Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Keith Murray' _publ_contact_author_address ; School of Chemistry Monash University Building 23 Clayton campus Melbourne Victoria 3800 AUSTRALIA ; _publ_contact_author_email KEITH.MURRAY@SCI.MONASH.EDU.AU _publ_section_title ; New mixed-valence MnII2MnIII2 clusters exhibiting an unprecedented MnII/III oxidation state distribution in their magnetically coupled cores ; loop_ _publ_author_name 'Keith Wittick' 'Kevin J. Berry' 'Paul Jensen' 'leigh jones' 'Boujemaa Moubaraki' 'Leone Spiccia' ; L.M.Wittick ; data_1) #[Mn4(teaH2)2(teaH)2(Me3CCO2)2](Me3CCO2)2 _database_code_depnum_ccdc_archive 'CCDC 281690' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn4(teaH2)2(teaH)2(Me3CCO2)2](Me3CCO2)2' _chemical_formula_sum 'C44 H82 Mn4 N4 O20' _chemical_formula_weight 1206.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.577(2) _cell_length_b 11.019(2) _cell_length_c 13.590(3) _cell_angle_alpha 82.44(3) _cell_angle_beta 84.43(3) _cell_angle_gamma 63.95(3) _cell_volume 1409.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour red/brown _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26375 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 28.24 _reflns_number_total 6835 _reflns_number_gt 5820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XSeed _computing_publication_material XSeed _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+1.8736P] 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 6835 _refine_ls_number_parameters 366 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.87638(3) 0.52347(3) 0.31485(2) 0.01551(8) Uani 1 1 d . . . Mn2 Mn 0.86126(3) 0.61261(3) 0.54415(2) 0.01486(8) Uani 1 1 d . . . O1 O 0.80572(16) 0.69027(15) 0.41509(11) 0.0208(3) Uani 1 1 d . . . O2 O 0.67737(16) 0.51610(17) 0.29572(11) 0.0213(3) Uani 1 1 d D . . O3 O 0.93615(17) 0.50043(17) 0.15036(12) 0.0232(3) Uani 1 1 d D . . O4 O 0.91207(15) 0.51188(15) 0.67054(10) 0.0175(3) Uani 1 1 d . . . O5 O 0.90806(15) 0.44707(14) 0.48280(10) 0.0157(3) Uani 1 1 d . . . O6A O 0.5321(5) 0.9039(4) 0.5690(4) 0.0306(10) Uani 0.40 1 d PD A 1 H6A H 0.6173 0.8775 0.5804 0.037 Uiso 0.40 1 calc PR A 1 O6B O 0.3401(5) 0.8620(5) 0.6653(4) 0.0409(12) Uani 0.40 1 d PD B 2 H6B H 0.3227 0.8098 0.7095 0.049 Uiso 0.40 1 calc PRD B 2 O6C O 0.4711(10) 0.8118(10) 0.7243(7) 0.036(2) Uani 0.20 1 d PD C 3 H6C H 0.4303 0.7638 0.7490 0.043 Uiso 0.20 1 calc PRD C 3 O7 O 1.02344(16) 0.70505(15) 0.68427(11) 0.0220(3) Uani 1 1 d . . . O8 O 0.83109(16) 0.78166(15) 0.59361(11) 0.0211(3) Uani 1 1 d . . . O9 O 0.6648(2) 0.3510(2) 0.18691(13) 0.0368(4) Uani 1 1 d . . . O10 O 0.8057(2) 0.3890(2) 0.06941(14) 0.0485(6) Uani 1 1 d . . . N1 N 0.7418(2) 0.7355(2) 0.22051(14) 0.0242(4) Uani 1 1 d . . . N2 N 0.65905(19) 0.5748(2) 0.60052(14) 0.0224(4) Uani 1 1 d . . . C1 C 0.9111(2) 0.7957(2) 0.65337(16) 0.0199(4) Uani 1 1 d . . . C2 C 0.8565(3) 0.9371(3) 0.6889(2) 0.0335(6) Uani 1 1 d . . . C3 C 0.7723(6) 0.9316(4) 0.7861(3) 0.0879(16) Uani 1 1 d . . . H3A H 0.7294 1.0212 0.8110 0.132 Uiso 1 1 calc R . . H3B H 0.8353 0.8648 0.8353 0.132 Uiso 1 1 calc R . . H3C H 0.6983 0.9053 0.7741 0.132 Uiso 1 1 calc R . . C4 C 0.9785(4) 0.9661(3) 0.7071(4) 0.0735(13) Uani 1 1 d . . . H4A H 1.0336 0.9656 0.6447 0.110 Uiso 1 1 calc R . . H4B H 1.0385 0.8962 0.7563 0.110 Uiso 1 1 calc R . . H4C H 0.9426 1.0553 0.7320 0.110 Uiso 1 1 calc R . . C5 C 0.7597(4) 1.0473(3) 0.6156(3) 0.0599(10) Uani 1 1 d . . . H5A H 0.8101 1.0453 0.5509 0.090 Uiso 1 1 calc R . . H5B H 0.7297 1.1361 0.6400 0.090 Uiso 1 1 calc R . . H5C H 0.6769 1.0317 0.6084 0.090 Uiso 1 1 calc R . . C6 C 0.7250(2) 0.3380(2) 0.10200(17) 0.0240(5) Uani 1 1 d . . . C7 C 0.6987(3) 0.2494(3) 0.03513(17) 0.0284(5) Uani 1 1 d . . . C8 C 0.5561(4) 0.2479(5) 0.0603(3) 0.0735(13) Uani 1 1 d . . . H8B H 0.5459 0.1848 0.0207 0.110 Uiso 1 1 calc R . . H8A H 0.4811 0.3393 0.0454 0.110 Uiso 1 1 calc R . . H8C H 0.5494 0.2185 0.1311 0.110 Uiso 1 1 calc R . . C9 C 0.8135(5) 0.1071(3) 0.0543(3) 0.0687(12) Uani 1 1 d . . . H9A H 0.8012 0.0470 0.0128 0.103 Uiso 1 1 calc R . . H9B H 0.8080 0.0744 0.1245 0.103 Uiso 1 1 calc R . . H9C H 0.9056 0.1075 0.0381 0.103 Uiso 1 1 calc R . . C10 C 0.7081(5) 0.3000(4) -0.0727(2) 0.0606(11) Uani 1 1 d . . . H10A H 0.8024 0.2949 -0.0894 0.091 Uiso 1 1 calc R . . H10B H 0.6377 0.3944 -0.0843 0.091 Uiso 1 1 calc R . . H10C H 0.6903 0.2436 -0.1145 0.091 Uiso 1 1 calc R . . C11 C 0.7885(3) 0.8172(2) 0.36726(18) 0.0269(5) Uani 1 1 d . . . H11A H 0.8809 0.8139 0.3422 0.032 Uiso 1 1 calc R . . H11B H 0.7456 0.8877 0.4142 0.032 Uiso 1 1 calc R . . C12 C 0.6940(3) 0.8496(3) 0.28249(19) 0.0340(6) Uani 1 1 d . . . H12A H 0.5969 0.8708 0.3091 0.041 Uiso 1 1 calc R . . H12B H 0.6922 0.9311 0.2408 0.041 Uiso 1 1 calc R . . C13 C 0.5681(2) 0.6446(3) 0.26482(19) 0.0295(5) Uani 1 1 d . . . H13A H 0.5293 0.6981 0.3226 0.035 Uiso 1 1 calc R . . H13B H 0.4911 0.6315 0.2389 0.035 Uiso 1 1 calc R . . C14 C 0.6213(3) 0.7213(3) 0.18575(19) 0.0322(6) Uani 1 1 d . . . H14A H 0.6509 0.6726 0.1253 0.039 Uiso 1 1 calc R . . H14B H 0.5447 0.8124 0.1684 0.039 Uiso 1 1 calc R . . C15 C 0.9043(3) 0.6204(3) 0.08299(18) 0.0301(5) Uani 1 1 d . . . H15A H 0.8378 0.6263 0.0341 0.036 Uiso 1 1 calc R . . H15B H 0.9917 0.6157 0.0463 0.036 Uiso 1 1 calc R . . C16 C 0.8398(3) 0.7450(3) 0.1388(2) 0.0354(6) Uani 1 1 d . . . H16A H 0.9159 0.7580 0.1661 0.042 Uiso 1 1 calc R . . H16B H 0.7889 0.8255 0.0920 0.042 Uiso 1 1 calc R . . C21 C 0.7982(2) 0.5507(2) 0.74265(16) 0.0221(5) Uani 1 1 d . . . H21A H 0.7629 0.6483 0.7511 0.026 Uiso 1 1 calc R . . H21B H 0.8304 0.4978 0.8075 0.026 Uiso 1 1 calc R . . C22 C 0.6823(2) 0.5241(3) 0.70802(16) 0.0253(5) Uani 1 1 d . . . H22A H 0.7085 0.4254 0.7174 0.030 Uiso 1 1 calc R . . H22B H 0.5943 0.5707 0.7479 0.030 Uiso 1 1 calc R . . C23 C 0.8381(2) 0.3689(2) 0.52977(17) 0.0220(4) Uani 1 1 d . . . H23A H 0.8778 0.3261 0.5953 0.026 Uiso 1 1 calc R . . H23B H 0.8517 0.2961 0.4885 0.026 Uiso 1 1 calc R . . C24 C 0.6830(2) 0.4611(2) 0.54284(17) 0.0242(5) Uani 1 1 d . . . H24A H 0.6426 0.4978 0.4767 0.029 Uiso 1 1 calc R . . H24B H 0.6340 0.4080 0.5776 0.029 Uiso 1 1 calc R . . C25 C 0.5149(2) 0.6821(3) 0.58425(18) 0.0279(5) Uani 1 1 d D . . H25A H 0.4470 0.6476 0.6158 0.033 Uiso 1 1 calc R D 1 H25B H 0.5002 0.6994 0.5120 0.033 Uiso 1 1 calc R D 1 C26A C 0.481(4) 0.816(2) 0.6239(17) 0.0307(17) Uani 0.40 1 d PD A 1 H26A H 0.3775 0.8658 0.6312 0.037 Uiso 0.40 1 calc PR A 1 H26B H 0.5181 0.7951 0.6913 0.037 Uiso 0.40 1 calc PR A 1 C26B C 0.4846(14) 0.804(2) 0.639(2) 0.0307(17) Uani 0.40 1 d PD B 2 H26C H 0.5408 0.7757 0.6987 0.037 Uiso 0.40 1 calc PR B 2 H26D H 0.5093 0.8706 0.5951 0.037 Uiso 0.40 1 calc PR B 2 C26C C 0.475(8) 0.818(2) 0.6205(10) 0.0307(17) Uani 0.20 1 d PD C 3 H26E H 0.5441 0.8532 0.5923 0.037 Uiso 0.20 1 calc PR C 3 H26F H 0.3814 0.8832 0.5963 0.037 Uiso 0.20 1 calc PR C 3 H2 H 0.679(3) 0.462(3) 0.259(2) 0.039(8) Uiso 1 1 d D . . H3 H 0.897(3) 0.460(3) 0.128(2) 0.039(9) 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 0.01374(15) 0.01758(17) 0.01623(16) -0.00497(12) -0.00013(11) -0.00691(12) Mn2 0.01350(15) 0.01602(16) 0.01482(15) -0.00535(11) 0.00059(11) -0.00537(12) O1 0.0265(8) 0.0165(7) 0.0182(7) -0.0034(6) -0.0037(6) -0.0071(6) O2 0.0209(8) 0.0267(9) 0.0199(8) -0.0066(6) -0.0006(6) -0.0125(7) O3 0.0246(8) 0.0278(9) 0.0213(8) -0.0070(7) 0.0015(6) -0.0143(7) O4 0.0150(7) 0.0239(8) 0.0155(7) -0.0042(6) 0.0019(5) -0.0099(6) O5 0.0148(7) 0.0182(7) 0.0174(7) -0.0053(6) 0.0028(5) -0.0098(6) O6A 0.019(2) 0.021(2) 0.049(3) -0.0022(19) -0.0009(19) -0.0063(17) O6B 0.031(2) 0.034(3) 0.058(3) -0.016(2) 0.016(2) -0.014(2) O6C 0.037(5) 0.037(5) 0.034(5) -0.016(4) 0.014(4) -0.017(4) O7 0.0227(8) 0.0206(8) 0.0242(8) -0.0074(6) -0.0019(6) -0.0093(7) O8 0.0211(8) 0.0179(8) 0.0227(8) -0.0073(6) -0.0019(6) -0.0054(6) O9 0.0396(10) 0.0590(13) 0.0285(9) -0.0226(9) 0.0117(8) -0.0344(10) O10 0.0693(15) 0.0821(16) 0.0293(10) -0.0222(10) 0.0164(9) -0.0642(14) N1 0.0281(10) 0.0233(10) 0.0197(9) -0.0048(8) 0.0001(8) -0.0094(8) N2 0.0147(8) 0.0339(11) 0.0190(9) -0.0072(8) 0.0015(7) -0.0101(8) C1 0.0220(11) 0.0183(10) 0.0207(10) -0.0069(8) 0.0017(8) -0.0089(9) C2 0.0328(13) 0.0223(12) 0.0467(16) -0.0167(11) -0.0036(11) -0.0090(11) C3 0.136(4) 0.059(3) 0.067(3) -0.047(2) 0.048(3) -0.040(3) C4 0.051(2) 0.0330(17) 0.147(4) -0.032(2) -0.029(2) -0.0161(16) C5 0.058(2) 0.0199(14) 0.093(3) -0.0128(16) -0.0219(19) -0.0030(14) C6 0.0276(12) 0.0267(12) 0.0216(11) -0.0046(9) -0.0018(9) -0.0146(10) C7 0.0406(14) 0.0312(13) 0.0222(12) -0.0061(10) -0.0014(10) -0.0227(11) C8 0.070(2) 0.124(4) 0.069(2) -0.054(2) 0.0135(19) -0.072(3) C9 0.096(3) 0.0337(18) 0.073(3) -0.0146(17) -0.036(2) -0.0162(19) C10 0.121(3) 0.065(2) 0.0237(14) -0.0039(14) -0.0083(17) -0.065(2) C11 0.0359(13) 0.0198(11) 0.0266(12) -0.0028(9) -0.0041(10) -0.0128(10) C12 0.0448(15) 0.0226(12) 0.0284(13) -0.0038(10) -0.0050(11) -0.0078(11) C13 0.0177(11) 0.0357(14) 0.0328(13) -0.0039(10) -0.0018(9) -0.0092(10) C14 0.0283(13) 0.0346(14) 0.0298(13) -0.0017(11) -0.0061(10) -0.0096(11) C15 0.0353(13) 0.0349(14) 0.0215(12) -0.0043(10) 0.0061(10) -0.0175(11) C16 0.0465(16) 0.0309(14) 0.0313(14) -0.0012(11) 0.0035(11) -0.0206(12) C21 0.0201(10) 0.0338(13) 0.0158(10) -0.0047(9) 0.0043(8) -0.0153(10) C22 0.0226(11) 0.0375(13) 0.0190(11) -0.0048(9) 0.0040(9) -0.0165(10) C23 0.0255(11) 0.0244(11) 0.0236(11) -0.0038(9) 0.0018(9) -0.0178(10) C24 0.0230(11) 0.0368(13) 0.0208(11) -0.0045(9) 0.0017(8) -0.0204(10) C25 0.0188(11) 0.0377(14) 0.0269(12) -0.0068(10) -0.0003(9) -0.0112(10) C26A 0.023(2) 0.031(2) 0.033(5) -0.006(3) -0.0017(18) -0.0070(14) C26B 0.023(2) 0.031(2) 0.033(5) -0.006(3) -0.0017(18) -0.0070(14) C26C 0.023(2) 0.031(2) 0.033(5) -0.006(3) -0.0017(18) -0.0070(14) _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 2.121(2) 2_766 ? Mn1 O2 2.183(2) . ? Mn1 O1 2.247(2) . ? Mn1 O7 2.262(2) 2_766 ? Mn1 O3 2.279(2) . ? Mn1 O5 2.330(2) . ? Mn1 N1 2.403(2) . ? Mn1 Mn2 3.201(1) 2_766 ? Mn2 O1 1.876(2) . ? Mn2 O4 1.904(2) . ? Mn2 O8 1.947(2) . ? Mn2 O5 1.948(2) . ? Mn2 O5 2.236(2) 2_766 ? Mn2 N2 2.391(2) . ? Mn2 Mn2 3.149(2) 2_766 ? Mn2 Mn1 3.201(1) 2_766 ? O1 C11 1.405(3) . ? O2 C13 1.420(3) . ? O2 H2 0.82(2) . ? O3 C15 1.432(3) . ? O3 H3 0.83(2) . ? O4 C21 1.422(2) . ? O4 Mn1 2.121(2) 2_766 ? O5 C23 1.421(2) . ? O5 Mn2 2.236(2) 2_766 ? O6A C26A 1.401(1) . ? O6A H6A 0.8400 . ? O6B C26B 1.405(1) . ? O6B H6B 0.8400 . ? O6C C26C 1.400(1) . ? O6C H6C 0.8400 . ? O7 C1 1.237(3) . ? O7 Mn1 2.262(2) 2_766 ? O8 C1 1.297(3) . ? O9 C6 1.256(3) . ? O10 C6 1.234(3) . ? N1 C16 1.469(3) . ? N1 C12 1.478(3) . ? N1 C14 1.478(3) . ? N2 C25 1.478(3) . ? N2 C24 1.480(3) . ? N2 C22 1.497(3) . ? C1 C2 1.532(3) . ? C2 C4 1.507(4) . ? C2 C5 1.518(4) . ? C2 C3 1.529(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.542(3) . ? C7 C10 1.508(4) . ? C7 C9 1.511(4) . ? C7 C8 1.521(4) . ? C8 H8B 0.9800 . ? C8 H8A 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.502(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.499(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.509(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 C22 1.509(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.511(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26C 1.509(2) . ? C25 C26B 1.514(1) . ? C25 C26A 1.516(1) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C26C H26E 0.9900 . ? C26C H26F 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O2 168.37(6) 2_766 . ? O4 Mn1 O1 89.08(6) 2_766 . ? O2 Mn1 O1 101.04(7) . . ? O4 Mn1 O7 82.15(7) 2_766 2_766 ? O2 Mn1 O7 86.31(7) . 2_766 ? O1 Mn1 O7 142.50(6) . 2_766 ? O4 Mn1 O3 85.89(6) 2_766 . ? O2 Mn1 O3 90.50(7) . . ? O1 Mn1 O3 136.77(6) . . ? O7 Mn1 O3 79.09(7) 2_766 . ? O4 Mn1 O5 78.20(6) 2_766 . ? O2 Mn1 O5 100.59(6) . . ? O1 Mn1 O5 65.89(6) . . ? O7 Mn1 O5 76.63(6) 2_766 . ? O3 Mn1 O5 152.50(6) . . ? O4 Mn1 N1 112.98(7) 2_766 . ? O2 Mn1 N1 76.08(7) . . ? O1 Mn1 N1 71.53(6) . . ? O7 Mn1 N1 145.00(6) 2_766 . ? O3 Mn1 N1 71.19(7) . . ? O5 Mn1 N1 135.81(6) . . ? O4 Mn1 Mn2 35.03(4) 2_766 2_766 ? O2 Mn1 Mn2 140.10(5) . 2_766 ? O1 Mn1 Mn2 82.53(5) . 2_766 ? O7 Mn1 Mn2 69.49(5) 2_766 2_766 ? O3 Mn1 Mn2 114.13(5) . 2_766 ? O5 Mn1 Mn2 44.31(4) . 2_766 ? N1 Mn1 Mn2 140.03(5) . 2_766 ? O1 Mn2 O4 171.33(7) . . ? O1 Mn2 O8 95.28(7) . . ? O4 Mn2 O8 92.86(7) . . ? O1 Mn2 O5 81.23(7) . . ? O4 Mn2 O5 90.99(7) . . ? O8 Mn2 O5 172.95(6) . . ? O1 Mn2 O5 97.55(7) . 2_766 ? O4 Mn2 O5 85.14(7) . 2_766 ? O8 Mn2 O5 91.83(7) . 2_766 ? O5 Mn2 O5 82.61(7) . 2_766 ? O1 Mn2 N2 98.17(7) . . ? O4 Mn2 N2 76.65(7) . . ? O8 Mn2 N2 106.00(7) . . ? O5 Mn2 N2 80.64(7) . . ? O5 Mn2 N2 154.93(6) 2_766 . ? O1 Mn2 Mn2 89.94(6) . 2_766 ? O4 Mn2 Mn2 87.17(6) . 2_766 ? O8 Mn2 Mn2 129.54(5) . 2_766 ? O5 Mn2 Mn2 44.77(5) . 2_766 ? O5 Mn2 Mn2 37.84(4) 2_766 2_766 ? N2 Mn2 Mn2 122.86(5) . 2_766 ? O1 Mn2 Mn1 144.14(5) . 2_766 ? O4 Mn2 Mn1 39.75(5) . 2_766 ? O8 Mn2 Mn1 84.95(5) . 2_766 ? O5 Mn2 Mn1 94.28(5) . 2_766 ? O5 Mn2 Mn1 46.70(4) 2_766 2_766 ? N2 Mn2 Mn1 116.29(5) . 2_766 ? Mn2 Mn2 Mn1 63.84(3) 2_766 2_766 ? C11 O1 Mn2 129.82(1) . . ? C11 O1 Mn1 114.98(1) . . ? Mn2 O1 Mn1 108.74(7) . . ? C13 O2 Mn1 113.37(1) . . ? C13 O2 H2 107(2) . . ? Mn1 O2 H2 117(2) . . ? C15 O3 Mn1 118.59(1) . . ? C15 O3 H3 105(2) . . ? Mn1 O3 H3 110(2) . . ? C21 O4 Mn2 112.90(13) . . ? C21 O4 Mn1 128.78(12) . 2_766 ? Mn2 O4 Mn1 105.22(7) . 2_766 ? C23 O5 Mn2 113.65(12) . . ? C23 O5 Mn2 129.41(13) . 2_766 ? Mn2 O5 Mn2 97.39(6) . 2_766 ? C23 O5 Mn1 119.07(12) . . ? Mn2 O5 Mn1 103.06(7) . . ? Mn2 O5 Mn1 88.99(6) 2_766 . ? C26B O6B H6B 109.5 . . ? C1 O7 Mn1 132.93(1) . 2_766 ? C1 O8 Mn2 125.84(1) . . ? C16 N1 C12 111.9(2) . . ? C16 N1 C14 112.7(2) . . ? C12 N1 C14 111.4(2) . . ? C16 N1 Mn1 104.01(1) . . ? C12 N1 Mn1 110.89(1) . . ? C14 N1 Mn1 105.50(1) . . ? C25 N2 C24 108.64(2) . . ? C25 N2 C22 112.17(2) . . ? C24 N2 C22 109.67(2) . . ? C25 N2 Mn2 121.20(2) . . ? C24 N2 Mn2 99.90(1) . . ? C22 N2 Mn2 104.32(1) . . ? O7 C1 O8 125.48(2) . . ? O7 C1 C2 119.0(2) . . ? O8 C1 C2 115.50(2) . . ? C4 C2 C5 110.1(3) . . ? C4 C2 C3 110.4(3) . . ? C5 C2 C3 108.9(3) . . ? C4 C2 C1 110.1(2) . . ? C5 C2 C1 112.1(2) . . ? C3 C2 C1 105.2(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O10 C6 O9 124.5(2) . . ? O10 C6 C7 117.9(2) . . ? O9 C6 C7 117.5(2) . . ? C10 C7 C9 109.4(3) . . ? C10 C7 C8 110.0(3) . . ? C9 C7 C8 109.1(3) . . ? C10 C7 C6 110.2(2) . . ? C9 C7 C6 106.7(2) . . ? C8 C7 C6 111.4(2) . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? C7 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 107.33(2) . . ? O1 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O1 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N1 C12 C11 111.8(2) . . ? N1 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N1 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? O2 C13 C14 111.2(2) . . ? O2 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? O2 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N1 C14 C13 110.5(2) . . ? N1 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O3 C15 C16 110.40(2) . . ? O3 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? O3 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N1 C16 C15 112.6(2) . . ? N1 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? N1 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? O4 C21 C22 108.72(2) . . ? O4 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? O4 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? N2 C22 C21 109.73(2) . . ? N2 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? N2 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? O5 C23 C24 108.83(2) . . ? O5 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? O5 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? N2 C24 C23 111.44(2) . . ? N2 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? N2 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N2 C25 C26C 118(3) . . ? N2 C25 C26B 111.5(8) . . ? C26C C25 C26B 10.5(12) . . ? N2 C25 C26A 115.5(17) . . ? C26C C25 C26A 3(4) . . ? C26B C25 C26A 8(2) . . ? N2 C25 H25A 108.4 . . ? C26C C25 H25A 107.6 . . ? C26B C25 H25A 103.9 . . ? C26A C25 H25A 108.4 . . ? N2 C25 H25B 108.4 . . ? C26C C25 H25B 106.3 . . ? C26B C25 H25B 116.7 . . ? C26A C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? O6A C26A C25 118.3(9) . . ? O6A C26A H26A 107.7 . . ? C25 C26A H26A 107.7 . . ? O6A C26A H26B 107.7 . . ? C25 C26A H26B 107.7 . . ? H26A C26A H26B 107.1 . . ? O6B C26B C25 107.2(9) . . ? O6B C26B H26C 110.3 . . ? C25 C26B H26C 110.3 . . ? O6B C26B H26D 110.3 . . ? C25 C26B H26D 110.3 . . ? H26C C26B H26D 108.5 . . ? O6C C26C C25 112.4(12) . . ? O6C C26C H26E 109.1 . . ? C25 C26C H26E 109.1 . . ? O6C C26C H26F 109.1 . . ? C25 C26C H26F 109.1 . . ? H26E C26C H26F 107.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6A H6A O8 0.84 2.05 2.876(5) 168.8 . O6B H6B O9 0.84 2.08 2.897(6) 165.1 2_666 O6C H6C O9 0.84 2.01 2.846(10) 177.8 2_666 O3 H3 O10 0.83(2) 1.78(3) 2.600(2) 173(3) . O2 H2 O9 0.82(2) 1.73(3) 2.544(2) 174(3) . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.637 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.071 #END data_2) #[Mn4(PhCO2)4(acac)2(teaH)2]_MeCN _database_code_depnum_ccdc_archive 'CCDC 281691' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn4(PhCO2)4(acac)2(teaH)2]_MeCN' _chemical_formula_sum 'C52 H65 Mn4 N3 O18' _chemical_formula_weight 1239.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.531(4) _cell_length_b 13.406(3) _cell_length_c 22.257(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5529.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square plate' _exptl_crystal_colour Red/Brown _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62888 _diffrn_reflns_av_R_equivalents 0.1004 _diffrn_reflns_av_sigmaI/netI 0.1126 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 30.51 _reflns_number_total 16738 _reflns_number_gt 11055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XSeed _computing_publication_material XSeed _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00138(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(12) _refine_ls_number_reflns 16738 _refine_ls_number_parameters 704 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.958 _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 0.09829(3) 0.65801(4) -0.00395(2) 0.01357(11) Uani 1 1 d . . . Mn2 Mn 0.19178(3) 0.83507(4) 0.04759(2) 0.01406(11) Uani 1 1 d . . . Mn3 Mn 0.01184(3) 0.87966(4) 0.01877(3) 0.01437(11) Uani 1 1 d . . . Mn4 Mn 0.10479(3) 1.08597(4) 0.03875(2) 0.01485(11) Uani 1 1 d . . . O1 O 0.01227(12) 0.58824(17) 0.02084(12) 0.0173(5) Uani 1 1 d . . . O2 O 0.11147(13) 0.56597(17) -0.06958(11) 0.0184(5) Uani 1 1 d . . . C1 C -0.10193(19) 0.5109(3) 0.01071(19) 0.0278(9) Uani 1 1 d . . . H1A H -0.1014 0.5116 0.0547 0.042 Uiso 1 1 calc R . . H1B H -0.1167 0.4448 -0.0035 0.042 Uiso 1 1 calc R . . H1C H -0.1362 0.5610 -0.0039 0.042 Uiso 1 1 calc R . . C2 C -0.02769(18) 0.5344(3) -0.01261(17) 0.0194(8) Uani 1 1 d . . . C3 C -0.0061(2) 0.4960(3) -0.06852(18) 0.0256(9) Uani 1 1 d . . . H3A H -0.0137 0.4230 -0.0665 0.031 Uiso 1 1 calc R . . H3B H -0.0411 0.5217 -0.0984 0.031 Uiso 1 1 calc R . . C4 C 0.0622(2) 0.5102(3) -0.09315(17) 0.0223(8) Uani 1 1 d . . . C5 C 0.0838(2) 0.4576(3) -0.14928(19) 0.0336(10) Uani 1 1 d . . . H5A H 0.1044 0.5057 -0.1776 0.050 Uiso 1 1 calc R . . H5B H 0.0413 0.4260 -0.1673 0.050 Uiso 1 1 calc R . . H5C H 0.1198 0.4064 -0.1398 0.050 Uiso 1 1 calc R . . O3 O 0.16938(12) 0.57543(17) 0.05459(11) 0.0171(5) Uani 1 1 d . . . O4 O 0.23320(13) 0.70462(18) 0.09204(11) 0.0198(6) Uani 1 1 d . . . C6 C 0.21809(19) 0.6132(3) 0.08770(16) 0.0167(7) Uani 1 1 d . . . C7 C 0.26154(19) 0.5421(3) 0.12625(16) 0.0183(7) Uani 1 1 d . . . C8 C 0.2434(2) 0.4424(3) 0.12941(18) 0.0256(9) Uani 1 1 d . . . H8 H 0.2030 0.4178 0.1077 0.031 Uiso 1 1 calc R . . C9 C 0.2845(2) 0.3780(3) 0.16453(18) 0.0286(9) Uani 1 1 d . . . H9 H 0.2716 0.3096 0.1671 0.034 Uiso 1 1 calc R . . C10 C 0.3437(2) 0.4126(3) 0.19555(18) 0.0309(10) Uani 1 1 d . . . H10 H 0.3714 0.3682 0.2195 0.037 Uiso 1 1 calc R . . C11 C 0.3629(2) 0.5119(3) 0.19177(18) 0.0310(10) Uani 1 1 d . . . H11 H 0.4044 0.5356 0.2123 0.037 Uiso 1 1 calc R . . C12 C 0.3210(2) 0.5770(3) 0.15782(17) 0.0241(8) Uani 1 1 d . . . H12 H 0.3332 0.6458 0.1562 0.029 Uiso 1 1 calc R . . N1 N 0.28171(15) 0.8733(2) -0.02047(13) 0.0171(6) Uani 1 1 d . . . O5 O 0.17295(12) 0.73799(17) -0.03191(11) 0.0152(5) Uani 1 1 d . . . O6 O 0.13815(12) 0.96152(17) 0.00304(11) 0.0160(5) Uani 1 1 d . . . O7 O 0.42468(13) 0.73549(18) -0.00846(12) 0.0247(6) Uani 1 1 d . . . H7 H 0.4574 0.7693 -0.0247 0.030 Uiso 1 1 calc R . . C13 C 0.24110(18) 0.7056(3) -0.05434(17) 0.0169(7) Uani 1 1 d . . . H13A H 0.2344 0.6628 -0.0902 0.020 Uiso 1 1 calc R . . H13B H 0.2672 0.6669 -0.0233 0.020 Uiso 1 1 calc R . . C14 C 0.28315(19) 0.7987(3) -0.07071(16) 0.0173(7) Uani 1 1 d . . . H14A H 0.3338 0.7804 -0.0797 0.021 Uiso 1 1 calc R . . H14B H 0.2620 0.8290 -0.1073 0.021 Uiso 1 1 calc R . . C15 C 0.17436(19) 0.9696(3) -0.05380(16) 0.0200(8) Uani 1 1 d . . . H15A H 0.1593 1.0318 -0.0743 0.024 Uiso 1 1 calc R . . H15B H 0.1609 0.9125 -0.0797 0.024 Uiso 1 1 calc R . . C16 C 0.25556(19) 0.9705(3) -0.04431(17) 0.0217(8) Uani 1 1 d . . . H16A H 0.2799 0.9848 -0.0830 0.026 Uiso 1 1 calc R . . H16B H 0.2683 1.0243 -0.0157 0.026 Uiso 1 1 calc R . . C17 C 0.38822(19) 0.7949(3) 0.03471(18) 0.0218(8) Uani 1 1 d . . . H17A H 0.4232 0.8149 0.0661 0.026 Uiso 1 1 calc R . . H17B H 0.3506 0.7536 0.0542 0.026 Uiso 1 1 calc R . . C18 C 0.35259(18) 0.8890(3) 0.00939(17) 0.0211(8) Uani 1 1 d . . . H18A H 0.3459 0.9372 0.0426 0.025 Uiso 1 1 calc R . . H18B H 0.3860 0.9197 -0.0200 0.025 Uiso 1 1 calc R . . N2 N -0.03267(15) 0.8442(2) 0.11865(13) 0.0165(6) Uani 1 1 d . . . N3 N -0.0633(4) 0.4855(4) -0.2559(3) 0.0848(19) Uani 1 1 d . . . O8 O 0.01800(13) 0.76084(18) -0.05053(11) 0.0170(5) Uani 1 1 d . . . O9 O -0.09417(13) 0.7563(2) -0.08776(12) 0.0261(6) Uani 1 1 d . . . O10 O 0.21973(15) 0.91718(18) 0.12453(11) 0.0238(6) Uani 1 1 d . . . O11 O 0.17226(15) 1.0707(2) 0.11802(12) 0.0270(6) Uani 1 1 d . . . O12 O 0.08403(12) 0.76056(17) 0.05807(10) 0.0150(5) Uani 1 1 d . . . O13 O -0.10886(13) 0.85906(19) 0.01168(12) 0.0212(6) Uani 1 1 d D . . O14 O 0.02907(13) 1.01004(19) 0.07094(11) 0.0199(5) Uani 1 1 d . . . O15 O -0.00241(13) 0.96913(18) -0.06100(11) 0.0179(5) Uani 1 1 d . . . O16 O 0.03929(12) 1.12307(18) -0.04195(11) 0.0189(5) Uani 1 1 d . . . O17 O 0.06661(12) 1.20509(17) 0.07748(11) 0.0180(5) Uani 1 1 d . . . O18 O 0.17777(12) 1.16535(18) -0.00088(12) 0.0198(5) Uani 1 1 d . . . C19 C -0.02709(19) 0.7577(3) -0.09463(17) 0.0179(8) Uani 1 1 d . . . C20 C 0.0021(2) 0.7572(3) -0.15686(17) 0.0187(8) Uani 1 1 d . . . C21 C -0.0456(2) 0.7698(3) -0.20498(17) 0.0222(8) Uani 1 1 d . . . H21 H -0.0959 0.7761 -0.1977 0.027 Uiso 1 1 calc R . . C22 C -0.0193(2) 0.7729(3) -0.26359(18) 0.0262(9) Uani 1 1 d . . . H22 H -0.0517 0.7816 -0.2963 0.031 Uiso 1 1 calc R . . C23 C 0.0538(2) 0.7634(3) -0.27423(18) 0.0295(10) Uani 1 1 d . . . H23 H 0.0717 0.7657 -0.3142 0.035 Uiso 1 1 calc R . . C24 C 0.1011(2) 0.7504(3) -0.22649(18) 0.0278(9) Uani 1 1 d . . . H24 H 0.1513 0.7428 -0.2342 0.033 Uiso 1 1 calc R . . C25 C 0.0762(2) 0.7484(3) -0.16779(17) 0.0199(8) Uani 1 1 d . . . H25 H 0.1091 0.7411 -0.1353 0.024 Uiso 1 1 calc R . . C26 C 0.21130(19) 1.0058(3) 0.14198(16) 0.0171(7) Uani 1 1 d . . . C27 C 0.25200(19) 1.0373(3) 0.19751(15) 0.0161(7) Uani 1 1 d . . . C28 C 0.3053(2) 0.9770(3) 0.22183(17) 0.0226(8) Uani 1 1 d . . . H28 H 0.3153 0.9138 0.2045 0.027 Uiso 1 1 calc R . . C29 C 0.3447(2) 1.0096(3) 0.27234(18) 0.0284(9) Uani 1 1 d . . . H29 H 0.3820 0.9692 0.2886 0.034 Uiso 1 1 calc R . . C30 C 0.3287(2) 1.1013(3) 0.29803(18) 0.0317(10) Uani 1 1 d . . . H30 H 0.3554 1.1238 0.3318 0.038 Uiso 1 1 calc R . . C31 C 0.2744(2) 1.1597(3) 0.27507(17) 0.0288(9) Uani 1 1 d . . . H31 H 0.2631 1.2216 0.2935 0.035 Uiso 1 1 calc R . . C32 C 0.2359(2) 1.1279(3) 0.22458(17) 0.0229(8) Uani 1 1 d . . . H32 H 0.1984 1.1686 0.2087 0.028 Uiso 1 1 calc R . . C33 C 0.06928(19) 0.7272(3) 0.11833(15) 0.0170(7) Uani 1 1 d . . . H33A H 0.1000 0.7645 0.1469 0.020 Uiso 1 1 calc R . . H33B H 0.0813 0.6555 0.1219 0.020 Uiso 1 1 calc R . . C34 C -0.0091(2) 0.7428(3) 0.13425(18) 0.0176(8) Uani 1 1 d . . . H34A H -0.0391 0.6936 0.1124 0.021 Uiso 1 1 calc R . . H34B H -0.0160 0.7316 0.1778 0.021 Uiso 1 1 calc R . . C35 C -0.14312(19) 0.8095(3) 0.06056(15) 0.0209(8) Uani 1 1 d . . . H35A H -0.1339 0.7369 0.0585 0.025 Uiso 1 1 calc R . . H35B H -0.1959 0.8207 0.0592 0.025 Uiso 1 1 calc R . . C36 C -0.11170(19) 0.8526(3) 0.11793(17) 0.0205(8) Uani 1 1 d . . . H36A H -0.1256 0.9237 0.1214 0.025 Uiso 1 1 calc R . . H36B H -0.1319 0.8167 0.1529 0.025 Uiso 1 1 calc R . . C37 C 0.0009(2) 1.0208(3) 0.12965(17) 0.0219(8) Uani 1 1 d . . . H37A H -0.0486 1.0484 0.1279 0.026 Uiso 1 1 calc R . . H37B H 0.0315 1.0670 0.1532 0.026 Uiso 1 1 calc R . . C38 C -0.00013(19) 0.9188(3) 0.15918(17) 0.0195(8) Uani 1 1 d . . . H38A H 0.0498 0.8985 0.1693 0.023 Uiso 1 1 calc R . . H38B H -0.0282 0.9221 0.1970 0.023 Uiso 1 1 calc R . . C39 C 0.00481(19) 1.0596(3) -0.07264(16) 0.0167(7) Uani 1 1 d . . . C40 C -0.03437(19) 1.0979(3) -0.12833(17) 0.0185(8) Uani 1 1 d . . . C41 C -0.0848(2) 1.0377(3) -0.15606(18) 0.0247(8) Uani 1 1 d . . . H41 H -0.0911 0.9707 -0.1431 0.030 Uiso 1 1 calc R . . C42 C -0.1265(2) 1.0751(3) -0.20302(18) 0.0313(10) Uani 1 1 d . . . H42 H -0.1611 1.0335 -0.2222 0.038 Uiso 1 1 calc R . . C43 C -0.1177(2) 1.1721(4) -0.22157(18) 0.0338(11) Uani 1 1 d . . . H43 H -0.1472 1.1978 -0.2529 0.041 Uiso 1 1 calc R . . C44 C -0.0662(2) 1.2328(3) -0.19516(19) 0.0313(10) Uani 1 1 d . . . H44 H -0.0592 1.2990 -0.2092 0.038 Uiso 1 1 calc R . . C45 C -0.0244(2) 1.1959(3) -0.14743(18) 0.0247(9) Uani 1 1 d . . . H45 H 0.0104 1.2373 -0.1284 0.030 Uiso 1 1 calc R . . C46 C 0.0389(2) 1.3736(3) 0.09792(18) 0.0260(9) Uani 1 1 d . . . H46A H -0.0131 1.3633 0.0926 0.039 Uiso 1 1 calc R . . H46B H 0.0520 1.4403 0.0836 0.039 Uiso 1 1 calc R . . H46C H 0.0512 1.3674 0.1406 0.039 Uiso 1 1 calc R . . C47 C 0.07943(19) 1.2966(3) 0.06265(17) 0.0195(8) Uani 1 1 d . . . C48 C 0.1278(2) 1.3249(3) 0.01796(18) 0.0213(8) Uani 1 1 d . . . H48A H 0.0986 1.3560 -0.0143 0.026 Uiso 1 1 calc R . . H48B H 0.1578 1.3788 0.0354 0.026 Uiso 1 1 calc R . . C49 C 0.17495(18) 1.2602(3) -0.01022(16) 0.0187(7) Uani 1 1 d . . . C50 C 0.2285(2) 1.2996(3) -0.0545(2) 0.0300(9) Uani 1 1 d . . . H50A H 0.2773 1.2807 -0.0419 0.045 Uiso 1 1 calc R . . H50B H 0.2248 1.3725 -0.0563 0.045 Uiso 1 1 calc R . . H50C H 0.2184 1.2714 -0.0942 0.045 Uiso 1 1 calc R . . C51 C -0.1101(4) 0.5153(5) -0.2270(4) 0.074(2) Uani 1 1 d . . . C52 C -0.1658(4) 0.5533(6) -0.1880(4) 0.103(3) Uani 1 1 d . . . H52A H -0.1856 0.4986 -0.1639 0.154 Uiso 1 1 calc R . . H52B H -0.2043 0.5830 -0.2123 0.154 Uiso 1 1 calc R . . H52C H -0.1453 0.6041 -0.1613 0.154 Uiso 1 1 calc R . . H13C H -0.113(3) 0.827(3) -0.0203(13) 0.046(15) 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 0.0136(2) 0.0113(2) 0.0158(3) -0.0009(2) -0.0004(2) -0.0013(2) Mn2 0.0135(2) 0.0116(2) 0.0172(3) -0.0003(2) -0.0006(2) 0.00018(19) Mn3 0.0152(2) 0.0120(2) 0.0159(2) -0.0003(2) -0.0004(2) 0.0007(2) Mn4 0.0148(2) 0.0107(2) 0.0191(3) 0.0000(2) -0.0012(2) -0.00031(19) O1 0.0181(12) 0.0143(11) 0.0195(12) 0.0001(11) 0.0017(10) -0.0034(9) O2 0.0211(13) 0.0152(13) 0.0188(13) -0.0026(10) 0.0005(11) -0.0015(10) C1 0.0197(18) 0.026(2) 0.038(2) -0.0026(17) 0.0022(18) -0.0062(15) C2 0.0210(18) 0.0106(16) 0.026(2) 0.0023(15) -0.0027(16) 0.0004(13) C3 0.025(2) 0.0186(19) 0.033(2) -0.0003(17) -0.0088(18) -0.0038(16) C4 0.029(2) 0.0136(18) 0.024(2) 0.0004(15) -0.0060(17) -0.0022(15) C5 0.034(2) 0.034(2) 0.033(2) -0.010(2) -0.001(2) -0.0069(19) O3 0.0162(11) 0.0143(12) 0.0209(14) -0.0011(10) -0.0042(11) 0.0003(9) O4 0.0224(13) 0.0120(12) 0.0250(14) 0.0033(10) -0.0026(11) 0.0006(10) C6 0.0158(17) 0.0165(18) 0.0179(17) 0.0018(14) 0.0056(15) 0.0009(14) C7 0.0179(18) 0.0189(18) 0.0183(18) -0.0001(15) 0.0023(15) 0.0050(14) C8 0.029(2) 0.0177(19) 0.030(2) -0.0003(16) -0.0001(18) 0.0034(16) C9 0.037(2) 0.0147(19) 0.034(2) 0.0067(17) -0.002(2) 0.0075(17) C10 0.043(3) 0.027(2) 0.024(2) 0.0011(18) -0.0047(19) 0.0112(19) C11 0.033(2) 0.034(2) 0.026(2) 0.0003(18) -0.0138(19) 0.0073(19) C12 0.025(2) 0.020(2) 0.028(2) 0.0022(16) -0.0056(17) 0.0022(16) N1 0.0141(14) 0.0151(15) 0.0222(16) -0.0011(12) 0.0035(13) 0.0011(11) O5 0.0124(11) 0.0126(12) 0.0205(13) -0.0003(10) 0.0004(10) -0.0018(9) O6 0.0154(12) 0.0164(12) 0.0162(12) 0.0034(10) 0.0013(10) 0.0037(9) O7 0.0230(13) 0.0176(13) 0.0335(15) -0.0003(12) 0.0003(13) -0.0001(10) C13 0.0136(17) 0.0159(18) 0.0213(19) -0.0012(14) 0.0040(15) 0.0014(14) C14 0.0164(17) 0.0179(18) 0.0176(18) -0.0035(14) 0.0025(15) 0.0011(14) C15 0.0188(18) 0.021(2) 0.0197(18) -0.0007(15) 0.0021(15) 0.0029(15) C16 0.0202(18) 0.0188(19) 0.026(2) 0.0042(16) 0.0047(16) -0.0011(15) C17 0.0171(17) 0.0212(18) 0.027(2) 0.0022(16) -0.0018(16) -0.0006(14) C18 0.0163(17) 0.0169(18) 0.030(2) -0.0064(16) 0.0032(16) -0.0022(13) N2 0.0136(14) 0.0163(15) 0.0195(15) -0.0030(12) 0.0027(12) 0.0021(11) N3 0.092(5) 0.053(4) 0.109(5) 0.029(3) -0.007(4) 0.005(3) O8 0.0172(12) 0.0161(13) 0.0176(13) -0.0004(10) -0.0012(11) 0.0019(10) O9 0.0177(13) 0.0388(17) 0.0216(14) -0.0033(12) 0.0001(11) -0.0011(12) O10 0.0351(15) 0.0162(13) 0.0202(14) -0.0047(11) -0.0050(12) 0.0041(12) O11 0.0355(16) 0.0196(14) 0.0259(15) -0.0041(11) -0.0142(13) 0.0065(12) O12 0.0162(12) 0.0132(12) 0.0157(12) -0.0014(9) -0.0010(10) -0.0002(9) O13 0.0197(13) 0.0246(15) 0.0194(14) 0.0014(11) -0.0007(11) -0.0002(10) O14 0.0243(13) 0.0174(13) 0.0181(12) -0.0019(10) 0.0039(11) -0.0063(10) O15 0.0208(13) 0.0136(12) 0.0193(13) 0.0003(10) -0.0007(10) -0.0012(10) O16 0.0176(12) 0.0150(13) 0.0240(14) -0.0002(11) -0.0053(11) -0.0021(10) O17 0.0203(13) 0.0102(12) 0.0236(14) -0.0011(10) -0.0002(11) 0.0006(10) O18 0.0151(11) 0.0136(12) 0.0307(15) 0.0022(11) -0.0011(11) -0.0008(10) C19 0.0176(18) 0.0168(18) 0.0194(19) -0.0008(15) -0.0061(15) 0.0014(14) C20 0.0264(19) 0.0104(16) 0.0192(19) -0.0012(14) -0.0027(16) -0.0010(14) C21 0.025(2) 0.022(2) 0.0202(19) -0.0003(16) -0.0035(17) 0.0043(15) C22 0.039(2) 0.020(2) 0.0195(19) 0.0012(16) -0.0072(18) 0.0034(18) C23 0.044(3) 0.025(2) 0.020(2) 0.0018(16) 0.0073(19) 0.0027(19) C24 0.034(2) 0.024(2) 0.026(2) 0.0006(17) 0.0098(19) 0.0047(18) C25 0.0220(18) 0.0152(18) 0.0224(19) 0.0012(15) 0.0003(16) 0.0008(14) C26 0.0148(17) 0.0205(19) 0.0161(18) 0.0035(15) -0.0013(15) -0.0031(14) C27 0.0180(17) 0.0161(17) 0.0143(17) -0.0005(14) 0.0009(14) -0.0037(14) C28 0.0237(19) 0.023(2) 0.022(2) 0.0041(16) -0.0025(16) -0.0014(16) C29 0.032(2) 0.028(2) 0.026(2) 0.0075(17) -0.0078(18) -0.0006(18) C30 0.041(2) 0.033(2) 0.022(2) 0.0011(18) -0.0108(19) -0.0111(19) C31 0.049(3) 0.018(2) 0.019(2) -0.0039(15) -0.0020(19) -0.0008(18) C32 0.026(2) 0.0177(19) 0.025(2) 0.0020(16) -0.0006(17) 0.0015(16) C33 0.0221(18) 0.0196(18) 0.0093(16) 0.0030(14) -0.0018(15) -0.0020(15) C34 0.0227(19) 0.0114(17) 0.0189(18) 0.0054(14) 0.0042(15) -0.0016(14) C35 0.0155(17) 0.0227(19) 0.024(2) -0.0026(15) 0.0065(15) -0.0010(14) C36 0.0203(18) 0.0179(18) 0.023(2) 0.0000(15) 0.0051(16) 0.0007(15) C37 0.026(2) 0.021(2) 0.0189(19) -0.0079(15) 0.0053(16) -0.0011(16) C38 0.0177(18) 0.0184(18) 0.0225(19) -0.0024(15) 0.0025(15) -0.0001(14) C39 0.0149(17) 0.0168(18) 0.0183(18) -0.0014(14) 0.0026(14) 0.0014(14) C40 0.0165(17) 0.0159(18) 0.0231(19) -0.0004(15) 0.0012(15) 0.0014(14) C41 0.025(2) 0.025(2) 0.025(2) -0.0028(17) -0.0021(17) 0.0015(16) C42 0.030(2) 0.041(3) 0.023(2) -0.0066(19) -0.0093(18) 0.0046(19) C43 0.035(2) 0.049(3) 0.017(2) 0.0059(19) -0.0031(18) 0.015(2) C44 0.032(2) 0.033(2) 0.029(2) 0.0114(19) 0.0050(19) 0.0099(19) C45 0.026(2) 0.021(2) 0.027(2) 0.0068(16) 0.0056(17) 0.0003(16) C46 0.034(2) 0.0138(18) 0.030(2) -0.0037(16) -0.0009(18) 0.0026(16) C47 0.0199(18) 0.0148(17) 0.024(2) -0.0014(15) -0.0115(16) 0.0039(14) C48 0.0246(19) 0.0152(18) 0.0241(19) -0.0004(16) -0.0054(17) -0.0030(14) C49 0.0206(18) 0.0159(17) 0.0197(19) 0.0023(15) -0.0069(16) -0.0051(14) C50 0.031(2) 0.024(2) 0.035(2) 0.0046(18) 0.0062(19) -0.0017(17) C51 0.068(5) 0.051(4) 0.103(6) 0.033(4) -0.014(4) 0.000(3) C52 0.072(5) 0.095(6) 0.142(8) 0.027(6) 0.006(5) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 1.858(2) . ? Mn1 O2 1.928(2) . ? Mn1 O1 1.929(2) . ? Mn1 O12 1.966(2) . ? Mn1 O3 2.158(2) . ? Mn1 O8 2.278(2) . ? Mn2 O10 2.101(3) . ? Mn2 O4 2.151(2) . ? Mn2 O6 2.201(2) . ? Mn2 O5 2.224(2) . ? Mn2 O12 2.245(2) . ? Mn2 N1 2.310(3) . ? Mn3 O14 2.123(3) . ? Mn3 O15 2.159(2) . ? Mn3 O8 2.220(3) . ? Mn3 O12 2.259(2) . ? Mn3 O13 2.259(3) . ? Mn3 N2 2.418(3) . ? Mn3 O6 2.609(2) . ? Mn4 O14 1.876(2) . ? Mn4 O18 1.934(2) . ? Mn4 O17 1.948(2) . ? Mn4 O6 1.949(2) . ? Mn4 O11 2.172(3) . ? Mn4 O16 2.224(2) . ? O1 C2 1.274(4) . ? O2 C4 1.291(4) . ? C1 C2 1.504(5) . ? C2 C3 1.405(5) . ? C3 C4 1.393(6) . ? C4 C5 1.489(6) . ? O3 C6 1.270(4) . ? O4 C6 1.261(4) . ? C6 C7 1.514(5) . ? C7 C8 1.380(5) . ? C7 C12 1.389(5) . ? C8 C9 1.391(5) . ? C9 C10 1.377(6) . ? C10 C11 1.380(6) . ? C11 C12 1.391(5) . ? N1 C18 1.487(5) . ? N1 C16 1.489(4) . ? N1 C14 1.500(4) . ? O5 C13 1.426(4) . ? O6 C15 1.436(4) . ? O7 C17 1.419(4) . ? C13 C14 1.516(5) . ? C15 C16 1.519(5) . ? C17 C18 1.531(5) . ? N2 C36 1.469(4) . ? N2 C34 1.469(4) . ? N2 C38 1.476(5) . ? N3 C51 1.152(9) . ? O8 C19 1.290(4) . ? O9 C19 1.253(4) . ? O10 C26 1.259(4) . ? O11 C26 1.251(4) . ? O12 C33 1.440(4) . ? O13 C35 1.424(4) . ? O14 C37 1.414(4) . ? O15 C39 1.247(4) . ? O16 C39 1.264(4) . ? O17 C47 1.292(4) . ? O18 C49 1.289(4) . ? C19 C20 1.487(5) . ? C20 C25 1.399(5) . ? C20 C21 1.400(5) . ? C21 C22 1.393(6) . ? C22 C23 1.382(6) . ? C23 C24 1.388(6) . ? C24 C25 1.386(5) . ? C26 C27 1.508(5) . ? C27 C28 1.387(5) . ? C27 C32 1.389(5) . ? C28 C29 1.410(6) . ? C29 C30 1.387(6) . ? C30 C31 1.372(6) . ? C31 C32 1.398(5) . ? C33 C34 1.510(5) . ? C35 C36 1.517(5) . ? C37 C38 1.517(5) . ? C39 C40 1.525(5) . ? C40 C41 1.381(5) . ? C40 C45 1.393(5) . ? C41 C42 1.394(6) . ? C42 C43 1.375(6) . ? C43 C44 1.385(6) . ? C44 C45 1.405(6) . ? C46 C47 1.499(5) . ? C47 C48 1.392(5) . ? C48 C49 1.382(5) . ? C49 C50 1.494(5) . ? C51 C52 1.441(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 O2 91.22(1) . . ? O5 Mn1 O1 172.40(1) . . ? O2 Mn1 O1 90.63(1) . . ? O5 Mn1 O12 86.09(1) . . ? O2 Mn1 O12 175.32(1) . . ? O1 Mn1 O12 91.56(1) . . ? O5 Mn1 O3 92.51(1) . . ? O2 Mn1 O3 92.97(1) . . ? O1 Mn1 O3 94.76(1) . . ? O12 Mn1 O3 90.97(1) . . ? O5 Mn1 O8 89.12(1) . . ? O2 Mn1 O8 97.19(1) . . ? O1 Mn1 O8 83.33(1) . . ? O12 Mn1 O8 78.97(9) . . ? O3 Mn1 O8 169.67(9) . . ? O10 Mn2 O4 87.88(1) . . ? O10 Mn2 O6 94.30(9) . . ? O4 Mn2 O6 174.02(9) . . ? O10 Mn2 O5 173.67(1) . . ? O4 Mn2 O5 86.91(9) . . ? O6 Mn2 O5 91.23(9) . . ? O10 Mn2 O12 111.58(1) . . ? O4 Mn2 O12 84.71(9) . . ? O6 Mn2 O12 89.31(9) . . ? O5 Mn2 O12 71.50(8) . . ? O10 Mn2 N1 103.92(1) . . ? O4 Mn2 N1 102.97(1) . . ? O6 Mn2 N1 81.93(9) . . ? O5 Mn2 N1 73.81(9) . . ? O12 Mn2 N1 143.97(1) . . ? O14 Mn3 O15 90.62(1) . . ? O14 Mn3 O8 164.39(9) . . ? O15 Mn3 O8 80.42(9) . . ? O14 Mn3 O12 106.32(9) . . ? O15 Mn3 O12 141.58(9) . . ? O8 Mn3 O12 74.42(9) . . ? O14 Mn3 O13 106.73(9) . . ? O15 Mn3 O13 83.65(9) . . ? O8 Mn3 O13 85.11(9) . . ? O12 Mn3 O13 121.80(9) . . ? O14 Mn3 N2 73.17(1) . . ? O15 Mn3 N2 145.45(1) . . ? O8 Mn3 N2 120.99(1) . . ? O12 Mn3 N2 72.96(9) . . ? O13 Mn3 N2 72.69(9) . . ? O14 Mn3 O6 65.92(9) . . ? O15 Mn3 O6 76.45(8) . . ? O8 Mn3 O6 99.35(8) . . ? O12 Mn3 O6 79.51(8) . . ? O13 Mn3 O6 158.49(8) . . ? N2 Mn3 O6 120.80(9) . . ? O14 Mn4 O18 174.89(1) . . ? O14 Mn4 O17 90.24(1) . . ? O18 Mn4 O17 90.27(1) . . ? O14 Mn4 O6 85.90(1) . . ? O18 Mn4 O6 93.63(1) . . ? O17 Mn4 O6 176.10(1) . . ? O14 Mn4 O11 93.97(1) . . ? O18 Mn4 O11 91.13(1) . . ? O17 Mn4 O11 85.81(1) . . ? O6 Mn4 O11 93.90(1) . . ? O14 Mn4 O16 91.23(1) . . ? O18 Mn4 O16 83.70(1) . . ? O17 Mn4 O16 88.61(1) . . ? O6 Mn4 O16 92.02(1) . . ? O11 Mn4 O16 172.38(1) . . ? C2 O1 Mn1 126.0(2) . . ? C4 O2 Mn1 126.1(2) . . ? O1 C2 C3 124.1(3) . . ? O1 C2 C1 116.7(3) . . ? C3 C2 C1 119.3(3) . . ? C4 C3 C2 123.8(3) . . ? O2 C4 C3 124.2(4) . . ? O2 C4 C5 115.2(3) . . ? C3 C4 C5 120.6(3) . . ? C6 O3 Mn1 125.4(2) . . ? C6 O4 Mn2 132.5(2) . . ? O4 C6 O3 126.1(3) . . ? O4 C6 C7 116.8(3) . . ? O3 C6 C7 117.1(3) . . ? C8 C7 C12 119.6(3) . . ? C8 C7 C6 120.6(3) . . ? C12 C7 C6 119.7(3) . . ? C7 C8 C9 119.7(4) . . ? C10 C9 C8 120.6(4) . . ? C9 C10 C11 119.9(4) . . ? C10 C11 C12 119.7(4) . . ? C7 C12 C11 120.3(4) . . ? C18 N1 C16 108.8(3) . . ? C18 N1 C14 114.3(3) . . ? C16 N1 C14 108.9(3) . . ? C18 N1 Mn2 112.1(2) . . ? C16 N1 Mn2 101.13(2) . . ? C14 N1 Mn2 110.7(2) . . ? C13 O5 Mn1 127.0(2) . . ? C13 O5 Mn2 108.54(2) . . ? Mn1 O5 Mn2 100.84(1) . . ? C15 O6 Mn4 116.3(2) . . ? C15 O6 Mn2 104.11(2) . . ? Mn4 O6 Mn2 128.24(1) . . ? C15 O6 Mn3 124.7(2) . . ? Mn4 O6 Mn3 91.19(8) . . ? Mn2 O6 Mn3 91.19(8) . . ? O5 C13 C14 106.8(3) . . ? N1 C14 C13 111.1(3) . . ? O6 C15 C16 109.9(3) . . ? N1 C16 C15 111.4(3) . . ? O7 C17 C18 114.7(3) . . ? N1 C18 C17 115.4(3) . . ? C36 N2 C34 111.7(3) . . ? C36 N2 C38 111.2(3) . . ? C34 N2 C38 111.2(3) . . ? C36 N2 Mn3 108.3(2) . . ? C34 N2 Mn3 107.3(2) . . ? C38 N2 Mn3 106.8(2) . . ? C19 O8 Mn3 121.2(2) . . ? C19 O8 Mn1 138.6(2) . . ? Mn3 O8 Mn1 98.72(1) . . ? C26 O10 Mn2 135.7(2) . . ? C26 O11 Mn4 138.1(2) . . ? C33 O12 Mn1 117.5(2) . . ? C33 O12 Mn2 113.83(2) . . ? Mn1 O12 Mn2 96.81(9) . . ? C33 O12 Mn3 117.89(2) . . ? Mn1 O12 Mn3 107.57(1) . . ? Mn2 O12 Mn3 99.90(9) . . ? C35 O13 Mn3 116.4(2) . . ? C37 O14 Mn4 125.0(2) . . ? C37 O14 Mn3 122.3(2) . . ? Mn4 O14 Mn3 110.52(1) . . ? C39 O15 Mn3 134.3(2) . . ? C39 O16 Mn4 124.2(2) . . ? C47 O17 Mn4 126.8(2) . . ? C49 O18 Mn4 126.0(2) . . ? O9 C19 O8 123.4(3) . . ? O9 C19 C20 118.4(3) . . ? O8 C19 C20 118.2(3) . . ? C25 C20 C21 119.8(3) . . ? C25 C20 C19 121.3(3) . . ? C21 C20 C19 118.8(3) . . ? C22 C21 C20 120.0(4) . . ? C23 C22 C21 120.0(4) . . ? C22 C23 C24 120.0(4) . . ? C25 C24 C23 120.9(4) . . ? C24 C25 C20 119.3(4) . . ? O11 C26 O10 126.6(3) . . ? O11 C26 C27 116.3(3) . . ? O10 C26 C27 117.1(3) . . ? C28 C27 C32 119.6(3) . . ? C28 C27 C26 120.9(3) . . ? C32 C27 C26 119.5(3) . . ? C27 C28 C29 120.0(4) . . ? C30 C29 C28 119.5(4) . . ? C31 C30 C29 120.6(4) . . ? C30 C31 C32 120.0(4) . . ? C27 C32 C31 120.3(3) . . ? O12 C33 C34 111.0(3) . . ? N2 C34 C33 111.0(3) . . ? O13 C35 C36 107.1(3) . . ? N2 C36 C35 111.3(3) . . ? O14 C37 C38 108.3(3) . . ? N2 C38 C37 110.6(3) . . ? O15 C39 O16 126.6(3) . . ? O15 C39 C40 116.4(3) . . ? O16 C39 C40 116.9(3) . . ? C41 C40 C45 120.3(4) . . ? C41 C40 C39 119.3(3) . . ? C45 C40 C39 120.1(3) . . ? C40 C41 C42 120.0(4) . . ? C43 C42 C41 120.0(4) . . ? C42 C43 C44 120.7(4) . . ? C43 C44 C45 119.6(4) . . ? C40 C45 C44 119.3(4) . . ? O17 C47 C48 124.1(3) . . ? O17 C47 C46 115.3(3) . . ? C48 C47 C46 120.6(3) . . ? C49 C48 C47 124.1(3) . . ? O18 C49 C48 124.9(3) . . ? O18 C49 C50 115.3(3) . . ? C48 C49 C50 119.8(3) . . ? N3 C51 C52 176.8(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O16 0.84 2.13 2.943(4) 163.5 4_575 O13 H13C O9 0.835(10) 1.809(17) 2.621(4) 164(5) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.564 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.113 #END data_3) #[Mn4(teaH)2(acac)4(MeOH)2](ClO4)2 _database_code_depnum_ccdc_archive 'CCDC 281692' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn4(teaH)2(acac)4(MeOH)2](ClO4)2' _chemical_formula_sum 'C34 H66 Cl2 Mn4 N2 O24' _chemical_formula_weight 1177.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.570(2) _cell_length_b 12.636(3) _cell_length_c 20.096(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.60(3) _cell_angle_gamma 90.00 _cell_volume 2380.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block shape' _exptl_crystal_colour red/brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.234 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.72410 _exptl_absorpt_correction_T_max 0.91249 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30976 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.20 _reflns_number_total 5784 _reflns_number_gt 4251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XSeed _computing_publication_material XSeed _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+1.5703P] 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 5784 _refine_ls_number_parameters 306 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.31840(4) 0.66276(3) -0.063674(19) 0.01613(10) Uani 1 1 d . . . Mn2 Mn 0.48790(4) 0.55416(3) 0.084915(19) 0.01497(10) Uani 1 1 d . . . O1 O 0.14670(18) 0.58245(15) -0.14487(9) 0.0231(4) Uani 1 1 d D . . C1 C 0.0970(3) 0.6279(2) -0.21082(16) 0.0348(7) Uiso 1 1 d . . . H1A H 0.0346 0.6882 -0.2070 0.052 Uiso 1 1 calc R . . H1B H 0.0438 0.5746 -0.2412 0.052 Uiso 1 1 calc R . . H1C H 0.1788 0.6521 -0.2293 0.052 Uiso 1 1 calc R . . O2 O 0.30195(18) 0.78837(13) -0.11746(9) 0.0220(4) Uani 1 1 d . . . O3 O 0.17516(18) 0.71312(13) -0.01699(9) 0.0217(4) Uani 1 1 d . . . C2 C 0.2107(3) 0.9425(2) -0.17620(16) 0.0339(7) Uani 1 1 d . . . H2A H 0.3051 0.9758 -0.1671 0.051 Uiso 1 1 calc R . . H2B H 0.1376 0.9964 -0.1752 0.051 Uiso 1 1 calc R . . H2C H 0.1937 0.9089 -0.2211 0.051 Uiso 1 1 calc R . . C3 C 0.2043(3) 0.8607(2) -0.12313(13) 0.0223(6) Uani 1 1 d . . . C4 C 0.1001(3) 0.8642(2) -0.08430(14) 0.0250(6) Uani 1 1 d . . . H4A H 0.0073 0.8603 -0.1166 0.030 Uiso 1 1 calc R . . H4B H 0.1055 0.9356 -0.0637 0.030 Uiso 1 1 calc R . . C5 C 0.0920(3) 0.7931(2) -0.03250(13) 0.0216(6) Uani 1 1 d . . . C6 C -0.0179(3) 0.8065(2) 0.01041(15) 0.0279(6) Uani 1 1 d . . . H6A H -0.0579 0.7372 0.0182 0.042 Uiso 1 1 calc R . . H6B H -0.0943 0.8529 -0.0130 0.042 Uiso 1 1 calc R . . H6C H 0.0265 0.8380 0.0541 0.042 Uiso 1 1 calc R . . O4 O 0.50256(17) 0.69802(13) 0.02749(9) 0.0197(4) Uani 1 1 d . . . O5 O 0.69628(17) 0.59842(13) 0.13961(9) 0.0196(4) Uani 1 1 d . . . C7 C 0.5581(3) 0.8742(2) 0.00317(16) 0.0330(7) Uani 1 1 d . . . H7A H 0.5678 0.8595 -0.0436 0.050 Uiso 1 1 calc R . . H7B H 0.6262 0.9294 0.0226 0.050 Uiso 1 1 calc R . . H7C H 0.4609 0.8984 0.0033 0.050 Uiso 1 1 calc R . . C8 C 0.5879(3) 0.77585(19) 0.04462(13) 0.0198(5) Uani 1 1 d . . . C9 C 0.7068(3) 0.7735(2) 0.09818(14) 0.0224(6) Uani 1 1 d . . . H9A H 0.7880 0.7973 0.0783 0.027 Uiso 1 1 calc R . . H9B H 0.6903 0.8304 0.1296 0.027 Uiso 1 1 calc R . . C10 C 0.7582(3) 0.6877(2) 0.13960(13) 0.0199(5) Uani 1 1 d . . . C11 C 0.8998(3) 0.6976(2) 0.18856(15) 0.0321(7) Uani 1 1 d . . . H11A H 0.8847 0.6934 0.2353 0.048 Uiso 1 1 calc R . . H11B H 0.9435 0.7658 0.1817 0.048 Uiso 1 1 calc R . . H11C H 0.9630 0.6401 0.1805 0.048 Uiso 1 1 calc R . . N1 N 0.2895(2) 0.47656(16) 0.11918(10) 0.0176(4) Uani 1 1 d . . . O6 O 0.33864(16) 0.53326(13) -0.01193(8) 0.0153(4) Uani 1 1 d . . . O7 O 0.54845(17) 0.39450(13) 0.11058(9) 0.0189(4) Uani 1 1 d . . . O8 O 0.4131(2) 0.66996(15) 0.15900(10) 0.0272(4) Uani 1 1 d D . . H8 H 0.422(4) 0.7385(10) 0.1508(18) 0.053(11) Uiso 1 1 d D . . C12 C 0.2189(2) 0.4686(2) -0.00559(13) 0.0185(5) Uani 1 1 d . . . H12A H 0.2454 0.3930 -0.0075 0.022 Uiso 1 1 calc R . . H12B H 0.1391 0.4828 -0.0442 0.022 Uiso 1 1 calc R . . C13 C 0.1704(3) 0.4899(2) 0.06037(13) 0.0202(5) Uani 1 1 d . . . H13A H 0.1329 0.5629 0.0600 0.024 Uiso 1 1 calc R . . H13B H 0.0924 0.4405 0.0646 0.024 Uiso 1 1 calc R . . C14 C 0.4775(3) 0.3450(2) 0.15772(13) 0.0214(6) Uani 1 1 d . . . H14A H 0.5100 0.3759 0.2035 0.026 Uiso 1 1 calc R . . H14B H 0.4989 0.2683 0.1602 0.026 Uiso 1 1 calc R . . C15 C 0.3186(3) 0.3625(2) 0.13395(14) 0.0230(6) Uani 1 1 d . . . H15A H 0.2833 0.3202 0.0925 0.028 Uiso 1 1 calc R . . H15B H 0.2676 0.3389 0.1696 0.028 Uiso 1 1 calc R . . C16 C 0.2758(3) 0.6494(2) 0.17522(15) 0.0270(6) Uani 1 1 d . . . H16A H 0.1989 0.6777 0.1392 0.032 Uiso 1 1 calc R . . H16B H 0.2690 0.6835 0.2188 0.032 Uiso 1 1 calc R . . C17 C 0.2621(3) 0.5310(2) 0.18053(14) 0.0259(6) Uani 1 1 d . . . H17A H 0.3308 0.5053 0.2209 0.031 Uiso 1 1 calc R . . H17B H 0.1648 0.5133 0.1868 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.28454(7) 0.96016(5) 0.13687(3) 0.02572(16) Uani 1 1 d . . . O9 O 0.4024(2) 0.88978(17) 0.13532(12) 0.0453(6) Uani 1 1 d . . . O10 O 0.3388(3) 1.05355(17) 0.17316(12) 0.0492(6) Uani 1 1 d . . . O11 O 0.1835(3) 0.90813(18) 0.16956(11) 0.0456(6) Uani 1 1 d . . . O12 O 0.2184(2) 0.9854(2) 0.06838(11) 0.0477(6) Uani 1 1 d . . . H1D H 0.194(3) 0.5225(17) -0.148(2) 0.065(12) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01567(19) 0.01614(19) 0.0165(2) 0.00408(15) 0.00304(14) 0.00391(14) Mn2 0.01404(19) 0.01540(19) 0.0144(2) 0.00216(15) 0.00026(14) 0.00004(14) O1 0.0202(9) 0.0278(10) 0.0187(10) 0.0019(8) -0.0024(7) 0.0046(8) O2 0.0242(9) 0.0198(9) 0.0232(10) 0.0067(7) 0.0074(8) 0.0062(7) O3 0.0209(9) 0.0219(9) 0.0233(10) 0.0059(8) 0.0070(7) 0.0081(7) C2 0.0498(18) 0.0239(15) 0.0301(17) 0.0100(12) 0.0129(14) 0.0133(13) C3 0.0277(14) 0.0178(13) 0.0194(14) 0.0010(11) -0.0003(11) 0.0036(11) C4 0.0289(14) 0.0215(13) 0.0236(15) 0.0006(11) 0.0032(11) 0.0080(11) C5 0.0226(13) 0.0204(13) 0.0211(14) -0.0025(11) 0.0031(11) 0.0035(10) C6 0.0246(14) 0.0254(14) 0.0353(17) 0.0001(12) 0.0097(12) 0.0066(11) O4 0.0196(9) 0.0170(9) 0.0208(10) 0.0017(7) 0.0002(7) -0.0010(7) O5 0.0179(9) 0.0204(9) 0.0185(9) -0.0013(7) -0.0011(7) -0.0001(7) C7 0.0338(16) 0.0197(14) 0.0436(19) 0.0047(13) 0.0031(14) -0.0041(12) C8 0.0208(13) 0.0163(12) 0.0245(14) -0.0021(11) 0.0093(11) 0.0007(10) C9 0.0219(13) 0.0188(13) 0.0283(15) -0.0099(11) 0.0095(11) -0.0031(10) C10 0.0175(12) 0.0244(13) 0.0183(13) -0.0078(11) 0.0049(10) -0.0031(10) C11 0.0272(15) 0.0371(17) 0.0285(16) -0.0050(13) -0.0027(12) -0.0060(13) N1 0.0181(10) 0.0177(10) 0.0178(11) 0.0036(9) 0.0055(8) 0.0032(8) O6 0.0134(8) 0.0165(8) 0.0151(9) 0.0037(7) 0.0007(7) 0.0005(6) O7 0.0182(9) 0.0184(9) 0.0214(10) 0.0075(7) 0.0071(7) 0.0039(7) O8 0.0287(10) 0.0238(11) 0.0316(11) -0.0036(9) 0.0124(8) 0.0006(8) C12 0.0130(12) 0.0196(13) 0.0215(14) 0.0025(10) 0.0004(10) -0.0033(9) C13 0.0147(12) 0.0220(13) 0.0240(14) 0.0043(11) 0.0044(10) 0.0020(10) C14 0.0251(14) 0.0212(13) 0.0192(14) 0.0094(11) 0.0074(11) 0.0050(10) C15 0.0232(13) 0.0189(13) 0.0283(15) 0.0084(11) 0.0085(11) 0.0017(10) C16 0.0272(14) 0.0301(15) 0.0265(15) -0.0021(12) 0.0125(12) 0.0024(12) C17 0.0272(14) 0.0291(15) 0.0246(15) 0.0031(12) 0.0127(12) 0.0048(11) Cl1 0.0324(4) 0.0231(3) 0.0220(3) -0.0011(3) 0.0062(3) 0.0018(3) O9 0.0410(13) 0.0332(12) 0.0599(16) -0.0013(11) 0.0060(11) 0.0131(10) O10 0.0715(16) 0.0334(13) 0.0469(15) -0.0155(11) 0.0222(13) -0.0144(11) O11 0.0647(15) 0.0408(13) 0.0391(13) -0.0051(11) 0.0291(12) -0.0146(11) O12 0.0405(13) 0.0629(16) 0.0337(13) 0.0202(12) -0.0069(10) -0.0030(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 O7 1.876(2) 3_665 ? Mn1 O2 1.909(2) . ? Mn1 O3 1.918(2) . ? Mn1 O6 1.927(2) . ? Mn1 O1 2.305(2) . ? Mn1 O4 2.315(2) . ? Mn2 O7 2.133(2) . ? Mn2 O5 2.148(2) . ? Mn2 O4 2.172(2) . ? Mn2 O6 2.186(2) . ? Mn2 O8 2.302(2) . ? Mn2 N1 2.359(2) . ? Mn2 O6 2.665(2) 3_665 ? O1 C1 1.435(3) . ? O1 H1D 0.891(1) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C3 1.295(3) . ? O3 C5 1.285(3) . ? C2 C3 1.496(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.385(4) . ? C4 C5 1.389(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.498(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O4 C8 1.280(3) . ? O5 C10 1.275(3) . ? C7 C8 1.491(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.400(4) . ? C9 C10 1.395(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.511(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N1 C13 1.478(3) . ? N1 C17 1.481(3) . ? N1 C15 1.486(3) . ? O6 C12 1.434(3) . ? O7 C14 1.417(3) . ? O7 Mn1 1.8758(2) 3_665 ? O8 C16 1.439(3) . ? O8 H8 0.888(1) . ? C12 C13 1.514(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.516(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.508(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? Cl1 O10 1.429(2) . ? Cl1 O12 1.431(2) . ? Cl1 O11 1.434(2) . ? Cl1 O9 1.441(2) . ? 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 O7 Mn1 O2 91.33(7) 3_665 . ? O7 Mn1 O3 176.31(8) 3_665 . ? O2 Mn1 O3 90.88(7) . . ? O7 Mn1 O6 86.50(7) 3_665 . ? O2 Mn1 O6 177.75(7) . . ? O3 Mn1 O6 91.26(7) . . ? O7 Mn1 O1 86.22(7) 3_665 . ? O2 Mn1 O1 89.96(7) . . ? O3 Mn1 O1 90.83(7) . . ? O6 Mn1 O1 89.32(7) . . ? O7 Mn1 O4 89.19(7) 3_665 . ? O2 Mn1 O4 104.53(7) . . ? O3 Mn1 O4 93.11(7) . . ? O6 Mn1 O4 76.03(6) . . ? O1 Mn1 O4 164.90(6) . . ? O7 Mn2 O5 86.76(7) . . ? O7 Mn2 O4 151.18(6) . . ? O5 Mn2 O4 84.35(7) . . ? O7 Mn2 O6 101.42(6) . . ? O5 Mn2 O6 149.30(6) . . ? O4 Mn2 O6 74.26(6) . . ? O7 Mn2 O8 123.33(7) . . ? O5 Mn2 O8 83.18(7) . . ? O4 Mn2 O8 82.73(7) . . ? O6 Mn2 O8 114.83(7) . . ? O7 Mn2 N1 74.44(7) . . ? O5 Mn2 N1 132.65(7) . . ? O4 Mn2 N1 130.13(7) . . ? O6 Mn2 N1 77.85(7) . . ? O8 Mn2 N1 72.67(7) . . ? O7 Mn2 O6 64.67(6) . 3_665 ? O5 Mn2 O6 76.86(6) . 3_665 ? O4 Mn2 O6 86.59(6) . 3_665 ? O6 Mn2 O6 80.08(6) . 3_665 ? O8 Mn2 O6 158.18(6) . 3_665 ? N1 Mn2 O6 127.96(6) . 3_665 ? C1 O1 Mn1 122.27(2) . . ? C1 O1 H1D 111(3) . . ? Mn1 O1 H1D 97(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 O2 Mn1 127.74(2) . . ? C5 O3 Mn1 127.64(2) . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 C4 124.1(2) . . ? O2 C3 C2 114.7(2) . . ? C4 C3 C2 121.2(2) . . ? C3 C4 C5 123.8(2) . . ? C3 C4 H4A 106.4 . . ? C5 C4 H4A 106.4 . . ? C3 C4 H4B 106.4 . . ? C5 C4 H4B 106.4 . . ? H4A C4 H4B 106.4 . . ? O3 C5 C4 124.4(2) . . ? O3 C5 C6 114.9(2) . . ? C4 C5 C6 120.7(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 O4 Mn2 127.27(2) . . ? C8 O4 Mn1 134.69(2) . . ? Mn2 O4 Mn1 97.99(7) . . ? C10 O5 Mn2 127.88(2) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O4 C8 C9 124.5(2) . . ? O4 C8 C7 116.8(2) . . ? C9 C8 C7 118.8(2) . . ? C10 C9 C8 127.5(2) . . ? C10 C9 H9A 105.4 . . ? C8 C9 H9A 105.4 . . ? C10 C9 H9B 105.4 . . ? C8 C9 H9B 105.4 . . ? H9A C9 H9B 106.0 . . ? O5 C10 C9 125.5(2) . . ? O5 C10 C11 115.4(2) . . ? C9 C10 C11 119.1(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 N1 C17 112.07(2) . . ? C13 N1 C15 110.7(2) . . ? C17 N1 C15 110.0(2) . . ? C13 N1 Mn2 104.83(1) . . ? C17 N1 Mn2 109.74(2) . . ? C15 N1 Mn2 109.41(1) . . ? C12 O6 Mn1 122.44(1) . . ? C12 O6 Mn2 112.36(1) . . ? Mn1 O6 Mn2 110.76(8) . . ? C14 O7 Mn1 129.13(2) . 3_665 ? C14 O7 Mn2 115.80(1) . . ? Mn1 O7 Mn2 114.97(8) 3_665 . ? C16 O8 Mn2 116.65(2) . . ? C16 O8 H8 110(2) . . ? Mn2 O8 H8 117(2) . . ? O6 C12 C13 111.6(2) . . ? O6 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? O6 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? N1 C13 C12 110.91(2) . . ? N1 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.0 . . ? O7 C14 C15 108.1(2) . . ? O7 C14 H14A 110.1 . . ? C15 C14 H14A 110.1 . . ? O7 C14 H14B 110.1 . . ? C15 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? N1 C15 C14 109.9(2) . . ? N1 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? N1 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? O8 C16 C17 107.0(2) . . ? O8 C16 H16A 110.3 . . ? C17 C16 H16A 110.3 . . ? O8 C16 H16B 110.3 . . ? C17 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? N1 C17 C16 111.7(2) . . ? N1 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? N1 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? O10 Cl1 O12 110.59(2) . . ? O10 Cl1 O11 110.77(1) . . ? O12 Cl1 O11 109.54(1) . . ? O10 Cl1 O9 108.35(1) . . ? O12 Cl1 O9 108.27(2) . . ? O11 Cl1 O9 109.27(1) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 O9 0.888(10) 1.940(12) 2.817(3) 169(3) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.720 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.085 #END data_4) #[Mn4(bheapH)2(acac)4(MeOH)2].2ClO4 _database_code_depnum_ccdc_archive 'CCDC 281693' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Mn4(bheapH)2(acac)4(MeOH)2).2ClO4 _chemical_melting_point ? _chemical_formula_moiety '[Mn4(bheapH)2(acac)4(MeOH)2].2ClO4' _chemical_formula_sum 'C36 H66 Cl2 Mn4 N2 O24' _chemical_formula_weight 1201.57 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 9.6236(1) _cell_length_b 12.8569(2) _cell_length_c 20.3485(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.532(1) _cell_angle_gamma 90.00 _cell_volume 2457.73(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red/brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 1.197 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26572 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 28.22 _reflns_number_total 6005 _reflns_number_gt 4761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+3.8617P] 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 6005 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.18181(4) 0.65949(3) 0.064592(19) 0.01954(11) Uani 1 1 d . . . Mn2 Mn 0.01144(4) 0.55227(3) -0.082855(18) 0.01739(10) Uani 1 1 d . . . Cl1 Cl 0.78353(9) 0.04092(6) 0.13130(4) 0.03781(19) Uani 1 1 d . . . O1 O 0.3493(2) 0.58051(17) 0.14801(9) 0.0304(4) Uani 1 1 d . . . H8 H 0.3942 0.5181 0.1386 0.036 Uiso 1 1 calc R . . O2 O 0.1984(2) 0.78444(15) 0.11655(9) 0.0273(4) Uani 1 1 d . . . O3 O 0.32620(19) 0.70660(15) 0.01967(9) 0.0250(4) Uani 1 1 d . . . O4 O -0.00074(19) 0.69604(14) -0.02687(9) 0.0217(4) Uani 1 1 d . . . O5 O -0.19518(18) 0.59822(14) -0.13887(9) 0.0222(4) Uani 1 1 d . . . O6 O 0.16094(17) 0.53116(13) 0.01445(8) 0.0173(3) Uani 1 1 d . . . O7 O -0.0476(2) 0.39486(14) -0.10996(9) 0.0241(4) Uani 1 1 d . . . O8 O 0.0886(2) 0.66309(17) -0.15418(12) 0.0385(5) Uani 1 1 d . . . H2 H 0.0348 0.7230 -0.1710 0.046 Uiso 1 1 calc R . . O9 O 0.6765(4) 0.0671(2) 0.16729(14) 0.0652(8) Uani 1 1 d . . . O10 O 0.8565(5) 0.1317(3) 0.1191(2) 0.1082(16) Uani 1 1 d . . . O11 O 0.7174(3) -0.0027(3) 0.06927(16) 0.0808(11) Uani 1 1 d . . . O12 O 0.8825(4) -0.0307(3) 0.1668(2) 0.0985(13) Uani 1 1 d . . . N1 N 0.2113(2) 0.47659(18) -0.11428(11) 0.0241(5) Uani 1 1 d . . . C1 C 0.2809(3) 0.4684(2) 0.00954(13) 0.0222(5) Uani 1 1 d . . . H1A H 0.2552 0.3941 0.0116 0.027 Uiso 1 1 calc R . . H1B H 0.3601 0.4833 0.0484 0.027 Uiso 1 1 calc R . . C2 C 0.3301(3) 0.4885(2) -0.05523(13) 0.0222(5) Uani 1 1 d . . . H2A H 0.3691 0.5598 -0.0545 0.027 Uiso 1 1 calc R . . H2B H 0.4069 0.4390 -0.0588 0.027 Uiso 1 1 calc R . . C3 C 0.2381(4) 0.5270(3) -0.17452(16) 0.0405(8) Uani 1 1 d . . . H3A H 0.1712 0.4987 -0.2145 0.049 Uiso 1 1 calc R . . H3B H 0.3360 0.5100 -0.1790 0.049 Uiso 1 1 calc R . . C4 C 0.2222(4) 0.6403(3) -0.17359(17) 0.0392(7) Uani 1 1 d . . . H4 H 0.3033 0.6717 -0.1404 0.047 Uiso 1 1 calc R . . C5 C 0.2131(4) 0.6890(3) -0.24439(17) 0.0430(8) Uani 1 1 d . . . H5A H 0.2932 0.6643 -0.2628 0.064 Uiso 1 1 calc R . . H5B H 0.2170 0.7649 -0.2405 0.064 Uiso 1 1 calc R . . H5C H 0.1234 0.6683 -0.2744 0.064 Uiso 1 1 calc R . . C6 C 0.1818(3) 0.3626(3) -0.12654(19) 0.0412(8) Uani 1 1 d . . . H6A H 0.2348 0.3368 -0.1598 0.049 Uiso 1 1 calc R . . H6B H 0.2154 0.3238 -0.0841 0.049 Uiso 1 1 calc R . . C7 C 0.0274(4) 0.3433(3) -0.15188(17) 0.0395(8) Uani 1 1 d . . . H7A H -0.0030 0.3693 -0.1986 0.047 Uiso 1 1 calc R . . H7B H 0.0077 0.2677 -0.1519 0.047 Uiso 1 1 calc R . . C8 C 0.5113(3) 0.8019(2) -0.01077(16) 0.0323(6) Uani 1 1 d . . . H8A H 0.5492 0.7338 -0.0196 0.048 Uiso 1 1 calc R . . H8B H 0.5892 0.8462 0.0129 0.048 Uiso 1 1 calc R . . H8C H 0.4658 0.8347 -0.0535 0.048 Uiso 1 1 calc R . . C9 C 0.4036(3) 0.7883(2) 0.03210(14) 0.0255(6) Uani 1 1 d . . . C10 C 0.3939(3) 0.8614(2) 0.08117(15) 0.0305(6) Uani 1 1 d . . . C11 C 0.2922(3) 0.8569(2) 0.12030(13) 0.0266(6) Uani 1 1 d . . . C12 C 0.2854(4) 0.9394(2) 0.17152(16) 0.0397(8) Uani 1 1 d . . . H12A H 0.1888 0.9680 0.1635 0.060 Uiso 1 1 calc R . . H12B H 0.3528 0.9951 0.1678 0.060 Uiso 1 1 calc R . . H12C H 0.3101 0.9091 0.2167 0.060 Uiso 1 1 calc R . . C13 C -0.0506(4) 0.8719(2) -0.00552(17) 0.0378(7) Uani 1 1 d . . . H13A H -0.0508 0.8580 0.0418 0.057 Uiso 1 1 calc R . . H13B H -0.1231 0.9243 -0.0232 0.057 Uiso 1 1 calc R . . H13C H 0.0432 0.8978 -0.0091 0.057 Uiso 1 1 calc R . . C14 C -0.0830(3) 0.7738(2) -0.04533(14) 0.0237(5) Uani 1 1 d . . . C15 C -0.2026(3) 0.7714(2) -0.09938(15) 0.0275(6) Uani 1 1 d . . . C16 C -0.2547(3) 0.6867(2) -0.14053(13) 0.0239(5) Uani 1 1 d . . . C17 C -0.3939(3) 0.6982(3) -0.19060(16) 0.0379(7) Uani 1 1 d . . . H17A H -0.3768 0.6965 -0.2363 0.057 Uiso 1 1 calc R . . H17B H -0.4380 0.7646 -0.1832 0.057 Uiso 1 1 calc R . . H17C H -0.4574 0.6410 -0.1849 0.057 Uiso 1 1 calc R . . C18 C 0.3857(5) 0.6254(3) 0.21383(17) 0.0566(11) Uani 1 1 d . . . H18A H 0.4382 0.6903 0.2121 0.085 Uiso 1 1 calc R . . H18B H 0.4452 0.5766 0.2448 0.085 Uiso 1 1 calc R . . H18C H 0.2986 0.6400 0.2297 0.085 Uiso 1 1 calc R . . H10 H 0.461(4) 0.915(3) 0.0886(18) 0.044(10) Uiso 1 1 d . . . H15 H -0.257(3) 0.831(3) -0.1047(16) 0.030(8) Uiso 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 0.0205(2) 0.0187(2) 0.02021(19) -0.00341(14) 0.00624(15) -0.00537(16) Mn2 0.01674(18) 0.01718(19) 0.01833(18) -0.00281(14) 0.00398(14) -0.00051(15) Cl1 0.0476(4) 0.0325(4) 0.0314(4) 0.0009(3) 0.0043(3) -0.0132(3) O1 0.0273(10) 0.0347(11) 0.0261(10) 0.0011(8) -0.0006(8) -0.0038(9) O2 0.0329(10) 0.0232(10) 0.0276(10) -0.0074(8) 0.0108(8) -0.0100(8) O3 0.0236(9) 0.0240(10) 0.0290(10) -0.0033(8) 0.0094(8) -0.0072(8) O4 0.0217(9) 0.0177(9) 0.0253(9) -0.0024(7) 0.0046(7) 0.0007(7) O5 0.0197(9) 0.0239(10) 0.0224(9) 0.0013(7) 0.0037(7) -0.0006(8) O6 0.0158(8) 0.0177(9) 0.0183(8) -0.0022(6) 0.0034(6) 0.0008(7) O7 0.0292(10) 0.0200(9) 0.0269(10) -0.0061(7) 0.0146(8) -0.0066(8) O8 0.0440(13) 0.0277(11) 0.0538(14) 0.0044(10) 0.0326(11) 0.0018(10) O9 0.090(2) 0.0630(18) 0.0511(16) -0.0008(14) 0.0350(16) -0.0067(16) O10 0.176(4) 0.0477(18) 0.136(3) -0.026(2) 0.111(3) -0.058(2) O11 0.0566(18) 0.111(3) 0.066(2) -0.0503(19) -0.0060(15) 0.0075(18) O12 0.070(2) 0.120(3) 0.098(3) 0.059(2) 0.0002(19) 0.012(2) N1 0.0213(11) 0.0299(12) 0.0220(11) -0.0067(9) 0.0067(8) -0.0002(10) C1 0.0187(12) 0.0254(14) 0.0231(13) 0.0029(10) 0.0060(10) 0.0051(10) C2 0.0161(11) 0.0273(14) 0.0241(13) -0.0009(10) 0.0061(10) 0.0004(11) C3 0.0381(17) 0.061(2) 0.0263(15) 0.0043(14) 0.0164(13) 0.0120(16) C4 0.0412(18) 0.0440(19) 0.0376(17) 0.0032(14) 0.0204(14) -0.0041(15) C5 0.0460(19) 0.044(2) 0.0454(19) 0.0004(15) 0.0238(16) -0.0011(16) C6 0.0325(16) 0.0364(18) 0.057(2) -0.0262(15) 0.0145(15) -0.0001(14) C7 0.0481(19) 0.0336(17) 0.0455(18) -0.0144(14) 0.0296(16) -0.0086(15) C8 0.0283(14) 0.0302(15) 0.0413(17) 0.0018(13) 0.0140(12) -0.0060(13) C9 0.0234(13) 0.0237(14) 0.0285(14) 0.0036(11) 0.0039(11) -0.0031(11) C10 0.0329(15) 0.0247(15) 0.0341(15) -0.0027(12) 0.0077(12) -0.0148(13) C11 0.0338(15) 0.0206(13) 0.0239(13) -0.0018(10) 0.0029(11) -0.0076(12) C12 0.057(2) 0.0274(16) 0.0373(17) -0.0096(13) 0.0165(15) -0.0158(15) C13 0.0433(18) 0.0200(14) 0.0485(19) -0.0078(13) 0.0064(15) 0.0032(13) C14 0.0268(13) 0.0178(13) 0.0290(13) 0.0007(10) 0.0116(11) 0.0007(11) C15 0.0258(14) 0.0218(14) 0.0361(15) 0.0057(11) 0.0095(11) 0.0062(12) C16 0.0201(12) 0.0283(14) 0.0247(13) 0.0081(11) 0.0077(10) 0.0029(11) C17 0.0283(15) 0.0410(18) 0.0400(17) 0.0051(14) -0.0025(13) 0.0081(14) C18 0.076(3) 0.050(2) 0.0312(18) 0.0000(16) -0.0165(17) -0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O7 1.8779(18) 3_565 ? Mn1 O2 1.9108(18) . ? Mn1 O3 1.9195(18) . ? Mn1 O6 1.9273(17) . ? Mn1 O1 2.307(2) . ? Mn1 O4 2.3134(18) . ? Mn2 O7 2.1416(18) . ? Mn2 O5 2.1491(18) . ? Mn2 O4 2.1878(18) . ? Mn2 O6 2.1973(16) . ? Mn2 O8 2.271(2) . ? Mn2 N1 2.364(2) . ? Cl1 O11 1.402(3) . ? Cl1 O12 1.406(3) . ? Cl1 O10 1.411(3) . ? Cl1 O9 1.427(3) . ? O1 C18 1.430(4) . ? O2 C11 1.288(3) . ? O3 C9 1.281(3) . ? O4 C14 1.280(3) . ? O5 C16 1.271(3) . ? O6 C1 1.429(3) . ? O7 C7 1.398(3) . ? O7 Mn1 1.8779(18) 3_565 ? O8 C4 1.455(4) . ? N1 C3 1.458(4) . ? N1 C2 1.475(3) . ? N1 C6 1.503(4) . ? C1 C2 1.516(3) . ? C3 C4 1.466(5) . ? C4 C5 1.556(5) . ? C6 C7 1.484(5) . ? C8 C9 1.503(4) . ? C9 C10 1.389(4) . ? C10 C11 1.390(4) . ? C11 C12 1.498(4) . ? C13 C14 1.495(4) . ? C14 C15 1.409(4) . ? C15 C16 1.398(4) . ? C16 C17 1.504(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Mn1 O2 91.40(8) 3_565 . ? O7 Mn1 O3 176.16(9) 3_565 . ? O2 Mn1 O3 90.92(8) . . ? O7 Mn1 O6 86.44(7) 3_565 . ? O2 Mn1 O6 177.81(8) . . ? O3 Mn1 O6 91.21(8) . . ? O7 Mn1 O1 85.41(8) 3_565 . ? O2 Mn1 O1 90.11(8) . . ? O3 Mn1 O1 91.53(8) . . ? O6 Mn1 O1 89.35(7) . . ? O7 Mn1 O4 89.30(8) 3_565 . ? O2 Mn1 O4 103.41(8) . . ? O3 Mn1 O4 93.13(7) . . ? O6 Mn1 O4 76.96(7) . . ? O1 Mn1 O4 165.61(7) . . ? O7 Mn2 O5 87.71(7) . . ? O7 Mn2 O4 153.04(7) . . ? O5 Mn2 O4 84.03(7) . . ? O7 Mn2 O6 101.57(7) . . ? O5 Mn2 O6 149.48(7) . . ? O4 Mn2 O6 74.55(6) . . ? O7 Mn2 O8 122.25(8) . . ? O5 Mn2 O8 83.21(8) . . ? O4 Mn2 O8 82.21(7) . . ? O6 Mn2 O8 114.36(8) . . ? O7 Mn2 N1 74.17(7) . . ? O5 Mn2 N1 133.09(7) . . ? O4 Mn2 N1 128.84(7) . . ? O6 Mn2 N1 77.34(7) . . ? O8 Mn2 N1 71.78(8) . . ? O11 Cl1 O12 109.0(3) . . ? O11 Cl1 O10 108.5(3) . . ? O12 Cl1 O10 109.0(3) . . ? O11 Cl1 O9 108.64(19) . . ? O12 Cl1 O9 112.0(2) . . ? O10 Cl1 O9 109.7(2) . . ? C18 O1 Mn1 120.1(2) . . ? C11 O2 Mn1 127.88(18) . . ? C9 O3 Mn1 127.94(18) . . ? C14 O4 Mn2 127.35(17) . . ? C14 O4 Mn1 135.08(17) . . ? Mn2 O4 Mn1 97.48(7) . . ? C16 O5 Mn2 128.31(17) . . ? C1 O6 Mn1 121.82(15) . . ? C1 O6 Mn2 112.79(14) . . ? Mn1 O6 Mn2 110.12(8) . . ? C7 O7 Mn1 128.65(18) . 3_565 ? C7 O7 Mn2 117.53(17) . . ? Mn1 O7 Mn2 113.41(8) 3_565 . ? C4 O8 Mn2 118.56(18) . . ? C3 N1 C2 113.0(2) . . ? C3 N1 C6 110.8(2) . . ? C2 N1 C6 108.8(2) . . ? C3 N1 Mn2 110.32(18) . . ? C2 N1 Mn2 105.60(15) . . ? C6 N1 Mn2 108.08(16) . . ? O6 C1 C2 112.0(2) . . ? N1 C2 C1 110.9(2) . . ? N1 C3 C4 113.1(3) . . ? O8 C4 C3 107.7(3) . . ? O8 C4 C5 107.2(3) . . ? C3 C4 C5 111.9(3) . . ? C7 C6 N1 111.1(3) . . ? O7 C7 C6 108.6(3) . . ? O3 C9 C10 124.7(3) . . ? O3 C9 C8 115.2(2) . . ? C10 C9 C8 120.1(3) . . ? C9 C10 C11 123.3(3) . . ? O2 C11 C10 124.6(3) . . ? O2 C11 C12 114.7(3) . . ? C10 C11 C12 120.8(3) . . ? O4 C14 C15 124.0(2) . . ? O4 C14 C13 117.2(2) . . ? C15 C14 C13 118.7(3) . . ? C16 C15 C14 127.7(3) . . ? O5 C16 C15 125.4(2) . . ? O5 C16 C17 115.8(3) . . ? C15 C16 C17 118.7(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.540 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.082 #END