Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;One-dimensional coordination polymers of antiferromagnetically-coupled [Mn4] Single-Molecule Magnets ; _publ_contact_author_name 'Olivier Roubeau' _publ_contact_author_email ROUBEAU@CRPP-BORDEAUX.CNRS.FR loop_ _publ_author_name 'Olivier Roubeau' 'Rodolphe Clerac' 'Claude Coulon' 'X.F.Le Goff' 'Lollita Lecren' ; Yang-Guang Li ; 'Hitoshi Miyasaka' 'Florent Richard' 'Wolfgang Wernsdorfer' # Attachment 'Dalton4-AC3B.CIF' data_ac3b _database_code_depnum_ccdc_archive 'CCDC 223056' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common catena-(Mn4(hmp)6(OOCCH3)2(ClO4)2)H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H84 Cl4 Mn8 N12 O38' _chemical_formula_weight 2402.91 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.958(2) _cell_length_b 12.333(3) _cell_length_c 19.546(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.30(3) _cell_angle_gamma 90.00 _cell_volume 2354.0(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details MULABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10542 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3356 _reflns_number_gt 2455 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Non hydrogens were refined anisotropically. The perchlorate oxygens were refined with displacment parameters restrains. All hydrogens were fixed at calculated positions on their riding atom except those of the water molecule that could not be found nor fixed and are therefore omitted from the structural model. ; _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^)+(0.0438P)^2^+5.8261P] 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 3356 _refine_ls_number_parameters 361 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.039 _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 Mn2 Mn 0.50406(8) 0.87626(7) 0.02583(4) 0.0248(2) Uani 1 1 d . . . Mn1 Mn 0.20431(8) 1.00661(7) -0.01161(4) 0.0246(2) Uani 1 1 d . . . N1 N 0.2029(4) 1.1514(4) 0.0568(2) 0.0311(11) Uani 1 1 d . . . N2 N 0.5091(5) 0.7150(4) -0.0228(3) 0.0346(12) Uani 1 1 d . . . N3 N 0.4818(4) 0.8046(4) 0.1192(2) 0.0306(11) Uani 1 1 d . . . O1 O 0.4277(3) 1.0357(3) 0.04745(17) 0.0251(8) Uani 1 1 d . . . O2 O 0.3222(3) 0.8624(3) -0.02315(18) 0.0274(8) Uani 1 1 d . . . O3 O 0.6821(3) 0.8929(3) 0.07519(18) 0.0292(9) Uani 1 1 d . . . O100 O 0.1169(4) 0.9241(3) 0.06555(19) 0.0354(10) Uani 1 1 d . . . O200 O 0.0550(4) 0.9936(3) -0.10222(19) 0.0336(9) Uani 1 1 d . . . C1 C 0.1018(6) 1.2242(5) 0.0510(3) 0.0394(15) Uani 1 1 d . . . H1 H 0.0274 1.2190 0.0125 0.047 Uiso 1 1 calc R . . C2 C 0.1008(6) 1.3067(5) 0.0987(3) 0.0434(16) Uani 1 1 d . . . H2 H 0.0279 1.3577 0.0927 0.052 Uiso 1 1 calc R . . C3 C 0.2068(6) 1.3134(5) 0.1546(3) 0.0402(15) Uani 1 1 d . . . H3 H 0.2070 1.3685 0.1886 0.048 Uiso 1 1 calc R . . C4 C 0.3128(6) 1.2409(5) 0.1619(3) 0.0385(15) Uani 1 1 d . . . H4 H 0.3875 1.2452 0.2004 0.046 Uiso 1 1 calc R . . C5 C 0.3082(6) 1.1610(5) 0.1114(3) 0.0309(13) Uani 1 1 d . . . C6 C 0.4240(6) 1.0796(5) 0.1146(3) 0.0328(14) Uani 1 1 d . . . H6A H 0.5124 1.1157 0.1334 0.039 Uiso 1 1 calc R . . H6B H 0.4119 1.0200 0.1468 0.039 Uiso 1 1 calc R . . C7 C 0.6127(6) 0.6425(5) -0.0167(4) 0.0463(17) Uani 1 1 d . . . H7 H 0.6956 0.6561 0.0155 0.056 Uiso 1 1 calc R . . C8 C 0.6004(9) 0.5482(6) -0.0568(5) 0.064(2) Uani 1 1 d . . . H8 H 0.6739 0.4979 -0.0522 0.077 Uiso 1 1 calc R . . C9 C 0.4806(10) 0.5295(6) -0.1028(5) 0.070(2) Uani 1 1 d . . . H9 H 0.4710 0.4666 -0.1315 0.084 Uiso 1 1 calc R . . C10 C 0.3744(8) 0.6012(5) -0.1078(4) 0.0530(18) Uani 1 1 d . . . H10 H 0.2899 0.5879 -0.1388 0.064 Uiso 1 1 calc R . . C11 C 0.3922(6) 0.6927(5) -0.0671(3) 0.0363(14) Uani 1 1 d . . . C12 C 0.2802(6) 0.7747(5) -0.0681(4) 0.0501(18) Uani 1 1 d . . . H12A H 0.2502 0.8022 -0.1162 0.060 Uiso 1 1 calc R . . H12B H 0.2008 0.7388 -0.0541 0.060 Uiso 1 1 calc R . . C13 C 0.3725(6) 0.7505(5) 0.1328(3) 0.0361(14) Uani 1 1 d . . . H13 H 0.2900 0.7509 0.0988 0.043 Uiso 1 1 calc R . . C14 C 0.3755(6) 0.6946(5) 0.1941(3) 0.0418(16) Uani 1 1 d . . . H14 H 0.2966 0.6580 0.2027 0.050 Uiso 1 1 calc R . . C15 C 0.4965(7) 0.6934(5) 0.2426(3) 0.0438(16) Uani 1 1 d . . . H15 H 0.5024 0.6550 0.2852 0.053 Uiso 1 1 calc R . . C16 C 0.6092(6) 0.7486(5) 0.2288(3) 0.0416(15) Uani 1 1 d . . . H16 H 0.6932 0.7482 0.2617 0.050 Uiso 1 1 calc R . . C17 C 0.5984(5) 0.8041(4) 0.1666(3) 0.0298(13) Uani 1 1 d . . . C18 C 0.7135(6) 0.8680(5) 0.1471(3) 0.0386(15) Uani 1 1 d . . . H18A H 0.7274 0.9358 0.1747 0.046 Uiso 1 1 calc R . . H18B H 0.7992 0.8253 0.1577 0.046 Uiso 1 1 calc R . . C100 C 0.0574(5) 0.9575(4) 0.1128(3) 0.0264(13) Uani 1 1 d . . . C101 C 0.1251(6) 0.9359(6) 0.1869(3) 0.0447(16) Uani 1 1 d . . . H10A H 0.0689 0.9660 0.2182 0.067 Uiso 1 1 calc R . . H10B H 0.2157 0.9700 0.1966 0.067 Uiso 1 1 calc R . . H10C H 0.1349 0.8575 0.1944 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.9568(2) 0.5863(2) 0.17321(16) 0.0971(9) Uani 1 1 d . . . O11 O 0.8463(13) 0.5953(14) 0.2101(8) 0.145(5) Uani 0.60 1 d PDU A 1 O12 O 1.0033(13) 0.6979(9) 0.1582(8) 0.132(5) Uani 0.60 1 d PDU A 1 O13 O 1.0675(18) 0.5286(15) 0.2101(9) 0.088(5) Uani 0.60 1 d PDU A 1 O14 O 0.9102(13) 0.5392(11) 0.1045(7) 0.094(4) Uani 0.60 1 d PU A 1 O21 O 0.898(3) 0.486(2) 0.2130(14) 0.170(7) Uani 0.40 1 d PDU A 2 O22 O 0.934(2) 0.6717(17) 0.2176(14) 0.133(6) Uani 0.40 1 d PDU A 2 O23 O 1.089(3) 0.566(3) 0.1875(19) 0.118(8) Uani 0.40 1 d PDU A 2 O24 O 0.874(2) 0.5861(18) 0.1118(13) 0.103(6) Uani 0.40 1 d PU A 2 O2W O 1.1138(15) 0.5884(14) 0.0298(11) 0.164(8) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn2 0.0229(4) 0.0256(5) 0.0260(5) 0.0018(4) 0.0048(3) 0.0002(4) Mn1 0.0214(4) 0.0280(5) 0.0247(5) -0.0015(4) 0.0056(3) 0.0011(4) N1 0.028(3) 0.029(3) 0.039(3) -0.006(2) 0.014(2) -0.005(2) N2 0.029(3) 0.030(3) 0.049(3) 0.006(2) 0.017(2) 0.004(2) N3 0.030(3) 0.030(3) 0.032(3) 0.004(2) 0.008(2) 0.005(2) O1 0.0253(19) 0.031(2) 0.0202(19) -0.0020(16) 0.0087(15) 0.0018(16) O2 0.0253(19) 0.028(2) 0.028(2) -0.0054(17) 0.0047(15) 0.0012(17) O3 0.0245(19) 0.036(2) 0.026(2) 0.0050(17) 0.0018(15) -0.0004(17) O100 0.042(2) 0.033(2) 0.034(2) -0.0010(18) 0.0157(19) -0.0037(19) O200 0.024(2) 0.044(2) 0.032(2) 0.0019(19) 0.0053(16) 0.0020(19) C1 0.030(3) 0.038(4) 0.051(4) -0.007(3) 0.010(3) -0.007(3) C2 0.037(4) 0.039(4) 0.058(4) -0.012(3) 0.020(3) -0.006(3) C3 0.046(4) 0.040(4) 0.038(4) -0.017(3) 0.017(3) -0.008(3) C4 0.042(4) 0.042(4) 0.033(3) -0.007(3) 0.010(3) -0.004(3) C5 0.037(3) 0.029(3) 0.030(3) -0.002(3) 0.014(3) -0.002(3) C6 0.040(3) 0.034(3) 0.024(3) -0.002(3) 0.006(3) -0.002(3) C7 0.043(4) 0.041(4) 0.063(5) 0.020(3) 0.029(3) 0.009(3) C8 0.081(6) 0.033(4) 0.097(7) 0.008(4) 0.060(5) 0.020(4) C9 0.107(7) 0.032(4) 0.085(6) -0.004(4) 0.057(6) -0.003(5) C10 0.066(5) 0.035(4) 0.062(5) -0.013(3) 0.025(4) -0.006(4) C11 0.036(3) 0.030(3) 0.046(4) -0.004(3) 0.015(3) -0.006(3) C12 0.033(3) 0.045(4) 0.069(5) -0.024(4) 0.002(3) -0.003(3) C13 0.031(3) 0.030(3) 0.050(4) 0.001(3) 0.014(3) 0.003(3) C14 0.045(4) 0.036(4) 0.052(4) 0.004(3) 0.029(3) 0.000(3) C15 0.059(4) 0.041(4) 0.035(4) 0.012(3) 0.019(3) 0.006(3) C16 0.042(4) 0.048(4) 0.034(4) 0.008(3) 0.005(3) 0.001(3) C17 0.031(3) 0.029(3) 0.029(3) 0.004(3) 0.006(3) 0.002(3) C18 0.034(3) 0.051(4) 0.027(3) 0.007(3) -0.002(3) -0.007(3) C100 0.026(3) 0.027(3) 0.027(3) 0.002(2) 0.007(2) -0.007(3) C101 0.043(4) 0.054(4) 0.033(4) 0.001(3) 0.001(3) 0.012(3) Cl1 0.0686(15) 0.0657(15) 0.134(2) -0.0327(15) -0.0368(15) 0.0138(12) O11 0.088(8) 0.174(11) 0.184(10) -0.039(9) 0.052(8) 0.046(8) O12 0.113(9) 0.059(7) 0.201(13) -0.006(8) -0.027(9) -0.015(6) O13 0.083(9) 0.085(12) 0.091(10) 0.015(7) 0.005(6) 0.048(8) O14 0.084(8) 0.108(10) 0.076(7) -0.033(7) -0.017(6) 0.026(7) O21 0.169(9) 0.163(10) 0.174(9) 0.008(7) 0.021(7) -0.016(7) O22 0.102(11) 0.099(11) 0.189(13) -0.052(11) 0.004(10) 0.017(9) O23 0.059(10) 0.121(19) 0.161(19) -0.012(14) -0.006(12) 0.023(12) O24 0.100(9) 0.109(9) 0.089(8) -0.002(7) -0.004(7) 0.000(7) O2W 0.086(10) 0.114(13) 0.27(2) 0.044(14) -0.025(12) -0.003(9) _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 Mn2 O3 1.856(3) . ? Mn2 O2 1.883(3) . ? Mn2 O1 2.018(3) 3_675 ? Mn2 N3 2.078(4) . ? Mn2 O1 2.180(4) . ? Mn2 N2 2.209(5) . ? Mn2 Mn2 3.2110(17) 3_675 ? Mn1 O200 2.084(4) . ? Mn1 O100 2.140(4) . ? Mn1 O2 2.167(4) . ? Mn1 O3 2.216(4) 3_675 ? Mn1 N1 2.232(4) . ? Mn1 O1 2.324(4) . ? N1 C1 1.337(7) . ? N1 C5 1.347(7) . ? N2 C11 1.336(7) . ? N2 C7 1.353(7) . ? N3 C17 1.336(7) . ? N3 C13 1.347(7) . ? O1 C6 1.427(6) . ? O1 Mn2 2.018(3) 3_675 ? O2 C12 1.405(7) . ? O3 C18 1.413(6) . ? O3 Mn1 2.216(4) 3_675 ? O100 C100 1.260(6) . ? O200 C100 1.252(6) 3_575 ? C1 C2 1.380(8) . ? C1 H1 0.9500 . ? C2 C3 1.366(8) . ? C2 H2 0.9500 . ? C3 C4 1.369(8) . ? C3 H3 0.9500 . ? C4 C5 1.390(8) . ? C4 H4 0.9500 . ? C5 C6 1.521(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.394(10) . ? C7 H7 0.9500 . ? C8 C9 1.366(11) . ? C8 H8 0.9500 . ? C9 C10 1.367(10) . ? C9 H9 0.9500 . ? C10 C11 1.371(8) . ? C10 H10 0.9500 . ? C11 C12 1.503(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.377(8) . ? C13 H13 0.9500 . ? C14 C15 1.379(9) . ? C14 H14 0.9500 . ? C15 C16 1.384(8) . ? C15 H15 0.9500 . ? C16 C17 1.380(8) . ? C16 H16 0.9500 . ? C17 C18 1.501(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C100 O200 1.252(6) 3_575 ? C100 C101 1.497(8) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? Cl1 O23 1.31(3) . ? Cl1 O24 1.32(2) . ? Cl1 O13 1.389(15) . ? Cl1 O22 1.41(2) . ? Cl1 O11 1.433(12) . ? Cl1 O14 1.453(12) . ? Cl1 O12 1.499(12) . ? Cl1 O21 1.63(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mn2 O2 178.59(17) . . ? O3 Mn2 O1 83.64(15) . 3_675 ? O2 Mn2 O1 96.43(15) . 3_675 ? O3 Mn2 N3 81.15(17) . . ? O2 Mn2 N3 98.65(17) . . ? O1 Mn2 N3 163.87(17) 3_675 . ? O3 Mn2 O1 97.66(15) . . ? O2 Mn2 O1 80.97(14) . . ? O1 Mn2 O1 80.27(13) 3_675 . ? N3 Mn2 O1 96.45(15) . . ? O3 Mn2 N2 102.92(17) . . ? O2 Mn2 N2 78.47(16) . . ? O1 Mn2 N2 98.02(15) 3_675 . ? N3 Mn2 N2 90.59(18) . . ? O1 Mn2 N2 159.05(16) . . ? O3 Mn2 Mn2 91.20(12) . 3_675 ? O2 Mn2 Mn2 87.92(11) . 3_675 ? O1 Mn2 Mn2 41.99(10) 3_675 3_675 ? N3 Mn2 Mn2 132.85(13) . 3_675 ? O1 Mn2 Mn2 38.28(9) . 3_675 ? N2 Mn2 Mn2 136.19(13) . 3_675 ? O200 Mn1 O100 103.98(15) . . ? O200 Mn1 O2 99.16(14) . . ? O100 Mn1 O2 89.23(14) . . ? O200 Mn1 O3 85.64(13) . 3_675 ? O100 Mn1 O3 169.63(14) . 3_675 ? O2 Mn1 O3 93.10(13) . 3_675 ? O200 Mn1 N1 118.90(16) . . ? O100 Mn1 N1 84.68(15) . . ? O2 Mn1 N1 141.82(16) . . ? O3 Mn1 N1 87.26(15) 3_675 . ? O200 Mn1 O1 152.63(13) . . ? O100 Mn1 O1 101.84(13) . . ? O2 Mn1 O1 72.15(12) . . ? O3 Mn1 O1 69.40(12) 3_675 . ? N1 Mn1 O1 72.35(14) . . ? C1 N1 C5 117.6(5) . . ? C1 N1 Mn1 125.5(4) . . ? C5 N1 Mn1 116.7(4) . . ? C11 N2 C7 118.2(5) . . ? C11 N2 Mn2 112.0(4) . . ? C7 N2 Mn2 129.7(4) . . ? C17 N3 C13 119.1(5) . . ? C17 N3 Mn2 112.6(3) . . ? C13 N3 Mn2 127.8(4) . . ? C6 O1 Mn2 121.5(3) . 3_675 ? C6 O1 Mn2 126.4(3) . . ? Mn2 O1 Mn2 99.73(13) 3_675 . ? C6 O1 Mn1 108.7(3) . . ? Mn2 O1 Mn1 98.81(14) 3_675 . ? Mn2 O1 Mn1 95.77(13) . . ? C12 O2 Mn2 121.7(3) . . ? C12 O2 Mn1 126.6(3) . . ? Mn2 O2 Mn1 111.06(16) . . ? C18 O3 Mn2 119.7(3) . . ? C18 O3 Mn1 129.9(3) . 3_675 ? Mn2 O3 Mn1 108.11(16) . 3_675 ? C100 O100 Mn1 132.5(4) . . ? C100 O200 Mn1 124.7(3) 3_575 . ? N1 C1 C2 122.9(6) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.5(6) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.2(6) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 118.1(6) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 122.5(5) . . ? N1 C5 C6 116.2(5) . . ? C4 C5 C6 121.3(5) . . ? O1 C6 C5 111.6(4) . . ? O1 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? O1 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 121.3(7) . . ? N2 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 118.7(7) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 120.0(7) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C11 118.8(7) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? N2 C11 C10 122.9(6) . . ? N2 C11 C12 114.7(5) . . ? C10 C11 C12 122.4(6) . . ? O2 C12 C11 112.5(5) . . ? O2 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? O2 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? N3 C13 C14 122.6(6) . . ? N3 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C13 C14 C15 118.1(6) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? C14 C15 C16 119.5(6) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 119.3(6) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? N3 C17 C16 121.4(5) . . ? N3 C17 C18 115.1(5) . . ? C16 C17 C18 123.5(5) . . ? O3 C18 C17 109.6(4) . . ? O3 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? O3 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? O200 C100 O100 124.7(5) 3_575 . ? O200 C100 C101 117.6(5) 3_575 . ? O100 C100 C101 117.6(5) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? O23 Cl1 O24 128(2) . . ? O24 Cl1 O13 139.9(13) . . ? O23 Cl1 O22 107(2) . . ? O24 Cl1 O22 114.5(13) . . ? O13 Cl1 O22 105.6(13) . . ? O23 Cl1 O11 138.0(16) . . ? O24 Cl1 O11 92.9(12) . . ? O13 Cl1 O11 112.8(8) . . ? O22 Cl1 O11 53.2(10) . . ? O23 Cl1 O14 104.2(19) . . ? O13 Cl1 O14 110.6(10) . . ? O22 Cl1 O14 143.8(10) . . ? O11 Cl1 O14 111.0(9) . . ? O23 Cl1 O12 83.2(14) . . ? O24 Cl1 O12 89.3(12) . . ? O13 Cl1 O12 109.1(9) . . ? O22 Cl1 O12 61.8(11) . . ? O11 Cl1 O12 108.9(8) . . ? O14 Cl1 O12 104.0(9) . . ? O23 Cl1 O21 101.1(13) . . ? O24 Cl1 O21 102.2(14) . . ? O13 Cl1 O21 71.7(12) . . ? O22 Cl1 O21 99.1(13) . . ? O11 Cl1 O21 55.7(10) . . ? O14 Cl1 O21 93.3(11) . . ? O12 Cl1 O21 160.7(11) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.947 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.084 # Attachment 'Dalton5-ACCL3.CIF' data_accl3 _database_code_depnum_ccdc_archive 'CCDC 223058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common catena-(Mn4(hmp)6(OOCCH2Cl)2(ClO4)2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 Cl2 Mn2 N3 O9.60' _chemical_formula_weight 636.79 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' 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' _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 10.151(2) _cell_length_b 10.544(2) _cell_length_c 11.974(2) _cell_angle_alpha 88.43(3) _cell_angle_beta 89.87(3) _cell_angle_gamma 75.63(3) _cell_volume 1241.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details MULABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10544 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5643 _reflns_number_gt 3762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. All non hydrogens were refined anisotropically. The perchlorate anion was found to be disordered over two positions and these were refined with displacement parameters and distance restrains. The occupancies of these two positions were refined together with that of a water oxygen atom (O1W) siting at ca 1.7 angstrom from a perchlorate O (O17). Hydrogens were fixed at calculated positions on their riding, except for the partial water molecule for which hydrogens could not be found found and are therefore missing from this model. ; _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^)+(0.0491P)^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 5643 _refine_ls_number_parameters 362 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1112 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.035 _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 Mn2 Mn -0.47911(4) 0.95407(4) 0.63007(4) 0.01888(13) Uani 1 1 d . . . Mn1 Mn -0.22010(4) 1.00707(4) 0.48543(4) 0.01921(14) Uani 1 1 d . . . Cl2 Cl 0.19513(10) 0.55496(9) 0.47642(9) 0.0498(3) Uani 1 1 d . . . O1 O -0.39281(18) 0.90535(18) 0.46610(16) 0.0191(4) Uani 1 1 d . . . O3 O -0.61793(18) 0.8689(2) 0.62213(17) 0.0235(5) Uani 1 1 d . . . O2 O -0.33837(18) 1.0413(2) 0.63613(16) 0.0220(5) Uani 1 1 d . . . O100 O -0.0691(2) 0.8650(2) 0.57824(18) 0.0316(5) Uani 1 1 d . . . O200 O -0.1411(2) 1.1683(2) 0.49163(19) 0.0311(5) Uani 1 1 d . . . N1 N -0.1642(2) 0.8665(3) 0.3470(2) 0.0265(6) Uani 1 1 d . . . N3 N -0.3781(2) 0.7746(3) 0.7043(2) 0.0242(6) Uani 1 1 d . . . N2 N -0.5213(2) 1.0496(3) 0.7905(2) 0.0259(6) Uani 1 1 d . . . C100 C 0.0417(3) 0.7936(3) 0.5433(2) 0.0233(7) Uani 1 1 d . . . C11 C -0.4367(3) 1.1257(3) 0.8100(3) 0.0283(7) Uani 1 1 d . . . C17 C -0.4555(3) 0.6875(3) 0.7078(3) 0.0254(7) Uani 1 1 d . . . C5 C -0.2299(3) 0.7708(3) 0.3434(3) 0.0255(7) Uani 1 1 d . . . C6 C -0.3428(3) 0.7765(3) 0.4273(3) 0.0267(7) Uani 1 1 d . . . H6A H -0.4164 0.7478 0.3927 0.032 Uiso 1 1 calc R . . H6B H -0.3089 0.7174 0.4901 0.032 Uiso 1 1 calc R . . C16 C -0.4113(3) 0.5668(3) 0.7624(3) 0.0343(8) Uani 1 1 d . . . H16 H -0.4653 0.5073 0.7643 0.041 Uiso 1 1 calc R . . C101 C 0.0500(3) 0.6484(3) 0.5444(3) 0.0344(8) Uani 1 1 d . . . H10A H -0.0308 0.6347 0.5085 0.041 Uiso 1 1 calc R . . H10B H 0.0504 0.6169 0.6213 0.041 Uiso 1 1 calc R . . C8 C -0.6425(4) 1.1249(4) 0.9560(3) 0.0445(10) Uani 1 1 d . . . H8 H -0.7127 1.1226 1.0055 0.053 Uiso 1 1 calc R . . C15 C -0.2854(3) 0.5367(4) 0.8140(3) 0.0396(9) Uani 1 1 d . . . H15 H -0.2537 0.4561 0.8509 0.048 Uiso 1 1 calc R . . C7 C -0.6222(3) 1.0472(4) 0.8639(3) 0.0349(8) Uani 1 1 d . . . H7 H -0.6790 0.9919 0.8519 0.042 Uiso 1 1 calc R . . C14 C -0.2071(3) 0.6254(4) 0.8109(3) 0.0385(9) Uani 1 1 d . . . H14 H -0.1227 0.6062 0.8463 0.046 Uiso 1 1 calc R . . C12 C -0.3237(3) 1.1183(4) 0.7269(3) 0.0352(8) Uani 1 1 d . . . H12A H -0.3240 1.2059 0.6998 0.042 Uiso 1 1 calc R . . H12B H -0.2371 1.0811 0.7635 0.042 Uiso 1 1 calc R . . C1 C -0.0633(3) 0.8670(4) 0.2730(3) 0.0346(8) Uani 1 1 d . . . H1 H -0.0186 0.9340 0.2744 0.042 Uiso 1 1 calc R . . C18 C -0.5894(3) 0.7321(3) 0.6470(3) 0.0305(8) Uani 1 1 d . . . H18A H -0.5859 0.6848 0.5783 0.037 Uiso 1 1 calc R . . H18B H -0.6614 0.7132 0.6930 0.037 Uiso 1 1 calc R . . C2 C -0.0249(3) 0.7700(4) 0.1951(3) 0.0398(9) Uani 1 1 d . . . H2 H 0.0446 0.7720 0.1449 0.048 Uiso 1 1 calc R . . C4 C -0.1954(3) 0.6695(3) 0.2683(3) 0.0328(8) Uani 1 1 d . . . H4 H -0.2409 0.6031 0.2685 0.039 Uiso 1 1 calc R . . C10 C -0.4528(4) 1.2062(4) 0.9020(3) 0.0403(9) Uani 1 1 d . . . H10 H -0.3937 1.2592 0.9144 0.048 Uiso 1 1 calc R . . C3 C -0.0911(3) 0.6701(4) 0.1928(3) 0.0404(9) Uani 1 1 d . . . H3 H -0.0661 0.6040 0.1414 0.049 Uiso 1 1 calc R . . C13 C -0.2552(3) 0.7437(4) 0.7546(3) 0.0320(8) Uani 1 1 d . . . H13 H -0.2015 0.8035 0.7512 0.038 Uiso 1 1 calc R . . C9 C -0.5583(4) 1.2053(4) 0.9738(3) 0.0488(10) Uani 1 1 d . . . H9 H -0.5724 1.2597 1.0349 0.059 Uiso 1 1 calc R . . O1W O 0.1014(6) 1.0232(6) 1.0747(6) 0.099(2) Uani 0.601(5) 1 d P . . O14 O -0.1308(4) 1.3214(5) 1.2103(3) 0.1141(15) Uani 1 1 d U . . O15 O -0.0978(4) 1.3860(4) 1.0321(3) 0.0902(11) Uani 1 1 d U . . Cl1 Cl -0.1784(3) 1.3287(4) 1.09806(19) 0.0540(7) Uani 0.601(5) 1 d PU A 1 O16 O -0.3134(6) 1.3996(8) 1.0968(6) 0.122(3) Uani 0.601(5) 1 d PU A 1 O12 O -0.1951(15) 1.1974(12) 1.0843(10) 0.150(5) Uani 0.601(5) 1 d PU A 1 Cl11 Cl -0.1142(5) 1.2629(6) 1.1086(3) 0.0593(11) Uani 0.399(5) 1 d PU A 2 O17 O 0.0128(10) 1.1706(12) 1.0999(9) 0.111(4) Uani 0.399(5) 1 d PU A 2 O13 O -0.1875(17) 1.228(2) 1.0293(12) 0.127(6) Uani 0.399(5) 1 d PU 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 Mn2 0.0165(2) 0.0205(3) 0.0199(3) 0.00085(19) -0.00037(18) -0.00517(18) Mn1 0.0133(2) 0.0200(3) 0.0241(3) -0.00034(19) 0.00075(18) -0.00369(18) Cl2 0.0482(5) 0.0252(5) 0.0756(7) -0.0117(5) 0.0121(5) -0.0072(4) O1 0.0154(9) 0.0165(11) 0.0244(11) -0.0058(9) 0.0038(8) -0.0019(8) O3 0.0189(10) 0.0217(12) 0.0298(12) 0.0069(9) -0.0032(9) -0.0059(9) O2 0.0161(10) 0.0280(12) 0.0228(11) -0.0058(9) 0.0008(8) -0.0067(9) O100 0.0230(11) 0.0344(14) 0.0306(13) 0.0054(11) -0.0005(10) 0.0052(10) O200 0.0225(11) 0.0237(12) 0.0493(15) -0.0009(11) -0.0003(10) -0.0100(9) N1 0.0213(13) 0.0307(16) 0.0255(15) -0.0007(12) -0.0002(11) -0.0027(11) N3 0.0197(13) 0.0324(16) 0.0197(14) 0.0027(12) 0.0001(11) -0.0052(11) N2 0.0207(13) 0.0335(16) 0.0213(14) 0.0023(12) -0.0012(11) -0.0031(12) C100 0.0225(16) 0.0235(17) 0.0231(17) 0.0033(13) -0.0085(13) -0.0047(13) C11 0.0262(16) 0.037(2) 0.0203(17) -0.0027(15) -0.0029(13) -0.0051(15) C17 0.0231(15) 0.0260(18) 0.0264(18) 0.0026(14) 0.0007(13) -0.0050(13) C5 0.0247(16) 0.0223(17) 0.0252(17) 0.0004(14) -0.0025(13) 0.0021(13) C6 0.0281(17) 0.0232(18) 0.0275(18) -0.0024(14) 0.0021(14) -0.0040(14) C16 0.0318(18) 0.0267(19) 0.043(2) 0.0070(16) 0.0003(16) -0.0054(15) C101 0.0276(17) 0.0239(19) 0.052(2) 0.0034(16) -0.0007(16) -0.0068(14) C8 0.035(2) 0.061(3) 0.027(2) 0.0080(19) 0.0080(16) 0.0070(19) C15 0.0339(19) 0.034(2) 0.041(2) 0.0115(17) 0.0004(16) 0.0088(16) C7 0.0207(16) 0.052(2) 0.0293(19) 0.0124(17) -0.0014(14) -0.0043(15) C14 0.0208(16) 0.051(2) 0.038(2) 0.0051(18) -0.0033(15) 0.0025(16) C12 0.0318(18) 0.045(2) 0.035(2) -0.0153(17) 0.0047(15) -0.0199(16) C1 0.0220(16) 0.046(2) 0.032(2) 0.0023(17) 0.0035(15) -0.0025(15) C18 0.0266(16) 0.0273(19) 0.039(2) 0.0066(15) -0.0069(15) -0.0105(14) C2 0.0285(18) 0.054(3) 0.031(2) -0.0068(18) 0.0083(15) 0.0010(17) C4 0.0366(19) 0.030(2) 0.0274(19) -0.0032(15) -0.0029(15) -0.0004(15) C10 0.048(2) 0.048(2) 0.0257(19) -0.0062(17) -0.0040(17) -0.0112(18) C3 0.037(2) 0.043(2) 0.032(2) -0.0120(17) 0.0043(16) 0.0084(17) C13 0.0205(16) 0.046(2) 0.0300(19) -0.0003(16) 0.0026(14) -0.0088(15) C9 0.056(2) 0.057(3) 0.026(2) -0.0070(19) 0.0000(18) 0.001(2) O1W 0.094(5) 0.082(5) 0.120(6) 0.018(4) -0.006(4) -0.021(4) O14 0.118(3) 0.206(5) 0.047(2) 0.001(2) -0.006(2) -0.095(3) O15 0.080(2) 0.131(3) 0.054(2) -0.001(2) 0.0130(18) -0.017(2) Cl1 0.0419(13) 0.093(2) 0.0312(11) -0.0158(12) 0.0046(10) -0.0241(13) O16 0.061(4) 0.166(7) 0.119(6) 0.015(5) 0.037(4) 0.008(4) O12 0.172(10) 0.116(6) 0.187(14) -0.056(8) -0.041(10) -0.075(6) Cl11 0.050(2) 0.093(3) 0.0427(18) 0.0007(19) 0.0007(17) -0.032(2) O17 0.087(6) 0.132(8) 0.101(8) -0.002(6) -0.029(5) -0.005(5) O13 0.076(7) 0.258(16) 0.078(9) -0.046(10) 0.003(6) -0.095(9) _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 Mn2 O3 1.854(2) . ? Mn2 O2 1.883(2) . ? Mn2 O1 2.042(2) 2_476 ? Mn2 N3 2.091(3) . ? Mn2 O1 2.1704(19) . ? Mn2 N2 2.185(3) . ? Mn2 Mn2 3.2339(12) 2_476 ? Mn1 O200 2.054(2) . ? Mn1 O100 2.146(2) . ? Mn1 O2 2.1538(19) . ? Mn1 O3 2.219(2) 2_476 ? Mn1 N1 2.232(3) . ? Mn1 O1 2.286(2) . ? Cl2 C101 1.767(3) . ? O1 C6 1.418(3) . ? O1 Mn2 2.042(2) 2_476 ? O3 C18 1.422(4) . ? O3 Mn1 2.219(2) 2_476 ? O2 C12 1.404(4) . ? O100 C100 1.266(3) . ? O200 C100 1.243(3) 2_576 ? N1 C5 1.341(4) . ? N1 C1 1.354(4) . ? N3 C13 1.348(4) . ? N3 C17 1.348(4) . ? N2 C11 1.337(4) . ? N2 C7 1.353(4) . ? C100 O200 1.243(3) 2_576 ? C100 C101 1.512(4) . ? C11 C10 1.395(5) . ? C11 C12 1.505(4) . ? C17 C16 1.386(4) . ? C17 C18 1.505(4) . ? C5 C4 1.393(4) . ? C5 C6 1.513(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C16 C15 1.381(5) . ? C16 H16 0.9300 . ? C101 H10A 0.9700 . ? C101 H10B 0.9700 . ? C8 C9 1.367(6) . ? C8 C7 1.376(5) . ? C8 H8 0.9300 . ? C15 C14 1.369(5) . ? C15 H15 0.9300 . ? C7 H7 0.9300 . ? C14 C13 1.379(5) . ? C14 H14 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C1 C2 1.385(5) . ? C1 H1 0.9300 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C2 C3 1.384(5) . ? C2 H2 0.9300 . ? C4 C3 1.391(5) . ? C4 H4 0.9300 . ? C10 C9 1.373(5) . ? C10 H10 0.9300 . ? C3 H3 0.9300 . ? C13 H13 0.9300 . ? C9 H9 0.9300 . ? O1W O17 1.627(12) . ? O14 Cl11 1.371(5) . ? O14 Cl1 1.423(4) . ? O15 Cl1 1.369(4) . ? O15 Cl11 1.610(6) . ? Cl1 O16 1.389(7) . ? Cl1 O12 1.449(11) . ? Cl11 O13 1.324(16) . ? Cl11 O17 1.416(12) . ? 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 Mn2 O2 179.25(9) . . ? O3 Mn2 O1 83.78(8) . 2_476 ? O2 Mn2 O1 95.66(9) . 2_476 ? O3 Mn2 N3 81.33(9) . . ? O2 Mn2 N3 99.14(10) . . ? O1 Mn2 N3 163.01(9) 2_476 . ? O3 Mn2 O1 97.80(9) . . ? O2 Mn2 O1 81.59(8) . . ? O1 Mn2 O1 79.75(8) 2_476 . ? N3 Mn2 O1 94.18(9) . . ? O3 Mn2 N2 101.34(9) . . ? O2 Mn2 N2 79.23(9) . . ? O1 Mn2 N2 97.76(9) 2_476 . ? N3 Mn2 N2 93.17(10) . . ? O1 Mn2 N2 160.32(9) . . ? O3 Mn2 Mn2 91.30(7) . 2_476 ? O2 Mn2 Mn2 87.95(7) . 2_476 ? O1 Mn2 Mn2 41.33(5) 2_476 2_476 ? N3 Mn2 Mn2 130.75(7) . 2_476 ? O1 Mn2 Mn2 38.42(5) . 2_476 ? N2 Mn2 Mn2 135.82(7) . 2_476 ? O200 Mn1 O100 100.94(9) . . ? O200 Mn1 O2 97.31(9) . . ? O100 Mn1 O2 88.15(8) . . ? O200 Mn1 O3 86.02(8) . 2_476 ? O100 Mn1 O3 172.25(8) . 2_476 ? O2 Mn1 O3 94.40(8) . 2_476 ? O200 Mn1 N1 120.49(9) . . ? O100 Mn1 N1 84.10(9) . . ? O2 Mn1 N1 142.19(9) . . ? O3 Mn1 N1 89.43(9) 2_476 . ? O200 Mn1 O1 153.75(8) . . ? O100 Mn1 O1 103.21(8) . . ? O2 Mn1 O1 73.46(7) . . ? O3 Mn1 O1 70.64(7) 2_476 . ? N1 Mn1 O1 72.47(8) . . ? C6 O1 Mn2 120.95(18) . 2_476 ? C6 O1 Mn2 125.15(18) . . ? Mn2 O1 Mn2 100.25(8) 2_476 . ? C6 O1 Mn1 110.86(16) . . ? Mn2 O1 Mn1 98.46(8) 2_476 . ? Mn2 O1 Mn1 95.45(8) . . ? C18 O3 Mn2 119.41(17) . . ? C18 O3 Mn1 129.45(18) . 2_476 ? Mn2 O3 Mn1 107.05(9) . 2_476 ? C12 O2 Mn2 121.76(17) . . ? C12 O2 Mn1 128.81(17) . . ? Mn2 O2 Mn1 109.39(9) . . ? C100 O100 Mn1 128.1(2) . . ? C100 O200 Mn1 139.7(2) 2_576 . ? C5 N1 C1 119.1(3) . . ? C5 N1 Mn1 116.58(19) . . ? C1 N1 Mn1 124.2(2) . . ? C13 N3 C17 119.4(3) . . ? C13 N3 Mn2 127.8(2) . . ? C17 N3 Mn2 112.49(19) . . ? C11 N2 C7 119.2(3) . . ? C11 N2 Mn2 111.47(19) . . ? C7 N2 Mn2 129.2(2) . . ? O200 C100 O100 126.4(3) 2_576 . ? O200 C100 C101 118.4(3) 2_576 . ? O100 C100 C101 115.2(3) . . ? N2 C11 C10 121.6(3) . . ? N2 C11 C12 115.9(3) . . ? C10 C11 C12 122.5(3) . . ? N3 C17 C16 121.3(3) . . ? N3 C17 C18 114.6(3) . . ? C16 C17 C18 124.2(3) . . ? N1 C5 C4 122.3(3) . . ? N1 C5 C6 116.6(3) . . ? C4 C5 C6 121.1(3) . . ? O1 C6 C5 111.1(3) . . ? O1 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? O1 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C15 C16 C17 118.6(3) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C100 C101 Cl2 113.7(2) . . ? C100 C101 H10A 108.8 . . ? Cl2 C101 H10A 108.8 . . ? C100 C101 H10B 108.8 . . ? Cl2 C101 H10B 108.8 . . ? H10A C101 H10B 107.7 . . ? C9 C8 C7 119.1(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C14 C15 C16 120.1(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? N2 C7 C8 121.4(4) . . ? N2 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C15 C14 C13 119.0(3) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? O2 C12 C11 111.3(3) . . ? O2 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? O2 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N1 C1 C2 121.6(3) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? O3 C18 C17 110.1(3) . . ? O3 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? O3 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C3 C4 C5 118.4(3) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C9 C10 C11 118.3(4) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? N3 C13 C14 121.5(3) . . ? N3 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? O15 Cl1 O16 112.4(4) . . ? O15 Cl1 O14 108.9(3) . . ? O16 Cl1 O14 107.7(4) . . ? O15 Cl1 O12 124.5(6) . . ? O16 Cl1 O12 100.4(7) . . ? O14 Cl1 O12 101.5(6) . . ? O13 Cl11 O14 139.9(9) . . ? O13 Cl11 O17 102.8(11) . . ? O14 Cl11 O17 112.3(6) . . ? O13 Cl11 O15 90.4(9) . . ? O14 Cl11 O15 99.0(4) . . ? O17 Cl11 O15 104.2(5) . . ? Cl11 O17 O1W 150.3(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.552 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.086 data_bb _database_code_depnum_ccdc_archive 'CCDC 616293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 Cl2 Mn4 N6 O24 ' _chemical_formula_weight 1281.46 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' 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' _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 10.808(2) _cell_length_b 11.190(3) _cell_length_c 11.360(2) _cell_angle_alpha 83.94(3) _cell_angle_beta 81.91(3) _cell_angle_gamma 79.58(2) _cell_volume 1333.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details MULABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8807 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5420 _reflns_number_gt 3900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. All non hydrogens were refined anisotropically. The perchlorate anion was disordered and refined with displacement parameters and distance constrains. Hydrogens were placed geometrically on their riding atom except for a number of lattice water molecules for which hydrogens could not be found nor fixed and are therefore missing from the structural model. ; _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^)+(0.0990P)^2^+1.8669P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.009(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5420 _refine_ls_number_parameters 380 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1973 _refine_ls_wR_factor_gt 0.1768 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.068 _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 0.67305(7) 0.11092(7) 0.61534(6) 0.0534(3) Uani 1 1 d . . . Mn2 Mn 0.40314(6) 0.12702(6) 0.49044(6) 0.0430(2) Uani 1 1 d . . . OW1 O 0.8060(5) 0.0117(6) 0.7380(4) 0.1124(19) Uani 1 1 d . . . O1 O 0.5104(3) -0.0040(3) 0.6186(2) 0.0423(7) Uani 1 1 d . . . O2 O 0.2668(3) 0.0448(3) 0.4961(3) 0.0553(8) Uani 1 1 d . . . O3 O 0.5386(3) 0.2101(3) 0.4918(3) 0.0491(7) Uani 1 1 d . . . O11 O 0.8356(4) 0.1958(5) 0.5007(4) 0.0821(12) Uani 1 1 d . . . O12 O 0.7175(5) 0.2961(4) 0.6411(4) 0.0908(14) Uani 1 1 d . . . N1 N 0.5367(4) 0.1317(4) 0.7889(3) 0.0585(11) Uani 1 1 d . . . N2 N 0.2814(4) 0.2196(4) 0.6199(4) 0.0581(10) Uani 1 1 d . . . N3 N 0.3599(4) 0.2780(4) 0.3546(4) 0.0544(10) Uani 1 1 d . . . C1 C 0.4480(5) 0.0617(4) 0.8166(4) 0.0507(11) Uani 1 1 d . . . C2 C 0.3603(6) 0.0732(5) 0.9186(4) 0.0651(14) Uani 1 1 d . . . H2A H 0.2958 0.0242 0.9344 0.078 Uiso 1 1 calc R . . C3 C 0.3688(7) 0.1564(6) 0.9955(5) 0.0832(19) Uani 1 1 d . . . H3A H 0.3104 0.1654 1.0661 0.100 Uiso 1 1 calc R . . C4 C 0.4618(8) 0.2267(6) 0.9704(5) 0.092(2) Uani 1 1 d . . . H4A H 0.4697 0.2845 1.0232 0.111 Uiso 1 1 calc R . . C5 C 0.5430(7) 0.2118(5) 0.8676(5) 0.0816(19) Uani 1 1 d . . . H5A H 0.6077 0.2606 0.8505 0.098 Uiso 1 1 calc R . . C6 C 0.4458(5) -0.0329(4) 0.7330(4) 0.0490(10) Uani 1 1 d . . . H6A H 0.4866 -0.1134 0.7661 0.059 Uiso 1 1 calc R . . H6B H 0.3568 -0.0380 0.7253 0.059 Uiso 1 1 calc R . . C7 C 0.1717(5) 0.1761(6) 0.6482(5) 0.0682(15) Uani 1 1 d . . . C8 C 0.0802(7) 0.2296(8) 0.7342(6) 0.096(2) Uani 1 1 d . . . H8A H 0.0029 0.1989 0.7549 0.116 Uiso 1 1 calc R . . C9 C 0.1004(8) 0.3256(9) 0.7891(7) 0.113(3) Uani 1 1 d . . . H9A H 0.0373 0.3624 0.8474 0.136 Uiso 1 1 calc R . . C10 C 0.2128(9) 0.3687(7) 0.7595(6) 0.099(2) Uani 1 1 d . . . H10A H 0.2287 0.4354 0.7970 0.119 Uiso 1 1 calc R . . C11 C 0.3017(7) 0.3136(5) 0.6748(5) 0.0749(16) Uani 1 1 d . . . H11A H 0.3799 0.3427 0.6544 0.090 Uiso 1 1 calc R . . C12 C 0.1594(5) 0.0729(7) 0.5816(5) 0.0755(17) Uani 1 1 d . . . H12A H 0.1503 0.0004 0.6381 0.091 Uiso 1 1 calc R . . H12B H 0.0822 0.0942 0.5408 0.091 Uiso 1 1 calc R . . C13 C 0.4507(5) 0.3465(4) 0.3338(4) 0.0585(12) Uani 1 1 d . . . C14 C 0.4437(8) 0.4454(5) 0.2495(6) 0.088(2) Uani 1 1 d . . . H14A H 0.5085 0.4942 0.2362 0.105 Uiso 1 1 calc R . . C15 C 0.3435(9) 0.4722(6) 0.1859(7) 0.100(3) Uani 1 1 d . . . H15A H 0.3389 0.5388 0.1266 0.120 Uiso 1 1 calc R . . C16 C 0.2500(8) 0.4038(6) 0.2070(6) 0.091(2) Uani 1 1 d . . . H16A H 0.1785 0.4231 0.1643 0.109 Uiso 1 1 calc R . . C17 C 0.2605(6) 0.3051(5) 0.2922(5) 0.0683(14) Uani 1 1 d . . . H17A H 0.1962 0.2558 0.3065 0.082 Uiso 1 1 calc R . . C18 C 0.5581(5) 0.3093(5) 0.4075(5) 0.0634(14) Uani 1 1 d . . . H18A H 0.6378 0.2865 0.3543 0.076 Uiso 1 1 calc R . . H18B H 0.5674 0.3795 0.4498 0.076 Uiso 1 1 calc R . . C21 C 0.8045(6) 0.2905(6) 0.5574(6) 0.0747(17) Uani 1 1 d . . . C22 C 0.8723(8) 0.3974(8) 0.5184(8) 0.106(3) Uani 1 1 d . . . H22A H 0.9583 0.3782 0.5410 0.160 Uiso 1 1 calc R . . H22B H 0.8259 0.4693 0.5572 0.160 Uiso 1 1 calc R . . H22C H 0.8766 0.4142 0.4316 0.160 Uiso 1 1 calc R . . Cl1 Cl 0.8195(3) 0.2770(5) 1.0605(3) 0.1900(19) Uani 1 1 d D . . O21 O 0.9151(14) 0.3312(14) 1.0862(14) 0.159(5) Uani 0.60 1 d PDU A 1 O22 O 0.8157(14) 0.1667(10) 1.1341(11) 0.189(5) Uani 0.70 1 d PDU A 1 O23 O 0.7054(18) 0.363(2) 1.080(2) 0.270(11) Uani 0.60 1 d PDU A 1 O24 O 0.8212(12) 0.2596(14) 0.9390(8) 0.137(4) Uani 0.50 1 d PDU A 1 O21A O 0.6899(12) 0.267(3) 1.097(2) 0.170(8) Uani 0.40 1 d PDU A 2 O22A O 0.812(4) 0.323(3) 1.1781(18) 0.207(13) Uani 0.30 1 d PDU A 2 O23A O 0.850(3) 0.3955(16) 1.017(3) 0.226(12) Uani 0.40 1 d PDU A 2 O24A O 0.9537(9) 0.2315(17) 1.0617(15) 0.153(5) Uani 0.50 1 d PDU A 2 OW2 O 0.9937(5) -0.1760(8) 0.6928(5) 0.137(3) Uani 1 1 d . . . OW3 O 0.9004(11) 0.0192(12) 0.9429(9) 0.234(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0573(5) 0.0668(5) 0.0440(4) -0.0076(3) -0.0068(3) -0.0290(4) Mn2 0.0406(4) 0.0437(4) 0.0436(4) -0.0068(3) 0.0013(3) -0.0071(3) OW1 0.087(3) 0.180(6) 0.075(3) 0.014(3) -0.036(3) -0.030(3) O1 0.0451(16) 0.0478(16) 0.0345(15) -0.0085(12) 0.0013(12) -0.0114(13) O2 0.0377(16) 0.074(2) 0.0558(19) -0.0102(16) 0.0001(14) -0.0139(15) O3 0.0555(18) 0.0447(16) 0.0486(18) -0.0031(13) -0.0033(14) -0.0153(14) O11 0.073(3) 0.106(3) 0.076(3) -0.005(2) -0.003(2) -0.046(2) O12 0.123(4) 0.094(3) 0.071(3) -0.018(2) 0.004(3) -0.067(3) N1 0.085(3) 0.055(2) 0.041(2) -0.0111(17) -0.004(2) -0.026(2) N2 0.054(2) 0.059(2) 0.053(2) -0.0059(19) 0.0025(19) 0.0065(19) N3 0.058(2) 0.050(2) 0.052(2) -0.0066(17) -0.0042(19) -0.0019(18) C1 0.065(3) 0.049(2) 0.036(2) -0.0044(18) -0.003(2) -0.007(2) C2 0.077(4) 0.069(3) 0.046(3) -0.011(2) 0.007(3) -0.011(3) C3 0.125(6) 0.077(4) 0.044(3) -0.020(3) 0.012(3) -0.015(4) C4 0.159(7) 0.075(4) 0.050(3) -0.025(3) -0.008(4) -0.028(4) C5 0.134(6) 0.070(4) 0.053(3) -0.019(3) -0.007(3) -0.044(4) C6 0.055(3) 0.050(2) 0.042(2) -0.0056(19) 0.005(2) -0.017(2) C7 0.047(3) 0.095(4) 0.051(3) -0.001(3) 0.004(2) 0.007(3) C8 0.065(4) 0.133(6) 0.075(4) -0.017(4) 0.022(3) 0.008(4) C9 0.099(6) 0.139(7) 0.075(5) -0.018(5) 0.026(4) 0.032(5) C10 0.134(7) 0.078(4) 0.069(4) -0.023(3) 0.004(4) 0.019(4) C11 0.093(4) 0.059(3) 0.064(3) -0.012(3) 0.003(3) 0.007(3) C12 0.042(3) 0.124(5) 0.060(3) -0.014(3) 0.005(2) -0.018(3) C13 0.081(4) 0.042(2) 0.052(3) -0.005(2) -0.003(3) -0.011(2) C14 0.144(6) 0.049(3) 0.081(4) 0.009(3) -0.038(4) -0.032(4) C15 0.173(8) 0.047(3) 0.090(5) 0.007(3) -0.058(5) -0.018(4) C16 0.128(6) 0.066(4) 0.081(4) -0.014(3) -0.047(4) 0.012(4) C17 0.073(4) 0.064(3) 0.065(3) -0.018(3) -0.008(3) 0.002(3) C18 0.077(4) 0.055(3) 0.062(3) 0.007(2) -0.009(3) -0.028(3) C21 0.089(4) 0.086(4) 0.065(4) 0.003(3) -0.028(3) -0.050(4) C22 0.116(6) 0.111(6) 0.109(6) 0.015(5) -0.024(5) -0.073(5) Cl1 0.0952(17) 0.290(5) 0.139(2) 0.111(3) -0.0049(17) 0.006(2) O21 0.174(9) 0.129(7) 0.166(9) 0.002(7) 0.019(7) -0.041(7) O22 0.224(9) 0.190(8) 0.169(8) 0.024(7) -0.058(7) -0.075(7) O23 0.249(13) 0.284(14) 0.268(13) 0.000(10) -0.046(9) -0.026(10) O24 0.106(7) 0.192(9) 0.097(7) 0.031(7) -0.004(6) -0.011(7) O21A 0.156(11) 0.173(11) 0.178(11) -0.032(9) 0.007(9) -0.033(9) O22A 0.206(16) 0.201(15) 0.200(15) 0.018(10) -0.018(10) -0.019(10) O23A 0.214(14) 0.243(15) 0.211(14) -0.002(10) -0.021(10) -0.028(10) O24A 0.146(9) 0.157(9) 0.146(9) -0.018(8) -0.014(7) 0.002(7) OW2 0.062(3) 0.261(8) 0.083(3) 0.022(4) -0.011(3) -0.033(4) OW3 0.221(10) 0.329(15) 0.174(9) -0.019(10) -0.025(8) -0.102(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 2.210(4) 2_656 ? Mn1 OW1 2.214(5) . ? Mn1 O3 2.230(3) . ? Mn1 O12 2.267(4) . ? Mn1 N1 2.295(4) . ? Mn1 O11 2.320(4) . ? Mn1 O1 2.352(3) . ? Mn2 O2 1.864(3) . ? Mn2 O3 1.874(3) . ? Mn2 O1 1.968(3) 2_656 ? Mn2 N2 2.061(4) . ? Mn2 N3 2.196(4) . ? Mn2 O1 2.241(3) . ? Mn2 Mn2 3.2181(17) 2_656 ? O1 C6 1.421(5) . ? O1 Mn2 1.968(3) 2_656 ? O2 C12 1.416(6) . ? O2 Mn1 2.210(4) 2_656 ? O3 C18 1.414(6) . ? O11 C21 1.267(8) . ? O12 C21 1.238(8) . ? N1 C1 1.330(6) . ? N1 C5 1.348(6) . ? N2 C11 1.343(7) . ? N2 C7 1.347(7) . ? N3 C13 1.332(7) . ? N3 C17 1.342(7) . ? C1 C2 1.391(7) . ? C1 C6 1.499(6) . ? C2 C3 1.366(8) . ? C2 H2A 0.9500 . ? C3 C4 1.367(10) . ? C3 H3A 0.9500 . ? C4 C5 1.364(9) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.388(8) . ? C7 C12 1.481(9) . ? C8 C9 1.363(12) . ? C8 H8A 0.9500 . ? C9 C10 1.372(12) . ? C9 H9A 0.9500 . ? C10 C11 1.372(9) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.383(8) . ? C13 C18 1.499(8) . ? C14 C15 1.357(10) . ? C14 H14A 0.9500 . ? C15 C16 1.355(11) . ? C15 H15A 0.9500 . ? C16 C17 1.389(9) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C21 C22 1.509(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? Cl1 O21 1.367(9) . ? Cl1 O24 1.412(8) . ? Cl1 O22 1.419(8) . ? Cl1 O21A 1.426(10) . ? Cl1 O23 1.427(10) . ? Cl1 O23A 1.443(10) . ? Cl1 O24A 1.449(9) . ? Cl1 O22A 1.468(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 O2 Mn1 OW1 86.66(19) 2_656 . ? O2 Mn1 O3 93.20(12) 2_656 . ? OW1 Mn1 O3 179.74(18) . . ? O2 Mn1 O12 142.34(15) 2_656 . ? OW1 Mn1 O12 93.8(2) . . ? O3 Mn1 O12 86.41(16) . . ? O2 Mn1 N1 130.84(13) 2_656 . ? OW1 Mn1 N1 82.74(19) . . ? O3 Mn1 N1 97.18(14) . . ? O12 Mn1 N1 86.37(16) . . ? O2 Mn1 O11 85.81(15) 2_656 . ? OW1 Mn1 O11 90.85(18) . . ? O3 Mn1 O11 89.35(14) . . ? O12 Mn1 O11 56.53(17) . . ? N1 Mn1 O11 141.93(16) . . ? O2 Mn1 O1 68.16(11) 2_656 . ? OW1 Mn1 O1 107.44(17) . . ? O3 Mn1 O1 72.31(11) . . ? O12 Mn1 O1 145.03(16) . . ? N1 Mn1 O1 69.71(12) . . ? O11 Mn1 O1 146.60(13) . . ? O2 Mn2 O3 177.55(14) . . ? O2 Mn2 O1 83.77(13) . 2_656 ? O3 Mn2 O1 98.04(13) . 2_656 ? O2 Mn2 N2 81.46(17) . . ? O3 Mn2 N2 96.56(16) . . ? O1 Mn2 N2 164.06(16) 2_656 . ? O2 Mn2 N3 102.13(16) . . ? O3 Mn2 N3 79.30(15) . . ? O1 Mn2 N3 97.54(14) 2_656 . ? N2 Mn2 N3 91.42(16) . . ? O2 Mn2 O1 97.05(13) . . ? O3 Mn2 O1 81.68(12) . . ? O1 Mn2 O1 80.46(12) 2_656 . ? N2 Mn2 O1 95.39(14) . . ? N3 Mn2 O1 160.41(14) . . ? O2 Mn2 Mn2 91.10(11) . 2_656 ? O3 Mn2 Mn2 89.13(10) . 2_656 ? O1 Mn2 Mn2 43.37(9) 2_656 2_656 ? N2 Mn2 Mn2 130.80(12) . 2_656 ? N3 Mn2 Mn2 137.41(11) . 2_656 ? O1 Mn2 Mn2 37.09(7) . 2_656 ? C6 O1 Mn2 123.7(3) . 2_656 ? C6 O1 Mn2 118.0(3) . . ? Mn2 O1 Mn2 99.54(12) 2_656 . ? C6 O1 Mn1 115.8(2) . . ? Mn2 O1 Mn1 99.65(12) 2_656 . ? Mn2 O1 Mn1 95.01(11) . . ? C12 O2 Mn2 119.3(3) . . ? C12 O2 Mn1 131.0(3) . 2_656 ? Mn2 O2 Mn1 108.38(15) . 2_656 ? C18 O3 Mn2 121.0(3) . . ? C18 O3 Mn1 127.0(3) . . ? Mn2 O3 Mn1 110.99(14) . . ? C21 O11 Mn1 89.9(4) . . ? C21 O12 Mn1 93.1(4) . . ? C1 N1 C5 117.0(5) . . ? C1 N1 Mn1 120.2(3) . . ? C5 N1 Mn1 122.8(4) . . ? C11 N2 C7 120.1(5) . . ? C11 N2 Mn2 127.1(4) . . ? C7 N2 Mn2 112.8(4) . . ? C13 N3 C17 119.4(5) . . ? C13 N3 Mn2 111.5(3) . . ? C17 N3 Mn2 129.1(4) . . ? N1 C1 C2 122.5(4) . . ? N1 C1 C6 117.1(4) . . ? C2 C1 C6 120.4(4) . . ? C3 C2 C1 118.8(6) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 119.5(6) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 118.4(5) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? N1 C5 C4 123.7(6) . . ? N1 C5 H5A 118.1 . . ? C4 C5 H5A 118.1 . . ? O1 C6 C1 111.0(3) . . ? O1 C6 H6A 109.4 . . ? C1 C6 H6A 109.4 . . ? O1 C6 H6B 109.4 . . ? C1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 119.4(7) . . ? N2 C7 C12 115.4(5) . . ? C8 C7 C12 125.3(6) . . ? C9 C8 C7 120.6(7) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 119.4(7) . . ? C8 C9 H9A 120.3 . . ? C10 C9 H9A 120.3 . . ? C11 C10 C9 118.7(8) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? N2 C11 C10 121.9(7) . . ? N2 C11 H11A 119.1 . . ? C10 C11 H11A 119.1 . . ? O2 C12 C7 110.9(5) . . ? O2 C12 H12A 109.5 . . ? C7 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N3 C13 C14 121.1(6) . . ? N3 C13 C18 115.7(4) . . ? C14 C13 C18 123.3(5) . . ? C15 C14 C13 119.5(6) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C16 C15 C14 120.0(6) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 118.9(6) . . ? C15 C16 H16A 120.6 . . ? C17 C16 H16A 120.6 . . ? N3 C17 C16 121.2(6) . . ? N3 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? O3 C18 C13 112.0(4) . . ? O3 C18 H18A 109.2 . . ? C13 C18 H18A 109.2 . . ? O3 C18 H18B 109.2 . . ? C13 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? O12 C21 O11 120.3(5) . . ? O12 C21 C22 120.8(7) . . ? O11 C21 C22 118.9(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O21 Cl1 O24 115.5(9) . . ? O21 Cl1 O22 109.5(9) . . ? O24 Cl1 O22 111.8(9) . . ? O21 Cl1 O21A 142.5(13) . . ? O24 Cl1 O21A 96.9(12) . . ? O22 Cl1 O21A 71.9(12) . . ? O21 Cl1 O23 106.5(15) . . ? O24 Cl1 O23 100.7(12) . . ? O22 Cl1 O23 112.5(14) . . ? O21A Cl1 O23 46.0(12) . . ? O21 Cl1 O23A 51.3(13) . . ? O24 Cl1 O23A 85.1(14) . . ? O22 Cl1 O23A 159.8(15) . . ? O21A Cl1 O23A 118.5(17) . . ? O23 Cl1 O23A 73.0(16) . . ? O21 Cl1 O24A 48.8(8) . . ? O24 Cl1 O24A 94.3(9) . . ? O22 Cl1 O24A 79.2(9) . . ? O21A Cl1 O24A 151.1(14) . . ? O23 Cl1 O24A 155.2(15) . . ? O23A Cl1 O24A 88.9(15) . . ? O21 Cl1 O22A 60.3(16) . . ? O24 Cl1 O22A 167.6(16) . . ? O22 Cl1 O22A 80.2(15) . . ? O21A Cl1 O22A 83.9(18) . . ? O23 Cl1 O22A 71.1(17) . . ? O23A Cl1 O22A 84(2) . . ? O24A Cl1 O22A 90.6(16) . . ? 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 Mn2 O1 C6 -54.1(3) . . . . ? O3 Mn2 O1 C6 123.7(3) . . . . ? O1 Mn2 O1 C6 -136.6(3) 2_656 . . . ? N2 Mn2 O1 C6 27.9(3) . . . . ? N3 Mn2 O1 C6 137.7(4) . . . . ? Mn2 Mn2 O1 C6 -136.6(3) 2_656 . . . ? O2 Mn2 O1 Mn2 82.44(14) . . . 2_656 ? O3 Mn2 O1 Mn2 -99.67(14) . . . 2_656 ? O1 Mn2 O1 Mn2 0.0 2_656 . . 2_656 ? N2 Mn2 O1 Mn2 164.47(16) . . . 2_656 ? N3 Mn2 O1 Mn2 -85.7(4) . . . 2_656 ? O2 Mn2 O1 Mn1 -176.88(12) . . . . ? O3 Mn2 O1 Mn1 1.01(11) . . . . ? O1 Mn2 O1 Mn1 100.68(13) 2_656 . . . ? N2 Mn2 O1 Mn1 -94.85(15) . . . . ? N3 Mn2 O1 Mn1 15.0(4) . . . . ? Mn2 Mn2 O1 Mn1 100.68(13) 2_656 . . . ? O2 Mn1 O1 C6 133.7(3) 2_656 . . . ? OW1 Mn1 O1 C6 54.8(3) . . . . ? O3 Mn1 O1 C6 -125.3(3) . . . . ? O12 Mn1 O1 C6 -70.1(4) . . . . ? N1 Mn1 O1 C6 -20.3(3) . . . . ? O11 Mn1 O1 C6 175.1(3) . . . . ? O2 Mn1 O1 Mn2 -1.31(12) 2_656 . . 2_656 ? OW1 Mn1 O1 Mn2 -80.3(2) . . . 2_656 ? O3 Mn1 O1 Mn2 99.70(14) . . . 2_656 ? O12 Mn1 O1 Mn2 154.9(2) . . . 2_656 ? N1 Mn1 O1 Mn2 -155.36(17) . . . 2_656 ? O11 Mn1 O1 Mn2 40.1(3) . . . 2_656 ? O2 Mn1 O1 Mn2 -101.89(13) 2_656 . . . ? OW1 Mn1 O1 Mn2 179.15(17) . . . . ? O3 Mn1 O1 Mn2 -0.88(10) . . . . ? O12 Mn1 O1 Mn2 54.3(3) . . . . ? N1 Mn1 O1 Mn2 104.06(15) . . . . ? O11 Mn1 O1 Mn2 -60.5(3) . . . . ? O1 Mn2 O2 C12 169.7(4) 2_656 . . . ? N2 Mn2 O2 C12 -4.2(4) . . . . ? N3 Mn2 O2 C12 -93.9(4) . . . . ? O1 Mn2 O2 C12 90.2(4) . . . . ? Mn2 Mn2 O2 C12 126.9(4) 2_656 . . . ? O1 Mn2 O2 Mn1 1.61(14) 2_656 . . 2_656 ? N2 Mn2 O2 Mn1 -172.36(19) . . . 2_656 ? N3 Mn2 O2 Mn1 98.01(17) . . . 2_656 ? O1 Mn2 O2 Mn1 -77.94(16) . . . 2_656 ? Mn2 Mn2 O2 Mn1 -41.22(14) 2_656 . . 2_656 ? O1 Mn2 O3 C18 89.5(4) 2_656 . . . ? N2 Mn2 O3 C18 -97.0(4) . . . . ? N3 Mn2 O3 C18 -6.7(4) . . . . ? O1 Mn2 O3 C18 168.5(4) . . . . ? Mn2 Mn2 O3 C18 132.0(4) 2_656 . . . ? O1 Mn2 O3 Mn1 -80.19(16) 2_656 . . . ? N2 Mn2 O3 Mn1 93.38(17) . . . . ? N3 Mn2 O3 Mn1 -176.41(17) . . . . ? O1 Mn2 O3 Mn1 -1.14(13) . . . . ? Mn2 Mn2 O3 Mn1 -37.62(13) 2_656 . . . ? O2 Mn1 O3 C18 -101.9(4) 2_656 . . . ? O12 Mn1 O3 C18 40.4(4) . . . . ? N1 Mn1 O3 C18 126.2(4) . . . . ? O11 Mn1 O3 C18 -16.1(4) . . . . ? O1 Mn1 O3 C18 -167.8(4) . . . . ? O2 Mn1 O3 Mn2 66.99(16) 2_656 . . . ? O12 Mn1 O3 Mn2 -150.74(19) . . . . ? N1 Mn1 O3 Mn2 -64.86(17) . . . . ? O11 Mn1 O3 Mn2 152.76(18) . . . . ? O1 Mn1 O3 Mn2 1.13(13) . . . . ? O2 Mn1 O11 C21 177.8(4) 2_656 . . . ? OW1 Mn1 O11 C21 -95.6(4) . . . . ? O3 Mn1 O11 C21 84.6(4) . . . . ? O12 Mn1 O11 C21 -1.6(3) . . . . ? N1 Mn1 O11 C21 -16.3(5) . . . . ? O1 Mn1 O11 C21 139.9(3) . . . . ? O2 Mn1 O12 C21 0.6(5) 2_656 . . . ? OW1 Mn1 O12 C21 90.1(4) . . . . ? O3 Mn1 O12 C21 -90.0(4) . . . . ? N1 Mn1 O12 C21 172.6(4) . . . . ? O11 Mn1 O12 C21 1.6(4) . . . . ? O1 Mn1 O12 C21 -141.6(4) . . . . ? O2 Mn1 N1 C1 -23.3(5) 2_656 . . . ? OW1 Mn1 N1 C1 -102.5(4) . . . . ? O3 Mn1 N1 C1 77.3(4) . . . . ? O12 Mn1 N1 C1 163.2(4) . . . . ? O11 Mn1 N1 C1 175.5(3) . . . . ? O1 Mn1 N1 C1 9.2(4) . . . . ? O2 Mn1 N1 C5 155.6(4) 2_656 . . . ? OW1 Mn1 N1 C5 76.4(5) . . . . ? O3 Mn1 N1 C5 -103.9(5) . . . . ? O12 Mn1 N1 C5 -18.0(5) . . . . ? O11 Mn1 N1 C5 -5.7(6) . . . . ? O1 Mn1 N1 C5 -172.0(5) . . . . ? O2 Mn2 N2 C11 -177.6(5) . . . . ? O3 Mn2 N2 C11 3.8(5) . . . . ? O1 Mn2 N2 C11 160.0(5) 2_656 . . . ? N3 Mn2 N2 C11 -75.6(5) . . . . ? O1 Mn2 N2 C11 86.0(4) . . . . ? Mn2 Mn2 N2 C11 98.3(4) 2_656 . . . ? O2 Mn2 N2 C7 2.5(4) . . . . ? O3 Mn2 N2 C7 -176.1(4) . . . . ? O1 Mn2 N2 C7 -19.9(8) 2_656 . . . ? N3 Mn2 N2 C7 104.5(4) . . . . ? O1 Mn2 N2 C7 -93.9(4) . . . . ? Mn2 Mn2 N2 C7 -81.6(4) 2_656 . . . ? O2 Mn2 N3 C13 -177.6(3) . . . . ? O3 Mn2 N3 C13 4.4(3) . . . . ? O1 Mn2 N3 C13 -92.4(3) 2_656 . . . ? N2 Mn2 N3 C13 100.8(3) . . . . ? O1 Mn2 N3 C13 -9.7(6) . . . . ? Mn2 Mn2 N3 C13 -72.4(4) 2_656 . . . ? O2 Mn2 N3 C17 0.5(4) . . . . ? O3 Mn2 N3 C17 -177.5(4) . . . . ? O1 Mn2 N3 C17 85.7(4) 2_656 . . . ? N2 Mn2 N3 C17 -81.1(4) . . . . ? O1 Mn2 N3 C17 168.4(4) . . . . ? Mn2 Mn2 N3 C17 105.7(4) 2_656 . . . ? C5 N1 C1 C2 3.2(8) . . . . ? Mn1 N1 C1 C2 -177.8(4) . . . . ? C5 N1 C1 C6 -176.3(5) . . . . ? Mn1 N1 C1 C6 2.6(6) . . . . ? N1 C1 C2 C3 -2.6(9) . . . . ? C6 C1 C2 C3 177.0(5) . . . . ? C1 C2 C3 C4 0.5(10) . . . . ? C2 C3 C4 C5 0.6(11) . . . . ? C1 N1 C5 C4 -2.1(10) . . . . ? Mn1 N1 C5 C4 179.0(6) . . . . ? C3 C4 C5 N1 0.2(11) . . . . ? Mn2 O1 C6 C1 151.1(3) 2_656 . . . ? Mn2 O1 C6 C1 -83.5(4) . . . . ? Mn1 O1 C6 C1 28.0(5) . . . . ? N1 C1 C6 O1 -20.3(6) . . . . ? C2 C1 C6 O1 160.1(4) . . . . ? C11 N2 C7 C8 0.1(8) . . . . ? Mn2 N2 C7 C8 -180.0(5) . . . . ? C11 N2 C7 C12 179.7(5) . . . . ? Mn2 N2 C7 C12 -0.4(6) . . . . ? N2 C7 C8 C9 0.4(10) . . . . ? C12 C7 C8 C9 -179.1(7) . . . . ? C7 C8 C9 C10 -0.6(12) . . . . ? C8 C9 C10 C11 0.2(12) . . . . ? C7 N2 C11 C10 -0.6(9) . . . . ? Mn2 N2 C11 C10 179.6(5) . . . . ? C9 C10 C11 N2 0.4(10) . . . . ? Mn2 O2 C12 C7 5.0(7) . . . . ? Mn1 O2 C12 C7 170.1(3) 2_656 . . . ? N2 C7 C12 O2 -2.7(7) . . . . ? C8 C7 C12 O2 176.8(6) . . . . ? C17 N3 C13 C14 0.4(8) . . . . ? Mn2 N3 C13 C14 178.7(5) . . . . ? C17 N3 C13 C18 -179.9(5) . . . . ? Mn2 N3 C13 C18 -1.5(5) . . . . ? N3 C13 C14 C15 -0.8(10) . . . . ? C18 C13 C14 C15 179.5(6) . . . . ? C13 C14 C15 C16 1.4(11) . . . . ? C14 C15 C16 C17 -1.5(11) . . . . ? C13 N3 C17 C16 -0.5(8) . . . . ? Mn2 N3 C17 C16 -178.6(4) . . . . ? C15 C16 C17 N3 1.1(10) . . . . ? Mn2 O3 C18 C13 7.8(6) . . . . ? Mn1 O3 C18 C13 175.7(3) . . . . ? N3 C13 C18 O3 -3.3(7) . . . . ? C14 C13 C18 O3 176.4(5) . . . . ? Mn1 O12 C21 O11 -2.8(6) . . . . ? Mn1 O12 C21 C22 175.0(5) . . . . ? Mn1 O11 C21 O12 2.8(6) . . . . ? Mn1 O11 C21 C22 -175.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.999 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.084 # Attachment 'Dalton2-LL406-B.CIF' data_ll406-b _database_code_depnum_ccdc_archive 'CCDC 616294' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Cl8 Mn4 N6 O20' _chemical_formula_weight 1428.14 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' 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' _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 11.169(2) _cell_length_b 11.475(2) _cell_length_c 12.184(3) _cell_angle_alpha 80.32(3) _cell_angle_beta 70.54(2) _cell_angle_gamma 65.73(3) _cell_volume 1341.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 1.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.64 _exptl_absorpt_process_details MULABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8723 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.43 _reflns_number_total 5865 _reflns_number_gt 4317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. All non hydrogens were refined anisotropically. Hydrogens were fixed at calculated positions on their riding atom except for the water molecules hydrogens. Those on O1w were found in difference Fourier maps and refined with distance restrains, while the rest could not be found nor fixed and is therefore missing from the structural model. ; _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^)+(0.0370P)^2^+0.6212P] 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 5865 _refine_ls_number_parameters 358 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.04204(4) 0.66894(4) 0.61512(4) 0.04046(13) Uani 1 1 d . . . Mn2 Mn 0.11658(4) 0.38164(4) 0.54541(4) 0.03575(12) Uani 1 1 d . . . Cl1 Cl 0.39610(9) 0.49800(10) 0.82919(9) 0.0767(3) Uani 1 1 d . . . Cl2 Cl 0.25713(11) 0.70943(12) 0.98071(11) 0.0915(4) Uani 1 1 d . . . Cl3 Cl 0.13034(12) 0.53367(13) 0.99267(9) 0.0894(3) Uani 1 1 d . . . Cl10 Cl 0.35028(9) 0.81836(9) 0.30059(10) 0.0716(3) Uani 1 1 d . . . O1W O 0.0792(3) 0.8430(2) 0.5853(2) 0.0696(7) Uani 1 1 d D . . HW1A H 0.092(4) 0.850(4) 0.647(2) 0.084 Uiso 1 1 d D . . HW2A H 0.130(4) 0.859(4) 0.523(2) 0.084 Uiso 1 1 d D . . O1 O -0.05559(18) 0.53097(17) 0.61239(15) 0.0374(4) Uani 1 1 d . . . O2 O 0.20303(18) 0.49114(17) 0.54268(18) 0.0427(5) Uani 1 1 d . . . O3 O 0.03444(19) 0.27178(17) 0.53764(17) 0.0421(4) Uani 1 1 d . . . O4 O 0.1444(3) 0.6213(2) 0.7467(2) 0.0643(6) Uani 1 1 d . . . O5 O 0.1327(3) 0.8044(2) 0.7930(2) 0.0748(7) Uani 1 1 d . . . O101 O 0.3051(4) 0.8467(3) 0.1996(3) 0.1030(10) Uani 1 1 d . . . O102 O 0.2561(3) 0.9159(2) 0.3834(2) 0.0791(8) Uani 1 1 d . . . O103 O 0.3459(3) 0.6990(3) 0.3518(3) 0.1116(12) Uani 1 1 d . . . O104 O 0.4836(3) 0.8175(4) 0.2726(4) 0.1318(15) Uani 1 1 d . . . N1 N -0.1647(3) 0.7265(2) 0.7517(2) 0.0463(6) Uani 1 1 d . . . N2 N 0.3167(2) 0.2652(2) 0.4643(2) 0.0405(5) Uani 1 1 d . . . N3 N 0.1262(2) 0.2738(2) 0.7086(2) 0.0448(6) Uani 1 1 d . . . C1 C -0.2328(3) 0.6480(3) 0.7763(3) 0.0456(7) Uani 1 1 d . . . C2 C -0.3611(3) 0.6777(3) 0.8566(3) 0.0580(8) Uani 1 1 d . . . H2A H -0.4074 0.6206 0.8726 0.070 Uiso 1 1 calc R . . C3 C -0.4213(4) 0.7911(4) 0.9134(3) 0.0662(9) Uani 1 1 d . . . H3A H -0.5088 0.8126 0.9701 0.079 Uiso 1 1 calc R . . C4 C -0.3527(4) 0.8722(4) 0.8865(3) 0.0690(10) Uani 1 1 d . . . H4A H -0.3929 0.9518 0.9232 0.083 Uiso 1 1 calc R . . C5 C -0.2243(3) 0.8366(3) 0.8054(3) 0.0565(8) Uani 1 1 d . . . H5A H -0.1769 0.8929 0.7874 0.068 Uiso 1 1 calc R . . C6 C -0.1620(3) 0.5232(3) 0.7144(3) 0.0470(7) Uani 1 1 d . . . H6A H -0.1225 0.4530 0.7672 0.056 Uiso 1 1 calc R . . H6B H -0.2297 0.5041 0.6927 0.056 Uiso 1 1 calc R . . C7 C 0.4084(3) 0.3153(3) 0.4594(3) 0.0431(6) Uani 1 1 d . . . C8 C 0.5463(3) 0.2515(3) 0.4077(3) 0.0611(9) Uani 1 1 d . . . H8A H 0.6101 0.2877 0.4047 0.073 Uiso 1 1 calc R . . C9 C 0.5913(4) 0.1346(4) 0.3603(3) 0.0687(10) Uani 1 1 d . . . H9A H 0.6864 0.0899 0.3238 0.082 Uiso 1 1 calc R . . C10 C 0.4976(4) 0.0830(3) 0.3663(3) 0.0598(9) Uani 1 1 d . . . H10A H 0.5271 0.0024 0.3342 0.072 Uiso 1 1 calc R . . C11 C 0.3615(3) 0.1496(3) 0.4190(3) 0.0476(7) Uani 1 1 d . . . H11A H 0.2967 0.1138 0.4240 0.057 Uiso 1 1 calc R . . C12 C 0.3483(3) 0.4419(3) 0.5138(3) 0.0475(7) Uani 1 1 d . . . H12A H 0.3760 0.4322 0.5851 0.057 Uiso 1 1 calc R . . H12B H 0.3837 0.5024 0.4589 0.057 Uiso 1 1 calc R . . C13 C 0.0736(3) 0.1851(3) 0.7232(3) 0.0469(7) Uani 1 1 d . . . C14 C 0.0776(4) 0.0988(3) 0.8175(3) 0.0657(10) Uani 1 1 d . . . H14A H 0.0389 0.0364 0.8280 0.079 Uiso 1 1 calc R . . C15 C 0.1389(5) 0.1060(4) 0.8955(4) 0.0866(13) Uani 1 1 d . . . H15A H 0.1440 0.0472 0.9604 0.104 Uiso 1 1 calc R . . C16 C 0.1925(5) 0.1968(5) 0.8803(4) 0.0862(13) Uani 1 1 d . . . H16A H 0.2346 0.2022 0.9344 0.103 Uiso 1 1 calc R . . C17 C 0.1850(4) 0.2795(4) 0.7868(3) 0.0633(9) Uani 1 1 d . . . H17A H 0.2222 0.3430 0.7761 0.076 Uiso 1 1 calc R . . C18 C 0.0110(4) 0.1865(3) 0.6318(3) 0.0638(9) Uani 1 1 d . . . H18A H 0.0496 0.0992 0.6024 0.077 Uiso 1 1 calc R . . H18B H -0.0893 0.2108 0.6672 0.077 Uiso 1 1 calc R . . C19 C 0.1634(3) 0.6893(3) 0.8034(3) 0.0491(7) Uani 1 1 d . . . C20 C 0.2340(3) 0.6128(3) 0.8982(3) 0.0560(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0431(2) 0.0345(2) 0.0471(3) -0.00667(18) -0.0158(2) -0.01410(19) Mn2 0.0349(2) 0.0310(2) 0.0420(3) -0.00296(17) -0.01159(18) -0.01241(18) Cl1 0.0557(5) 0.0802(6) 0.0812(7) -0.0221(5) -0.0244(5) -0.0029(5) Cl2 0.0838(7) 0.1125(8) 0.0951(8) -0.0471(7) -0.0380(6) -0.0282(6) Cl3 0.0915(7) 0.1285(10) 0.0597(6) 0.0161(6) -0.0237(5) -0.0593(7) Cl10 0.0555(5) 0.0583(5) 0.0951(8) -0.0091(5) -0.0083(5) -0.0245(4) O1W 0.102(2) 0.0653(15) 0.0638(17) 0.0051(14) -0.0293(16) -0.0530(15) O1 0.0364(9) 0.0367(9) 0.0347(10) -0.0061(8) -0.0050(8) -0.0122(8) O2 0.0356(10) 0.0363(10) 0.0577(13) -0.0100(9) -0.0120(9) -0.0134(8) O3 0.0483(11) 0.0360(10) 0.0487(12) 0.0020(8) -0.0173(9) -0.0215(9) O4 0.0859(17) 0.0477(12) 0.0760(17) -0.0041(11) -0.0497(14) -0.0206(12) O5 0.107(2) 0.0557(15) 0.0773(18) -0.0078(13) -0.0393(16) -0.0348(15) O101 0.121(3) 0.113(2) 0.084(2) -0.0087(19) -0.020(2) -0.059(2) O102 0.0809(18) 0.0618(15) 0.0800(18) -0.0106(14) -0.0034(15) -0.0261(14) O103 0.108(2) 0.0551(16) 0.158(3) 0.0097(18) -0.028(2) -0.0320(17) O104 0.0597(18) 0.128(3) 0.203(4) -0.038(3) -0.006(2) -0.045(2) N1 0.0493(14) 0.0428(13) 0.0443(14) -0.0080(11) -0.0158(12) -0.0110(12) N2 0.0440(13) 0.0357(12) 0.0428(13) -0.0012(10) -0.0172(11) -0.0128(11) N3 0.0441(13) 0.0400(13) 0.0469(15) -0.0014(11) -0.0140(11) -0.0121(11) C1 0.0460(16) 0.0441(16) 0.0398(16) -0.0024(13) -0.0131(13) -0.0098(14) C2 0.0483(18) 0.064(2) 0.051(2) -0.0036(16) -0.0038(15) -0.0190(17) C3 0.0509(19) 0.070(2) 0.055(2) -0.0136(18) 0.0005(16) -0.0091(18) C4 0.070(2) 0.061(2) 0.063(2) -0.0241(18) -0.0154(19) -0.0074(19) C5 0.0562(19) 0.0509(18) 0.056(2) -0.0163(16) -0.0148(16) -0.0097(16) C6 0.0480(17) 0.0460(16) 0.0420(17) -0.0017(13) -0.0049(13) -0.0195(14) C7 0.0400(15) 0.0418(15) 0.0459(17) 0.0001(13) -0.0130(13) -0.0145(13) C8 0.0409(17) 0.061(2) 0.074(2) -0.0124(18) -0.0081(16) -0.0161(16) C9 0.0455(18) 0.064(2) 0.074(3) -0.0173(19) -0.0050(17) -0.0035(17) C10 0.067(2) 0.0434(17) 0.058(2) -0.0106(15) -0.0202(18) -0.0067(17) C11 0.0563(18) 0.0350(14) 0.0518(18) -0.0022(13) -0.0234(15) -0.0117(14) C12 0.0361(15) 0.0455(16) 0.063(2) -0.0084(14) -0.0135(14) -0.0156(13) C13 0.0476(17) 0.0350(14) 0.0476(18) -0.0033(13) -0.0085(14) -0.0091(13) C14 0.081(3) 0.0455(18) 0.054(2) 0.0058(16) -0.0080(19) -0.0209(18) C15 0.107(3) 0.078(3) 0.051(2) 0.014(2) -0.025(2) -0.016(3) C16 0.097(3) 0.103(3) 0.059(3) 0.008(2) -0.041(2) -0.029(3) C17 0.062(2) 0.076(2) 0.055(2) -0.0055(18) -0.0217(18) -0.0253(19) C18 0.089(3) 0.060(2) 0.064(2) 0.0138(17) -0.030(2) -0.050(2) C19 0.0460(17) 0.0520(18) 0.0499(19) -0.0160(15) -0.0111(14) -0.0164(15) C20 0.0487(17) 0.067(2) 0.055(2) -0.0173(16) -0.0156(15) -0.0179(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 2.143(2) . ? Mn1 O1W 2.152(2) . ? Mn1 O2 2.169(2) . ? Mn1 O3 2.194(2) 2_566 ? Mn1 N1 2.257(3) . ? Mn1 O1 2.2710(18) . ? Mn1 Mn2 3.2398(10) . ? Mn2 O2 1.8639(18) . ? Mn2 O3 1.8677(18) . ? Mn2 O1 2.004(2) . ? Mn2 N2 2.067(3) . ? Mn2 N3 2.168(2) . ? Mn2 O1 2.197(2) 2_566 ? Mn2 Mn2 3.2368(15) 2_566 ? Cl1 C20 1.766(3) . ? Cl2 C20 1.758(3) . ? Cl3 C20 1.765(4) . ? Cl10 O104 1.408(3) . ? Cl10 O103 1.419(3) . ? Cl10 O101 1.421(3) . ? Cl10 O102 1.443(3) . ? O1W HW1A 0.831(19) . ? O1W HW2A 0.830(19) . ? O1 C6 1.425(3) . ? O1 Mn2 2.197(2) 2_566 ? O2 C12 1.417(3) . ? O3 C18 1.405(4) . ? O3 Mn1 2.194(2) 2_566 ? O4 C19 1.243(3) . ? O5 C19 1.216(4) . ? N1 C5 1.328(4) . ? N1 C1 1.341(4) . ? N2 C7 1.347(3) . ? N2 C11 1.353(4) . ? N3 C13 1.332(4) . ? N3 C17 1.347(4) . ? C1 C2 1.381(4) . ? C1 C6 1.510(4) . ? C2 C3 1.377(5) . ? C2 H2A 0.9500 . ? C3 C4 1.370(5) . ? C3 H3A 0.9500 . ? C4 C5 1.382(5) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.374(4) . ? C7 C12 1.492(4) . ? C8 C9 1.378(5) . ? C8 H8A 0.9500 . ? C9 C10 1.377(5) . ? C9 H9A 0.9500 . ? C10 C11 1.367(5) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.385(4) . ? C13 C18 1.494(5) . ? C14 C15 1.373(6) . ? C14 H14A 0.9500 . ? C15 C16 1.361(6) . ? C15 H15A 0.9500 . ? C16 C17 1.357(5) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.556(5) . ? 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 O1W 86.25(10) . . ? O4 Mn1 O2 83.21(9) . . ? O1W Mn1 O2 120.82(10) . . ? O4 Mn1 O3 170.25(9) . 2_566 ? O1W Mn1 O3 86.68(9) . 2_566 ? O2 Mn1 O3 94.68(8) . 2_566 ? O4 Mn1 N1 90.93(10) . . ? O1W Mn1 N1 101.87(11) . . ? O2 Mn1 N1 136.24(8) . . ? O3 Mn1 N1 97.09(8) 2_566 . ? O4 Mn1 O1 113.65(8) . . ? O1W Mn1 O1 158.77(9) . . ? O2 Mn1 O1 71.17(7) . . ? O3 Mn1 O1 74.34(7) 2_566 . ? N1 Mn1 O1 71.82(8) . . ? O4 Mn1 Mn2 98.56(6) . . ? O1W Mn1 Mn2 151.25(8) . . ? O2 Mn1 Mn2 33.45(5) . . ? O3 Mn1 Mn2 84.53(6) 2_566 . ? N1 Mn1 Mn2 106.35(7) . . ? O1 Mn1 Mn2 37.73(5) . . ? O2 Mn2 O3 176.29(9) . . ? O2 Mn2 O1 83.81(8) . . ? O3 Mn2 O1 97.86(8) . . ? O2 Mn2 N2 81.16(9) . . ? O3 Mn2 N2 96.91(9) . . ? O1 Mn2 N2 164.42(8) . . ? O2 Mn2 N3 102.68(9) . . ? O3 Mn2 N3 80.46(9) . . ? O1 Mn2 N3 96.49(9) . . ? N2 Mn2 N3 90.81(10) . . ? O2 Mn2 O1 94.34(8) . 2_566 ? O3 Mn2 O1 82.75(8) . 2_566 ? O1 Mn2 O1 79.31(8) . 2_566 ? N2 Mn2 O1 97.71(9) . 2_566 ? N3 Mn2 O1 161.97(8) . 2_566 ? O2 Mn2 Mn2 89.12(6) . 2_566 ? O3 Mn2 Mn2 89.94(6) . 2_566 ? O1 Mn2 Mn2 41.84(6) . 2_566 ? N2 Mn2 Mn2 133.43(7) . 2_566 ? N3 Mn2 Mn2 135.69(7) . 2_566 ? O1 Mn2 Mn2 37.47(5) 2_566 2_566 ? O2 Mn2 Mn1 39.91(6) . . ? O3 Mn2 Mn1 141.72(6) . . ? O1 Mn2 Mn1 43.91(5) . . ? N2 Mn2 Mn1 121.01(7) . . ? N3 Mn2 Mn1 102.38(7) . . ? O1 Mn2 Mn1 86.85(5) 2_566 . ? Mn2 Mn2 Mn1 61.09(3) 2_566 . ? O104 Cl10 O103 111.0(2) . . ? O104 Cl10 O101 110.6(2) . . ? O103 Cl10 O101 109.6(2) . . ? O104 Cl10 O102 109.5(2) . . ? O103 Cl10 O102 108.0(2) . . ? O101 Cl10 O102 108.1(2) . . ? Mn1 O1W HW1A 103(3) . . ? Mn1 O1W HW2A 122(3) . . ? HW1A O1W HW2A 119(4) . . ? C6 O1 Mn2 124.26(16) . . ? C6 O1 Mn2 116.90(16) . 2_566 ? Mn2 O1 Mn2 100.69(8) . 2_566 ? C6 O1 Mn1 116.41(16) . . ? Mn2 O1 Mn1 98.36(7) . . ? Mn2 O1 Mn1 94.88(7) 2_566 . ? C12 O2 Mn2 118.98(16) . . ? C12 O2 Mn1 133.57(16) . . ? Mn2 O2 Mn1 106.64(8) . . ? C18 O3 Mn2 119.70(18) . . ? C18 O3 Mn1 131.26(17) . 2_566 ? Mn2 O3 Mn1 108.02(9) . 2_566 ? C19 O4 Mn1 131.5(2) . . ? C5 N1 C1 118.5(3) . . ? C5 N1 Mn1 123.0(2) . . ? C1 N1 Mn1 118.37(19) . . ? C7 N2 C11 119.4(3) . . ? C7 N2 Mn2 112.88(18) . . ? C11 N2 Mn2 127.7(2) . . ? C13 N3 C17 119.5(3) . . ? C13 N3 Mn2 111.17(19) . . ? C17 N3 Mn2 129.2(2) . . ? N1 C1 C2 121.9(3) . . ? N1 C1 C6 117.3(3) . . ? C2 C1 C6 120.7(3) . . ? C3 C2 C1 119.2(3) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 122.4(3) . . ? N1 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? O1 C6 C1 110.1(2) . . ? O1 C6 H6A 109.6 . . ? C1 C6 H6A 109.6 . . ? O1 C6 H6B 109.6 . . ? C1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C8 121.0(3) . . ? N2 C7 C12 115.0(2) . . ? C8 C7 C12 124.0(3) . . ? C7 C8 C9 119.5(3) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C11 C10 C9 119.0(3) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? N2 C11 C10 121.7(3) . . ? N2 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? O2 C12 C7 110.2(2) . . ? O2 C12 H12A 109.6 . . ? C7 C12 H12A 109.6 . . ? O2 C12 H12B 109.6 . . ? C7 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N3 C13 C14 121.3(3) . . ? N3 C13 C18 115.4(3) . . ? C14 C13 C18 123.3(3) . . ? C15 C14 C13 118.2(4) . . ? C15 C14 H14A 120.9 . . ? C13 C14 H14A 120.9 . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C17 C16 C15 119.0(4) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? N3 C17 C16 121.7(4) . . ? N3 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? O3 C18 C13 112.8(2) . . ? O3 C18 H18A 109.0 . . ? C13 C18 H18A 109.0 . . ? O3 C18 H18B 109.0 . . ? C13 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O5 C19 O4 127.7(3) . . ? O5 C19 C20 118.9(3) . . ? O4 C19 C20 113.4(3) . . ? C19 C20 Cl2 113.5(2) . . ? C19 C20 Cl3 108.0(2) . . ? Cl2 C20 Cl3 108.79(19) . . ? C19 C20 Cl1 108.6(2) . . ? Cl2 C20 Cl1 108.74(17) . . ? Cl3 C20 Cl1 109.18(19) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.358 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.063 # Attachment 'Dalton3-LL296B.CIF' data_ll296b _database_code_depnum_ccdc_archive 'CCDC 616295' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H62 Cl2 Mn4 N10 O22' _chemical_formula_weight 1541.84 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.484(3) _cell_length_b 24.639(5) _cell_length_c 10.849(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.80(3) _cell_angle_gamma 90.00 _cell_volume 3369.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details MULABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21012 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.71 _reflns_number_total 7609 _reflns_number_gt 5111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. All non hydrogens were refined anisotropically. The perchlorate anion was disordered and refined with displacement parameters and distance constrains. Hydrogens were placed geometrically on their riding atom except for the water ones (O200) that were found in difference Fourier map and refined with distance restrains. ; _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^)+(0.0383P)^2^+1.6936P] 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 7609 _refine_ls_number_parameters 459 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.035 _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 0.62662(3) 0.455024(17) 0.25776(4) 0.02009(12) Uani 1 1 d . . . Mn2 Mn 0.51054(3) 0.445074(16) -0.07482(4) 0.01809(11) Uani 1 1 d . . . C1 C 0.7083(2) 0.37658(11) -0.0396(3) 0.0252(6) Uani 1 1 d . . . H1 H 0.6936 0.3583 0.0290 0.030 Uiso 1 1 calc R . . C2 C 0.7975(2) 0.36293(12) -0.0649(3) 0.0308(7) Uani 1 1 d . . . H2 H 0.8439 0.3355 -0.0150 0.037 Uiso 1 1 calc R . . C3 C 0.8189(2) 0.39002(13) -0.1651(3) 0.0332(7) Uani 1 1 d . . . H3 H 0.8812 0.3818 -0.1833 0.040 Uiso 1 1 calc R . . C4 C 0.7491(2) 0.42885(13) -0.2377(3) 0.0298(7) Uani 1 1 d . . . H4 H 0.7620 0.4473 -0.3074 0.036 Uiso 1 1 calc R . . C5 C 0.6599(2) 0.44063(12) -0.2079(3) 0.0229(6) Uani 1 1 d . . . C6 C 0.5781(2) 0.48143(12) -0.2816(3) 0.0254(6) Uani 1 1 d . . . H6A H 0.6117 0.5175 -0.2761 0.030 Uiso 1 1 calc R . . H6B H 0.5472 0.4710 -0.3757 0.030 Uiso 1 1 calc R . . C7 C 0.3611(2) 0.35345(12) -0.2730(3) 0.0267(7) Uani 1 1 d . . . H7 H 0.3547 0.3773 -0.3442 0.032 Uiso 1 1 calc R . . C8 C 0.3152(2) 0.30301(14) -0.2998(3) 0.0355(8) Uani 1 1 d . . . H8 H 0.2762 0.2925 -0.3881 0.043 Uiso 1 1 calc R . . C9 C 0.3262(3) 0.26768(14) -0.1968(3) 0.0385(8) Uani 1 1 d . . . H9 H 0.2966 0.2323 -0.2134 0.046 Uiso 1 1 calc R . . C10 C 0.3806(2) 0.28454(13) -0.0705(3) 0.0336(7) Uani 1 1 d . . . H10 H 0.3888 0.2609 0.0016 0.040 Uiso 1 1 calc R . . C11 C 0.4236(2) 0.33643(11) -0.0482(3) 0.0238(6) Uani 1 1 d . . . C12 C 0.4789(2) 0.35912(12) 0.0868(3) 0.0272(7) Uani 1 1 d . . . H12A H 0.4260 0.3663 0.1289 0.033 Uiso 1 1 calc R . . H12B H 0.5297 0.3319 0.1412 0.033 Uiso 1 1 calc R . . C13 C 0.8591(2) 0.41887(12) 0.2715(3) 0.0277(7) Uani 1 1 d . . . H13 H 0.8500 0.3929 0.3312 0.033 Uiso 1 1 calc R . . C14 C 0.9531(2) 0.41932(13) 0.2493(3) 0.0322(7) Uani 1 1 d . . . H14 H 1.0078 0.3941 0.2924 0.039 Uiso 1 1 calc R . . C15 C 0.9666(2) 0.45730(13) 0.1628(3) 0.0329(7) Uani 1 1 d . . . H15 H 1.0314 0.4590 0.1467 0.039 Uiso 1 1 calc R . . C16 C 0.8851(2) 0.49272(13) 0.1003(3) 0.0297(7) Uani 1 1 d . . . H16 H 0.8926 0.5188 0.0397 0.036 Uiso 1 1 calc R . . C17 C 0.7917(2) 0.48976(11) 0.1270(3) 0.0217(6) Uani 1 1 d . . . C18 C 0.7015(2) 0.52816(12) 0.0619(3) 0.0237(6) Uani 1 1 d . . . H18A H 0.7184 0.5642 0.1044 0.028 Uiso 1 1 calc R . . H18B H 0.6927 0.5324 -0.0322 0.028 Uiso 1 1 calc R . . CB1 C 0.6199(2) 0.37700(12) 0.4318(3) 0.0241(6) Uani 1 1 d . . . CB2 C 0.6410(2) 0.33146(11) 0.5302(3) 0.0242(6) Uani 1 1 d . . . CB3 C 0.5757(2) 0.32320(13) 0.6028(3) 0.0295(7) Uani 1 1 d . . . HB3 H 0.5158 0.3459 0.5891 0.035 Uiso 1 1 calc R . . CB4 C 0.5978(3) 0.28187(13) 0.6953(3) 0.0365(8) Uani 1 1 d . . . HB4 H 0.5538 0.2767 0.7459 0.044 Uiso 1 1 calc R . . CB5 C 0.6837(3) 0.24810(13) 0.7141(3) 0.0365(8) Uani 1 1 d . . . HB5 H 0.6979 0.2194 0.7764 0.044 Uiso 1 1 calc R . . CB6 C 0.7489(3) 0.25618(12) 0.6425(3) 0.0336(7) Uani 1 1 d . . . HB6 H 0.8078 0.2328 0.6551 0.040 Uiso 1 1 calc R . . CB7 C 0.7289(2) 0.29828(12) 0.5521(3) 0.0276(7) Uani 1 1 d . . . HB7 H 0.7754 0.3044 0.5050 0.033 Uiso 1 1 calc R . . C100 C 0.0046(3) 0.26533(18) 0.3889(4) 0.0551(10) Uani 1 1 d . . . C101 C 0.0405(3) 0.23235(17) 0.3022(4) 0.0586(11) Uani 1 1 d . . . H10A H -0.0115 0.2036 0.2631 0.088 Uiso 1 1 calc R . . H10B H 0.1091 0.2160 0.3529 0.088 Uiso 1 1 calc R . . H10C H 0.0481 0.2552 0.2321 0.088 Uiso 1 1 calc R . . C200 C 0.9880(3) 0.43433(16) 0.6100(3) 0.0415(8) Uani 1 1 d . . . C201 C 1.0870(3) 0.40411(16) 0.6437(4) 0.0505(10) Uani 1 1 d . . . H20A H 1.0750 0.3710 0.5905 0.076 Uiso 1 1 calc R . . H20B H 1.1122 0.3945 0.7375 0.076 Uiso 1 1 calc R . . H20C H 1.1404 0.4266 0.6259 0.076 Uiso 1 1 calc R . . N200 N 0.9111(2) 0.45787(15) 0.5830(3) 0.0535(9) Uani 1 1 d . . . Cl10 Cl 0.16185(6) 0.36134(3) 0.10367(9) 0.0418(2) Uani 1 1 d D . . O104 O 0.2125(2) 0.41032(10) 0.1649(2) 0.0559(7) Uani 1 1 d D A . O102 O 0.23270(19) 0.32649(12) 0.0711(3) 0.0598(7) Uani 1 1 d D A . O101 O 0.0879(8) 0.3807(5) -0.0230(10) 0.074(4) Uani 0.50 1 d PDU A 1 O100 O 0.1041(11) 0.3333(7) 0.1709(14) 0.111(5) Uani 0.50 1 d PDU A 1 O111 O 0.0649(9) 0.3703(6) 0.0040(13) 0.100(4) Uani 0.50 1 d PDU A 2 O110 O 0.1501(11) 0.3366(7) 0.2171(14) 0.110(5) Uani 0.50 1 d PDU A 2 N100 N -0.0244(3) 0.29167(18) 0.4546(4) 0.0821(12) Uani 1 1 d . . . O1 O 0.60562(13) 0.50874(7) 0.07158(17) 0.0187(4) Uani 1 1 d . . . O2 O 0.53370(14) 0.40754(7) 0.08378(17) 0.0214(4) Uani 1 1 d . . . OB2 O 0.68252(15) 0.38150(8) 0.36856(18) 0.0288(5) Uani 1 1 d . . . O7 O 0.71843(16) 0.50864(9) 0.42478(19) 0.0328(5) Uani 1 1 d . . . OB1 O 0.54333(16) 0.40901(8) 0.4133(2) 0.0321(5) Uani 1 1 d . . . N3 N 0.77902(17) 0.45359(9) 0.2125(2) 0.0222(5) Uani 1 1 d . . . N2 N 0.41517(17) 0.37020(9) -0.1489(2) 0.0222(5) Uani 1 1 d . . . N1 N 0.64058(17) 0.41517(9) -0.1088(2) 0.0204(5) Uani 1 1 d . . . O3 O 0.49701(14) 0.48425(7) -0.22747(17) 0.0219(4) Uani 1 1 d . . . O200 O 0.65018(18) 0.58722(9) 0.5550(2) 0.0356(5) Uani 1 1 d D . . H201 H 0.704(2) 0.5927(14) 0.629(2) 0.043 Uiso 1 1 d D . . H202 H 0.5871(17) 0.5851(14) 0.561(3) 0.043 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0213(2) 0.0213(2) 0.0179(2) 0.00235(17) 0.00736(17) 0.00357(18) Mn2 0.0194(2) 0.0176(2) 0.0180(2) 0.00144(17) 0.00758(16) 0.00205(17) C1 0.0279(15) 0.0212(15) 0.0250(15) 0.0003(12) 0.0076(12) 0.0049(12) C2 0.0279(16) 0.0278(17) 0.0352(17) -0.0019(14) 0.0093(13) 0.0084(13) C3 0.0267(16) 0.0404(19) 0.0347(18) -0.0057(15) 0.0135(13) 0.0064(14) C4 0.0275(16) 0.0413(19) 0.0236(16) 0.0004(14) 0.0127(13) 0.0015(14) C5 0.0235(15) 0.0264(16) 0.0184(14) -0.0026(12) 0.0069(11) 0.0010(12) C6 0.0268(15) 0.0323(17) 0.0210(14) 0.0053(13) 0.0133(12) 0.0048(13) C7 0.0256(15) 0.0306(17) 0.0245(16) -0.0051(13) 0.0097(12) 0.0014(13) C8 0.0260(16) 0.043(2) 0.0360(18) -0.0169(16) 0.0094(14) -0.0064(14) C9 0.0378(19) 0.0307(18) 0.049(2) -0.0134(16) 0.0184(16) -0.0098(15) C10 0.0372(18) 0.0252(17) 0.0399(19) -0.0010(14) 0.0158(15) -0.0046(14) C11 0.0227(15) 0.0197(15) 0.0311(16) -0.0014(12) 0.0121(12) -0.0023(12) C12 0.0362(17) 0.0221(15) 0.0227(15) 0.0034(12) 0.0095(12) -0.0073(13) C13 0.0288(16) 0.0294(17) 0.0249(16) 0.0031(13) 0.0095(12) 0.0089(13) C14 0.0271(16) 0.0381(19) 0.0295(17) 0.0008(14) 0.0077(13) 0.0095(14) C15 0.0216(15) 0.044(2) 0.0361(18) -0.0013(15) 0.0139(13) 0.0046(14) C16 0.0280(16) 0.0304(17) 0.0328(17) 0.0008(14) 0.0134(13) 0.0012(13) C17 0.0215(14) 0.0217(15) 0.0218(15) -0.0025(12) 0.0074(11) -0.0004(12) C18 0.0235(15) 0.0227(15) 0.0275(15) -0.0002(12) 0.0124(12) -0.0021(12) CB1 0.0286(16) 0.0247(16) 0.0156(14) -0.0004(12) 0.0036(12) -0.0009(13) CB2 0.0283(15) 0.0222(15) 0.0199(14) -0.0016(12) 0.0059(12) -0.0013(12) CB3 0.0302(16) 0.0316(17) 0.0270(16) 0.0026(14) 0.0102(13) 0.0001(13) CB4 0.045(2) 0.0375(19) 0.0298(17) 0.0076(15) 0.0161(15) -0.0074(16) CB5 0.049(2) 0.0277(18) 0.0253(16) 0.0083(14) 0.0039(15) -0.0045(15) CB6 0.0402(19) 0.0255(17) 0.0289(17) 0.0015(14) 0.0045(14) 0.0079(14) CB7 0.0360(17) 0.0279(16) 0.0181(15) 0.0001(12) 0.0085(12) 0.0032(13) C100 0.053(2) 0.053(3) 0.051(2) -0.001(2) 0.007(2) -0.006(2) C101 0.059(3) 0.059(3) 0.062(3) 0.010(2) 0.027(2) 0.001(2) C200 0.0327(19) 0.059(2) 0.0294(18) -0.0073(16) 0.0064(14) -0.0033(18) C201 0.039(2) 0.047(2) 0.061(2) -0.0074(19) 0.0111(18) 0.0038(17) N200 0.0334(17) 0.084(3) 0.0386(17) -0.0077(17) 0.0072(13) 0.0095(17) Cl10 0.0327(4) 0.0318(5) 0.0640(6) 0.0047(4) 0.0210(4) 0.0057(4) O104 0.0560(16) 0.0475(16) 0.0556(16) -0.0046(13) 0.0093(13) -0.0088(13) O102 0.0432(14) 0.072(2) 0.0671(17) -0.0031(15) 0.0226(13) 0.0254(14) O101 0.057(6) 0.036(4) 0.082(5) 0.002(3) -0.033(4) 0.007(4) O100 0.124(11) 0.051(4) 0.228(11) 0.007(7) 0.147(9) -0.009(7) O111 0.035(4) 0.081(8) 0.141(7) -0.062(6) -0.021(5) 0.020(5) O110 0.141(11) 0.057(5) 0.206(10) 0.059(7) 0.155(10) 0.035(7) N100 0.089(3) 0.083(3) 0.063(3) -0.017(2) 0.013(2) 0.012(2) O1 0.0161(9) 0.0199(10) 0.0208(10) 0.0014(8) 0.0073(7) -0.0005(8) O2 0.0260(10) 0.0170(10) 0.0205(10) 0.0017(8) 0.0072(8) -0.0025(8) OB2 0.0352(12) 0.0281(12) 0.0252(11) 0.0082(9) 0.0134(9) 0.0052(9) O7 0.0308(12) 0.0358(13) 0.0277(11) -0.0066(10) 0.0054(9) 0.0003(10) OB1 0.0313(11) 0.0302(12) 0.0356(12) 0.0066(10) 0.0129(9) 0.0099(10) N3 0.0225(12) 0.0247(13) 0.0199(12) 0.0007(10) 0.0080(10) 0.0034(10) N2 0.0223(12) 0.0235(13) 0.0223(12) -0.0013(10) 0.0098(10) 0.0015(10) N1 0.0237(12) 0.0188(12) 0.0188(12) -0.0009(10) 0.0075(9) 0.0011(10) O3 0.0214(10) 0.0251(11) 0.0210(10) 0.0040(8) 0.0098(8) 0.0047(8) O200 0.0342(13) 0.0444(14) 0.0292(12) 0.0001(11) 0.0125(10) 0.0037(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 OB2 2.157(2) . ? Mn1 O3 2.1763(18) 3_665 ? Mn1 O2 2.1959(19) . ? Mn1 O7 2.229(2) . ? Mn1 N3 2.276(2) . ? Mn1 O1 2.3463(18) . ? Mn2 O3 1.8690(18) . ? Mn2 O2 1.8793(18) . ? Mn2 O1 1.9464(18) 3_665 ? Mn2 N1 2.053(2) . ? Mn2 N2 2.229(2) . ? Mn2 O1 2.2761(19) . ? Mn2 Mn2 3.2203(9) 3_665 ? C1 N1 1.347(3) . ? C1 C2 1.367(4) . ? C1 H1 0.9500 . ? C2 C3 1.391(4) . ? C2 H2 0.9500 . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 N1 1.347(3) . ? C5 C6 1.496(4) . ? C6 O3 1.414(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.348(3) . ? C7 C8 1.373(4) . ? C7 H7 0.9500 . ? C8 C9 1.383(5) . ? C8 H8 0.9500 . ? C9 C10 1.369(4) . ? C9 H9 0.9500 . ? C10 C11 1.389(4) . ? C10 H10 0.9500 . ? C11 N2 1.345(3) . ? C11 C12 1.496(4) . ? C12 O2 1.410(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N3 1.348(3) . ? C13 C14 1.372(4) . ? C13 H13 0.9500 . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(4) . ? C15 H15 0.9500 . ? C16 C17 1.392(4) . ? C16 H16 0.9500 . ? C17 N3 1.340(3) . ? C17 C18 1.504(4) . ? C18 O1 1.418(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? CB1 OB1 1.258(3) . ? CB1 OB2 1.268(3) . ? CB1 CB2 1.505(4) . ? CB2 CB3 1.389(4) . ? CB2 CB7 1.389(4) . ? CB3 CB4 1.385(4) . ? CB3 HB3 0.9500 . ? CB4 CB5 1.381(5) . ? CB4 HB4 0.9500 . ? CB5 CB6 1.379(5) . ? CB5 HB5 0.9500 . ? CB6 CB7 1.386(4) . ? CB6 HB6 0.9500 . ? CB7 HB7 0.9500 . ? C100 N100 1.131(5) . ? C100 C101 1.450(6) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C200 N200 1.132(4) . ? C200 C201 1.458(5) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? Cl10 O111 1.387(8) . ? Cl10 O102 1.420(2) . ? Cl10 O100 1.421(7) . ? Cl10 O104 1.429(2) . ? Cl10 O110 1.432(8) . ? Cl10 O101 1.461(6) . ? O1 Mn2 1.9464(18) 3_665 ? O3 Mn1 2.1763(18) 3_665 ? O200 H201 0.879(18) . ? O200 H202 0.877(18) . ? 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 OB2 Mn1 O3 139.37(7) . 3_665 ? OB2 Mn1 O2 90.65(7) . . ? O3 Mn1 O2 93.66(7) 3_665 . ? OB2 Mn1 O7 93.52(8) . . ? O3 Mn1 O7 83.67(8) 3_665 . ? O2 Mn1 O7 175.75(7) . . ? OB2 Mn1 N3 86.76(8) . . ? O3 Mn1 N3 132.84(8) 3_665 . ? O2 Mn1 N3 95.14(8) . . ? O7 Mn1 N3 84.33(8) . . ? OB2 Mn1 O1 149.89(7) . . ? O3 Mn1 O1 68.31(7) 3_665 . ? O2 Mn1 O1 72.72(7) . . ? O7 Mn1 O1 103.17(7) . . ? N3 Mn1 O1 70.45(7) . . ? O3 Mn2 O2 176.06(8) . . ? O3 Mn2 O1 83.57(8) . 3_665 ? O2 Mn2 O1 98.30(8) . 3_665 ? O3 Mn2 N1 81.19(8) . . ? O2 Mn2 N1 96.49(9) . . ? O1 Mn2 N1 163.21(8) 3_665 . ? O3 Mn2 N2 104.24(8) . . ? O2 Mn2 N2 79.03(8) . . ? O1 Mn2 N2 97.21(8) 3_665 . ? N1 Mn2 N2 93.35(8) . . ? O3 Mn2 O1 96.66(8) . . ? O2 Mn2 O1 80.27(7) . . ? O1 Mn2 O1 80.90(7) 3_665 . ? N1 Mn2 O1 93.86(8) . . ? N2 Mn2 O1 158.71(7) . . ? O3 Mn2 Mn2 90.82(6) . 3_665 ? O2 Mn2 Mn2 88.15(6) . 3_665 ? O1 Mn2 Mn2 44.26(5) 3_665 3_665 ? N1 Mn2 Mn2 128.78(7) . 3_665 ? N2 Mn2 Mn2 137.26(6) . 3_665 ? O1 Mn2 Mn2 36.64(4) . 3_665 ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 118.8(3) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 115.1(2) . . ? C4 C5 C6 123.6(3) . . ? O3 C6 C5 110.1(2) . . ? O3 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O3 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.2 . . ? N2 C7 C8 122.1(3) . . ? N2 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C7 C8 C9 119.2(3) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N2 C11 C10 121.2(3) . . ? N2 C11 C12 115.7(2) . . ? C10 C11 C12 123.1(3) . . ? O2 C12 C11 112.1(2) . . ? O2 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? O2 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N3 C13 C14 123.1(3) . . ? N3 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C15 118.5(3) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.7 . . ? C16 C15 C14 119.2(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? N3 C17 C16 121.7(3) . . ? N3 C17 C18 117.6(2) . . ? C16 C17 C18 120.6(3) . . ? O1 C18 C17 111.0(2) . . ? O1 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? O1 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? OB1 CB1 OB2 121.7(3) . . ? OB1 CB1 CB2 121.2(3) . . ? OB2 CB1 CB2 117.1(2) . . ? CB3 CB2 CB7 119.4(3) . . ? CB3 CB2 CB1 120.9(3) . . ? CB7 CB2 CB1 119.6(3) . . ? CB4 CB3 CB2 120.1(3) . . ? CB4 CB3 HB3 120.0 . . ? CB2 CB3 HB3 120.0 . . ? CB5 CB4 CB3 120.3(3) . . ? CB5 CB4 HB4 119.9 . . ? CB3 CB4 HB4 119.9 . . ? CB6 CB5 CB4 119.9(3) . . ? CB6 CB5 HB5 120.1 . . ? CB4 CB5 HB5 120.1 . . ? CB5 CB6 CB7 120.3(3) . . ? CB5 CB6 HB6 119.9 . . ? CB7 CB6 HB6 119.9 . . ? CB6 CB7 CB2 120.0(3) . . ? CB6 CB7 HB7 120.0 . . ? CB2 CB7 HB7 120.0 . . ? N100 C100 C101 178.7(5) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N200 C200 C201 179.5(4) . . ? C200 C201 H20A 109.5 . . ? C200 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? O111 Cl10 O102 115.7(7) . . ? O111 Cl10 O100 86.6(9) . . ? O102 Cl10 O100 111.9(7) . . ? O111 Cl10 O104 113.0(6) . . ? O102 Cl10 O104 111.97(17) . . ? O100 Cl10 O104 115.5(7) . . ? O111 Cl10 O110 112.1(9) . . ? O102 Cl10 O110 104.2(7) . . ? O104 Cl10 O110 98.1(8) . . ? O102 Cl10 O101 104.9(6) . . ? O100 Cl10 O101 109.0(8) . . ? O104 Cl10 O101 102.5(5) . . ? O110 Cl10 O101 134.4(8) . . ? C18 O1 Mn2 124.41(16) . 3_665 ? C18 O1 Mn2 118.91(15) . . ? Mn2 O1 Mn2 99.10(7) 3_665 . ? C18 O1 Mn1 114.83(15) . . ? Mn2 O1 Mn1 99.56(7) 3_665 . ? Mn2 O1 Mn1 94.47(7) . . ? C12 O2 Mn2 121.32(16) . . ? C12 O2 Mn1 125.06(15) . . ? Mn2 O2 Mn1 112.54(9) . . ? CB1 OB2 Mn1 101.96(17) . . ? C17 N3 C13 118.2(2) . . ? C17 N3 Mn1 119.04(17) . . ? C13 N3 Mn1 122.70(19) . . ? C11 N2 C7 118.8(2) . . ? C11 N2 Mn2 110.34(17) . . ? C7 N2 Mn2 130.63(19) . . ? C1 N1 C5 119.2(2) . . ? C1 N1 Mn2 127.34(19) . . ? C5 N1 Mn2 113.31(17) . . ? C6 O3 Mn2 119.71(16) . . ? C6 O3 Mn1 129.40(16) . 3_665 ? Mn2 O3 Mn1 108.50(8) . 3_665 ? H201 O200 H202 117(3) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.591 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.080