Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Qiutian Liu' _publ_contact_author_address ; Fujian Institute of Research on the Structure of Matter Chinese Academy of Science 155 West Yangqiao Road, Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email LQT@MS.FJIRSM.AC.CN _publ_section_title ; Syntheses and Structural Characterizations of 24-Membered Di-Metal (Mn, Ni, Fe) Macrocyclic Complexes and the C-S Bond Formation between Acetylacetone and Mercapto N-Heterocycle ; loop_ _publ_author_name 'Qiutian Liu' 'Hui Chen' 'Changneng Chen' 'Chengbing Ma' ; Xiaofeng Zhang ; data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 281993' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [MnL(H2O)(dmso)]2[dmso]2 ; _chemical_name_common (MnL(H2O)(dmso))2(dmso)2 _chemical_melting_point ? _chemical_formula_moiety 'C28 H40 Mn2 N4 O12 S8, 2(C2 H6 O S)' _chemical_formula_sum 'C32 H52 Mn2 N4 O14 S10' _chemical_formula_weight 1147.26 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 10.0088(8) _cell_length_b 11.3527(9) _cell_length_c 11.9496(9) _cell_angle_alpha 69.390(2) _cell_angle_beta 81.425(2) _cell_angle_gamma 84.084(2) _cell_volume 1254.83(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2257 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .36 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .4926 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6475 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4353 _reflns_number_gt 3117 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL, enCIFer (Allen et al., 2004)' _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 hydrogens of coordinated H2O were solved by Fourier maps without refinement. ; _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^)+(0.0000P)^2^+12.2738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap for water' _refine_ls_hydrogen_treatment 'constr, H2O refall with restraints' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4353 _refine_ls_number_parameters 294 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1556 _refine_ls_R_factor_gt 0.1064 _refine_ls_wR_factor_ref 0.2181 _refine_ls_wR_factor_gt 0.1893 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.244 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.72272(15) 0.90957(13) 0.92385(12) 0.0333(4) Uani 1 1 d . . . S1 S 0.7916(3) 1.2626(3) 0.5037(2) 0.0493(7) Uani 1 1 d . . . S2 S 1.0264(3) 1.2563(3) 0.6464(2) 0.0450(7) Uani 1 1 d . . . S3 S 1.3021(3) 1.3671(3) 0.6191(2) 0.0548(8) Uani 1 1 d . . . S4 S 1.0723(3) 0.9017(3) 0.8534(3) 0.0536(8) Uani 1 1 d . . . S5 S 0.5076(4) 0.5975(4) 0.8141(4) 0.0773(11) Uani 1 1 d . . . O1 O 0.7295(7) 0.9233(6) 0.7414(5) 0.0394(16) Uani 1 1 d . . . O2 O 0.6621(6) 1.1043(5) 0.8468(5) 0.0367(15) Uani 1 1 d . . . O3 O 1.2072(7) 1.2714(6) 0.9695(6) 0.0427(17) Uani 1 1 d . . . O4 O 1.3086(7) 1.0617(6) 0.9079(6) 0.0439(17) Uani 1 1 d . . . O5 O 0.9343(7) 0.9622(6) 0.8770(7) 0.0482(18) Uani 1 1 d . . . O6 O 0.5218(7) 0.8365(7) 0.9625(8) 0.056(2) Uani 1 1 d D . . H6A H 0.491(8) 0.777(6) 0.950(10) 0.067 Uiso 1 1 d D . . H6B H 0.455(6) 0.887(7) 0.964(10) 0.067 Uiso 1 1 d D . . O7 O 0.4240(10) 0.6604(10) 0.8928(9) 0.096(3) Uani 1 1 d . . . N1 N 1.0258(9) 1.3735(8) 0.4191(7) 0.049(2) Uani 1 1 d . . . N2 N 1.1475(8) 1.3994(8) 0.4469(7) 0.046(2) Uani 1 1 d . . . C1 C 0.7997(14) 0.9836(12) 0.5347(9) 0.069(4) Uani 1 1 d . . . H1B H 0.8171 0.8941 0.5568 0.104 Uiso 1 1 calc R . . H1C H 0.8801 1.0254 0.4917 0.104 Uiso 1 1 calc R . . H1D H 0.7282 1.0099 0.4843 0.104 Uiso 1 1 calc R . . C2 C 0.7580(10) 1.0176(10) 0.6477(8) 0.042(2) Uani 1 1 d . . . C3 C 0.7487(10) 1.1445(8) 0.6444(8) 0.036(2) Uani 1 1 d . . . C4 C 0.6900(9) 1.1815(8) 0.7444(8) 0.033(2) Uani 1 1 d . . . C5 C 0.6582(11) 1.3183(9) 0.7272(10) 0.054(3) Uani 1 1 d . . . H5B H 0.6031 1.3261 0.7974 0.082 Uiso 1 1 calc R . . H5C H 0.6102 1.3567 0.6582 0.082 Uiso 1 1 calc R . . H5D H 0.7408 1.3597 0.7148 0.082 Uiso 1 1 calc R . . C6 C 0.9537(9) 1.3015(8) 0.5124(7) 0.035(2) Uani 1 1 d . . . C7 C 1.1584(10) 1.3475(8) 0.5604(8) 0.038(2) Uani 1 1 d . . . C8 C 1.1692(13) 1.4637(10) 0.8168(11) 0.064(3) Uani 1 1 d . . . H8B H 1.0966 1.4741 0.7695 0.096 Uiso 1 1 calc R . . H8C H 1.2414 1.5154 0.7690 0.096 Uiso 1 1 calc R . . H8D H 1.1371 1.4883 0.8856 0.096 Uiso 1 1 calc R . . C9 C 1.2206(9) 1.3270(9) 0.8586(10) 0.041(2) Uani 1 1 d . . . C10 C 1.2769(10) 1.2689(9) 0.7713(8) 0.039(2) Uani 1 1 d . . . C11 C 1.3191(9) 1.1399(9) 0.8022(9) 0.038(2) Uani 1 1 d . . . C12 C 1.3776(11) 1.0830(11) 0.7077(9) 0.056(3) Uani 1 1 d . . . H12B H 1.4110 0.9980 0.7462 0.085 Uiso 1 1 calc R . . H12C H 1.4505 1.1317 0.6569 0.085 Uiso 1 1 calc R . . H12D H 1.3086 1.0831 0.6599 0.085 Uiso 1 1 calc R . . C13 C 1.1208(12) 0.8061(12) 0.9947(11) 0.069(4) Uani 1 1 d . . . H13A H 1.1264 0.8577 1.0424 0.103 Uiso 1 1 calc R . . H13B H 1.2075 0.7644 0.9833 0.103 Uiso 1 1 calc R . . H13C H 1.0550 0.7444 1.0353 0.103 Uiso 1 1 calc R . . C14 C 1.0467(14) 0.7786(12) 0.8021(12) 0.076(4) Uani 1 1 d . . . H14A H 0.9829 0.7231 0.8593 0.114 Uiso 1 1 calc R . . H14B H 1.1311 0.7323 0.7933 0.114 Uiso 1 1 calc R . . H14C H 1.0121 0.8134 0.7257 0.114 Uiso 1 1 calc R . . C15 C 0.5244(16) 0.7177(17) 0.6701(15) 0.114(6) Uani 1 1 d . . . H15A H 0.4372 0.7582 0.6523 0.171 Uiso 1 1 calc R . . H15B H 0.5610 0.6812 0.6100 0.171 Uiso 1 1 calc R . . H15C H 0.5841 0.7788 0.6701 0.171 Uiso 1 1 calc R . . C16 C 0.6762(13) 0.5916(12) 0.8396(12) 0.075(4) Uani 1 1 d . . . H16A H 0.6983 0.6731 0.8365 0.113 Uiso 1 1 calc R . . H16B H 0.7344 0.5676 0.7789 0.113 Uiso 1 1 calc R . . H16C H 0.6884 0.5309 0.9175 0.113 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 Mn 0.0412(9) 0.0294(8) 0.0259(7) -0.0066(6) -0.0013(6) -0.0009(6) S1 0.0488(16) 0.0559(17) 0.0325(14) 0.0028(12) -0.0094(11) -0.0143(13) S2 0.0445(15) 0.0524(16) 0.0261(12) 0.0029(11) -0.0010(10) -0.0127(12) S3 0.0507(17) 0.0658(19) 0.0333(14) 0.0072(13) -0.0054(12) -0.0249(14) S4 0.0390(16) 0.0488(16) 0.0654(19) -0.0138(14) 0.0046(13) -0.0054(13) S5 0.067(2) 0.085(3) 0.100(3) -0.062(2) 0.019(2) -0.0274(19) O1 0.057(4) 0.034(4) 0.028(3) -0.011(3) -0.001(3) -0.009(3) O2 0.041(4) 0.027(3) 0.033(4) -0.003(3) -0.002(3) 0.003(3) O3 0.056(5) 0.030(4) 0.033(4) -0.004(3) -0.006(3) 0.009(3) O4 0.060(5) 0.033(4) 0.037(4) -0.012(3) -0.001(3) 0.001(3) O5 0.037(4) 0.041(4) 0.069(5) -0.022(4) -0.009(3) 0.002(3) O6 0.039(4) 0.050(5) 0.086(6) -0.038(4) 0.008(4) -0.004(4) O7 0.082(7) 0.117(8) 0.118(8) -0.089(7) 0.039(6) -0.032(6) N1 0.052(6) 0.056(6) 0.031(5) -0.006(4) 0.002(4) -0.010(4) N2 0.043(5) 0.054(5) 0.032(5) -0.001(4) -0.003(4) -0.012(4) C1 0.102(11) 0.075(9) 0.032(6) -0.022(6) -0.002(6) -0.012(8) C2 0.048(6) 0.054(7) 0.026(5) -0.013(5) -0.007(4) -0.007(5) C3 0.042(6) 0.033(5) 0.026(5) 0.001(4) -0.008(4) -0.007(4) C4 0.035(5) 0.028(5) 0.040(5) -0.016(4) -0.008(4) 0.001(4) C5 0.057(7) 0.037(6) 0.059(7) -0.011(5) 0.006(6) -0.001(5) C6 0.041(6) 0.038(5) 0.020(4) -0.003(4) -0.010(4) 0.003(4) C7 0.041(6) 0.032(5) 0.029(5) 0.001(4) 0.005(4) -0.013(4) C8 0.082(9) 0.046(7) 0.056(7) -0.004(6) -0.018(6) 0.004(6) C9 0.030(5) 0.029(5) 0.058(7) -0.003(5) -0.022(5) 0.000(4) C10 0.046(6) 0.042(6) 0.024(5) -0.005(4) -0.004(4) -0.012(5) C11 0.035(6) 0.044(6) 0.038(6) -0.014(5) -0.002(4) -0.013(5) C12 0.046(7) 0.083(9) 0.043(6) -0.026(6) 0.001(5) -0.011(6) C13 0.057(8) 0.067(8) 0.082(9) -0.023(7) -0.023(7) 0.006(6) C14 0.086(10) 0.073(9) 0.076(9) -0.041(8) 0.003(8) 0.006(8) C15 0.077(11) 0.150(17) 0.112(14) -0.048(13) -0.005(10) 0.012(11) C16 0.087(10) 0.072(9) 0.073(9) -0.035(7) -0.004(7) -0.003(8) _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 Mn O3 2.113(6) 2_777 ? Mn O4 2.121(6) 2_777 ? Mn O1 2.121(6) . ? Mn O2 2.135(6) . ? Mn O6 2.178(7) . ? Mn O5 2.197(7) . ? S1 C6 1.752(10) . ? S1 C3 1.768(9) . ? S2 C7 1.733(9) . ? S2 C6 1.747(9) . ? S3 C7 1.757(10) . ? S3 C10 1.763(9) . ? S4 O5 1.512(7) . ? S4 C13 1.764(12) . ? S4 C14 1.766(12) . ? S5 O7 1.487(8) . ? S5 C16 1.750(14) . ? S5 C15 1.778(17) . ? O1 C2 1.267(11) . ? O2 C4 1.240(10) . ? O3 C9 1.245(11) . ? O3 Mn 2.113(6) 2_777 ? O4 C11 1.259(11) . ? O4 Mn 2.121(6) 2_777 ? O6 H6A 0.840(10) . ? O6 H6B 0.840(10) . ? N1 C6 1.293(11) . ? N1 N2 1.393(11) . ? N2 C7 1.291(11) . ? C1 C2 1.520(13) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.421(13) . ? C3 C4 1.429(13) . ? C4 C5 1.500(13) . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C5 H5D 0.9600 . ? C8 C9 1.513(13) . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C9 C10 1.439(14) . ? C10 C11 1.414(13) . ? C11 C12 1.508(13) . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 H12D 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mn O4 82.3(2) 2_777 2_777 ? O3 Mn O1 111.2(3) 2_777 . ? O4 Mn O1 166.4(3) 2_777 . ? O3 Mn O2 167.6(3) 2_777 . ? O4 Mn O2 86.3(2) 2_777 . ? O1 Mn O2 80.4(2) . . ? O3 Mn O6 87.4(3) 2_777 . ? O4 Mn O6 88.9(3) 2_777 . ? O1 Mn O6 89.9(3) . . ? O2 Mn O6 97.2(3) . . ? O3 Mn O5 88.1(3) 2_777 . ? O4 Mn O5 96.5(3) 2_777 . ? O1 Mn O5 86.2(3) . . ? O2 Mn O5 88.4(2) . . ? O6 Mn O5 172.5(3) . . ? C6 S1 C3 104.0(4) . . ? C7 S2 C6 85.5(4) . . ? C7 S3 C10 103.5(4) . . ? O5 S4 C13 107.0(5) . . ? O5 S4 C14 106.8(5) . . ? C13 S4 C14 97.2(6) . . ? O7 S5 C16 107.7(6) . . ? O7 S5 C15 103.8(7) . . ? C16 S5 C15 96.2(7) . . ? C2 O1 Mn 128.0(6) . . ? C4 O2 Mn 131.1(6) . . ? C9 O3 Mn 131.6(6) . 2_777 ? C11 O4 Mn 130.5(6) . 2_777 ? S4 O5 Mn 138.3(4) . . ? Mn O6 H6A 133(7) . . ? Mn O6 H6B 118(6) . . ? H6A O6 H6B 104(3) . . ? C6 N1 N2 112.4(8) . . ? C7 N2 N1 111.6(8) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C2 C3 124.6(8) . . ? O1 C2 C1 113.6(9) . . ? C3 C2 C1 121.8(9) . . ? C2 C3 C4 123.1(8) . . ? C2 C3 S1 117.5(7) . . ? C4 C3 S1 118.9(7) . . ? O2 C4 C3 122.6(8) . . ? O2 C4 C5 117.4(8) . . ? C3 C4 C5 120.0(8) . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? N1 C6 S2 114.7(7) . . ? N1 C6 S1 121.5(7) . . ? S2 C6 S1 123.7(5) . . ? N2 C7 S2 115.7(7) . . ? N2 C7 S3 120.7(7) . . ? S2 C7 S3 123.6(5) . . ? C9 C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 C8 H8D 109.5 . . ? H8B C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? O3 C9 C10 124.5(8) . . ? O3 C9 C8 115.6(10) . . ? C10 C9 C8 119.8(9) . . ? C11 C10 C9 123.5(8) . . ? C11 C10 S3 118.9(7) . . ? C9 C10 S3 117.5(7) . . ? O4 C11 C10 124.5(9) . . ? O4 C11 C12 113.8(9) . . ? C10 C11 C12 121.7(9) . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12B C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? S4 C13 H13A 109.5 . . ? S4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? S4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? S4 C14 H14A 109.5 . . ? S4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S5 C15 H15A 109.5 . . ? S5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S5 C16 H16A 109.5 . . ? S5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mn O1 C2 -143.8(8) 2_777 . . . ? O4 Mn O1 C2 44.3(16) 2_777 . . . ? O2 Mn O1 C2 31.7(8) . . . . ? O6 Mn O1 C2 129.1(8) . . . . ? O5 Mn O1 C2 -57.3(8) . . . . ? O3 Mn O2 C4 130.6(12) 2_777 . . . ? O4 Mn O2 C4 153.5(8) 2_777 . . . ? O1 Mn O2 C4 -29.4(8) . . . . ? O6 Mn O2 C4 -118.0(8) . . . . ? O5 Mn O2 C4 57.0(8) . . . . ? C13 S4 O5 Mn -77.0(8) . . . . ? C14 S4 O5 Mn 26.2(9) . . . . ? O3 Mn O5 S4 35.5(7) 2_777 . . . ? O4 Mn O5 S4 117.5(7) 2_777 . . . ? O1 Mn O5 S4 -75.9(7) . . . . ? O2 Mn O5 S4 -156.4(7) . . . . ? C6 N1 N2 C7 -1.5(12) . . . . ? Mn O1 C2 C3 -21.6(14) . . . . ? Mn O1 C2 C1 160.4(7) . . . . ? O1 C2 C3 C4 -7.9(16) . . . . ? C1 C2 C3 C4 170.0(10) . . . . ? O1 C2 C3 S1 -179.4(8) . . . . ? C1 C2 C3 S1 -1.5(14) . . . . ? C6 S1 C3 C2 -102.8(8) . . . . ? C6 S1 C3 C4 85.3(8) . . . . ? Mn O2 C4 C3 15.1(13) . . . . ? Mn O2 C4 C5 -165.7(7) . . . . ? C2 C3 C4 O2 11.5(15) . . . . ? S1 C3 C4 O2 -177.1(7) . . . . ? C2 C3 C4 C5 -167.6(9) . . . . ? S1 C3 C4 C5 3.7(12) . . . . ? N2 N1 C6 S2 0.0(11) . . . . ? N2 N1 C6 S1 176.1(7) . . . . ? C7 S2 C6 N1 1.0(8) . . . . ? C7 S2 C6 S1 -174.9(7) . . . . ? C3 S1 C6 N1 170.6(8) . . . . ? C3 S1 C6 S2 -13.7(8) . . . . ? N1 N2 C7 S2 2.4(11) . . . . ? N1 N2 C7 S3 -179.4(7) . . . . ? C6 S2 C7 N2 -2.0(8) . . . . ? C6 S2 C7 S3 179.8(7) . . . . ? C10 S3 C7 N2 -174.9(9) . . . . ? C10 S3 C7 S2 3.2(8) . . . . ? Mn O3 C9 C10 9.0(14) 2_777 . . . ? Mn O3 C9 C8 -172.8(7) 2_777 . . . ? O3 C9 C10 C11 2.3(15) . . . . ? C8 C9 C10 C11 -175.8(9) . . . . ? O3 C9 C10 S3 -174.1(8) . . . . ? C8 C9 C10 S3 7.7(13) . . . . ? C7 S3 C10 C11 85.8(8) . . . . ? C7 S3 C10 C9 -97.6(8) . . . . ? Mn O4 C11 C10 -17.6(14) 2_777 . . . ? Mn O4 C11 C12 164.4(6) 2_777 . . . ? C9 C10 C11 O4 2.2(15) . . . . ? S3 C10 C11 O4 178.6(8) . . . . ? C9 C10 C11 C12 -180.0(9) . . . . ? S3 C10 C11 C12 -3.6(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6A O7 0.840(10) 1.90(3) 2.732(11) 170(12) . _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.574 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.143 #==END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 281994' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [NiL(H2O)(dmf)]2(dmf)2 ; _chemical_name_common (NiL(H2O)(dmf))2(dmf)2 _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 N6 Ni2 O12 S6, 2(C3 H7 N O)' _chemical_formula_sum 'C36 H56 N8 Ni2 O14 S6' _chemical_formula_weight 1134.67 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' Ni Ni 0.3393 1.1124 '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 10.5249(14) _cell_length_b 11.7042(15) _cell_length_c 12.1680(15) _cell_angle_alpha 98.875(2) _cell_angle_beta 105.571(2) _cell_angle_gamma 107.445(2) _cell_volume 1331.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2001 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour 'light blue' _exptl_crystal_size_max .28 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .4490 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6986 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4677 _reflns_number_gt 2638 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement "Siemens SHELXTL'" _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL, enCIFer (Allen et al., 2004)' _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 hydrogens of coordinated H2O were solved by Fourier maps without refinement. ; _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^)+(0.0369P)^2^+3.7261P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap for water' _refine_ls_hydrogen_treatment 'constr, H2O refall with restraints' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4677 _refine_ls_number_parameters 312 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1534 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1467 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.68519(10) 0.81538(9) 0.78198(8) 0.0590(3) Uani 1 1 d D . . S1 S 0.7164(3) 1.1523(2) 0.5668(2) 0.0875(7) Uani 1 1 d . . . S2 S 0.9688(2) 1.24120(19) 0.79930(18) 0.0741(6) Uani 1 1 d . . . S3 S 1.2485(3) 1.4573(2) 0.9361(2) 0.0835(7) Uani 1 1 d . . . O1 O 0.7479(5) 0.8453(5) 0.6435(4) 0.0663(13) Uani 1 1 d . . . O2 O 0.5674(5) 0.9200(5) 0.7434(4) 0.0673(14) Uani 1 1 d . . . O3 O 1.3678(5) 1.2089(5) 1.0754(4) 0.0678(14) Uani 1 1 d . . . O4 O 1.1913(6) 1.2840(5) 1.1824(5) 0.0761(15) Uani 1 1 d . . . O5 O 0.5267(8) 0.6506(7) 0.6873(7) 0.125(3) Uani 1 1 d . . . O6 O 0.8493(5) 0.9781(5) 0.8833(4) 0.0688(14) Uani 1 1 d D . . H6B H 0.9352(18) 0.998(4) 0.887(5) 0.083 Uiso 1 1 d D . . H6A H 0.858(4) 1.021(4) 0.949(3) 0.083 Uiso 1 1 d D . . O7 O 1.1028(6) 0.9684(6) 0.8738(5) 0.0952(19) Uani 1 1 d . . . N1 N 0.9490(8) 1.3522(7) 0.6349(6) 0.083(2) Uani 1 1 d . . . N2 N 1.0761(8) 1.4249(6) 0.7216(6) 0.079(2) Uani 1 1 d . . . N3 N 0.3470(8) 0.4905(7) 0.5665(7) 0.086(2) Uani 1 1 d . . . N4 N 1.2010(8) 0.8375(7) 0.8074(6) 0.079(2) Uani 1 1 d . . . C1 C 0.8431(9) 0.9570(9) 0.5238(8) 0.093(3) Uani 1 1 d . . . H1B H 0.8892 0.8975 0.5245 0.139 Uiso 1 1 calc R . . H1C H 0.9129 1.0392 0.5513 0.139 Uiso 1 1 calc R . . H1D H 0.7833 0.9454 0.4448 0.139 Uiso 1 1 calc R . . C2 C 0.7553(8) 0.9396(8) 0.6032(6) 0.065(2) Uani 1 1 d . . . C3 C 0.6894(8) 1.0252(7) 0.6295(6) 0.0602(19) Uani 1 1 d . . . C4 C 0.5986(8) 1.0093(8) 0.6968(6) 0.064(2) Uani 1 1 d . . . C5 C 0.5278(10) 1.1002(9) 0.7173(9) 0.102(3) Uani 1 1 d . . . H5B H 0.4559 1.0666 0.7503 0.154 Uiso 1 1 calc R . . H5C H 0.4858 1.1162 0.6437 0.154 Uiso 1 1 calc R . . H5D H 0.5965 1.1761 0.7711 0.154 Uiso 1 1 calc R . . C6 C 0.8815(9) 1.2548(7) 0.6607(7) 0.068(2) Uani 1 1 d . . . C7 C 1.0982(8) 1.3787(7) 0.8125(7) 0.063(2) Uani 1 1 d . . . C8 C 1.3920(10) 1.2697(9) 0.9069(7) 0.092(3) Uani 1 1 d . . . H8B H 1.4460 1.3517 0.9062 0.138 Uiso 1 1 calc R . . H8C H 1.3145 1.2319 0.8340 0.138 Uiso 1 1 calc R . . H8D H 1.4513 1.2210 0.9157 0.138 Uiso 1 1 calc R . . C9 C 1.3363(8) 1.2768(7) 1.0077(7) 0.066(2) Uani 1 1 d . . . C10 C 1.2550(8) 1.3508(7) 1.0244(7) 0.062(2) Uani 1 1 d . . . C11 C 1.1885(9) 1.3515(7) 1.1104(7) 0.069(2) Uani 1 1 d . . . C12 C 1.0993(11) 1.4302(9) 1.1198(8) 0.106(3) Uani 1 1 d . . . H12B H 1.0335 1.4180 1.0433 0.159 Uiso 1 1 calc R . . H12C H 1.1593 1.5159 1.1498 0.159 Uiso 1 1 calc R . . H12D H 1.0485 1.4067 1.1725 0.159 Uiso 1 1 calc R . . C13 C 0.4371(12) 0.6060(12) 0.6131(11) 0.111(4) Uani 1 1 d . . . H13A H 0.4150 0.6598 0.5689 0.133 Uiso 1 1 calc R . . C14 C 0.2318(13) 0.4654(12) 0.4662(11) 0.163(6) Uani 1 1 d . . . H14B H 0.1488 0.4564 0.4880 0.245 Uiso 1 1 calc R . . H14C H 0.2180 0.3901 0.4124 0.245 Uiso 1 1 calc R . . H14D H 0.2488 0.5324 0.4290 0.245 Uiso 1 1 calc R . . C15 C 0.3633(15) 0.3905(12) 0.6143(11) 0.152(5) Uani 1 1 d . . . H15B H 0.4381 0.4221 0.6891 0.229 Uiso 1 1 calc R . . H15C H 0.3861 0.3365 0.5612 0.229 Uiso 1 1 calc R . . H15D H 0.2768 0.3452 0.6249 0.229 Uiso 1 1 calc R . . C16 C 1.1044(9) 0.8868(9) 0.7980(8) 0.084(3) Uani 1 1 d . . . H16A H 1.0293 0.8576 0.7272 0.101 Uiso 1 1 calc R . . C17 C 1.3183(11) 0.8761(12) 0.9172(10) 0.143(5) Uani 1 1 d . . . H17B H 1.3289 0.9559 0.9610 0.215 Uiso 1 1 calc R . . H17C H 1.4034 0.8809 0.9002 0.215 Uiso 1 1 calc R . . H17D H 1.3001 0.8169 0.9629 0.215 Uiso 1 1 calc R . . C18 C 1.1966(12) 0.7454(9) 0.7109(10) 0.120(4) Uani 1 1 d . . . H18B H 1.1881 0.6691 0.7334 0.181 Uiso 1 1 calc R . . H18C H 1.2820 0.7738 0.6923 0.181 Uiso 1 1 calc R . . H18D H 1.1169 0.7321 0.6429 0.181 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 Ni 0.0582(6) 0.0622(6) 0.0536(6) 0.0118(5) 0.0130(5) 0.0241(5) S1 0.0866(16) 0.0927(17) 0.0711(14) 0.0398(13) 0.0023(13) 0.0271(13) S2 0.0806(15) 0.0682(13) 0.0643(13) 0.0338(11) 0.0096(11) 0.0186(11) S3 0.0912(16) 0.0609(13) 0.0816(15) 0.0278(12) 0.0114(13) 0.0147(12) O1 0.066(3) 0.075(4) 0.060(3) 0.017(3) 0.020(3) 0.029(3) O2 0.053(3) 0.090(4) 0.071(3) 0.031(3) 0.023(3) 0.035(3) O3 0.070(3) 0.078(4) 0.064(3) 0.019(3) 0.025(3) 0.036(3) O4 0.103(4) 0.082(4) 0.070(3) 0.031(3) 0.038(3) 0.056(3) O5 0.098(6) 0.120(6) 0.087(5) -0.019(4) 0.008(4) -0.013(5) O6 0.047(3) 0.077(4) 0.066(3) 0.003(3) 0.007(3) 0.019(3) O7 0.069(4) 0.117(5) 0.081(4) -0.012(4) 0.013(3) 0.036(4) N1 0.090(5) 0.085(5) 0.074(5) 0.044(4) 0.017(4) 0.029(4) N2 0.090(5) 0.074(5) 0.071(5) 0.039(4) 0.021(4) 0.021(4) N3 0.085(5) 0.074(5) 0.075(5) -0.010(4) 0.014(4) 0.020(4) N4 0.072(5) 0.088(5) 0.092(6) 0.027(4) 0.040(5) 0.037(4) C1 0.085(6) 0.116(8) 0.095(7) 0.040(6) 0.046(6) 0.039(6) C2 0.055(5) 0.079(6) 0.053(5) 0.015(4) 0.013(4) 0.017(4) C3 0.052(4) 0.073(5) 0.048(4) 0.017(4) 0.004(4) 0.021(4) C4 0.055(5) 0.078(6) 0.046(4) 0.007(4) 0.000(4) 0.028(4) C5 0.118(8) 0.112(8) 0.103(7) 0.033(6) 0.035(6) 0.076(7) C6 0.083(6) 0.070(5) 0.066(5) 0.038(4) 0.025(5) 0.038(5) C7 0.073(5) 0.057(5) 0.066(5) 0.024(4) 0.026(4) 0.026(4) C8 0.108(7) 0.126(8) 0.070(6) 0.047(6) 0.042(6) 0.059(6) C9 0.061(5) 0.071(5) 0.057(5) 0.015(4) 0.012(4) 0.019(4) C10 0.061(5) 0.058(5) 0.061(5) 0.018(4) 0.009(4) 0.022(4) C11 0.078(6) 0.067(5) 0.061(5) 0.008(4) 0.014(5) 0.037(5) C12 0.153(9) 0.128(8) 0.083(6) 0.039(6) 0.039(6) 0.109(8) C13 0.087(8) 0.122(10) 0.100(9) -0.012(8) 0.016(7) 0.041(8) C14 0.150(11) 0.181(13) 0.117(10) 0.000(9) -0.032(9) 0.087(10) C15 0.208(14) 0.149(11) 0.127(10) 0.070(9) 0.058(10) 0.081(11) C16 0.068(6) 0.103(7) 0.064(6) -0.001(5) 0.009(5) 0.029(6) C17 0.098(8) 0.221(14) 0.125(10) 0.055(10) 0.024(8) 0.086(9) C18 0.136(9) 0.096(8) 0.157(10) 0.022(7) 0.088(9) 0.051(7) _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 Ni O3 1.995(5) 2_777 ? Ni O4 1.998(5) 2_777 ? Ni O2 2.009(5) . ? Ni O1 2.009(5) . ? Ni O5 2.045(7) . ? Ni O6 2.071(5) . ? S1 C6 1.740(9) . ? S1 C3 1.757(7) . ? S2 C7 1.721(8) . ? S2 C6 1.747(7) . ? S3 C7 1.742(8) . ? S3 C10 1.771(7) . ? O1 C2 1.264(8) . ? O2 C4 1.265(9) . ? O3 C9 1.277(8) . ? O3 Ni 1.995(5) 2_777 ? O4 C11 1.267(9) . ? O4 Ni 1.998(5) 2_777 ? O5 C13 1.038(11) . ? O6 H6B 0.850(10) . ? O6 H6A 0.847(10) . ? O7 C16 1.228(10) . ? N1 C6 1.284(9) . ? N1 N2 1.382(9) . ? N2 C7 1.300(8) . ? N3 C13 1.325(13) . ? N3 C14 1.389(11) . ? N3 C15 1.419(12) . ? N4 C16 1.300(10) . ? N4 C18 1.448(11) . ? N4 C17 1.451(12) . ? C1 C2 1.502(10) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.423(10) . ? C3 C4 1.407(10) . ? C4 C5 1.497(10) . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C5 H5D 0.9600 . ? C8 C9 1.497(10) . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C9 C10 1.417(10) . ? C10 C11 1.406(10) . ? C11 C12 1.513(10) . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 H12D 0.9600 . ? C13 H13A 0.9300 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14 H14D 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15 H15D 0.9600 . ? C16 H16A 0.9300 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C17 H17D 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C18 H18D 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ni O4 89.1(2) 2_777 2_777 ? O3 Ni O2 93.1(2) 2_777 . ? O4 Ni O2 177.4(2) 2_777 . ? O3 Ni O1 177.2(2) 2_777 . ? O4 Ni O1 90.0(2) 2_777 . ? O2 Ni O1 87.8(2) . . ? O3 Ni O5 88.8(3) 2_777 . ? O4 Ni O5 86.3(3) 2_777 . ? O2 Ni O5 95.2(3) . . ? O1 Ni O5 93.7(3) . . ? O3 Ni O6 89.7(2) 2_777 . ? O4 Ni O6 91.5(2) 2_777 . ? O2 Ni O6 87.0(2) . . ? O1 Ni O6 87.8(2) . . ? O5 Ni O6 177.4(3) . . ? C6 S1 C3 102.8(3) . . ? C7 S2 C6 86.5(4) . . ? C7 S3 C10 105.1(3) . . ? C2 O1 Ni 125.5(5) . . ? C4 O2 Ni 124.6(5) . . ? C9 O3 Ni 128.4(5) . 2_777 ? C11 O4 Ni 127.9(5) . 2_777 ? C13 O5 Ni 145.8(11) . . ? Ni O6 H6B 126(2) . . ? Ni O6 H6A 127(2) . . ? H6B O6 H6A 101(2) . . ? C6 N1 N2 113.9(6) . . ? C7 N2 N1 111.4(6) . . ? C13 N3 C14 118.9(10) . . ? C13 N3 C15 122.9(10) . . ? C14 N3 C15 118.3(10) . . ? C16 N4 C18 122.1(9) . . ? C16 N4 C17 119.6(8) . . ? C18 N4 C17 118.3(9) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C2 C3 124.7(7) . . ? O1 C2 C1 114.3(7) . . ? C3 C2 C1 121.0(7) . . ? C4 C3 C2 123.5(7) . . ? C4 C3 S1 119.0(6) . . ? C2 C3 S1 117.4(6) . . ? O2 C4 C3 125.0(7) . . ? O2 C4 C5 114.0(8) . . ? C3 C4 C5 120.9(8) . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? N1 C6 S1 121.9(6) . . ? N1 C6 S2 113.3(6) . . ? S1 C6 S2 124.7(5) . . ? N2 C7 S2 114.9(6) . . ? N2 C7 S3 120.0(6) . . ? S2 C7 S3 125.1(4) . . ? C9 C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 C8 H8D 109.5 . . ? H8B C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? O3 C9 C10 123.9(7) . . ? O3 C9 C8 113.5(7) . . ? C10 C9 C8 122.6(7) . . ? C11 C10 C9 124.9(7) . . ? C11 C10 S3 118.5(6) . . ? C9 C10 S3 116.5(6) . . ? O4 C11 C10 124.4(7) . . ? O4 C11 C12 113.9(8) . . ? C10 C11 C12 121.6(7) . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12B C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? O5 C13 N3 135.1(14) . . ? O5 C13 H13A 112.5 . . ? N3 C13 H13A 112.5 . . ? N3 C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C14 H14D 109.5 . . ? H14B C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? N3 C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C15 H15D 109.5 . . ? H15B C15 H15D 109.5 . . ? H15C C15 H15D 109.5 . . ? O7 C16 N4 126.1(8) . . ? O7 C16 H16A 116.9 . . ? N4 C16 H16A 116.9 . . ? N4 C17 H17B 109.5 . . ? N4 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C17 H17D 109.5 . . ? H17B C17 H17D 109.5 . . ? H17C C17 H17D 109.5 . . ? N4 C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C18 H18D 109.5 . . ? H18B C18 H18D 109.5 . . ? H18C C18 H18D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ni O1 C2 -150.8(6) 2_777 . . . ? O2 Ni O1 C2 27.9(6) . . . . ? O5 Ni O1 C2 122.9(6) . . . . ? O6 Ni O1 C2 -59.2(6) . . . . ? O3 Ni O2 C4 146.5(6) 2_777 . . . ? O1 Ni O2 C4 -30.9(6) . . . . ? O5 Ni O2 C4 -124.4(6) . . . . ? O6 Ni O2 C4 57.0(6) . . . . ? O3 Ni O5 C13 126.5(16) 2_777 . . . ? O4 Ni O5 C13 -144.4(16) 2_777 . . . ? O2 Ni O5 C13 33.5(16) . . . . ? O1 Ni O5 C13 -54.6(16) . . . . ? C6 N1 N2 C7 -1.2(10) . . . . ? Ni O1 C2 C3 -16.1(10) . . . . ? Ni O1 C2 C1 163.2(5) . . . . ? O1 C2 C3 C4 -5.1(11) . . . . ? C1 C2 C3 C4 175.6(7) . . . . ? O1 C2 C3 S1 178.6(6) . . . . ? C1 C2 C3 S1 -0.7(9) . . . . ? C6 S1 C3 C4 102.5(6) . . . . ? C6 S1 C3 C2 -81.0(6) . . . . ? Ni O2 C4 C3 22.5(10) . . . . ? Ni O2 C4 C5 -158.4(5) . . . . ? C2 C3 C4 O2 1.6(11) . . . . ? S1 C3 C4 O2 177.8(6) . . . . ? C2 C3 C4 C5 -177.5(7) . . . . ? S1 C3 C4 C5 -1.3(10) . . . . ? N2 N1 C6 S1 177.9(6) . . . . ? N2 N1 C6 S2 0.3(10) . . . . ? C3 S1 C6 N1 169.3(7) . . . . ? C3 S1 C6 S2 -13.4(6) . . . . ? C7 S2 C6 N1 0.4(7) . . . . ? C7 S2 C6 S1 -177.1(6) . . . . ? N1 N2 C7 S2 1.5(9) . . . . ? N1 N2 C7 S3 -177.4(5) . . . . ? C6 S2 C7 N2 -1.1(6) . . . . ? C6 S2 C7 S3 177.7(5) . . . . ? C10 S3 C7 N2 -169.0(7) . . . . ? C10 S3 C7 S2 12.3(6) . . . . ? Ni O3 C9 C10 0.6(11) 2_777 . . . ? Ni O3 C9 C8 -178.6(5) 2_777 . . . ? O3 C9 C10 C11 -5.8(12) . . . . ? C8 C9 C10 C11 173.4(8) . . . . ? O3 C9 C10 S3 169.7(6) . . . . ? C8 C9 C10 S3 -11.2(10) . . . . ? C7 S3 C10 C11 -91.3(7) . . . . ? C7 S3 C10 C9 92.9(6) . . . . ? Ni O4 C11 C10 12.7(12) 2_777 . . . ? Ni O4 C11 C12 -170.4(6) 2_777 . . . ? C9 C10 C11 O4 -1.3(13) . . . . ? S3 C10 C11 O4 -176.6(6) . . . . ? C9 C10 C11 C12 -177.9(8) . . . . ? S3 C10 C11 C12 6.7(11) . . . . ? Ni O5 C13 N3 178.9(8) . . . . ? C14 N3 C13 O5 176.7(14) . . . . ? C15 N3 C13 O5 -4(2) . . . . ? C18 N4 C16 O7 -177.3(9) . . . . ? C17 N4 C16 O7 2.1(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6B O7 0.850(10) 1.94(2) 2.736(7) 156(4) . O6 H6A O7 0.847(10) 2.06(4) 2.796(8) 145(6) 2_777 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.442 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.078 #==END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 281995' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [MnL(dmf)2]2 ; _chemical_name_common (MnL(dmf)2)2 _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 Mn2 N8 O12 S6' _chemical_formula_sum 'C36 H52 Mn2 N8 O12 S6' _chemical_formula_weight 1091.10 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 11.0902(8) _cell_length_b 11.2049(7) _cell_length_c 11.9250(8) _cell_angle_alpha 111.5750(10) _cell_angle_beta 107.8200(10) _cell_angle_gamma 96.0660(10) _cell_volume 1271.44(15) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4062 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.09 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .50 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 566 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .4845 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6649 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.09 _reflns_number_total 4457 _reflns_number_gt 4035 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL, enCIFer (Allen et al., 2004)' _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^)+(0.0000P)^2^+3.1399P] 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 4457 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.1468 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.326 _refine_ls_restrained_S_all 1.326 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.19595(8) 0.86901(8) 0.28887(8) 0.0501(2) Uani 1 1 d . . . S2 S 0.50017(14) 1.22312(14) 0.28096(13) 0.0519(4) Uani 1 1 d . . . S1 S 0.26252(15) 1.14010(15) 0.02914(14) 0.0563(4) Uani 1 1 d . . . S3 S 0.76549(17) 1.42365(17) 0.45051(16) 0.0734(5) Uani 1 1 d . . . O1 O 0.0987(4) 0.9965(4) 0.2180(4) 0.0583(10) Uani 1 1 d . . . O2 O 0.2665(4) 0.8498(4) 0.1382(4) 0.0567(10) Uani 1 1 d . . . O3 O 0.8446(4) 1.1337(5) 0.5483(4) 0.0730(12) Uani 1 1 d . . . O4 O 0.6877(4) 1.2608(4) 0.6699(4) 0.0601(10) Uani 1 1 d . . . O5 O 0.0378(6) 0.6945(5) 0.1708(6) 0.116(2) Uani 1 1 d . . . O6 O 0.3481(4) 1.0501(4) 0.4313(4) 0.0738(12) Uani 1 1 d . . . N1 N 0.4744(4) 1.3383(4) 0.1280(4) 0.0513(11) Uani 1 1 d . . . N2 N 0.5957(5) 1.4057(4) 0.2275(4) 0.0542(11) Uani 1 1 d . . . N3 N -0.1433(4) 0.5351(4) 0.0924(4) 0.0545(11) Uani 1 1 d . . . N4 N 0.3467(5) 1.1784(5) 0.6293(5) 0.0682(14) Uani 1 1 d . . . C1 C 0.0819(6) 1.1863(6) 0.1798(7) 0.0726(18) Uani 1 1 d . . . H1B H 0.0109 1.1808 0.2092 0.109 Uiso 1 1 calc R . . H1C H 0.0507 1.1888 0.0963 0.109 Uiso 1 1 calc R . . H1D H 0.1489 1.2653 0.2408 0.109 Uiso 1 1 calc R . . C2 C 0.1371(5) 1.0672(5) 0.1687(5) 0.0498(12) Uani 1 1 d . . . C3 C 0.2249(5) 1.0378(5) 0.1023(5) 0.0474(12) Uani 1 1 d . . . C4 C 0.2773(5) 0.9240(5) 0.0831(5) 0.0461(12) Uani 1 1 d . . . C5 C 0.3524(7) 0.8865(6) -0.0050(6) 0.0673(17) Uani 1 1 d . . . H5B H 0.4375 0.9463 0.0365 0.101 Uiso 1 1 calc R . . H5C H 0.3065 0.8915 -0.0850 0.101 Uiso 1 1 calc R . . H5D H 0.3611 0.7977 -0.0227 0.101 Uiso 1 1 calc R . . C6 C 0.4154(5) 1.2429(5) 0.1430(5) 0.0433(11) Uani 1 1 d . . . C7 C 0.6211(5) 1.3561(5) 0.3124(5) 0.0492(13) Uani 1 1 d . . . C8 C 0.8835(8) 1.1860(10) 0.3883(8) 0.107(3) Uani 1 1 d . . . H8B H 0.8172 1.1782 0.3103 0.160 Uiso 1 1 calc R . . H8C H 0.9121 1.1054 0.3718 0.160 Uiso 1 1 calc R . . H8D H 0.9563 1.2585 0.4160 0.160 Uiso 1 1 calc R . . C9 C 0.8283(6) 1.2107(7) 0.4936(6) 0.0614(15) Uani 1 1 d . . . C10 C 0.7601(5) 1.3115(6) 0.5226(5) 0.0546(14) Uani 1 1 d . . . C11 C 0.6940(6) 1.3321(6) 0.6108(5) 0.0548(13) Uani 1 1 d . . . C12 C 0.6202(8) 1.4383(7) 0.6335(7) 0.084(2) Uani 1 1 d . . . H12B H 0.5759 1.4324 0.6896 0.126 Uiso 1 1 calc R . . H12C H 0.5573 1.4267 0.5519 0.126 Uiso 1 1 calc R . . H12D H 0.6802 1.5237 0.6733 0.126 Uiso 1 1 calc R . . C13 C -0.0754(8) 0.6449(7) 0.1059(7) 0.080(2) Uani 1 1 d . . . H13A H -0.1195 0.6893 0.0606 0.096 Uiso 1 1 calc R . . C14 C -0.0855(8) 0.4586(8) 0.1580(8) 0.107(3) Uani 1 1 d . . . H14B H 0.0075 0.4936 0.1977 0.161 Uiso 1 1 calc R . . H14C H -0.1054 0.3681 0.0964 0.161 Uiso 1 1 calc R . . H14D H -0.1200 0.4629 0.2237 0.161 Uiso 1 1 calc R . . C15 C -0.2798(6) 0.4793(7) 0.0063(7) 0.0782(19) Uani 1 1 d . . . H15B H -0.3102 0.5396 -0.0294 0.117 Uiso 1 1 calc R . . H15C H -0.3309 0.4651 0.0543 0.117 Uiso 1 1 calc R . . H15D H -0.2884 0.3965 -0.0629 0.117 Uiso 1 1 calc R . . C16 C 0.3932(6) 1.0978(6) 0.5514(7) 0.0661(16) Uani 1 1 d . . . H16A H 0.4675 1.0742 0.5904 0.079 Uiso 1 1 calc R . . C17 C 0.2268(8) 1.2139(9) 0.5765(8) 0.116(3) Uani 1 1 d . . . H17B H 0.2005 1.1805 0.4839 0.175 Uiso 1 1 calc R . . H17C H 0.2412 1.3085 0.6136 0.175 Uiso 1 1 calc R . . H17D H 0.1594 1.1761 0.5972 0.175 Uiso 1 1 calc R . . C18 C 0.4073(8) 1.2331(9) 0.7695(7) 0.108(3) Uani 1 1 d . . . H18B H 0.3493 1.2010 0.8032 0.162 Uiso 1 1 calc R . . H18C H 0.4256 1.3280 0.8047 0.162 Uiso 1 1 calc R . . H18D H 0.4874 1.2066 0.7935 0.162 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 Mn 0.0541(5) 0.0530(5) 0.0528(5) 0.0286(4) 0.0248(4) 0.0129(4) S2 0.0603(8) 0.0549(8) 0.0520(8) 0.0355(7) 0.0210(7) 0.0105(6) S1 0.0618(9) 0.0663(9) 0.0528(8) 0.0393(7) 0.0192(7) 0.0171(7) S3 0.0722(11) 0.0756(11) 0.0683(10) 0.0454(9) 0.0117(8) -0.0090(8) O1 0.055(2) 0.076(3) 0.067(2) 0.043(2) 0.034(2) 0.027(2) O2 0.087(3) 0.048(2) 0.057(2) 0.0293(19) 0.044(2) 0.025(2) O3 0.090(3) 0.092(3) 0.082(3) 0.056(3) 0.059(3) 0.047(3) O4 0.077(3) 0.068(3) 0.065(2) 0.042(2) 0.042(2) 0.035(2) O5 0.080(4) 0.089(4) 0.136(5) 0.039(4) 0.011(4) -0.028(3) O6 0.067(3) 0.080(3) 0.056(3) 0.015(2) 0.020(2) 0.006(2) N1 0.064(3) 0.057(3) 0.053(3) 0.036(2) 0.030(2) 0.022(2) N2 0.068(3) 0.057(3) 0.060(3) 0.037(2) 0.035(3) 0.021(2) N3 0.057(3) 0.044(2) 0.060(3) 0.024(2) 0.017(2) 0.007(2) N4 0.057(3) 0.073(3) 0.058(3) 0.013(3) 0.017(2) 0.021(3) C1 0.080(4) 0.079(4) 0.089(5) 0.048(4) 0.048(4) 0.045(4) C2 0.050(3) 0.057(3) 0.043(3) 0.024(3) 0.015(2) 0.016(3) C3 0.055(3) 0.054(3) 0.044(3) 0.029(3) 0.021(2) 0.017(3) C4 0.052(3) 0.046(3) 0.038(3) 0.014(2) 0.019(2) 0.008(2) C5 0.093(5) 0.062(4) 0.066(4) 0.028(3) 0.051(4) 0.027(3) C6 0.057(3) 0.049(3) 0.045(3) 0.029(2) 0.030(2) 0.025(2) C7 0.053(3) 0.053(3) 0.059(3) 0.033(3) 0.031(3) 0.016(3) C8 0.097(6) 0.195(9) 0.102(6) 0.099(7) 0.075(5) 0.075(6) C9 0.053(3) 0.088(4) 0.056(3) 0.042(3) 0.024(3) 0.011(3) C10 0.052(3) 0.067(4) 0.051(3) 0.035(3) 0.017(3) 0.010(3) C11 0.061(4) 0.053(3) 0.048(3) 0.021(3) 0.018(3) 0.015(3) C12 0.130(6) 0.073(4) 0.081(5) 0.044(4) 0.057(5) 0.058(5) C13 0.094(6) 0.062(4) 0.089(5) 0.037(4) 0.034(4) 0.018(4) C14 0.095(6) 0.096(6) 0.121(7) 0.070(6) 0.001(5) 0.018(5) C15 0.064(4) 0.073(4) 0.085(5) 0.033(4) 0.011(4) 0.016(3) C16 0.051(3) 0.069(4) 0.078(5) 0.032(4) 0.022(3) 0.017(3) C17 0.100(6) 0.115(7) 0.101(6) 0.017(5) 0.017(5) 0.060(6) C18 0.108(6) 0.134(8) 0.059(4) 0.021(5) 0.026(4) 0.030(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 Mn O2 2.121(3) . ? Mn O3 2.133(4) 2_676 ? Mn O4 2.134(4) 2_676 ? Mn O1 2.138(4) . ? Mn O5 2.150(5) . ? Mn O6 2.199(4) . ? S2 C6 1.733(5) . ? S2 C7 1.737(5) . ? S1 C6 1.753(5) . ? S1 C3 1.762(5) . ? S3 C7 1.750(6) . ? S3 C10 1.770(5) . ? O1 C2 1.257(6) . ? O2 C4 1.251(6) . ? O3 C9 1.255(7) . ? O3 Mn 2.133(4) 2_676 ? O4 C11 1.253(6) . ? O4 Mn 2.134(4) 2_676 ? O5 C13 1.194(8) . ? O6 C16 1.236(7) . ? N1 C6 1.291(6) . ? N1 N2 1.392(6) . ? N2 C7 1.298(6) . ? N3 C13 1.300(8) . ? N3 C14 1.435(8) . ? N3 C15 1.454(7) . ? N4 C16 1.312(8) . ? N4 C18 1.447(8) . ? N4 C17 1.451(8) . ? C1 C2 1.506(7) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.425(7) . ? C3 C4 1.427(7) . ? C4 C5 1.503(7) . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C5 H5D 0.9600 . ? C8 C9 1.509(8) . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C9 C10 1.421(8) . ? C10 C11 1.423(8) . ? C11 C12 1.505(8) . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 H12D 0.9600 . ? C13 H13A 0.9300 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14 H14D 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15 H15D 0.9600 . ? C16 H16A 0.9300 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C17 H17D 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C18 H18D 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn O3 167.75(16) . 2_676 ? O2 Mn O4 86.75(14) . 2_676 ? O3 Mn O4 81.14(15) 2_676 2_676 ? O2 Mn O1 80.99(14) . . ? O3 Mn O1 111.07(15) 2_676 . ? O4 Mn O1 167.70(14) 2_676 . ? O2 Mn O5 94.1(2) . . ? O3 Mn O5 86.9(2) 2_676 . ? O4 Mn O5 86.2(2) 2_676 . ? O1 Mn O5 95.7(2) . . ? O2 Mn O6 93.71(16) . . ? O3 Mn O6 85.34(18) 2_676 . ? O4 Mn O6 94.13(17) 2_676 . ? O1 Mn O6 85.70(17) . . ? O5 Mn O6 172.1(2) . . ? C6 S2 C7 85.7(2) . . ? C6 S1 C3 102.4(2) . . ? C7 S3 C10 103.4(3) . . ? C2 O1 Mn 128.3(3) . . ? C4 O2 Mn 131.2(3) . . ? C9 O3 Mn 131.6(4) . 2_676 ? C11 O4 Mn 131.5(4) . 2_676 ? C13 O5 Mn 149.6(6) . . ? C16 O6 Mn 130.3(4) . . ? C6 N1 N2 112.6(4) . . ? C7 N2 N1 111.4(4) . . ? C13 N3 C14 121.6(6) . . ? C13 N3 C15 122.5(6) . . ? C14 N3 C15 115.9(5) . . ? C16 N4 C18 123.1(6) . . ? C16 N4 C17 120.3(6) . . ? C18 N4 C17 116.6(6) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C2 C3 123.6(5) . . ? O1 C2 C1 116.1(5) . . ? C3 C2 C1 120.3(5) . . ? C2 C3 C4 123.7(5) . . ? C2 C3 S1 118.6(4) . . ? C4 C3 S1 117.5(4) . . ? O2 C4 C3 123.6(5) . . ? O2 C4 C5 115.1(5) . . ? C3 C4 C5 121.3(5) . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? N1 C6 S2 115.0(4) . . ? N1 C6 S1 121.7(4) . . ? S2 C6 S1 123.3(3) . . ? N2 C7 S2 115.3(4) . . ? N2 C7 S3 121.5(4) . . ? S2 C7 S3 123.2(3) . . ? C9 C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 C8 H8D 109.5 . . ? H8B C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? O3 C9 C10 124.2(5) . . ? O3 C9 C8 114.7(6) . . ? C10 C9 C8 121.0(6) . . ? C9 C10 C11 124.3(5) . . ? C9 C10 S3 117.5(4) . . ? C11 C10 S3 118.1(4) . . ? O4 C11 C10 123.2(5) . . ? O4 C11 C12 115.5(5) . . ? C10 C11 C12 121.3(5) . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12B C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? O5 C13 N3 126.4(7) . . ? O5 C13 H13A 116.8 . . ? N3 C13 H13A 116.8 . . ? N3 C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C14 H14D 109.5 . . ? H14B C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? N3 C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C15 H15D 109.5 . . ? H15B C15 H15D 109.5 . . ? H15C C15 H15D 109.5 . . ? O6 C16 N4 126.4(6) . . ? O6 C16 H16A 116.8 . . ? N4 C16 H16A 116.8 . . ? N4 C17 H17B 109.5 . . ? N4 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C17 H17D 109.5 . . ? H17B C17 H17D 109.5 . . ? H17C C17 H17D 109.5 . . ? N4 C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C18 H18D 109.5 . . ? H18B C18 H18D 109.5 . . ? H18C C18 H18D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn O1 C2 -31.7(5) . . . . ? O3 Mn O1 C2 146.0(5) 2_676 . . . ? O4 Mn O1 C2 -26.9(10) 2_676 . . . ? O5 Mn O1 C2 -125.0(5) . . . . ? O6 Mn O1 C2 62.7(5) . . . . ? O3 Mn O2 C4 -147.3(8) 2_676 . . . ? O4 Mn O2 C4 -156.1(5) 2_676 . . . ? O1 Mn O2 C4 22.8(5) . . . . ? O5 Mn O2 C4 118.0(5) . . . . ? O6 Mn O2 C4 -62.2(5) . . . . ? O2 Mn O5 C13 -100.4(12) . . . . ? O3 Mn O5 C13 91.8(12) 2_676 . . . ? O4 Mn O5 C13 173.1(12) 2_676 . . . ? O1 Mn O5 C13 -19.1(12) . . . . ? O2 Mn O6 C16 -155.8(6) . . . . ? O3 Mn O6 C16 12.0(6) 2_676 . . . ? O4 Mn O6 C16 -68.8(6) 2_676 . . . ? O1 Mn O6 C16 123.6(6) . . . . ? C6 N1 N2 C7 0.2(6) . . . . ? Mn O1 C2 C3 26.9(8) . . . . ? Mn O1 C2 C1 -154.8(4) . . . . ? O1 C2 C3 C4 0.9(9) . . . . ? C1 C2 C3 C4 -177.4(5) . . . . ? O1 C2 C3 S1 176.1(4) . . . . ? C1 C2 C3 S1 -2.2(7) . . . . ? C6 S1 C3 C2 100.4(4) . . . . ? C6 S1 C3 C4 -84.1(4) . . . . ? Mn O2 C4 C3 -8.6(8) . . . . ? Mn O2 C4 C5 170.4(4) . . . . ? C2 C3 C4 O2 -10.7(8) . . . . ? S1 C3 C4 O2 174.0(4) . . . . ? C2 C3 C4 C5 170.4(5) . . . . ? S1 C3 C4 C5 -4.9(7) . . . . ? N2 N1 C6 S2 0.1(6) . . . . ? N2 N1 C6 S1 -178.6(3) . . . . ? C7 S2 C6 N1 -0.2(4) . . . . ? C7 S2 C6 S1 178.4(3) . . . . ? C3 S1 C6 N1 -176.4(4) . . . . ? C3 S1 C6 S2 5.1(4) . . . . ? N1 N2 C7 S2 -0.4(6) . . . . ? N1 N2 C7 S3 -178.5(4) . . . . ? C6 S2 C7 N2 0.3(4) . . . . ? C6 S2 C7 S3 178.4(4) . . . . ? C10 S3 C7 N2 -174.0(5) . . . . ? C10 S3 C7 S2 8.0(4) . . . . ? Mn O3 C9 C10 -8.1(10) 2_676 . . . ? Mn O3 C9 C8 173.9(5) 2_676 . . . ? O3 C9 C10 C11 -4.5(10) . . . . ? C8 C9 C10 C11 173.3(6) . . . . ? O3 C9 C10 S3 172.0(5) . . . . ? C8 C9 C10 S3 -10.1(8) . . . . ? C7 S3 C10 C9 95.9(5) . . . . ? C7 S3 C10 C11 -87.3(5) . . . . ? Mn O4 C11 C10 19.7(8) 2_676 . . . ? Mn O4 C11 C12 -163.3(4) 2_676 . . . ? C9 C10 C11 O4 -1.3(9) . . . . ? S3 C10 C11 O4 -177.9(4) . . . . ? C9 C10 C11 C12 -178.1(6) . . . . ? S3 C10 C11 C12 5.4(8) . . . . ? Mn O5 C13 N3 -148.9(8) . . . . ? C14 N3 C13 O5 0.2(12) . . . . ? C15 N3 C13 O5 -177.1(8) . . . . ? Mn O6 C16 N4 -87.2(8) . . . . ? C18 N4 C16 O6 -178.2(7) . . . . ? C17 N4 C16 O6 3.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.341 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.063 #==END data_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 281996' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [MnL(dmf)(dmso)]2 ; _chemical_name_common (MnL(dmf)(dmso))2 _chemical_melting_point ? _chemical_formula_moiety 'C34 H50 Mn2 N6 O12 S8' _chemical_formula_sum 'C34 H50 Mn2 N6 O12 S8' _chemical_formula_weight 1101.16 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 10.89890(10) _cell_length_b 11.0697(3) _cell_length_c 11.7666(3) _cell_angle_alpha 107.7100(10) _cell_angle_beta 109.1140(10) _cell_angle_gamma 99.8060(10) _cell_volume 1218.97(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3051 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 25.16 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max .42 _exptl_crystal_size_mid .34 _exptl_crystal_size_min .28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .6785 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6325 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.16 _reflns_number_total 4239 _reflns_number_gt 3266 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL, enCIFer (Allen et al., 2004)' _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^)+(0.0232P)^2^+4.8641P] 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 4239 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1441 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.184 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.15074(10) 0.82473(10) 0.22738(9) 0.0436(3) Uani 1 1 d . . . S1 S -0.14422(18) 0.73662(17) 0.48210(16) 0.0540(4) Uani 1 1 d . . . S2 S -0.23198(17) 0.49843(17) 0.22532(16) 0.0494(4) Uani 1 1 d . . . S3 S -0.4454(2) 0.2260(2) 0.05204(19) 0.0700(6) Uani 1 1 d . . . S4 S 0.39903(19) 1.11017(19) 0.34597(19) 0.0622(5) Uani 1 1 d . . . O1 O 0.1609(4) 0.7517(5) 0.3754(4) 0.0518(11) Uani 1 1 d . . . O2 O 0.0073(4) 0.9059(4) 0.2875(4) 0.0497(11) Uani 1 1 d . . . O3 O -0.1692(5) 0.1275(5) -0.0700(4) 0.0583(12) Uani 1 1 d . . . O4 O -0.2814(5) 0.2900(5) -0.1836(4) 0.0574(12) Uani 1 1 d . . . O5 O 0.3221(5) 1.0004(5) 0.3685(5) 0.0676(14) Uani 1 1 d . . . O6 O -0.0320(5) 0.6581(5) 0.0751(5) 0.0690(14) Uani 1 1 d . . . N1 N -0.3487(5) 0.5135(5) 0.3844(5) 0.0469(12) Uani 1 1 d . . . N2 N -0.4192(5) 0.3910(5) 0.2823(5) 0.0495(13) Uani 1 1 d . . . N3 N -0.1593(7) 0.6552(6) -0.1195(6) 0.0718(18) Uani 1 1 d . . . C1 C 0.1132(7) 0.6562(8) 0.5120(7) 0.066(2) Uani 1 1 d . . . H1B H 0.0530 0.5669 0.4662 0.099 Uiso 1 1 calc R . . H1C H 0.1018 0.6975 0.5908 0.099 Uiso 1 1 calc R . . H1D H 0.2057 0.6546 0.5332 0.099 Uiso 1 1 calc R . . C2 C 0.0808(6) 0.7341(6) 0.4269(6) 0.0441(14) Uani 1 1 d . . . C3 C -0.0362(6) 0.7794(6) 0.4077(5) 0.0395(13) Uani 1 1 d . . . C4 C -0.0651(6) 0.8638(6) 0.3394(6) 0.0438(14) Uani 1 1 d . . . C5 C -0.1892(7) 0.9126(7) 0.3273(7) 0.0600(18) Uani 1 1 d . . . H5B H -0.1865 0.9780 0.2894 0.090 Uiso 1 1 calc R . . H5C H -0.1892 0.9515 0.4122 0.090 Uiso 1 1 calc R . . H5D H -0.2704 0.8391 0.2727 0.090 Uiso 1 1 calc R . . C6 C -0.2513(6) 0.5786(6) 0.3665(6) 0.0435(14) Uani 1 1 d . . . C7 C -0.3692(6) 0.3715(6) 0.1950(6) 0.0461(15) Uani 1 1 d . . . C8 C -0.2140(10) 0.1035(8) 0.1042(8) 0.084(3) Uani 1 1 d . . . H8B H -0.2813 0.0197 0.0738 0.126 Uiso 1 1 calc R . . H8C H -0.2203 0.1661 0.1776 0.126 Uiso 1 1 calc R . . H8D H -0.1249 0.0921 0.1300 0.126 Uiso 1 1 calc R . . C9 C -0.2382(7) 0.1551(6) -0.0043(6) 0.0536(17) Uani 1 1 d . . . C10 C -0.3317(7) 0.2298(6) -0.0249(6) 0.0490(16) Uani 1 1 d . . . C11 C -0.3468(7) 0.2949(6) -0.1129(6) 0.0497(15) Uani 1 1 d . . . C12 C -0.4404(8) 0.3799(8) -0.1243(7) 0.070(2) Uani 1 1 d . . . H12B H -0.3937 0.4679 -0.0585 0.105 Uiso 1 1 calc R . . H12C H -0.5192 0.3421 -0.1127 0.105 Uiso 1 1 calc R . . H12D H -0.4680 0.3840 -0.2090 0.105 Uiso 1 1 calc R . . C13 C -0.0927(9) 0.6097(7) -0.0454(7) 0.079(3) Uani 1 1 d . . . H13A H -0.0871 0.5258 -0.0863 0.095 Uiso 1 1 calc R . . C14 C -0.2198(11) 0.5870(10) -0.2610(8) 0.106(3) Uani 1 1 d . . . H14B H -0.1961 0.5061 -0.2848 0.159 Uiso 1 1 calc R . . H14C H -0.1862 0.6433 -0.2990 0.159 Uiso 1 1 calc R . . H14D H -0.3170 0.5668 -0.2925 0.159 Uiso 1 1 calc R . . C15 C -0.1849(11) 0.7798(10) -0.0669(9) 0.109(4) Uani 1 1 d . . . H15B H -0.1440 0.8134 0.0267 0.164 Uiso 1 1 calc R . . H15C H -0.2813 0.7659 -0.0962 0.164 Uiso 1 1 calc R . . H15D H -0.1464 0.8428 -0.0961 0.164 Uiso 1 1 calc R . . C16 C 0.4902(8) 1.2421(8) 0.5009(8) 0.081(3) Uani 1 1 d . . . H16B H 0.4272 1.2745 0.5336 0.121 Uiso 1 1 calc R . . H16C H 0.5469 1.3128 0.4928 0.121 Uiso 1 1 calc R . . H16D H 0.5460 1.2106 0.5602 0.121 Uiso 1 1 calc R . . C17 C 0.5410(8) 1.0643(8) 0.3267(8) 0.079(2) Uani 1 1 d . . . H17B H 0.5923 1.0488 0.4017 0.118 Uiso 1 1 calc R . . H17C H 0.5976 1.1346 0.3181 0.118 Uiso 1 1 calc R . . H17D H 0.5101 0.9846 0.2500 0.118 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 Mn 0.0432(5) 0.0498(6) 0.0434(5) 0.0205(4) 0.0212(4) 0.0153(4) S1 0.0584(10) 0.0522(10) 0.0494(10) 0.0121(8) 0.0312(8) 0.0070(8) S2 0.0478(9) 0.0537(10) 0.0459(9) 0.0144(8) 0.0269(8) 0.0063(8) S3 0.0650(12) 0.0635(12) 0.0633(12) 0.0021(9) 0.0383(10) -0.0079(9) S4 0.0542(11) 0.0593(11) 0.0637(12) 0.0263(9) 0.0130(9) 0.0112(9) O1 0.046(3) 0.071(3) 0.058(3) 0.040(2) 0.027(2) 0.026(2) O2 0.050(3) 0.054(3) 0.057(3) 0.029(2) 0.026(2) 0.021(2) O3 0.079(3) 0.069(3) 0.052(3) 0.034(2) 0.038(3) 0.039(3) O4 0.070(3) 0.069(3) 0.052(3) 0.030(2) 0.035(3) 0.036(3) O5 0.058(3) 0.069(3) 0.063(3) 0.020(3) 0.023(3) -0.001(3) O6 0.065(3) 0.056(3) 0.063(3) 0.019(3) 0.005(3) 0.011(3) N1 0.047(3) 0.051(3) 0.048(3) 0.020(3) 0.024(3) 0.017(3) N2 0.045(3) 0.055(3) 0.052(3) 0.020(3) 0.027(3) 0.011(3) N3 0.074(4) 0.058(4) 0.066(4) 0.018(3) 0.010(3) 0.026(3) C1 0.059(5) 0.082(5) 0.071(5) 0.049(4) 0.025(4) 0.023(4) C2 0.048(4) 0.041(3) 0.034(3) 0.011(3) 0.014(3) 0.003(3) C3 0.040(3) 0.040(3) 0.040(3) 0.016(3) 0.020(3) 0.009(3) C4 0.044(3) 0.039(3) 0.045(3) 0.012(3) 0.019(3) 0.012(3) C5 0.053(4) 0.063(4) 0.080(5) 0.036(4) 0.034(4) 0.027(4) C6 0.043(3) 0.050(4) 0.044(3) 0.022(3) 0.021(3) 0.015(3) C7 0.044(3) 0.048(4) 0.046(3) 0.017(3) 0.021(3) 0.008(3) C8 0.133(8) 0.079(6) 0.074(5) 0.046(5) 0.059(6) 0.049(6) C9 0.072(5) 0.042(4) 0.040(3) 0.011(3) 0.023(3) 0.006(3) C10 0.054(4) 0.043(4) 0.038(3) 0.003(3) 0.021(3) 0.004(3) C11 0.048(4) 0.052(4) 0.042(3) 0.013(3) 0.014(3) 0.016(3) C12 0.063(5) 0.093(6) 0.061(5) 0.026(4) 0.027(4) 0.043(4) C13 0.114(7) 0.041(4) 0.049(4) 0.014(4) 0.007(5) 0.000(4) C14 0.134(9) 0.106(8) 0.060(6) 0.024(5) 0.027(6) 0.032(7) C15 0.124(9) 0.097(7) 0.090(7) 0.022(6) 0.018(6) 0.070(7) C16 0.059(5) 0.066(5) 0.089(6) -0.002(4) 0.027(4) 0.014(4) C17 0.072(5) 0.068(5) 0.080(6) 0.000(4) 0.046(5) 0.004(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 Mn O1 2.112(4) . ? Mn O3 2.133(4) 2_565 ? Mn O2 2.137(4) . ? Mn O4 2.146(4) 2_565 ? Mn O5 2.189(5) . ? Mn O6 2.231(5) . ? S1 C6 1.758(6) . ? S1 C3 1.765(6) . ? S2 C7 1.723(6) . ? S2 C6 1.728(6) . ? S3 C10 1.759(6) . ? S3 C7 1.759(6) . ? S4 O5 1.499(5) . ? S4 C17 1.769(8) . ? S4 C16 1.773(8) . ? O1 C2 1.236(7) . ? O2 C4 1.255(7) . ? O3 C9 1.254(8) . ? O3 Mn 2.133(4) 2_565 ? O4 C11 1.256(7) . ? O4 Mn 2.146(4) 2_565 ? O6 C13 1.240(8) . ? N1 C6 1.292(7) . ? N1 N2 1.386(7) . ? N2 C7 1.292(7) . ? N3 C13 1.232(9) . ? N3 C15 1.445(10) . ? N3 C14 1.457(10) . ? C1 C2 1.505(9) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.424(8) . ? C3 C4 1.417(8) . ? C4 C5 1.521(8) . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C5 H5D 0.9600 . ? C8 C9 1.517(9) . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C9 C10 1.424(9) . ? C10 C11 1.415(9) . ? C11 C12 1.503(9) . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 H12D 0.9600 . ? C13 H13A 0.9300 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14 H14D 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15 H15D 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C16 H16D 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C17 H17D 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn O3 167.29(17) . 2_565 ? O1 Mn O2 81.52(16) . . ? O3 Mn O2 111.13(17) 2_565 . ? O1 Mn O4 86.70(17) . 2_565 ? O3 Mn O4 80.58(17) 2_565 2_565 ? O2 Mn O4 166.90(17) . 2_565 ? O1 Mn O5 89.99(18) . . ? O3 Mn O5 90.67(19) 2_565 . ? O2 Mn O5 92.72(18) . . ? O4 Mn O5 93.00(19) 2_565 . ? O1 Mn O6 94.28(19) . . ? O3 Mn O6 85.9(2) 2_565 . ? O2 Mn O6 84.79(19) . . ? O4 Mn O6 90.42(19) 2_565 . ? O5 Mn O6 174.68(19) . . ? C6 S1 C3 102.0(3) . . ? C7 S2 C6 85.2(3) . . ? C10 S3 C7 104.8(3) . . ? O5 S4 C17 106.0(4) . . ? O5 S4 C16 106.2(4) . . ? C17 S4 C16 97.0(4) . . ? C2 O1 Mn 131.5(4) . . ? C4 O2 Mn 128.6(4) . . ? C9 O3 Mn 133.0(4) . 2_565 ? C11 O4 Mn 133.5(4) . 2_565 ? S4 O5 Mn 129.2(3) . . ? C13 O6 Mn 138.0(5) . . ? C6 N1 N2 111.6(5) . . ? C7 N2 N1 111.6(5) . . ? C13 N3 C15 120.0(7) . . ? C13 N3 C14 123.3(7) . . ? C15 N3 C14 116.7(7) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C2 C3 124.3(6) . . ? O1 C2 C1 115.0(6) . . ? C3 C2 C1 120.7(6) . . ? C4 C3 C2 123.4(5) . . ? C4 C3 S1 118.6(4) . . ? C2 C3 S1 117.9(4) . . ? O2 C4 C3 124.6(5) . . ? O2 C4 C5 115.0(6) . . ? C3 C4 C5 120.4(5) . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? N1 C6 S2 115.7(5) . . ? N1 C6 S1 121.2(5) . . ? S2 C6 S1 123.1(3) . . ? N2 C7 S2 115.9(5) . . ? N2 C7 S3 120.4(5) . . ? S2 C7 S3 123.6(4) . . ? C9 C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 C8 H8D 109.5 . . ? H8B C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? O3 C9 C10 124.7(6) . . ? O3 C9 C8 114.6(7) . . ? C10 C9 C8 120.7(6) . . ? C11 C10 C9 123.7(6) . . ? C11 C10 S3 118.7(5) . . ? C9 C10 S3 117.3(5) . . ? O4 C11 C10 123.5(6) . . ? O4 C11 C12 115.1(6) . . ? C10 C11 C12 121.4(6) . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12B C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? N3 C13 O6 130.2(8) . . ? N3 C13 H13A 114.9 . . ? O6 C13 H13A 114.9 . . ? N3 C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C14 H14D 109.5 . . ? H14B C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? N3 C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C15 H15D 109.5 . . ? H15B C15 H15D 109.5 . . ? H15C C15 H15D 109.5 . . ? S4 C16 H16B 109.5 . . ? S4 C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S4 C16 H16D 109.5 . . ? H16B C16 H16D 109.5 . . ? H16C C16 H16D 109.5 . . ? S4 C17 H17B 109.5 . . ? S4 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S4 C17 H17D 109.5 . . ? H17B C17 H17D 109.5 . . ? H17C C17 H17D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mn O1 C2 -153.5(8) 2_565 . . . ? O2 Mn O1 C2 20.7(5) . . . . ? O4 Mn O1 C2 -153.5(6) 2_565 . . . ? O5 Mn O1 C2 113.5(6) . . . . ? O6 Mn O1 C2 -63.3(6) . . . . ? O1 Mn O2 C4 -26.5(5) . . . . ? O3 Mn O2 C4 152.1(5) 2_565 . . . ? O4 Mn O2 C4 -0.3(11) 2_565 . . . ? O5 Mn O2 C4 -116.1(5) . . . . ? O6 Mn O2 C4 68.6(5) . . . . ? C17 S4 O5 Mn -93.7(4) . . . . ? C16 S4 O5 Mn 163.8(4) . . . . ? O1 Mn O5 S4 173.7(4) . . . . ? O3 Mn O5 S4 6.4(4) 2_565 . . . ? O2 Mn O5 S4 -104.8(4) . . . . ? O4 Mn O5 S4 87.0(4) 2_565 . . . ? O1 Mn O6 C13 -164.2(8) . . . . ? O3 Mn O6 C13 3.1(8) 2_565 . . . ? O2 Mn O6 C13 114.7(8) . . . . ? O4 Mn O6 C13 -77.5(8) 2_565 . . . ? C6 N1 N2 C7 0.8(7) . . . . ? Mn O1 C2 C3 -9.5(9) . . . . ? Mn O1 C2 C1 169.1(5) . . . . ? O1 C2 C3 C4 -7.8(10) . . . . ? C1 C2 C3 C4 173.7(6) . . . . ? O1 C2 C3 S1 176.4(5) . . . . ? C1 C2 C3 S1 -2.1(8) . . . . ? C6 S1 C3 C4 98.6(5) . . . . ? C6 S1 C3 C2 -85.4(5) . . . . ? Mn O2 C4 C3 21.9(9) . . . . ? Mn O2 C4 C5 -159.5(4) . . . . ? C2 C3 C4 O2 1.0(10) . . . . ? S1 C3 C4 O2 176.7(5) . . . . ? C2 C3 C4 C5 -177.6(6) . . . . ? S1 C3 C4 C5 -1.9(8) . . . . ? N2 N1 C6 S2 -0.9(7) . . . . ? N2 N1 C6 S1 -179.3(4) . . . . ? C7 S2 C6 N1 0.7(5) . . . . ? C7 S2 C6 S1 179.0(4) . . . . ? C3 S1 C6 N1 -178.5(5) . . . . ? C3 S1 C6 S2 3.2(5) . . . . ? N1 N2 C7 S2 -0.3(7) . . . . ? N1 N2 C7 S3 -177.3(4) . . . . ? C6 S2 C7 N2 -0.2(5) . . . . ? C6 S2 C7 S3 176.8(5) . . . . ? C10 S3 C7 N2 -171.6(6) . . . . ? C10 S3 C7 S2 11.6(5) . . . . ? Mn O3 C9 C10 1.7(10) 2_565 . . . ? Mn O3 C9 C8 -177.5(5) 2_565 . . . ? O3 C9 C10 C11 -7.4(10) . . . . ? C8 C9 C10 C11 171.7(7) . . . . ? O3 C9 C10 S3 166.1(5) . . . . ? C8 C9 C10 S3 -14.7(9) . . . . ? C7 S3 C10 C11 -88.9(5) . . . . ? C7 S3 C10 C9 97.2(5) . . . . ? Mn O4 C11 C10 9.4(10) 2_565 . . . ? Mn O4 C11 C12 -172.7(5) 2_565 . . . ? C9 C10 C11 O4 1.9(10) . . . . ? S3 C10 C11 O4 -171.5(5) . . . . ? C9 C10 C11 C12 -175.9(6) . . . . ? S3 C10 C11 C12 10.7(9) . . . . ? C15 N3 C13 O6 -5.2(16) . . . . ? C14 N3 C13 O6 177.1(9) . . . . ? Mn O6 C13 N3 -68.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.700 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.085 #==END data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 281997' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [MnL(H2O)2]2(H2O)6 ; _chemical_name_common (MnL(H2O)2)2(H2O)6 _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Mn2 N4 O12 S6, 6(H2O)' _chemical_formula_sum 'C24 H44 Mn2 N4 O18 S6' _chemical_formula_weight 978.87 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 Orthorhombic _symmetry_space_group_name_H-M Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 18.5969(7) _cell_length_b 22.4917(7) _cell_length_c 10.3271(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4319.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3573 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 25.04 _exptl_crystal_description rhombic _exptl_crystal_colour yellow _exptl_crystal_size_max .42 _exptl_crystal_size_mid .34 _exptl_crystal_size_min .28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.944 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .6868 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7849 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.04 _reflns_number_total 1898 _reflns_number_gt 1363 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL, enCIFer (Allen et al., 2004), platon (Spek, 2003)' _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 hydrogens of coordinated water were solved by Fourier maps, but the hydrogens of solvate watercan not be added from Fourier maps. Therefore, hydrogen bondings are not given in this CIF. platon_squeeze_void_count_electrons is 59.8.Therefore solvate water/unit is six. ; _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^)+(0.0770P)^2^+9.3548P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap for water' _refine_ls_hydrogen_treatment 'constr, H2O refall with restraints' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1898 _refine_ls_number_parameters 137 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.22078(5) 0.7500 1.2500 0.0437(3) Uani 1 2 d S . . N1 N 0.0366(2) 0.46016(16) 1.2358(5) 0.0572(11) Uani 1 1 d . . . S1 S 0.15217(6) 0.52783(5) 1.18682(15) 0.0566(4) Uani 1 1 d . . . S2 S 0.0000 0.56949(7) 1.2500 0.0556(5) Uani 1 2 d S . . O1 O 0.1484(2) 0.70084(15) 1.1300(3) 0.0672(10) Uani 1 1 d . . . O2 O 0.20070(19) 0.67477(13) 1.3708(3) 0.0503(8) Uani 1 1 d . . . O3 O 0.3064(2) 0.7159(2) 1.1300(3) 0.0732(11) Uani 1 1 d D . . H3A H 0.302(3) 0.703(3) 1.053(3) 0.110 Uiso 1 1 d D . . H3B H 0.3480(17) 0.704(3) 1.152(5) 0.10(3) Uiso 1 1 d D . . O4 O 0.0301(7) 0.7883(6) 1.0790(14) 0.156(6) Uani 0.50 1 d P . . O5 O 0.4363(3) 0.6632(3) 1.1642(7) 0.131(2) Uani 1 1 d . A 1 C1 C 0.1163(3) 0.6253(3) 0.9856(5) 0.0755(16) Uani 1 1 d . . . H1A H 0.0696 0.6077 0.9957 0.113 Uiso 1 1 calc R . . H1B H 0.1489 0.5965 0.9502 0.113 Uiso 1 1 calc R . . H1C H 0.1130 0.6588 0.9281 0.113 Uiso 1 1 calc R . . C2 C 0.1435(2) 0.6457(2) 1.1156(4) 0.0478(11) Uani 1 1 d . . . C3 C 0.1604(2) 0.60454(19) 1.2167(4) 0.0442(11) Uani 1 1 d . . . C4 C 0.1837(2) 0.62208(18) 1.3420(4) 0.0433(10) Uani 1 1 d . . . C5 C 0.1870(4) 0.5778(2) 1.4499(5) 0.0706(16) Uani 1 1 d . . . H5A H 0.2263 0.5509 1.4353 0.106 Uiso 1 1 calc R . . H5B H 0.1428 0.5558 1.4531 0.106 Uiso 1 1 calc R . . H5C H 0.1940 0.5982 1.5306 0.106 Uiso 1 1 calc R . . C6 C 0.0619(2) 0.51361(19) 1.2252(5) 0.0467(11) 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 Mn 0.0694(7) 0.0301(5) 0.0315(5) 0.0011(4) 0.000 0.000 N1 0.051(2) 0.033(2) 0.088(3) -0.003(2) -0.004(2) -0.0011(17) S1 0.0481(7) 0.0391(7) 0.0825(9) -0.0208(6) 0.0063(6) -0.0005(5) S2 0.0505(9) 0.0287(8) 0.0876(13) 0.000 0.0117(9) 0.000 O1 0.101(3) 0.049(2) 0.052(2) 0.0079(17) -0.0282(19) -0.0082(19) O2 0.083(2) 0.0339(17) 0.0337(16) 0.0032(13) -0.0096(15) -0.0101(15) O3 0.088(3) 0.089(3) 0.042(2) -0.011(2) 0.0023(19) 0.028(2) O4 0.143(10) 0.191(13) 0.135(10) 0.068(9) 0.043(8) 0.091(9) O5 0.116(4) 0.116(4) 0.159(6) 0.016(4) 0.002(4) 0.025(3) C1 0.091(4) 0.085(4) 0.050(3) -0.009(3) -0.016(3) -0.013(3) C2 0.052(3) 0.048(3) 0.043(3) -0.006(2) -0.007(2) -0.007(2) C3 0.045(2) 0.035(2) 0.052(3) -0.009(2) -0.0012(19) -0.0035(19) C4 0.051(2) 0.034(2) 0.045(2) 0.0019(19) -0.003(2) -0.0028(19) C5 0.104(4) 0.043(3) 0.064(3) 0.015(3) -0.018(3) -0.015(3) C6 0.045(2) 0.036(2) 0.059(3) -0.006(2) -0.008(2) 0.0004(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O2 2.135(3) 8_467 ? Mn O2 2.135(3) . ? Mn O1 2.138(3) . ? Mn O1 2.138(3) 8_467 ? Mn O3 2.158(4) 8_467 ? Mn O3 2.158(4) . ? N1 C6 1.296(6) . ? N1 N1 1.393(8) 3_557 ? S1 C6 1.754(5) . ? S1 C3 1.759(4) . ? S2 C6 1.724(4) . ? S2 C6 1.724(4) 3_557 ? O1 C2 1.252(6) . ? O2 C4 1.263(5) . ? O3 H3A 0.852(10) . ? O3 H3B 0.851(10) . ? C1 C2 1.506(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.431(7) . ? C3 C4 1.420(6) . ? C4 C5 1.496(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn O2 159.85(19) 8_467 . ? O2 Mn O1 87.75(13) 8_467 . ? O2 Mn O1 79.57(12) . . ? O2 Mn O1 79.57(12) 8_467 8_467 ? O2 Mn O1 87.75(13) . 8_467 ? O1 Mn O1 102.0(2) . 8_467 ? O2 Mn O3 100.57(15) 8_467 8_467 ? O2 Mn O3 94.28(14) . 8_467 ? O1 Mn O3 168.82(17) . 8_467 ? O1 Mn O3 87.00(17) 8_467 8_467 ? O2 Mn O3 94.28(14) 8_467 . ? O2 Mn O3 100.57(15) . . ? O1 Mn O3 87.00(17) . . ? O1 Mn O3 168.82(17) 8_467 . ? O3 Mn O3 85.0(2) 8_467 . ? C6 N1 N1 111.9(3) . 3_557 ? C6 S1 C3 102.9(2) . . ? C6 S2 C6 86.4(3) . 3_557 ? C2 O1 Mn 128.8(3) . . ? C4 O2 Mn 130.5(3) . . ? Mn O3 H3A 126(4) . . ? Mn O3 H3B 129(4) . . ? H3A O3 H3B 102.8(16) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.6(4) . . ? O1 C2 C1 115.6(4) . . ? C3 C2 C1 121.8(4) . . ? C4 C3 C2 123.5(4) . . ? C4 C3 S1 117.3(3) . . ? C2 C3 S1 119.2(3) . . ? O2 C4 C3 123.5(4) . . ? O2 C4 C5 116.0(4) . . ? C3 C4 C5 120.4(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 S2 114.9(3) . . ? N1 C6 S1 122.4(3) . . ? S2 C6 S1 122.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn O1 C2 159.1(4) 8_467 . . . ? O2 Mn O1 C2 -36.7(4) . . . . ? O1 Mn O1 C2 -122.1(5) 8_467 . . . ? O3 Mn O1 C2 20.6(10) 8_467 . . . ? O3 Mn O1 C2 64.6(4) . . . . ? O2 Mn O2 C4 79.4(4) 8_467 . . . ? O1 Mn O2 C4 27.6(4) . . . . ? O1 Mn O2 C4 130.2(4) 8_467 . . . ? O3 Mn O2 C4 -143.0(4) 8_467 . . . ? O3 Mn O2 C4 -57.4(4) . . . . ? Mn O1 C2 C3 30.7(7) . . . . ? Mn O1 C2 C1 -151.1(4) . . . . ? O1 C2 C3 C4 0.5(7) . . . . ? C1 C2 C3 C4 -177.6(5) . . . . ? O1 C2 C3 S1 -179.7(4) . . . . ? C1 C2 C3 S1 2.2(6) . . . . ? C6 S1 C3 C4 92.2(4) . . . . ? C6 S1 C3 C2 -87.5(4) . . . . ? Mn O2 C4 C3 -12.8(7) . . . . ? Mn O2 C4 C5 169.0(4) . . . . ? C2 C3 C4 O2 -9.8(7) . . . . ? S1 C3 C4 O2 170.5(4) . . . . ? C2 C3 C4 C5 168.3(5) . . . . ? S1 C3 C4 C5 -11.4(6) . . . . ? N1 N1 C6 S2 0.5(7) 3_557 . . . ? N1 N1 C6 S1 -178.8(4) 3_557 . . . ? C6 S2 C6 N1 -0.2(3) 3_557 . . . ? C6 S2 C6 S1 179.1(4) 3_557 . . . ? C3 S1 C6 N1 -168.8(4) . . . . ? C3 S1 C6 S2 11.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.999 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.078 #==END data_Compound_8 _database_code_depnum_ccdc_archive 'CCDC 281998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Fe2L2(dmf)2(SO4)](CH2Cl2)2 ; _chemical_name_common (Fe2L2(dmf)2(SO4))(CH2Cl2)2 _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 Fe2 N6 O14 S7, 2(C H2 Cl2)' _chemical_formula_sum 'C32 H42 Cl4 Fe2 N6 O14 S7' _chemical_formula_weight 1212.64 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 11.4902(8) _cell_length_b 15.0401(9) _cell_length_c 15.0968(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.810(2) _cell_angle_gamma 90.00 _cell_volume 2544.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2200 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max .34 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.131 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .5243 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7328 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4449 _reflns_number_gt 2244 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL, enCIFer (Allen et al., 2004)' _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^)+(0.1690P)^2^+6.3786P] 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 4449 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1725 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.3269 _refine_ls_wR_factor_gt 0.2475 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Fe Fe 0.57114(11) 0.34131(8) 0.13197(9) 0.0669(5) Uani 1 1 d . . . S1 S 0.9291(3) 0.5250(2) 0.2953(2) 0.0963(10) Uani 1 1 d . . . S2 S 0.7917(2) 0.64202(17) 0.14111(18) 0.0812(8) Uani 1 1 d . . . S3 S 0.7920(2) 0.82499(17) 0.0532(2) 0.0861(9) Uani 1 1 d . . . S4 S 0.5388(7) 0.4787(4) -0.0272(4) 0.100(2) Uani 0.50 1 d P . 1 O1 O 0.6069(6) 0.4191(4) 0.2394(4) 0.0780(18) Uani 1 1 d . A . O2 O 0.7413(6) 0.3501(4) 0.1287(5) 0.0748(17) Uani 1 1 d . A . O3 O 0.4588(5) 0.7449(4) -0.0298(4) 0.0729(17) Uani 1 1 d . . . O4 O 0.5946(6) 0.6796(5) -0.1416(4) 0.0783(18) Uani 1 1 d . . . O5 O 0.5291(7) 0.4401(4) 0.0515(5) 0.097(2) Uani 1 1 d . . . O6 O 0.6127(7) 0.2347(5) 0.2145(6) 0.104(3) Uani 1 1 d . A 1 O7 O 0.4905(15) 0.4170(9) -0.1016(9) 0.099(5) Uani 0.50 1 d P B 1 O8 O 0.6651(12) 0.5107(10) -0.0100(10) 0.097(4) Uani 0.50 1 d P C 1 N1 N 0.9870(8) 0.6887(6) 0.2502(6) 0.083(2) Uani 1 1 d . . . N2 N 0.9528(7) 0.7610(5) 0.1917(6) 0.083(2) Uani 1 1 d . . . N3 N 0.7072(11) 0.1297(7) 0.3075(8) 0.123(4) Uani 1 1 d . . . C1 C 0.6812(12) 0.5351(8) 0.3388(8) 0.108(4) Uani 1 1 d . A . H1B H 0.6818 0.5934 0.3132 0.162 Uiso 1 1 calc R . . H1D H 0.7451 0.5301 0.3917 0.162 Uiso 1 1 calc R . . H1C H 0.6064 0.5253 0.3555 0.162 Uiso 1 1 calc R . . C2 C 0.6974(10) 0.4674(6) 0.2707(6) 0.072(2) Uani 1 1 d . . . C3 C 0.8033(8) 0.4617(6) 0.2383(6) 0.070(2) Uani 1 1 d . A . C4 C 0.8213(8) 0.4040(6) 0.1690(7) 0.070(2) Uani 1 1 d . . . C5 C 0.9339(9) 0.4032(8) 0.1368(8) 0.095(3) Uani 1 1 d . A . H5A H 0.9999 0.3942 0.1875 0.142 Uiso 1 1 calc R . . H5B H 0.9432 0.4590 0.1083 0.142 Uiso 1 1 calc R . . H5C H 0.9316 0.3559 0.0938 0.142 Uiso 1 1 calc R . . C6 C 0.9120(8) 0.6237(6) 0.2314(6) 0.072(2) Uani 1 1 d . . . C7 C 0.8540(8) 0.7449(6) 0.1329(7) 0.070(2) Uani 1 1 d . . . C8 C 0.8004(10) 0.7084(9) -0.1120(8) 0.105(4) Uani 1 1 d . . . H8A H 0.8511 0.6716 -0.0676 0.157 Uiso 1 1 calc R . . H8B H 0.8363 0.7659 -0.1130 0.157 Uiso 1 1 calc R . . H8C H 0.7898 0.6813 -0.1708 0.157 Uiso 1 1 calc R . . C9 C 0.6805(9) 0.7184(7) -0.0876(6) 0.072(2) Uani 1 1 d . . . C10 C 0.6665(8) 0.7674(6) -0.0108(6) 0.067(2) Uani 1 1 d . . . C11 C 0.5555(8) 0.7779(6) 0.0151(6) 0.065(2) Uani 1 1 d . . . C12 C 0.5434(11) 0.8285(8) 0.0986(8) 0.102(4) Uani 1 1 d . . . H12A H 0.4620 0.8261 0.1047 0.153 Uiso 1 1 calc R . . H12B H 0.5662 0.8893 0.0933 0.153 Uiso 1 1 calc R . . H12C H 0.5943 0.8023 0.1512 0.153 Uiso 1 1 calc R . . C13 C 0.6904(13) 0.2039(9) 0.2652(10) 0.114(4) Uani 1 1 d . A . H13A H 0.7566 0.2411 0.2790 0.137 Uiso 1 1 calc R D 1 C14 C 0.671(3) 0.040(2) 0.264(3) 0.168(13) Uiso 0.50 1 d P E 1 H14A H 0.7218 0.0250 0.2239 0.253 Uiso 0.50 1 calc PR E 1 H14B H 0.5896 0.0422 0.2312 0.253 Uiso 0.50 1 calc PR E 1 H14C H 0.6792 -0.0046 0.3111 0.253 Uiso 0.50 1 calc PR E 1 C14' C 0.594(3) 0.092(2) 0.326(3) 0.158(12) Uiso 0.50 1 d P E 2 H14D H 0.6051 0.0790 0.3894 0.237 Uiso 0.50 1 calc PR E 2 H14E H 0.5731 0.0390 0.2911 0.237 Uiso 0.50 1 calc PR E 2 H14F H 0.5309 0.1352 0.3089 0.237 Uiso 0.50 1 calc PR E 2 C15 C 0.8108(16) 0.1100(14) 0.3760(14) 0.189(8) Uani 1 1 d . E . H15A H 0.8683 0.1567 0.3784 0.284 Uiso 1 1 calc R . . H15B H 0.8445 0.0548 0.3619 0.284 Uiso 1 1 calc R . . H15C H 0.7893 0.1052 0.4337 0.284 Uiso 1 1 calc R . . C16 C 1.1946(11) 0.8418(8) -0.0510(10) 0.113(4) Uani 1 1 d . . . H16A H 1.2598 0.8008 -0.0289 0.136 Uiso 1 1 calc R . . H16B H 1.1480 0.8182 -0.1076 0.136 Uiso 1 1 calc R . . Cl1 Cl 1.2518(5) 0.9416(3) -0.0715(4) 0.179(2) Uani 1 1 d . . . Cl2 Cl 1.1063(4) 0.8468(4) 0.0264(4) 0.173(2) 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 Fe 0.0692(9) 0.0639(8) 0.0647(9) 0.0053(6) 0.0084(6) 0.0009(6) S1 0.100(2) 0.0890(19) 0.0829(19) 0.0127(14) -0.0165(15) -0.0237(16) S2 0.0764(16) 0.0723(16) 0.0843(18) 0.0074(13) -0.0049(13) -0.0129(12) S3 0.0810(17) 0.0705(16) 0.097(2) 0.0103(14) -0.0018(14) -0.0141(13) S4 0.149(6) 0.085(4) 0.067(4) 0.015(3) 0.027(3) 0.023(4) O1 0.088(5) 0.087(4) 0.058(4) -0.002(3) 0.015(3) -0.012(4) O2 0.071(4) 0.064(4) 0.086(5) -0.002(3) 0.010(3) -0.003(3) O3 0.058(4) 0.072(4) 0.086(4) -0.006(3) 0.009(3) 0.004(3) O4 0.072(4) 0.095(5) 0.068(4) -0.007(3) 0.014(3) -0.003(4) O5 0.137(6) 0.076(4) 0.079(5) 0.026(4) 0.028(4) 0.030(4) O6 0.093(5) 0.095(5) 0.112(6) 0.044(5) 0.001(5) 0.000(4) O7 0.149(13) 0.076(9) 0.064(8) -0.015(7) 0.003(8) -0.013(9) O8 0.066(8) 0.111(11) 0.110(12) 0.003(9) 0.010(8) -0.023(8) N1 0.085(6) 0.082(5) 0.071(5) -0.001(4) -0.005(4) -0.022(5) N2 0.082(6) 0.077(5) 0.080(6) -0.001(4) -0.001(4) -0.010(4) N3 0.126(9) 0.093(7) 0.133(9) 0.061(7) -0.007(7) 0.007(6) C1 0.133(10) 0.093(8) 0.094(8) -0.025(7) 0.020(7) -0.010(7) C2 0.089(7) 0.074(6) 0.050(5) 0.005(4) 0.008(5) -0.004(5) C3 0.067(6) 0.068(6) 0.065(6) 0.011(5) -0.004(4) -0.013(5) C4 0.062(5) 0.063(5) 0.084(7) 0.024(5) 0.013(5) 0.004(5) C5 0.074(7) 0.100(8) 0.105(9) 0.001(7) 0.010(6) -0.004(6) C6 0.070(6) 0.064(5) 0.074(6) 0.006(5) -0.001(5) -0.010(5) C7 0.061(5) 0.064(5) 0.084(7) 0.006(5) 0.012(5) -0.007(4) C8 0.081(7) 0.130(10) 0.112(9) -0.001(8) 0.040(6) 0.011(7) C9 0.076(6) 0.079(6) 0.058(6) 0.008(5) 0.008(5) 0.006(5) C10 0.065(5) 0.058(5) 0.069(6) 0.014(4) -0.001(4) -0.008(4) C11 0.058(5) 0.062(5) 0.071(6) 0.000(4) 0.006(4) -0.002(4) C12 0.095(8) 0.117(9) 0.092(8) -0.039(7) 0.019(6) 0.008(7) C13 0.123(11) 0.110(10) 0.115(11) 0.042(9) 0.040(9) 0.027(9) C15 0.155(15) 0.207(19) 0.197(19) 0.100(17) 0.023(14) -0.005(15) C16 0.096(9) 0.097(9) 0.131(11) -0.026(8) -0.007(8) 0.004(7) Cl1 0.205(5) 0.108(3) 0.209(5) -0.011(3) 0.017(4) -0.011(3) Cl2 0.147(4) 0.205(5) 0.171(4) -0.065(4) 0.045(3) -0.003(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 Fe O5 1.912(6) . ? Fe O4 1.967(6) 3_665 ? Fe O1 1.968(6) . ? Fe O2 1.972(7) . ? Fe O3 1.986(6) 3_665 ? Fe O6 2.022(7) . ? S1 C6 1.758(9) . ? S1 C3 1.784(9) . ? S2 C7 1.721(9) . ? S2 C6 1.735(9) . ? S3 C7 1.740(9) . ? S3 C10 1.773(9) . ? S4 O5 1.349(8) . ? S4 O5 1.452(8) 3_665 ? S4 O7 1.468(14) . ? S4 S4 1.483(12) 3_665 ? S4 O8 1.496(14) . ? O1 C2 1.270(11) . ? O2 C4 1.274(11) . ? O3 C11 1.268(10) . ? O3 Fe 1.986(6) 3_665 ? O4 C9 1.274(11) . ? O4 Fe 1.967(6) 3_665 ? O5 S4 1.452(8) 3_665 ? O6 C13 1.138(14) . ? N1 C6 1.292(11) . ? N1 N2 1.400(11) . ? N2 C7 1.300(11) . ? N3 C13 1.280(15) . ? N3 C15 1.424(18) . ? N3 C14' 1.50(3) . ? N3 C14 1.52(4) . ? C1 C2 1.488(14) . ? C1 H1B 0.9600 . ? C1 H1D 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.411(13) . ? C3 C4 1.410(14) . ? C4 C5 1.479(13) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C8 C9 1.510(14) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.412(13) . ? C10 C11 1.424(13) . ? C11 C12 1.505(13) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 Cl1 1.695(13) . ? C16 Cl2 1.710(15) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? 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 Fe O4 93.3(3) . 3_665 ? O5 Fe O1 92.2(3) . . ? O4 Fe O1 93.6(3) 3_665 . ? O5 Fe O2 92.5(3) . . ? O4 Fe O2 174.0(3) 3_665 . ? O1 Fe O2 87.4(3) . . ? O5 Fe O3 92.2(3) . 3_665 ? O4 Fe O3 87.1(3) 3_665 3_665 ? O1 Fe O3 175.5(3) . 3_665 ? O2 Fe O3 91.5(3) . 3_665 ? O5 Fe O6 178.4(3) . . ? O4 Fe O6 85.9(3) 3_665 . ? O1 Fe O6 89.2(3) . . ? O2 Fe O6 88.2(3) . . ? O3 Fe O6 86.4(3) 3_665 . ? C6 S1 C3 101.9(4) . . ? C7 S2 C6 85.8(4) . . ? C7 S3 C10 101.4(4) . . ? O5 S4 O5 116.2(5) . 3_665 ? O5 S4 O7 108.1(8) . . ? O5 S4 O7 104.3(8) 3_665 . ? O5 S4 S4 61.5(5) . 3_665 ? O5 S4 S4 54.7(5) 3_665 3_665 ? O7 S4 S4 121.7(10) . 3_665 ? O5 S4 O8 104.6(8) . . ? O5 S4 O8 102.7(8) 3_665 . ? O7 S4 O8 121.5(10) . . ? S4 S4 O8 116.3(9) 3_665 . ? C2 O1 Fe 130.5(6) . . ? C4 O2 Fe 130.2(6) . . ? C11 O3 Fe 130.7(6) . 3_665 ? C9 O4 Fe 130.7(6) . 3_665 ? S4 O5 S4 63.8(5) . 3_665 ? S4 O5 Fe 146.7(6) . . ? S4 O5 Fe 149.4(6) 3_665 . ? C13 O6 Fe 141.3(9) . . ? C6 N1 N2 111.6(7) . . ? C7 N2 N1 111.5(8) . . ? C13 N3 C15 123.6(14) . . ? C13 N3 C14' 112.2(17) . . ? C15 N3 C14' 114.1(17) . . ? C13 N3 C14 124.6(19) . . ? C15 N3 C14 103.3(18) . . ? C14' N3 C14 65.1(18) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? H1D C1 H1C 109.5 . . ? O1 C2 C3 122.3(9) . . ? O1 C2 C1 115.5(10) . . ? C3 C2 C1 122.0(10) . . ? C4 C3 C2 125.0(8) . . ? C4 C3 S1 116.7(7) . . ? C2 C3 S1 118.0(8) . . ? O2 C4 C3 122.5(8) . . ? O2 C4 C5 115.4(10) . . ? C3 C4 C5 122.1(9) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 S2 115.4(7) . . ? N1 C6 S1 122.0(7) . . ? S2 C6 S1 122.5(5) . . ? N2 C7 S2 115.6(7) . . ? N2 C7 S3 120.4(7) . . ? S2 C7 S3 124.0(5) . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 C10 123.5(9) . . ? O4 C9 C8 114.6(9) . . ? C10 C9 C8 121.9(9) . . ? C9 C10 C11 123.7(8) . . ? C9 C10 S3 118.4(7) . . ? C11 C10 S3 117.8(7) . . ? O3 C11 C10 122.9(8) . . ? O3 C11 C12 114.4(8) . . ? C10 C11 C12 122.7(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O6 C13 N3 134.4(15) . . ? O6 C13 H13A 112.8 . . ? N3 C13 H13A 112.8 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C14' H14D 109.5 . . ? N3 C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? N3 C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Cl1 C16 Cl2 113.5(7) . . ? Cl1 C16 H16A 108.9 . . ? Cl2 C16 H16A 108.9 . . ? Cl1 C16 H16B 108.9 . . ? Cl2 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Fe O1 C2 -77.6(8) . . . . ? O4 Fe O1 C2 -171.1(8) 3_665 . . . ? O2 Fe O1 C2 14.8(8) . . . . ? O6 Fe O1 C2 103.1(8) . . . . ? O5 Fe O2 C4 77.5(8) . . . . ? O1 Fe O2 C4 -14.6(8) . . . . ? O3 Fe O2 C4 169.7(8) 3_665 . . . ? O6 Fe O2 C4 -103.9(8) . . . . ? O5 S4 O5 S4 0.0 3_665 . . 3_665 ? O7 S4 O5 S4 -116.8(11) . . . 3_665 ? O8 S4 O5 S4 112.3(9) . . . 3_665 ? O5 S4 O5 Fe 176.2(12) 3_665 . . . ? O7 S4 O5 Fe 59.4(15) . . . . ? S4 S4 O5 Fe 176.2(12) 3_665 . . . ? O8 S4 O5 Fe -71.4(14) . . . . ? O4 Fe O5 S4 -130.3(12) 3_665 . . . ? O1 Fe O5 S4 136.0(12) . . . . ? O2 Fe O5 S4 48.5(12) . . . . ? O3 Fe O5 S4 -43.1(12) 3_665 . . . ? O4 Fe O5 S4 43.0(12) 3_665 . . 3_665 ? O1 Fe O5 S4 -50.7(12) . . . 3_665 ? O2 Fe O5 S4 -138.2(12) . . . 3_665 ? O3 Fe O5 S4 130.2(12) 3_665 . . 3_665 ? o4 Fe O6 C13 -156.0(17) 3_665 . . . ? O1 Fe O6 C13 -62.3(16) . . . . ? O2 Fe O6 C13 25.1(16) . . . . ? O3 Fe O6 C13 116.7(16) 3_665 . . . ? C6 N1 N2 C7 0.0(13) . . . . ? Fe O1 C2 C3 -11.0(13) . . . . ? Fe O1 C2 C1 164.7(7) . . . . ? O1 C2 C3 C4 0.5(14) . . . . ? C1 C2 C3 C4 -174.9(10) . . . . ? O1 C2 C3 S1 -173.9(7) . . . . ? C1 C2 C3 S1 10.7(13) . . . . ? C6 S1 C3 C4 92.4(8) . . . . ? C6 S1 C3 C2 -92.7(8) . . . . ? Fe O2 C4 C3 10.7(13) . . . . ? Fe O2 C4 C5 -168.1(6) . . . . ? C2 C3 C4 O2 -0.3(14) . . . . ? S1 C3 C4 O2 174.1(7) . . . . ? C2 C3 C4 C5 178.4(9) . . . . ? S1 C3 C4 C5 -7.2(12) . . . . ? N2 N1 C6 S2 0.1(12) . . . . ? N2 N1 C6 S1 -178.2(7) . . . . ? C7 S2 C6 N1 -0.1(9) . . . . ? C7 S2 C6 S1 178.2(7) . . . . ? C3 S1 C6 N1 -179.4(9) . . . . ? C3 S1 C6 S2 2.4(8) . . . . ? N1 N2 C7 S2 0.0(12) . . . . ? N1 N2 C7 S3 179.4(7) . . . . ? C6 S2 C7 N2 0.0(8) . . . . ? C6 S2 C7 S3 -179.3(7) . . . . ? C10 S3 C7 N2 177.4(8) . . . . ? C10 S3 C7 S2 -3.3(8) . . . . ? Fe O4 C9 C10 -9.4(14) 3_665 . . . ? Fe O4 C9 C8 170.8(7) 3_665 . . . ? O4 C9 C10 C11 0.7(14) . . . . ? C8 C9 C10 C11 -179.4(9) . . . . ? O4 C9 C10 S3 -175.2(7) . . . . ? C8 C9 C10 S3 4.6(12) . . . . ? C7 S3 C10 C9 -90.6(8) . . . . ? C7 S3 C10 C11 93.3(7) . . . . ? Fe O3 C11 C10 9.9(13) 3_665 . . . ? Fe O3 C11 C12 -169.5(7) 3_665 . . . ? C9 C10 C11 O3 -1.0(14) . . . . ? S3 C10 C11 O3 174.9(7) . . . . ? C9 C10 C11 C12 178.3(9) . . . . ? S3 C10 C11 C12 -5.7(12) . . . . ? Fe O6 C13 N3 -172.0(12) . . . . ? C15 N3 C13 O6 -173.3(18) . . . . ? C14' N3 C13 O6 -30(3) . . . . ? C14 N3 C13 O6 44(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.161 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.115 #==END data_H2L _database_code_depnum_ccdc_archive 'CCDC 281999' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 N2 O4 S3' _chemical_formula_sum 'C12 H14 N2 O4 S3' _chemical_formula_weight 346.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9134(2) _cell_length_b 8.7061(3) _cell_length_c 13.7625(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.259(2) _cell_angle_gamma 90.00 _cell_volume 1540.74(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2589 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.07 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max .42 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .7616 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4263 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.07 _reflns_number_total 2679 _reflns_number_gt 2266 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL, enCIFer (Allen et al., 2004)' _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 hydrogens of hydroxyl were solved by Fourier maps without refinement. ; _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^)+(0.0127P)^2^+2.6752P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap for hydroxyl' _refine_ls_hydrogen_treatment 'constr and refall with hydroxy' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0149(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2679 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.225 _refine_ls_restrained_S_all 1.225 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.53011(7) 0.31731(13) 0.28400(7) 0.0488(3) Uani 1 1 d . . . S2 S 0.37086(7) 0.28077(13) 0.43402(7) 0.0462(3) Uani 1 1 d . . . S3 S 0.34864(8) 0.27272(14) 0.65413(7) 0.0523(3) Uani 1 1 d . . . O1 O 0.2855(3) 0.1154(4) 0.1455(2) 0.0718(9) Uani 1 1 d . A 1 H1A H 0.255(4) 0.242(7) 0.126(4) 0.086 Uiso 1 1 d . B 1 O2 O 0.2641(2) 0.3950(4) 0.1281(2) 0.0674(9) Uani 1 1 d . A 2 O3 O 0.1001(2) 0.0384(4) 0.5533(2) 0.0631(8) Uani 1 1 d . C 1 H3A H 0.064(3) 0.152(6) 0.538(3) 0.076 Uiso 1 1 d . D 1 O4 O 0.0607(2) 0.3128(4) 0.5349(2) 0.0688(9) Uani 1 1 d . C 2 N1 N 0.5665(2) 0.3165(4) 0.4779(2) 0.0484(8) Uani 1 1 d . . . N2 N 0.5229(2) 0.3043(4) 0.5665(2) 0.0483(8) Uani 1 1 d . . . C1 C 0.4309(4) -0.0037(6) 0.2284(4) 0.0767(15) Uani 1 1 d . A . H1B H 0.4022 -0.0441 0.2851 0.115 Uiso 1 1 calc R . . H1C H 0.5030 0.0202 0.2442 0.115 Uiso 1 1 calc R . . H1D H 0.4242 -0.0786 0.1771 0.115 Uiso 1 1 calc R . . C2 C 0.3739(3) 0.1377(5) 0.1958(3) 0.0546(11) Uani 1 1 d . . . C3 C 0.4082(3) 0.2872(5) 0.2168(3) 0.0440(9) Uani 1 1 d . A . C4 C 0.3507(3) 0.4157(5) 0.1783(3) 0.0501(10) Uani 1 1 d . . . C5 C 0.3884(4) 0.5757(5) 0.1930(3) 0.0618(12) Uani 1 1 d . A . H5A H 0.3394 0.6452 0.1598 0.093 Uiso 1 1 calc R . . H5B H 0.4546 0.5865 0.1672 0.093 Uiso 1 1 calc R . . H5C H 0.3956 0.5991 0.2615 0.093 Uiso 1 1 calc R . . C6 C 0.4972(3) 0.3062(4) 0.4040(3) 0.0376(8) Uani 1 1 d . . . C7 C 0.4233(3) 0.2847(4) 0.5539(3) 0.0390(8) Uani 1 1 d . . . C8 C 0.2620(4) -0.0597(5) 0.6146(3) 0.0663(13) Uani 1 1 d . C . H8A H 0.2229 -0.1532 0.6058 0.099 Uiso 1 1 calc R . . H8B H 0.2893 -0.0507 0.6816 0.099 Uiso 1 1 calc R . . H8C H 0.3183 -0.0610 0.5737 0.099 Uiso 1 1 calc R . . C9 C 0.1934(3) 0.0727(5) 0.5880(3) 0.0473(10) Uani 1 1 d . . . C10 C 0.2246(3) 0.2271(5) 0.5982(3) 0.0435(9) Uani 1 1 d . C . C11 C 0.1524(3) 0.3464(5) 0.5708(3) 0.0531(10) Uani 1 1 d . . . C12 C 0.1790(4) 0.5127(5) 0.5821(4) 0.0695(13) Uani 1 1 d . C . H12A H 0.1193 0.5736 0.5606 0.104 Uiso 1 1 calc R . . H12B H 0.2351 0.5368 0.5435 0.104 Uiso 1 1 calc R . . H12C H 0.1997 0.5345 0.6494 0.104 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 S1 0.0331(5) 0.0705(7) 0.0437(5) 0.0042(5) 0.0081(4) -0.0012(5) S2 0.0282(5) 0.0722(7) 0.0378(5) -0.0013(5) 0.0017(4) -0.0050(4) S3 0.0418(5) 0.0787(8) 0.0368(5) -0.0029(5) 0.0055(4) -0.0058(5) O1 0.066(2) 0.081(2) 0.067(2) -0.0142(18) 0.0008(17) -0.0201(18) O2 0.0506(17) 0.091(3) 0.0570(19) 0.0005(17) -0.0125(14) 0.0046(17) O3 0.0437(16) 0.071(2) 0.075(2) -0.0012(17) 0.0069(14) -0.0111(15) O4 0.0378(16) 0.085(3) 0.084(2) 0.0092(19) 0.0061(15) 0.0127(16) N1 0.0334(16) 0.068(2) 0.0435(18) -0.0024(16) 0.0024(14) -0.0015(15) N2 0.0343(16) 0.068(2) 0.0419(17) -0.0060(16) 0.0005(13) -0.0006(16) C1 0.079(3) 0.054(3) 0.099(4) 0.000(3) 0.018(3) -0.001(3) C2 0.051(2) 0.069(3) 0.045(2) -0.005(2) 0.0147(19) -0.003(2) C3 0.0368(19) 0.061(3) 0.0351(19) -0.0028(18) 0.0068(15) 0.0013(18) C4 0.046(2) 0.068(3) 0.037(2) -0.0029(19) 0.0076(17) 0.005(2) C5 0.065(3) 0.061(3) 0.058(3) 0.000(2) 0.003(2) 0.011(2) C6 0.0297(17) 0.041(2) 0.042(2) -0.0030(16) 0.0064(15) 0.0004(15) C7 0.0337(18) 0.048(2) 0.0360(18) -0.0006(16) 0.0042(14) -0.0054(16) C8 0.073(3) 0.061(3) 0.065(3) 0.004(2) 0.007(2) 0.008(2) C9 0.041(2) 0.061(3) 0.041(2) 0.0003(19) 0.0097(16) 0.0012(19) C10 0.0346(19) 0.057(3) 0.040(2) -0.0001(18) 0.0090(15) 0.0021(18) C11 0.045(2) 0.063(3) 0.053(2) 0.008(2) 0.0181(19) 0.002(2) C12 0.074(3) 0.060(3) 0.077(3) 0.011(3) 0.019(3) 0.011(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 S1 C6 1.746(4) . ? S1 C3 1.771(4) . ? S2 C7 1.725(3) . ? S2 C6 1.734(3) . ? S3 C7 1.757(4) . ? S3 C10 1.758(4) . ? O1 C2 1.294(5) . ? O1 H1A 1.19(6) . ? O2 C4 1.273(5) . ? O3 C9 1.289(5) . ? O3 H3A 1.11(5) . ? O4 C11 1.275(5) . ? N1 C6 1.295(4) . ? N1 N2 1.393(4) . ? N2 C7 1.293(4) . ? C1 C2 1.482(6) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.396(6) . ? C3 C4 1.418(6) . ? C4 C5 1.484(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C8 C9 1.479(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.407(6) . ? C10 C11 1.423(6) . ? C11 C12 1.493(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 S1 C3 101.79(16) . . ? C7 S2 C6 85.97(16) . . ? C7 S3 C10 102.29(16) . . ? C2 O1 H1A 104(2) . . ? C9 O3 H3A 103(2) . . ? C6 N1 N2 112.1(3) . . ? C7 N2 N1 111.7(3) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C2 C3 119.9(4) . . ? O1 C2 C1 115.2(4) . . ? C3 C2 C1 124.9(4) . . ? C2 C3 C4 120.9(4) . . ? C2 C3 S1 119.7(3) . . ? C4 C3 S1 119.2(3) . . ? O2 C4 C3 119.7(4) . . ? O2 C4 C5 117.9(4) . . ? C3 C4 C5 122.4(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 S2 114.8(3) . . ? N1 C6 S1 121.9(3) . . ? S2 C6 S1 123.3(2) . . ? N2 C7 S2 115.4(3) . . ? N2 C7 S3 120.9(3) . . ? S2 C7 S3 123.7(2) . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 C10 120.5(4) . . ? O3 C9 C8 115.4(4) . . ? C10 C9 C8 124.0(4) . . ? C9 C10 C11 119.7(4) . . ? C9 C10 S3 120.1(3) . . ? C11 C10 S3 120.0(3) . . ? O4 C11 C10 119.9(4) . . ? O4 C11 C12 117.4(4) . . ? C10 C11 C12 122.7(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 N2 C7 0.4(5) . . . . ? O1 C2 C3 C4 -4.2(6) . . . . ? C1 C2 C3 C4 176.9(4) . . . . ? O1 C2 C3 S1 -179.0(3) . . . . ? C1 C2 C3 S1 2.1(6) . . . . ? C6 S1 C3 C2 -86.2(3) . . . . ? C6 S1 C3 C4 98.9(3) . . . . ? C2 C3 C4 O2 3.6(5) . . . . ? S1 C3 C4 O2 178.5(3) . . . . ? C2 C3 C4 C5 -175.4(4) . . . . ? S1 C3 C4 C5 -0.6(5) . . . . ? N2 N1 C6 S2 0.1(4) . . . . ? N2 N1 C6 S1 -179.9(3) . . . . ? C7 S2 C6 N1 -0.4(3) . . . . ? C7 S2 C6 S1 179.6(3) . . . . ? C3 S1 C6 N1 177.3(3) . . . . ? C3 S1 C6 S2 -2.7(3) . . . . ? N1 N2 C7 S2 -0.7(4) . . . . ? N1 N2 C7 S3 -177.7(3) . . . . ? C6 S2 C7 N2 0.6(3) . . . . ? C6 S2 C7 S3 177.6(3) . . . . ? C10 S3 C7 N2 -174.2(3) . . . . ? C10 S3 C7 S2 9.0(3) . . . . ? O3 C9 C10 C11 0.5(6) . . . . ? C8 C9 C10 C11 -179.7(4) . . . . ? O3 C9 C10 S3 175.1(3) . . . . ? C8 C9 C10 S3 -5.2(5) . . . . ? C7 S3 C10 C9 93.0(3) . . . . ? C7 S3 C10 C11 -92.5(3) . . . . ? C9 C10 C11 O4 -1.8(6) . . . . ? S3 C10 C11 O4 -176.4(3) . . . . ? C9 C10 C11 C12 178.3(4) . . . . ? S3 C10 C11 C12 3.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O2 1.19(6) 1.34(6) 2.460(5) 152(4) . O3 H3A O4 1.11(5) 1.40(5) 2.451(5) 155(4) . _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.322 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.062 #==END