# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_sada _database_code_depnum_ccdc_archive 'CCDC 765718' #TrackingRef '07038.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H27 Mn N4 O5' _chemical_formula_weight 470.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 30.200(18) _cell_length_b 30.200(18) _cell_length_c 10.016(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9135(13) _cell_formula_units_Z 16 _cell_measurement_temperature 202(2) _cell_measurement_reflns_used 6377 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 24.69 _exptl_crystal_description prism _exptl_crystal_colour dark_brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7906 _exptl_absorpt_correction_T_max 0.8367 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 202(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22111 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.82 _reflns_number_total 3905 _reflns_number_gt 2873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+30.9879P] 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 3905 _refine_ls_number_parameters 277 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.481129(18) 0.952505(18) 0.97655(6) 0.0230(2) Uani 1 1 d . . . N1 N 0.49673(10) 0.90796(11) 0.8400(3) 0.0283(8) Uani 1 1 d . . . N2 N 0.53281(11) 0.88027(11) 0.8735(3) 0.0314(8) Uani 1 1 d . . . N3 N 0.65158(11) 0.81435(11) 1.1589(3) 0.0298(8) Uani 1 1 d . . . O1 O 0.35681(10) 1.00299(11) 0.7787(3) 0.0469(8) Uani 1 1 d . . . O2 O 0.43067(9) 0.96898(9) 0.8729(3) 0.0285(6) Uani 1 1 d . . . O3 O 0.53158(8) 0.92401(8) 1.0623(3) 0.0276(6) Uani 1 1 d . . . O4 O 0.47518(8) 0.99671(8) 1.1081(2) 0.0252(6) Uani 1 1 d . . . C1 C 0.31612(18) 1.0205(2) 0.7291(6) 0.0618(16) Uani 1 1 d . . . H1A H 0.3030 1.0401 0.7964 0.093 Uiso 1 1 calc R . . H1B H 0.2957 0.9962 0.7096 0.093 Uiso 1 1 calc R . . H1C H 0.3218 1.0374 0.6473 0.093 Uiso 1 1 calc R . . C2 C 0.37880(14) 0.97405(14) 0.6968(4) 0.0349(10) Uani 1 1 d . . . C3 C 0.36546(15) 0.96275(16) 0.5706(5) 0.0422(11) Uani 1 1 d . . . H3B H 0.3393 0.9755 0.5348 0.051 Uiso 1 1 calc R . . C4 C 0.38990(16) 0.93275(17) 0.4938(5) 0.0475(12) Uani 1 1 d . . . H4A H 0.3804 0.9253 0.4062 0.057 Uiso 1 1 calc R . . C5 C 0.42720(16) 0.91433(16) 0.5446(4) 0.0417(11) Uani 1 1 d . . . H5A H 0.4438 0.8940 0.4923 0.050 Uiso 1 1 calc R . . C6 C 0.44154(13) 0.92514(14) 0.6749(4) 0.0322(10) Uani 1 1 d . . . C7 C 0.41849(13) 0.95611(13) 0.7523(4) 0.0282(9) Uani 1 1 d . . . C8 C 0.47934(14) 0.90202(14) 0.7243(4) 0.0320(9) Uani 1 1 d . . . H8A H 0.4926 0.8806 0.6674 0.038 Uiso 1 1 calc R . . C9 C 0.54725(13) 0.89161(12) 0.9903(4) 0.0261(9) Uani 1 1 d . . . C10 C 0.58437(13) 0.86524(13) 1.0462(4) 0.0279(9) Uani 1 1 d . . . C11 C 0.59140(14) 0.82226(14) 1.0057(4) 0.0335(10) Uani 1 1 d . . . H11A H 0.5735 0.8094 0.9380 0.040 Uiso 1 1 calc R . . C12 C 0.62479(14) 0.79806(14) 1.0648(4) 0.0335(10) Uani 1 1 d . . . H12A H 0.6290 0.7683 1.0372 0.040 Uiso 1 1 calc R . . C13 C 0.64516(14) 0.85649(14) 1.1948(4) 0.0360(10) Uani 1 1 d . . . H13A H 0.6644 0.8689 1.2599 0.043 Uiso 1 1 calc R . . C14 C 0.61225(14) 0.88295(14) 1.1428(4) 0.0341(10) Uani 1 1 d . . . H14A H 0.6087 0.9126 1.1723 0.041 Uiso 1 1 calc R . . C15 C 0.47489(18) 0.98720(16) 1.2458(4) 0.0446(12) Uani 1 1 d . . . H15A H 0.4715 1.0148 1.2963 0.067 Uiso 1 1 calc R . . H15B H 0.5028 0.9729 1.2707 0.067 Uiso 1 1 calc R . . H15C H 0.4502 0.9673 1.2661 0.067 Uiso 1 1 calc R . . N4 N 0.6788(2) 1.0117(2) 0.7291(6) 0.097(2) Uani 1 1 d . . . C16 C 0.6576(2) 0.99243(18) 0.8018(6) 0.0553(14) Uani 1 1 d . . . C17 C 0.63090(19) 0.96817(19) 0.8967(6) 0.0629(15) Uani 1 1 d . . . H17A H 0.6502 0.9533 0.9612 0.094 Uiso 1 1 calc R . . H17B H 0.6131 0.9460 0.8493 0.094 Uiso 1 1 calc R . . H17C H 0.6112 0.9887 0.9437 0.094 Uiso 1 1 calc R . . O5 O 0.5360(2) 0.8677(2) 0.4545(6) 0.1165(18) Uiso 1 1 d DU . . C18 C 0.5584(6) 0.9066(4) 0.457(2) 0.129(5) Uiso 0.50 1 d PDU A 1 H18A H 0.5356 0.9301 0.4622 0.155 Uiso 0.50 1 calc PR A 1 H18B H 0.5723 0.9096 0.3676 0.155 Uiso 0.50 1 calc PR A 1 C19 C 0.5920(6) 0.9181(6) 0.5522(17) 0.114(5) Uiso 0.50 1 d PDU A 1 H19A H 0.5804 0.9138 0.6427 0.171 Uiso 0.50 1 calc PR A 1 H19B H 0.6004 0.9492 0.5403 0.171 Uiso 0.50 1 calc PR A 1 H19C H 0.6180 0.8992 0.5388 0.171 Uiso 0.50 1 calc PR A 1 C20 C 0.5638(6) 0.8323(4) 0.479(2) 0.138(5) Uiso 0.50 1 d PDU A 1 H20A H 0.5646 0.8243 0.5745 0.166 Uiso 0.50 1 calc PR A 1 H20B H 0.5942 0.8378 0.4460 0.166 Uiso 0.50 1 calc PR A 1 C21 C 0.5397(6) 0.7978(6) 0.3953(19) 0.111(5) Uiso 0.50 1 d PDU A 1 H21A H 0.5076 0.8025 0.4021 0.166 Uiso 0.50 1 calc PR A 1 H21B H 0.5470 0.7681 0.4283 0.166 Uiso 0.50 1 calc PR A 1 H21C H 0.5488 0.8005 0.3018 0.166 Uiso 0.50 1 calc PR A 1 C18A C 0.5739(5) 0.8891(5) 0.5086(18) 0.113(5) Uiso 0.50 1 d PDU A 2 H18C H 0.6015 0.8773 0.4684 0.136 Uiso 0.50 1 calc PR A 2 H18D H 0.5753 0.8852 0.6066 0.136 Uiso 0.50 1 calc PR A 2 C19A C 0.5673(7) 0.9361(5) 0.4727(19) 0.115(5) Uiso 0.50 1 d PDU A 2 H19D H 0.5711 0.9398 0.3761 0.172 Uiso 0.50 1 calc PR A 2 H19E H 0.5891 0.9544 0.5197 0.172 Uiso 0.50 1 calc PR A 2 H19F H 0.5374 0.9453 0.4983 0.172 Uiso 0.50 1 calc PR A 2 C20A C 0.5543(7) 0.8285(4) 0.401(2) 0.166(6) Uiso 0.50 1 d PDU A 2 H20C H 0.5868 0.8270 0.4120 0.199 Uiso 0.50 1 calc PR A 2 H20D H 0.5463 0.8240 0.3061 0.199 Uiso 0.50 1 calc PR A 2 C21A C 0.5308(8) 0.7986(7) 0.490(2) 0.142(7) Uiso 0.50 1 d PDU A 2 H21D H 0.5497 0.7913 0.5667 0.213 Uiso 0.50 1 calc PR A 2 H21E H 0.5230 0.7714 0.4424 0.213 Uiso 0.50 1 calc PR A 2 H21F H 0.5037 0.8130 0.5224 0.213 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0223(3) 0.0214(3) 0.0252(3) 0.0004(2) -0.0022(2) 0.0006(2) N1 0.0280(18) 0.0264(18) 0.0304(19) -0.0006(15) -0.0018(15) 0.0035(14) N2 0.0294(19) 0.0304(19) 0.035(2) -0.0015(15) -0.0060(15) 0.0091(15) N3 0.0279(18) 0.0270(18) 0.035(2) 0.0003(15) -0.0033(15) 0.0055(14) O1 0.0344(17) 0.060(2) 0.0467(19) -0.0080(16) -0.0109(15) 0.0196(15) O2 0.0274(15) 0.0318(15) 0.0262(15) 0.0001(12) -0.0060(12) 0.0036(12) O3 0.0259(14) 0.0248(14) 0.0321(15) 0.0010(12) -0.0023(12) 0.0030(11) O4 0.0277(15) 0.0235(14) 0.0244(14) 0.0007(11) 0.0017(11) -0.0005(11) C1 0.049(3) 0.073(4) 0.064(4) -0.007(3) -0.019(3) 0.030(3) C2 0.030(2) 0.039(2) 0.036(3) 0.002(2) -0.0047(19) 0.0020(19) C3 0.036(3) 0.050(3) 0.041(3) 0.003(2) -0.014(2) 0.004(2) C4 0.048(3) 0.059(3) 0.035(3) -0.004(2) -0.016(2) -0.002(2) C5 0.043(3) 0.050(3) 0.032(2) -0.005(2) -0.007(2) 0.004(2) C6 0.031(2) 0.035(2) 0.031(2) -0.0028(19) -0.0066(18) 0.0010(18) C7 0.024(2) 0.032(2) 0.028(2) 0.0041(18) -0.0041(17) -0.0023(17) C8 0.034(2) 0.030(2) 0.032(2) -0.0075(18) -0.0036(19) 0.0038(17) C9 0.023(2) 0.022(2) 0.033(2) 0.0023(17) -0.0012(17) 0.0005(16) C10 0.025(2) 0.031(2) 0.028(2) 0.0020(17) -0.0005(17) 0.0015(16) C11 0.035(2) 0.030(2) 0.036(2) -0.0033(18) -0.0084(19) 0.0038(18) C12 0.034(2) 0.027(2) 0.040(2) -0.0028(19) -0.0060(19) 0.0062(18) C13 0.033(2) 0.036(2) 0.039(3) -0.004(2) -0.010(2) 0.0018(19) C14 0.037(2) 0.025(2) 0.041(3) -0.0016(19) -0.006(2) 0.0066(18) C15 0.064(3) 0.040(3) 0.030(3) 0.000(2) 0.005(2) -0.010(2) N4 0.116(5) 0.098(5) 0.075(4) 0.033(4) -0.019(4) -0.033(4) C16 0.065(4) 0.047(3) 0.054(3) 0.007(3) -0.018(3) -0.004(3) C17 0.058(3) 0.064(4) 0.067(4) 0.006(3) 0.007(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 1.885(3) . ? Mn1 O2 1.910(3) . ? Mn1 O3 1.949(3) . ? Mn1 N1 1.976(4) . ? Mn1 O4 2.194(3) 9_677 ? Mn1 N3 2.360(3) 12_768 ? Mn1 Mn1 3.122(2) 9_677 ? N1 C8 1.285(5) . ? N1 N2 1.414(4) . ? N2 C9 1.294(5) . ? N3 C12 1.336(5) . ? N3 C13 1.336(5) . ? N3 Mn1 2.360(3) 15_567 ? O1 C2 1.371(5) . ? O1 C1 1.428(5) . ? O2 C7 1.321(5) . ? O3 C9 1.305(5) . ? O4 C15 1.408(5) . ? O4 Mn1 2.194(3) 9_677 ? C2 C3 1.370(6) . ? C2 C7 1.428(6) . ? C3 C4 1.399(7) . ? C4 C5 1.355(7) . ? C5 C6 1.414(6) . ? C6 C7 1.400(6) . ? C6 C8 1.426(6) . ? C9 C10 1.485(5) . ? C10 C11 1.376(6) . ? C10 C14 1.390(6) . ? C11 C12 1.379(6) . ? C13 C14 1.378(6) . ? N4 C16 1.131(7) . ? C16 C17 1.446(8) . ? O5 C18 1.354(9) . ? O5 C20 1.380(9) . ? O5 C20A 1.412(9) . ? O5 C18A 1.421(9) . ? C18 C19 1.438(10) . ? C20 C21 1.521(10) . ? C18A C19A 1.479(10) . ? C20A C21A 1.457(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O2 96.86(12) . . ? O4 Mn1 O3 94.53(12) . . ? O2 Mn1 O3 168.02(11) . . ? O4 Mn1 N1 171.63(12) . . ? O2 Mn1 N1 89.50(14) . . ? O3 Mn1 N1 79.53(13) . . ? O4 Mn1 O4 80.36(12) . 9_677 ? O2 Mn1 O4 95.03(11) . 9_677 ? O3 Mn1 O4 90.51(11) . 9_677 ? N1 Mn1 O4 93.71(13) . 9_677 ? O4 Mn1 N3 93.79(13) . 12_768 ? O2 Mn1 N3 88.27(13) . 12_768 ? O3 Mn1 N3 87.30(12) . 12_768 ? N1 Mn1 N3 91.82(14) . 12_768 ? O4 Mn1 N3 173.58(11) 9_677 12_768 ? O4 Mn1 Mn1 43.84(8) . 9_677 ? O2 Mn1 Mn1 97.68(8) . 9_677 ? O3 Mn1 Mn1 93.09(8) . 9_677 ? N1 Mn1 Mn1 129.99(10) . 9_677 ? O4 Mn1 Mn1 36.52(7) 9_677 9_677 ? N3 Mn1 Mn1 137.57(10) 12_768 9_677 ? C8 N1 N2 116.5(3) . . ? C8 N1 Mn1 128.5(3) . . ? N2 N1 Mn1 114.9(2) . . ? C9 N2 N1 108.5(3) . . ? C12 N3 C13 116.9(3) . . ? C12 N3 Mn1 121.6(3) . 15_567 ? C13 N3 Mn1 121.2(3) . 15_567 ? C2 O1 C1 116.5(4) . . ? C7 O2 Mn1 130.0(2) . . ? C9 O3 Mn1 111.8(2) . . ? C15 O4 Mn1 122.7(3) . . ? C15 O4 Mn1 121.7(3) . 9_677 ? Mn1 O4 Mn1 99.64(12) . 9_677 ? C3 C2 O1 124.7(4) . . ? C3 C2 C7 120.8(4) . . ? O1 C2 C7 114.6(4) . . ? C2 C3 C4 120.9(4) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 C6 120.4(4) . . ? C7 C6 C5 120.9(4) . . ? C7 C6 C8 122.2(4) . . ? C5 C6 C8 116.9(4) . . ? O2 C7 C6 124.3(4) . . ? O2 C7 C2 118.6(4) . . ? C6 C7 C2 117.1(4) . . ? N1 C8 C6 124.8(4) . . ? N2 C9 O3 125.2(4) . . ? N2 C9 C10 116.9(3) . . ? O3 C9 C10 117.9(3) . . ? C11 C10 C14 118.3(4) . . ? C11 C10 C9 120.7(4) . . ? C14 C10 C9 120.9(4) . . ? C10 C11 C12 119.1(4) . . ? N3 C12 C11 123.4(4) . . ? N3 C13 C14 123.7(4) . . ? C13 C14 C10 118.5(4) . . ? N4 C16 C17 179.0(7) . . ? C18 O5 C20 111.5(9) . . ? C18 O5 C20A 122.5(13) . . ? C20 O5 C20A 34.9(11) . . ? C18 O5 C18A 36.8(8) . . ? C20 O5 C18A 78.2(9) . . ? C20A O5 C18A 102.1(8) . . ? O5 C18 C19 124.9(14) . . ? O5 C20 C21 98.3(12) . . ? O5 C18A C19A 103.5(12) . . ? O5 C20A C21A 95.5(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.82 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.600 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.077 data_sada _database_code_depnum_ccdc_archive 'CCDC 765719' #TrackingRef '07031.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Cl2 Mn N6 O8' _chemical_formula_weight 732.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.8865(15) _cell_length_b 8.9804(15) _cell_length_c 12.543(2) _cell_angle_alpha 69.358(2) _cell_angle_beta 76.853(2) _cell_angle_gamma 77.743(2) _cell_volume 801.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 202(2) _cell_measurement_reflns_used 3581 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 26.35 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 379 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8828 _exptl_absorpt_correction_T_max 0.9388 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 202(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5172 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3181 _reflns_number_gt 2550 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.3577P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3181 _refine_ls_number_parameters 219 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 1.0000 0.5000 0.5000 0.02573(15) Uani 1 2 d S . . Cl1 Cl 0.82829(9) 0.75445(7) 0.39133(5) 0.03472(17) Uani 1 1 d . . . O3 O 0.8614(3) 0.3127(2) 0.01886(15) 0.0419(5) Uani 1 1 d . . . O2 O 0.7452(2) 0.12728(19) -0.15733(14) 0.0339(4) Uani 1 1 d . . . H2B H 0.7702 0.1360 -0.0983 0.041 Uiso 1 1 d R . . O1 O 0.6652(3) 0.0656(2) -0.32507(15) 0.0396(5) Uani 1 1 d . . . O4 O 0.7616(3) 0.3961(2) 0.61625(17) 0.0396(4) Uani 1 1 d D . . H4O H 0.774(4) 0.3037(18) 0.663(2) 0.047 Uiso 1 1 d D . . N3 N 0.9815(3) 0.3831(2) 0.36979(18) 0.0305(5) Uani 1 1 d . . . N2 N 0.8327(3) 0.0642(2) 0.14259(17) 0.0294(5) Uani 1 1 d . . . H2A H 0.8382 -0.0069 0.2116 0.035 Uiso 1 1 d R . . N1 N 0.7883(3) 0.0291(2) 0.05569(17) 0.0280(4) Uani 1 1 d . . . C13 C 0.9893(4) 0.4712(3) 0.2583(2) 0.0330(6) Uani 1 1 d . . . H13 H 1.0197 0.5763 0.2344 0.040 Uiso 1 1 calc R . . C14 C 0.9553(4) 0.4168(3) 0.1764(2) 0.0331(6) Uani 1 1 d . . . H14 H 0.9624 0.4839 0.0981 0.040 Uiso 1 1 calc R . . C10 C 0.9105(3) 0.2637(3) 0.2088(2) 0.0264(5) Uani 1 1 d . . . C11 C 0.9072(4) 0.1691(3) 0.3237(2) 0.0320(6) Uani 1 1 d . . . H11 H 0.8813 0.0623 0.3492 0.038 Uiso 1 1 calc R . . C12 C 0.9425(4) 0.2335(3) 0.4002(2) 0.0333(6) Uani 1 1 d . . . H12 H 0.9388 0.1682 0.4788 0.040 Uiso 1 1 calc R . . C9 C 0.8673(3) 0.2166(3) 0.1152(2) 0.0286(5) Uani 1 1 d . . . C8 C 0.7406(3) -0.1063(3) 0.0743(2) 0.0296(5) Uani 1 1 d . . . H8 H 0.7346 -0.1849 0.1488 0.036 Uiso 1 1 calc R . . C6 C 0.6957(3) -0.1371(3) -0.0218(2) 0.0271(5) Uani 1 1 d . . . C5 C 0.6469(4) -0.2864(3) -0.0053(2) 0.0350(6) Uani 1 1 d . . . H5 H 0.6412 -0.3654 0.0690 0.042 Uiso 1 1 calc R . . C4 C 0.6076(4) -0.3197(3) -0.0947(2) 0.0389(6) Uani 1 1 d . . . H4 H 0.5779 -0.4223 -0.0823 0.047 Uiso 1 1 calc R . . C3 C 0.6109(4) -0.2043(3) -0.2036(2) 0.0346(6) Uani 1 1 d . . . H3 H 0.5821 -0.2275 -0.2651 0.042 Uiso 1 1 calc R . . C2 C 0.6561(3) -0.0564(3) -0.2217(2) 0.0291(5) Uani 1 1 d . . . C7 C 0.6996(3) -0.0209(3) -0.1315(2) 0.0266(5) Uani 1 1 d . . . C1 C 0.6047(4) 0.0404(4) -0.4153(2) 0.0424(7) Uani 1 1 d . . . H1A H 0.6101 0.1369 -0.4835 0.064 Uiso 1 1 calc R . . H1B H 0.4830 0.0183 -0.3894 0.064 Uiso 1 1 calc R . . H1C H 0.6796 -0.0514 -0.4351 0.064 Uiso 1 1 calc R . . C15 C 0.5884(5) 0.4698(4) 0.6429(3) 0.0612(9) Uani 1 1 d . . . H15A H 0.5674 0.4727 0.7223 0.092 Uiso 1 1 calc R . . H15B H 0.5052 0.4083 0.6357 0.092 Uiso 1 1 calc R . . H15C H 0.5720 0.5798 0.5894 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0377(3) 0.0188(3) 0.0230(3) -0.0067(2) -0.0085(2) -0.0051(2) Cl1 0.0479(4) 0.0229(3) 0.0323(3) -0.0060(2) -0.0136(3) -0.0004(3) O3 0.0697(14) 0.0315(10) 0.0281(10) -0.0015(8) -0.0180(9) -0.0185(9) O2 0.0535(12) 0.0260(9) 0.0266(9) -0.0055(7) -0.0121(8) -0.0140(8) O1 0.0590(12) 0.0356(10) 0.0276(9) -0.0070(8) -0.0168(9) -0.0093(9) O4 0.0426(11) 0.0257(9) 0.0430(11) -0.0032(8) -0.0020(9) -0.0084(8) N3 0.0441(13) 0.0214(10) 0.0284(11) -0.0082(8) -0.0085(9) -0.0066(9) N2 0.0432(13) 0.0266(10) 0.0212(10) -0.0061(8) -0.0118(9) -0.0066(9) N1 0.0346(11) 0.0297(11) 0.0238(10) -0.0095(8) -0.0091(9) -0.0067(9) C13 0.0480(16) 0.0227(12) 0.0304(13) -0.0077(10) -0.0061(11) -0.0113(11) C14 0.0490(16) 0.0282(13) 0.0217(12) -0.0051(10) -0.0062(11) -0.0093(11) C10 0.0318(13) 0.0242(12) 0.0255(12) -0.0099(9) -0.0052(10) -0.0045(10) C11 0.0483(16) 0.0235(12) 0.0271(12) -0.0059(10) -0.0111(11) -0.0099(11) C12 0.0517(16) 0.0257(12) 0.0233(12) -0.0037(10) -0.0109(11) -0.0098(11) C9 0.0341(13) 0.0285(12) 0.0241(12) -0.0078(10) -0.0074(10) -0.0048(10) C8 0.0393(14) 0.0258(12) 0.0237(12) -0.0060(10) -0.0055(10) -0.0080(10) C6 0.0295(13) 0.0271(12) 0.0266(12) -0.0100(10) -0.0047(10) -0.0054(10) C5 0.0472(16) 0.0289(13) 0.0294(13) -0.0051(10) -0.0057(12) -0.0147(12) C4 0.0525(17) 0.0315(14) 0.0389(15) -0.0129(11) -0.0055(13) -0.0187(13) C3 0.0409(15) 0.0392(14) 0.0318(13) -0.0176(11) -0.0077(11) -0.0102(12) C2 0.0329(14) 0.0304(13) 0.0253(12) -0.0094(10) -0.0060(10) -0.0051(10) C7 0.0288(13) 0.0267(12) 0.0265(12) -0.0102(10) -0.0045(10) -0.0058(10) C1 0.0472(17) 0.0555(18) 0.0284(14) -0.0160(13) -0.0143(12) -0.0026(14) C15 0.053(2) 0.0478(19) 0.066(2) -0.0083(16) -0.0001(17) 0.0002(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 2.2519(19) 2_766 ? Mn1 O4 2.2520(19) . ? Mn1 N3 2.274(2) 2_766 ? Mn1 N3 2.275(2) . ? Mn1 Cl1 2.4986(6) 2_766 ? Mn1 Cl1 2.4986(6) . ? O3 C9 1.216(3) . ? O2 C7 1.361(3) . ? O2 H2B 0.8399 . ? O1 C2 1.369(3) . ? O1 C1 1.425(3) . ? O4 C15 1.407(4) . ? O4 H4O 0.831(10) . ? N3 C13 1.337(3) . ? N3 C12 1.344(3) . ? N2 C9 1.360(3) . ? N2 N1 1.368(3) . ? N2 H2A 0.8800 . ? N1 C8 1.276(3) . ? C13 C14 1.379(3) . ? C13 H13 0.9500 . ? C14 C10 1.389(3) . ? C14 H14 0.9500 . ? C10 C11 1.389(3) . ? C10 C9 1.505(3) . ? C11 C12 1.384(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C8 C6 1.458(3) . ? C8 H8 0.9500 . ? C6 C7 1.402(3) . ? C6 C5 1.405(3) . ? C5 C4 1.370(4) . ? C5 H5 0.9500 . ? C4 C3 1.392(4) . ? C4 H4 0.9500 . ? C3 C2 1.376(4) . ? C3 H3 0.9500 . ? C2 C7 1.406(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O4 180.00(6) 2_766 . ? O4 Mn1 N3 90.36(8) 2_766 2_766 ? O4 Mn1 N3 89.64(8) . 2_766 ? O4 Mn1 N3 89.64(8) 2_766 . ? O4 Mn1 N3 90.36(8) . . ? N3 Mn1 N3 179.999(1) 2_766 . ? O4 Mn1 Cl1 94.70(5) 2_766 2_766 ? O4 Mn1 Cl1 85.30(5) . 2_766 ? N3 Mn1 Cl1 90.08(5) 2_766 2_766 ? N3 Mn1 Cl1 89.92(5) . 2_766 ? O4 Mn1 Cl1 85.30(5) 2_766 . ? O4 Mn1 Cl1 94.70(5) . . ? N3 Mn1 Cl1 89.92(5) 2_766 . ? N3 Mn1 Cl1 90.08(5) . . ? Cl1 Mn1 Cl1 180.0 2_766 . ? C7 O2 H2B 109.5 . . ? C2 O1 C1 116.1(2) . . ? C15 O4 Mn1 130.99(18) . . ? C15 O4 H4O 108(2) . . ? Mn1 O4 H4O 120(2) . . ? C13 N3 C12 116.9(2) . . ? C13 N3 Mn1 119.39(16) . . ? C12 N3 Mn1 123.24(16) . . ? C9 N2 N1 115.45(19) . . ? C9 N2 H2A 122.2 . . ? N1 N2 H2A 122.3 . . ? C8 N1 N2 120.7(2) . . ? N3 C13 C14 123.2(2) . . ? N3 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C10 119.7(2) . . ? C13 C14 H14 120.1 . . ? C10 C14 H14 120.1 . . ? C14 C10 C11 117.7(2) . . ? C14 C10 C9 116.3(2) . . ? C11 C10 C9 126.0(2) . . ? C12 C11 C10 118.8(2) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? N3 C12 C11 123.7(2) . . ? N3 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? O3 C9 N2 121.4(2) . . ? O3 C9 C10 120.9(2) . . ? N2 C9 C10 117.7(2) . . ? N1 C8 C6 118.2(2) . . ? N1 C8 H8 120.9 . . ? C6 C8 H8 120.9 . . ? C7 C6 C5 118.5(2) . . ? C7 C6 C8 121.6(2) . . ? C5 C6 C8 119.8(2) . . ? C4 C5 C6 121.0(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C4 C3 120.5(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? O1 C2 C3 124.8(2) . . ? O1 C2 C7 114.5(2) . . ? C3 C2 C7 120.7(2) . . ? O2 C7 C6 123.5(2) . . ? O2 C7 C2 116.9(2) . . ? C6 C7 C2 119.6(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O4 C15 H15A 109.5 . . ? O4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 N2 H2A Cl1 0.88 2.50 3.368(2) 167.7 1_545 O2 H2B N1 0.84 1.85 2.580(3) 143.9 . _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.337 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.060 data_08194_pl2149 _database_code_depnum_ccdc_archive 'CCDC 765720' #TrackingRef '08194_PL2149.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H40 Cl2 Mn3 N6 O11' _chemical_formula_weight 932.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.0173(18) _cell_length_b 10.2552(18) _cell_length_c 11.2365(13) _cell_angle_alpha 114.964(11) _cell_angle_beta 108.935(11) _cell_angle_gamma 98.289(2) _cell_volume 935.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4035 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 26.35 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 477 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6437 _exptl_absorpt_correction_T_max 0.7942 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8871 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.1035 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3372 _reflns_number_gt 2154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3372 _refine_ls_number_parameters 253 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.0000 0.5000 0.0217(3) Uani 1 2 d S . . Mn2 Mn 0.28087(10) 0.18736(9) 0.63208(9) 0.0249(3) Uani 1 1 d . . . Cl1 Cl 0.56948(16) 0.21371(14) 0.75759(14) 0.0272(4) Uani 1 1 d . . . N3 N 0.5612(5) 0.1778(5) 0.4318(5) 0.0245(11) Uani 1 1 d . . . N2 N 0.6504(6) 0.4897(5) 0.1974(5) 0.0310(12) Uani 1 1 d . . . N1 N 0.6859(5) 0.6243(5) 0.1925(5) 0.0268(12) Uani 1 1 d . . . O3 O 0.6802(4) 0.6643(4) 0.4248(4) 0.0277(9) Uani 1 1 d . . . O2 O 0.7761(4) 0.9325(4) 0.2904(4) 0.0296(10) Uani 1 1 d . . . O1 O 0.8588(5) 1.1476(4) 0.2383(5) 0.0466(12) Uani 1 1 d . . . O4 O 0.2806(4) 0.0266(4) 0.4673(4) 0.0222(9) Uani 1 1 d . . . O5 O 0.0322(4) 0.1672(4) 0.5345(4) 0.0382(11) Uani 1 1 d . . . H5A H -0.0370 0.0697 0.4590 0.046 Uiso 1 1 calc R . . C12 C 0.5485(7) 0.1444(6) 0.2986(7) 0.0346(16) Uani 1 1 d . . . H12 H 0.5169 0.0400 0.2273 0.041 Uiso 1 1 calc R . . C11 C 0.5778(7) 0.2496(6) 0.2582(7) 0.0344(15) Uani 1 1 d . . . H11 H 0.5656 0.2180 0.1617 0.041 Uiso 1 1 calc R . . C10 C 0.6256(6) 0.4036(6) 0.3600(6) 0.0284(14) Uani 1 1 d . . . C14 C 0.6444(7) 0.4409(6) 0.4991(6) 0.0322(15) Uani 1 1 d . . . H14 H 0.6788 0.5444 0.5734 0.039 Uiso 1 1 calc R . . C13 C 0.6128(7) 0.3262(6) 0.5279(7) 0.0325(15) Uani 1 1 d . . . H13 H 0.6290 0.3550 0.6249 0.039 Uiso 1 1 calc R . . C9 C 0.6527(6) 0.5249(6) 0.3235(6) 0.0246(13) Uani 1 1 d . . . C8 C 0.6901(6) 0.6106(6) 0.0742(6) 0.0304(14) Uani 1 1 d . . . H8 H 0.6642 0.5108 -0.0040 0.036 Uiso 1 1 calc R . . C6 C 0.7314(7) 0.7367(6) 0.0533(6) 0.0312(15) Uani 1 1 d . . . C5 C 0.7364(8) 0.7002(7) -0.0828(7) 0.0431(17) Uani 1 1 d . . . H5 H 0.7101 0.5970 -0.1548 0.052 Uiso 1 1 calc R . . C4 C 0.7787(8) 0.8128(8) -0.1082(7) 0.0494(19) Uani 1 1 d . . . H4 H 0.7823 0.7883 -0.1984 0.059 Uiso 1 1 calc R . . C3 C 0.8170(8) 0.9639(8) -0.0048(7) 0.0466(18) Uani 1 1 d . . . H3 H 0.8443 1.0418 -0.0254 0.056 Uiso 1 1 calc R . . C2 C 0.8156(7) 1.0016(7) 0.1269(7) 0.0366(16) Uani 1 1 d . . . C7 C 0.7708(6) 0.8865(6) 0.1580(6) 0.0290(14) Uani 1 1 d . . . C1 C 0.8983(10) 1.2686(8) 0.2109(9) 0.067(2) Uani 1 1 d . . . H1C H 0.9266 1.3667 0.2984 0.101 Uiso 1 1 calc R . . H1A H 0.8127 1.2592 0.1306 0.101 Uiso 1 1 calc R . . H1B H 0.9826 1.2628 0.1851 0.101 Uiso 1 1 calc R . . C15 C 0.1765(7) -0.0110(7) 0.3260(6) 0.0372(16) Uani 1 1 d . . . H15A H 0.0806 -0.0812 0.2991 0.056 Uiso 1 1 calc R . . H15B H 0.2154 -0.0595 0.2549 0.056 Uiso 1 1 calc R . . H15C H 0.1622 0.0821 0.3273 0.056 Uiso 1 1 calc R . . C16 C -0.0248(8) 0.2895(8) 0.5788(8) 0.060(2) Uani 1 1 d . . . H16A H -0.1317 0.2491 0.5506 0.089 Uiso 1 1 calc R . . H16B H -0.0099 0.3483 0.5317 0.089 Uiso 1 1 calc R . . H16C H 0.0280 0.3555 0.6846 0.089 Uiso 1 1 calc R . . O6 O 0.972(2) 0.478(3) -0.0544(19) 0.161(8) Uiso 0.50 1 d PD A -1 H6 H 1.0266 0.5694 -0.0019 0.241 Uiso 0.50 1 calc PR A -1 C17 C 0.919(3) 0.428(3) 0.031(3) 0.143(10) Uiso 0.50 1 d PD A -1 H17A H 0.9886 0.4928 0.1345 0.214 Uiso 0.50 1 calc PR A -1 H17B H 0.9143 0.3221 0.0003 0.214 Uiso 0.50 1 calc PR A -1 H17C H 0.8199 0.4368 0.0170 0.214 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0300(7) 0.0135(6) 0.0270(7) 0.0101(5) 0.0171(6) 0.0101(5) Mn2 0.0353(6) 0.0154(4) 0.0302(5) 0.0124(4) 0.0193(4) 0.0094(4) Cl1 0.0368(9) 0.0159(7) 0.0274(8) 0.0080(6) 0.0166(7) 0.0073(6) N3 0.025(3) 0.020(2) 0.032(3) 0.014(2) 0.015(2) 0.008(2) N2 0.042(3) 0.017(2) 0.037(3) 0.016(2) 0.017(2) 0.009(2) N1 0.035(3) 0.018(2) 0.034(3) 0.014(2) 0.020(2) 0.009(2) O3 0.037(2) 0.0174(19) 0.034(2) 0.0153(18) 0.0187(19) 0.0090(17) O2 0.043(3) 0.021(2) 0.033(2) 0.0146(18) 0.023(2) 0.0115(18) O1 0.072(3) 0.024(2) 0.058(3) 0.024(2) 0.038(3) 0.018(2) O4 0.026(2) 0.0185(19) 0.022(2) 0.0101(16) 0.0101(17) 0.0088(16) O5 0.034(2) 0.026(2) 0.048(3) 0.014(2) 0.016(2) 0.0098(19) C12 0.046(4) 0.015(3) 0.039(4) 0.006(3) 0.024(3) 0.007(3) C11 0.047(4) 0.025(3) 0.034(3) 0.012(3) 0.024(3) 0.011(3) C10 0.030(3) 0.023(3) 0.039(4) 0.016(3) 0.020(3) 0.012(3) C14 0.043(4) 0.018(3) 0.035(3) 0.012(3) 0.019(3) 0.008(3) C13 0.039(4) 0.027(3) 0.038(4) 0.016(3) 0.023(3) 0.013(3) C9 0.025(3) 0.018(3) 0.033(3) 0.010(3) 0.016(3) 0.011(2) C8 0.034(4) 0.026(3) 0.031(3) 0.012(3) 0.017(3) 0.009(3) C6 0.033(4) 0.030(3) 0.033(3) 0.018(3) 0.015(3) 0.008(3) C5 0.058(5) 0.038(4) 0.036(4) 0.018(3) 0.025(3) 0.011(3) C4 0.065(5) 0.052(4) 0.037(4) 0.024(4) 0.028(4) 0.017(4) C3 0.057(5) 0.046(4) 0.051(4) 0.034(4) 0.029(4) 0.012(4) C2 0.038(4) 0.035(4) 0.043(4) 0.024(3) 0.019(3) 0.011(3) C7 0.027(3) 0.030(3) 0.032(3) 0.015(3) 0.015(3) 0.010(3) C1 0.097(7) 0.039(4) 0.102(7) 0.048(5) 0.066(6) 0.025(4) C15 0.044(4) 0.033(3) 0.036(4) 0.016(3) 0.019(3) 0.016(3) C16 0.039(4) 0.039(4) 0.077(6) 0.015(4) 0.015(4) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 2.185(4) . ? Mn1 O4 2.185(4) 2_656 ? Mn1 N3 2.334(4) . ? Mn1 N3 2.334(4) 2_656 ? Mn1 Cl1 2.5619(14) . ? Mn1 Cl1 2.5620(14) 2_656 ? Mn2 O4 1.888(4) . ? Mn2 O2 1.903(4) 2_666 ? Mn2 O3 1.920(4) 2_666 ? Mn2 N1 1.975(4) 2_666 ? Mn2 O5 2.310(4) . ? Mn2 Cl1 2.6884(18) . ? N3 C13 1.332(7) . ? N3 C12 1.343(7) . ? N2 C9 1.297(7) . ? N2 N1 1.404(6) . ? N1 C8 1.293(7) . ? N1 Mn2 1.975(4) 2_666 ? O3 C9 1.313(6) . ? O3 Mn2 1.920(4) 2_666 ? O2 C7 1.337(7) . ? O2 Mn2 1.903(4) 2_666 ? O1 C2 1.369(7) . ? O1 C1 1.432(7) . ? O4 C15 1.432(7) . ? O5 C16 1.417(8) . ? O5 H5A 0.9500 . ? C12 C11 1.366(8) . ? C12 H12 0.9500 . ? C11 C10 1.390(8) . ? C11 H11 0.9500 . ? C10 C14 1.381(8) . ? C10 C9 1.482(7) . ? C14 C13 1.367(8) . ? C14 H14 0.9500 . ? C13 H13 0.9500 . ? C8 C6 1.436(8) . ? C8 H8 0.9500 . ? C6 C7 1.378(8) . ? C6 C5 1.434(8) . ? C5 C4 1.345(9) . ? C5 H5 0.9500 . ? C4 C3 1.385(9) . ? C4 H4 0.9500 . ? C3 C2 1.368(9) . ? C3 H3 0.9500 . ? C2 C7 1.420(8) . ? C1 H1C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O6 C17 1.460(10) . ? O6 H6 0.8400 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O4 180.0 . 2_656 ? O4 Mn1 N3 91.33(14) . . ? O4 Mn1 N3 88.67(14) 2_656 . ? O4 Mn1 N3 88.67(14) . 2_656 ? O4 Mn1 N3 91.33(14) 2_656 2_656 ? N3 Mn1 N3 180.00(18) . 2_656 ? O4 Mn1 Cl1 81.51(10) . . ? O4 Mn1 Cl1 98.49(10) 2_656 . ? N3 Mn1 Cl1 90.90(11) . . ? N3 Mn1 Cl1 89.10(11) 2_656 . ? O4 Mn1 Cl1 98.49(10) . 2_656 ? O4 Mn1 Cl1 81.51(10) 2_656 2_656 ? N3 Mn1 Cl1 89.10(11) . 2_656 ? N3 Mn1 Cl1 90.90(11) 2_656 2_656 ? Cl1 Mn1 Cl1 180.0 . 2_656 ? O4 Mn2 O2 96.66(15) . 2_666 ? O4 Mn2 O3 94.04(16) . 2_666 ? O2 Mn2 O3 168.11(17) 2_666 2_666 ? O4 Mn2 N1 169.94(17) . 2_666 ? O2 Mn2 N1 90.71(17) 2_666 2_666 ? O3 Mn2 N1 79.34(17) 2_666 2_666 ? O4 Mn2 O5 98.39(15) . . ? O2 Mn2 O5 86.47(16) 2_666 . ? O3 Mn2 O5 86.84(16) 2_666 . ? N1 Mn2 O5 88.86(17) 2_666 . ? O4 Mn2 Cl1 83.74(12) . . ? O2 Mn2 Cl1 91.61(13) 2_666 . ? O3 Mn2 Cl1 94.72(12) 2_666 . ? N1 Mn2 Cl1 89.23(15) 2_666 . ? O5 Mn2 Cl1 177.28(11) . . ? Mn1 Cl1 Mn2 81.00(4) . . ? C13 N3 C12 114.3(5) . . ? C13 N3 Mn1 120.3(4) . . ? C12 N3 Mn1 125.4(3) . . ? C9 N2 N1 108.4(4) . . ? C8 N1 N2 116.8(5) . . ? C8 N1 Mn2 127.8(4) . 2_666 ? N2 N1 Mn2 115.3(3) . 2_666 ? C9 O3 Mn2 112.9(3) . 2_666 ? C7 O2 Mn2 128.8(3) . 2_666 ? C2 O1 C1 117.4(5) . . ? C15 O4 Mn2 118.6(3) . . ? C15 O4 Mn1 119.8(3) . . ? Mn2 O4 Mn1 113.56(16) . . ? C16 O5 Mn2 124.9(4) . . ? C16 O5 H5A 117.6 . . ? Mn2 O5 H5A 117.6 . . ? N3 C12 C11 124.8(5) . . ? N3 C12 H12 117.6 . . ? C11 C12 H12 117.6 . . ? C12 C11 C10 119.2(5) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C14 C10 C11 117.0(5) . . ? C14 C10 C9 120.2(5) . . ? C11 C10 C9 122.7(5) . . ? C13 C14 C10 118.9(5) . . ? C13 C14 H14 120.6 . . ? C10 C14 H14 120.6 . . ? N3 C13 C14 125.7(6) . . ? N3 C13 H13 117.2 . . ? C14 C13 H13 117.2 . . ? N2 C9 O3 124.0(5) . . ? N2 C9 C10 119.5(5) . . ? O3 C9 C10 116.5(5) . . ? N1 C8 C6 124.1(5) . . ? N1 C8 H8 117.9 . . ? C6 C8 H8 117.9 . . ? C7 C6 C5 120.1(5) . . ? C7 C6 C8 123.5(5) . . ? C5 C6 C8 116.4(5) . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C4 C3 120.9(6) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C2 C3 C4 120.4(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C2 O1 124.6(6) . . ? C3 C2 C7 120.5(6) . . ? O1 C2 C7 114.9(5) . . ? O2 C7 C6 124.7(5) . . ? O2 C7 C2 117.0(5) . . ? C6 C7 C2 118.3(5) . . ? O1 C1 H1C 109.5 . . ? O1 C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O4 C15 H15A 109.5 . . ? O4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 H16A 109.5 . . ? O5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 O6 H6 109.5 . . ? O6 C17 H17A 109.5 . . ? O6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? 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 O5 H5A O2 0.95 1.94 2.824(5) 154.0 1_445 O5 H5A O5 0.95 2.47 3.094(8) 123.4 2_556 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.774 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.115