1153 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 18.99 _reflns_number_total 1425 _reflns_number_gt 1074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The high R factors are due to the presence of large pores in this structure, and the guest molecules in the pores are all structurally disorder. The low Theta(max) is related with the quality of the crystal. Because it is a framework structure with large pores, the high angle reflections are too weak to be determined. ; _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^)+(0.2500P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1425 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1448 _refine_ls_R_factor_gt 0.1221 _refine_ls_wR_factor_ref 0.3353 _refine_ls_wR_factor_gt 0.3106 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.56269(7) 0.43731(7) -0.2500 0.0251(12) Uani 1 2 d S . . Mn2 Mn 0.5000 0.5000 0.0000 0.0239(13) Uani 1 2 d S . . S2 S 0.2500 0.5496(2) 0.0942(3) 0.0539(17) Uani 1 2 d S . . S1 S 0.5067(2) 0.2500 -0.1283(3) 0.0471(16) Uani 1 2 d S . . C8 C 0.5004(4) 0.3668(5) -0.0721(10) 0.035(3) Uiso 1 1 d . . . O4 O 0.4063(4) 0.5078(3) -0.0105(5) 0.031(2) Uiso 1 1 d . . . O3 O 0.4909(3) 0.4903(3) 0.1675(6) 0.037(3) Uani 1 1 d . . . O2 O 0.5110(3) 0.3747(3) -0.1659(6) 0.050(3) Uani 1 1 d . . . C7 C 0.5196(6) 0.4804(6) 0.2500 0.045(5) Uiso 1 2 d S . . O1 O 0.4923(3) 0.4052(4) -0.0049(5) 0.036(2) Uani 1 1 d . . . C6 C 0.4992(5) 0.3049(5) -0.0380(8) 0.039(3) Uani 1 1 d . . . C5 C 0.3048(5) 0.5277(6) 0.0106(9) 0.044(3) Uani 1 1 d . . . C4 C 0.5641(8) 0.4359(8) 0.2500 0.097(10) Uiso 1 2 d S . . H4A H 0.5807 0.4326 0.3186 0.145 Uiso 0.50 1 calc PR . . H4B H 0.5944 0.4463 0.2012 0.145 Uiso 0.50 1 calc PR . . H4C H 0.5471 0.3990 0.2302 0.145 Uiso 0.50 1 calc PR . . C3 C 0.4881(9) 0.2831(6) 0.0595(12) 0.103(7) Uani 1 1 d . . . H3A H 0.4815 0.3061 0.1183 0.124 Uiso 1 1 calc R . . C2 C 0.2816(5) 0.5069(5) -0.0822(10) 0.046(4) Uani 1 1 d . . . H2A H 0.3043 0.4943 -0.1382 0.055 Uiso 1 1 calc R . . O5 O 0.3731(6) 0.5539(7) 0.1298(12) 0.016(4) Uiso 0.50 1 d P . . C1 C 0.3689(5) 0.5321(5) 0.0423(10) 0.050(4) Uani 1 1 d . . . O5' O 0.3803(8) 0.5763(9) 0.1210(14) 0.048(7) Uiso 0.50 1 d P . . 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 0.0250(15) 0.0250(15) 0.0251(19) 0.0012(6) 0.0012(6) -0.0005(10) Mn2 0.0246(18) 0.0214(18) 0.026(2) -0.0008(10) 0.0007(10) 0.0014(10) S2 0.022(3) 0.108(4) 0.031(3) -0.013(2) 0.000 0.000 S1 0.079(4) 0.026(3) 0.036(3) 0.000 0.022(2) 0.000 O3 0.050(5) 0.035(5) 0.026(6) 0.004(4) -0.013(4) 0.013(4) O2 0.087(6) 0.030(5) 0.032(5) -0.003(4) 0.010(4) -0.018(4) O1 0.048(5) 0.032(5) 0.029(4) 0.000(4) 0.003(3) -0.003(4) C6 0.062(8) 0.036(7) 0.021(7) 0.018(6) -0.001(5) -0.002(5) C5 0.038(8) 0.052(8) 0.042(8) -0.003(6) 0.003(6) 0.014(6) C3 0.21(2) 0.029(7) 0.067(11) 0.012(8) 0.077(12) 0.032(10) C2 0.035(6) 0.063(9) 0.040(8) -0.022(6) 0.012(6) 0.006(6) C1 0.045(9) 0.046(8) 0.060(9) 0.005(7) -0.013(7) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5' 2.124(17) 9_665 ? Mn1 O5' 2.124(17) 16 ? Mn1 O5 2.133(15) 16 ? Mn1 O5 2.133(15) 9_665 ? Mn1 O2 2.141(7) 8_664 ? Mn1 O2 2.141(7) . ? Mn1 O3 2.308(7) 9_665 ? Mn1 O3 2.308(7) 16 ? Mn2 O4 2.145(9) . ? Mn2 O4 2.145(9) 9_665 ? Mn2 O3 2.168(8) . ? Mn2 O3 2.168(8) 9_665 ? Mn2 O1 2.168(8) 9_665 ? Mn2 O1 2.168(8) . ? S2 C5 1.719(11) 14_655 ? S2 C5 1.719(11) . ? S1 C6 1.712(12) . ? S1 C6 1.712(12) 13_565 ? C8 O2 1.239(13) . ? C8 O1 1.240(13) . ? C8 C6 1.476(16) . ? O4 C1 1.221(13) . ? O3 C7 1.264(12) . ? O3 Mn1 2.308(7) 9_665 ? C7 O3 1.264(12) 8_665 ? C7 C4 1.43(3) . ? C6 C3 1.369(18) . ? C5 C2 1.384(16) . ? C5 C1 1.519(17) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C3 C3 1.51(3) 13_565 ? C3 H3A 0.9300 . ? C2 C2 1.44(2) 14_655 ? C2 H2A 0.9300 . ? O5 O5' 0.55(2) . ? O5 C1 1.230(17) . ? O5 Mn1 2.133(15) 9_665 ? C1 O5' 1.45(2) . ? O5' Mn1 2.124(17) 9_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5' Mn1 O5' 115.3(10) 9_665 16 ? O5' Mn1 O5 121.3(6) 9_665 16 ? O5' Mn1 O5 14.7(6) 16 16 ? O5' Mn1 O5 14.7(6) 9_665 9_665 ? O5' Mn1 O5 121.3(6) 16 9_665 ? O5 Mn1 O5 130.5(8) 16 9_665 ? O5' Mn1 O2 93.7(6) 9_665 8_664 ? O5' Mn1 O2 81.3(6) 16 8_664 ? O5 Mn1 O2 94.4(4) 16 8_664 ? O5 Mn1 O2 81.7(5) 9_665 8_664 ? O5' Mn1 O2 81.3(6) 9_665 . ? O5' Mn1 O2 93.7(6) 16 . ? O5 Mn1 O2 81.7(5) 16 . ? O5 Mn1 O2 94.4(4) 9_665 . ? O2 Mn1 O2 170.6(4) 8_664 . ? O5' Mn1 O3 94.1(5) 9_665 9_665 ? O5' Mn1 O3 150.5(5) 16 9_665 ? O5 Mn1 O3 140.5(5) 16 9_665 ? O5 Mn1 O3 88.0(4) 9_665 9_665 ? O2 Mn1 O3 100.9(3) 8_664 9_665 ? O2 Mn1 O3 87.4(3) . 9_665 ? O5' Mn1 O3 150.5(5) 9_665 16 ? O5' Mn1 O3 94.1(5) 16 16 ? O5 Mn1 O3 88.0(4) 16 16 ? O5 Mn1 O3 140.5(5) 9_665 16 ? O2 Mn1 O3 87.4(3) 8_664 16 ? O2 Mn1 O3 100.9(3) . 16 ? O3 Mn1 O3 56.9(4) 9_665 16 ? O4 Mn2 O4 180.0(4) . 9_665 ? O4 Mn2 O3 88.6(3) . . ? O4 Mn2 O3 91.4(3) 9_665 . ? O4 Mn2 O3 91.4(3) . 9_665 ? O4 Mn2 O3 88.6(3) 9_665 9_665 ? O3 Mn2 O3 180.0(4) . 9_665 ? O4 Mn2 O1 90.0(2) . 9_665 ? O4 Mn2 O1 90.0(2) 9_665 9_665 ? O3 Mn2 O1 94.6(3) . 9_665 ? O3 Mn2 O1 85.4(3) 9_665 9_665 ? O4 Mn2 O1 90.0(2) . . ? O4 Mn2 O1 90.0(2) 9_665 . ? O3 Mn2 O1 85.4(3) . . ? O3 Mn2 O1 94.6(3) 9_665 . ? O1 Mn2 O1 180.0(3) 9_665 . ? C5 S2 C5 93.0(9) 14_655 . ? C6 S1 C6 93.8(7) . 13_565 ? O2 C8 O1 126.9(10) . . ? O2 C8 C6 115.4(11) . . ? O1 C8 C6 117.7(10) . . ? C1 O4 Mn2 134.2(7) . . ? C7 O3 Mn2 142.8(8) . . ? C7 O3 Mn1 91.1(9) . 9_665 ? Mn2 O3 Mn1 115.6(3) . 9_665 ? C8 O2 Mn1 133.8(7) . . ? O3 C7 O3 120.9(17) . 8_665 ? O3 C7 C4 119.5(8) . . ? O3 C7 C4 119.5(8) 8_665 . ? C8 O1 Mn2 135.3(7) . . ? C3 C6 C8 128.3(12) . . ? C3 C6 S1 111.8(10) . . ? C8 C6 S1 119.7(8) . . ? C2 C5 C1 128.3(10) . . ? C2 C5 S2 111.0(9) . . ? C1 C5 S2 120.7(9) . . ? C7 C4 H4A 109.5 . . ? C7 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C7 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C3 C3 111.3(8) . 13_565 ? C6 C3 H3A 124.4 . . ? C3 C3 H3A 124.4 13_565 . ? C5 C2 C2 112.4(7) . 14_655 ? C5 C2 H2A 123.8 . . ? C2 C2 H2A 123.8 14_655 . ? O5' O5 C1 102(3) . . ? O5' O5 Mn1 82(3) . 9_665 ? C1 O5 Mn1 138.6(11) . 9_665 ? O4 C1 O5 129.3(12) . . ? O4 C1 O5' 125.1(12) . . ? O5 C1 O5' 21.6(10) . . ? O4 C1 C5 119.5(11) . . ? O5 C1 C5 110.3(12) . . ? O5' C1 C5 113.9(12) . . ? O5 O5' C1 56(3) . . ? O5 O5' Mn1 84(3) . 9_665 ? C1 O5' Mn1 123.4(12) . 9_665 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 0.250 -0.019 1095.7 -32.7 2 0.250 0.750 -0.061 698.7 -17.2 3 0.750 0.250 0.033 698.7 -17.3 4 0.750 0.750 -0.007 1095.7 -32.5 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 18.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.643 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.232 #end