# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Roberta Sessoli' 'Roberto Biagi' 'Daniele Bonacchi' 'Guillaume Chastanet' 'Andrea Cornia' 'Del Pennino,Umberto' 'D. Gatteschi' 'Matteo Mannini' 'Mirko Pacchioni' 'Chiara Zanardi' 'Laura Zobbi' _publ_contact_author_name 'Dr Roberta Sessoli' _publ_contact_author_address ; Dipartimento di Chimica Universita degli Studi di Firenze Via Della Lastruccia 3 50019 - Sesto Fiorentino Firenze 50019 ITALY ; _publ_contact_author_email ROBERTA.SESSOLI@UNIFI.IT _publ_requested_journal 'Chemical Communications' _publ_section_title ; Isolated Single Molecule Magnets on native gold ; _publ_section_references ; North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351--359. Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) SIR92. A program for crystal structure solution. J. Appl. Cryst. 26, 343--350. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565--565. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Nardelli, M. (1999), J. Appl. Cryst. 32, 563--571 Sheldrick, G. M. (1997). SHELX97. Programs for Crystal Structure Analysis (Release 97-2). University of Gottingen, Germany. ; data_mn12s1a _database_code_depnum_ccdc_archive 'CCDC 257821' # CHEMICAL DATA _audit_creation_method 'SHELXL-97 (Sheldrick, 1997)' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_iupac '[Mn12 O12 (C8 H7 O2 S)16 (H2 O)4].8(C H Cl3)' _chemical_formula_moiety 'Mn12 C128 H120 O48 S16,C8 H8 Cl24' _chemical_formula_sum 'C136 H128 Cl24 Mn12 O48 S16' _chemical_formula_weight 4553.42 _chemical_compound_source synthesis # CRYSTAL DATA loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4' _symmetry_space_group_name_Hall 'I -4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 19.9340(10) _cell_length_b 19.9340(10) _cell_length_c 25.343(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10070.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 4.84 _cell_measurement_theta_max 12.98 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4584 _exptl_absorpt_coefficient_mu 1.276 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.465 _exptl_absorpt_correction_T_max 0.511 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Siemens P4-RA' _diffrn_measurement_method theta-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -7 2 -1 1 9 2 -7 5 10 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 6172 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5988 _reflns_number_gt 5889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS, v2.2' _computing_cell_refinement 'Siemens XSCANS, v2.2' _computing_data_reduction 'Siemens XSCANS, v2.2' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'WINGX v1.64.05 (Farrugia, 1999)' # REFINEMENT DATA _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. Merohedrally-twinned crystals, with twinning law corresponding to a two-fold axis along the a-axis (TWIN 1 0 0 0 -1 0 0 0 -1 2; BASF 0.51356). All non-hydrogen atoms refined anisotropically, with the exception of disordered CHCl3 carbon atoms. Hydrogen atoms of coordinated water molecule set in calculated positions and held fixed (Nardelli, 1999). CHCl3 hydrogen atoms omitted. 12 low-angle reflections omitted in final refinement. Restraints applied to the anisotropic displacement parameters (ISOR) of C8, C21, C23, C26, to the C-Cl distances (DFIX) of a chloroform molecule (C35, Cl7, Cl8, Cl9A, Cl9B) and to the S3-C24 bond length. ; _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^)+(0.1135P)^2^+1.4110P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 5988 _refine_ls_number_parameters 563 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.94772(5) 0.94832(5) 0.96203(3) 0.01749(18) Uani 1 1 d . . . Mn2 Mn 0.84842(5) 0.85019(5) 0.95863(4) 0.02112(19) Uani 1 1 d . . . Mn3 Mn 0.79190(4) 1.00765(5) 0.99286(4) 0.0224(2) Uani 1 1 d . . . O1 O 0.9560(3) 0.9561(3) 1.03689(16) 0.0201(8) Uani 1 1 d . . . O2 O 0.8537(2) 1.0566(3) 1.03438(17) 0.0212(9) Uani 1 1 d . . . O3 O 0.8550(2) 0.9445(3) 0.96888(18) 0.0212(9) Uani 1 1 d . . . O4 O 0.9415(3) 0.9502(2) 0.88714(17) 0.0242(9) Uani 1 1 d . . . O5 O 0.8584(3) 0.8762(3) 0.87341(19) 0.0326(12) Uani 1 1 d . . . O6 O 0.8331(3) 0.8278(3) 1.04184(19) 0.0281(9) Uani 1 1 d . . . O7 O 0.9345(3) 0.7987(3) 1.0761(2) 0.0375(13) Uani 1 1 d . . . O8 O 0.7511(3) 0.8499(3) 0.9529(2) 0.0284(11) Uani 1 1 d . . . O9 O 0.7188(3) 0.9570(3) 0.9594(3) 0.0367(13) Uani 1 1 d . . . O10 O 0.8445(3) 0.7554(3) 0.9392(2) 0.0332(12) Uani 1 1 d . . . O11 O 0.9362(3) 0.7181(3) 0.9823(3) 0.0394(14) Uani 1 1 d . . . O12 O 0.7733(3) 0.9438(3) 1.0654(3) 0.0415(15) Uani 1 1 d . . . H12A H 0.7645 0.9428 1.0987 0.063 Uiso 1 1 d . . . H12B H 0.7811 0.9044 1.0556 0.063 Uiso 1 1 d . . . C1 C 0.8953(4) 0.9224(4) 0.8593(3) 0.0277(15) Uani 1 1 d . . . C2 C 0.8888(4) 0.9519(5) 0.8047(3) 0.0329(16) Uani 1 1 d . . . C3 C 0.9222(5) 1.0108(5) 0.7918(3) 0.044(2) Uani 1 1 d . . . H3 H 0.9477 1.0331 0.8181 0.053 Uiso 1 1 calc R . . C4 C 0.9195(5) 1.0374(6) 0.7422(4) 0.056(3) Uani 1 1 d . . . H4 H 0.9442 1.0768 0.7341 0.067 Uiso 1 1 calc R . . C5 C 0.8805(7) 1.0069(10) 0.7034(3) 0.078(4) Uani 1 1 d . . . C6 C 0.8455(8) 0.9489(7) 0.7166(4) 0.075(4) Uani 1 1 d . . . H6 H 0.8185 0.9277 0.6906 0.089 Uiso 1 1 calc R . . C7 C 0.8489(6) 0.9208(7) 0.7672(3) 0.060(3) Uani 1 1 d . . . H7 H 0.8244 0.8813 0.7756 0.072 Uiso 1 1 calc R . . S1 S 0.8761(3) 1.0358(3) 0.63841(13) 0.127(2) Uani 1 1 d . . . C8 C 0.9352(17) 1.094(2) 0.6364(8) 0.216(17) Uani 1 1 d U . . H8A H 0.9358 1.1150 0.6014 0.324 Uiso 1 1 calc R . . H8B H 0.9789 1.0737 0.6436 0.324 Uiso 1 1 calc R . . H8C H 0.9258 1.1285 0.6631 0.324 Uiso 1 1 calc R . . C9 C 0.8719(4) 0.8079(4) 1.0793(3) 0.0277(15) Uani 1 1 d . . . C10 C 0.8376(4) 0.7985(4) 1.1321(3) 0.0346(16) Uani 1 1 d . . . C11 C 0.8761(5) 0.7934(5) 1.1773(3) 0.044(2) Uani 1 1 d . . . H11 H 0.9234 0.7990 1.1754 0.053 Uiso 1 1 calc R . . C12 C 0.8446(6) 0.7794(6) 1.2273(4) 0.052(2) Uani 1 1 d . . . H12 H 0.8707 0.7760 1.2585 0.062 Uiso 1 1 calc R . . C13 C 0.7781(6) 0.7714(6) 1.2290(3) 0.056(3) Uani 1 1 d . . . C14 C 0.7384(6) 0.7773(8) 1.1839(4) 0.068(4) Uani 1 1 d . . . H14 H 0.6911 0.7720 1.1861 0.081 Uiso 1 1 calc R . . C15 C 0.7691(5) 0.7911(6) 1.1357(4) 0.052(2) Uani 1 1 d . . . H15 H 0.7424 0.7955 1.1048 0.063 Uiso 1 1 calc R . . S2 S 0.73079(18) 0.7579(3) 1.28779(14) 0.0854(13) Uani 1 1 d . . . C16 C 0.7912(11) 0.7388(9) 1.3370(5) 0.100(6) Uani 1 1 d . . . H16A H 0.7684 0.7301 1.3706 0.150 Uiso 1 1 calc R . . H16B H 0.8220 0.7768 1.3412 0.150 Uiso 1 1 calc R . . H16C H 0.8167 0.6989 1.3265 0.150 Uiso 1 1 calc R . . C17 C 0.7079(4) 0.8962(4) 0.9517(3) 0.0298(15) Uani 1 1 d . . . C18 C 0.6381(5) 0.8756(5) 0.9430(4) 0.037(2) Uani 1 1 d . . . C19 C 0.6181(5) 0.8106(6) 0.9443(7) 0.072(4) Uani 1 1 d . . . H19 H 0.6511 0.7765 0.9481 0.087 Uiso 1 1 calc R . . C20 C 0.5528(6) 0.7926(8) 0.9404(7) 0.077(4) Uani 1 1 d . . . H20 H 0.5402 0.7479 0.9486 0.093 Uiso 1 1 calc R . . C21 C 0.5043(6) 0.8375(7) 0.9248(6) 0.068(3) Uani 1 1 d U . . C22 C 0.5216(6) 0.9025(8) 0.9277(7) 0.079(4) Uani 1 1 d U . . H22 H 0.4875 0.9356 0.9254 0.095 Uiso 1 1 calc R . . C23 C 0.5884(5) 0.9232(6) 0.9340(5) 0.053(3) Uani 1 1 d U . . H23 H 0.5996 0.9695 0.9322 0.064 Uiso 1 1 calc R . . S3 S 0.4240(2) 0.8075(3) 0.9111(3) 0.138(3) Uani 1 1 d D . . C24 C 0.3790(9) 0.8804(14) 0.9021(8) 0.158(14) Uani 1 1 d D . . H24A H 0.3323 0.8693 0.8938 0.237 Uiso 1 1 calc R . . H24B H 0.3986 0.9061 0.8730 0.237 Uiso 1 1 calc R . . H24C H 0.3806 0.9072 0.9345 0.237 Uiso 1 1 calc R . . C25 C 0.8857(4) 0.7104(3) 0.9538(3) 0.0247(14) Uani 1 1 d . . . C26 C 0.8724(4) 0.6384(4) 0.9357(4) 0.0310(17) Uani 1 1 d U . . C27 C 0.8163(6) 0.6250(4) 0.9060(5) 0.054(3) Uani 1 1 d . . . H27 H 0.7883 0.6601 0.8935 0.065 Uiso 1 1 calc R . . C28 C 0.8022(7) 0.5582(6) 0.8949(7) 0.077(4) Uani 1 1 d . . . H28 H 0.7594 0.5461 0.8814 0.092 Uiso 1 1 calc R . . C29 C 0.8507(7) 0.5084(5) 0.9036(5) 0.055(3) Uani 1 1 d . . . C30 C 0.9056(7) 0.5255(6) 0.9338(6) 0.063(3) Uani 1 1 d . . . H30 H 0.9375 0.4919 0.9426 0.075 Uiso 1 1 calc R . . C31 C 0.9152(6) 0.5886(5) 0.9511(5) 0.051(3) Uani 1 1 d . . . H31 H 0.9517 0.5985 0.9739 0.062 Uiso 1 1 calc R . . S4 S 0.8332(3) 0.42735(17) 0.8800(3) 0.120(2) Uani 1 1 d . . . C32 C 0.9009(11) 0.3778(6) 0.9002(8) 0.101(7) Uani 1 1 d . . . H32A H 0.8949 0.3319 0.8872 0.152 Uiso 1 1 calc R . . H32B H 0.9032 0.3773 0.9389 0.152 Uiso 1 1 calc R . . H32C H 0.9427 0.3964 0.8860 0.152 Uiso 1 1 calc R . . Cl1 Cl 0.9523(4) 0.6962(5) 0.8241(4) 0.126(3) Uani 0.75 1 d P . . Cl2 Cl 1.0277(3) 0.8165(4) 0.8113(2) 0.1023(19) Uani 0.75 1 d P . . Cl3 Cl 0.9498(3) 0.7733(7) 0.7262(2) 0.147(4) Uani 0.75 1 d P . . C33 C 0.9549(12) 0.7715(12) 0.7917(10) 0.089(6) Uiso 0.75 1 d P . . Cl4 Cl 0.6550(14) 0.3080(7) -0.0007(6) 0.372(18) Uani 0.75 1 d P . . Cl5 Cl 0.6206(10) 0.4397(9) -0.0044(4) 0.219(7) Uani 0.75 1 d P . . Cl6 Cl 0.6711(11) 0.3817(7) -0.0905(6) 0.269(12) Uani 0.75 1 d P . . C34 C 0.639(2) 0.377(2) -0.0382(17) 0.151(13) Uiso 0.75 1 d P . . Cl7 Cl 0.9684(6) 0.3029(5) 1.1774(3) 0.103(3) Uani 0.50 1 d PD . . Cl8 Cl 1.0190(8) 0.3392(14) 1.2832(8) 0.211(11) Uani 0.50 1 d PD . . Cl9A Cl 0.9080(12) 0.4068(13) 1.2328(10) 0.123(8) Uani 0.25 1 d PD . . Cl9B Cl 0.8853(9) 0.3249(9) 1.2683(6) 0.090(4) Uani 0.25 1 d PD . . C35 C 0.9569(16) 0.338(2) 1.2383(13) 0.21(3) Uiso 0.50 1 d PD . . 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 0.0169(5) 0.0180(5) 0.0176(4) -0.0005(4) -0.0006(4) 0.0000(3) Mn2 0.0199(5) 0.0175(5) 0.0260(4) -0.0007(4) -0.0041(4) -0.0007(3) Mn3 0.0161(4) 0.0200(5) 0.0310(4) -0.0039(4) -0.0021(4) -0.0003(4) O1 0.020(2) 0.018(2) 0.0218(18) -0.004(2) 0.002(2) 0.0015(15) O2 0.011(2) 0.032(3) 0.0204(19) -0.001(2) 0.0012(19) 0.0012(18) O3 0.020(2) 0.018(2) 0.026(2) -0.0052(19) -0.004(2) -0.0012(17) O4 0.033(3) 0.021(3) 0.0190(18) 0.0000(18) -0.006(2) -0.003(2) O5 0.036(3) 0.035(3) 0.026(2) -0.009(2) -0.005(2) -0.009(3) O6 0.026(3) 0.032(3) 0.027(2) 0.004(2) -0.006(2) -0.0039(17) O7 0.027(3) 0.047(3) 0.039(3) 0.007(3) 0.002(2) -0.002(3) O8 0.022(2) 0.022(2) 0.041(3) -0.004(2) -0.002(2) -0.005(2) O9 0.022(2) 0.025(2) 0.063(4) -0.011(3) -0.009(3) -0.005(2) O10 0.032(3) 0.019(2) 0.049(3) -0.007(2) -0.006(3) 0.002(2) O11 0.035(3) 0.022(3) 0.062(4) -0.001(3) -0.016(3) -0.007(2) O12 0.049(3) 0.029(3) 0.046(3) 0.008(3) 0.023(3) 0.004(3) C1 0.025(3) 0.039(4) 0.019(3) 0.001(3) -0.002(3) 0.001(3) C2 0.031(4) 0.050(4) 0.017(3) 0.002(3) -0.012(3) 0.002(4) C3 0.038(4) 0.061(6) 0.034(4) 0.003(4) -0.006(4) -0.003(4) C4 0.046(5) 0.069(7) 0.051(5) 0.021(5) -0.001(4) -0.009(5) C5 0.085(9) 0.125(12) 0.024(4) 0.017(6) -0.017(5) -0.028(9) C6 0.100(10) 0.091(9) 0.032(4) 0.005(5) -0.030(6) -0.038(8) C7 0.067(6) 0.087(8) 0.026(4) 0.001(4) -0.017(4) -0.031(6) S1 0.157(5) 0.183(5) 0.0418(14) 0.055(2) -0.041(2) -0.074(4) C8 0.22(3) 0.35(4) 0.074(10) 0.090(17) -0.031(14) -0.20(3) C9 0.027(3) 0.025(3) 0.031(4) 0.007(3) -0.001(3) -0.002(3) C10 0.035(4) 0.030(4) 0.039(4) 0.000(3) 0.006(3) 0.001(3) C11 0.051(5) 0.049(5) 0.033(4) 0.006(4) 0.006(4) -0.007(4) C12 0.060(6) 0.062(6) 0.033(4) 0.006(4) -0.002(4) -0.010(5) C13 0.070(7) 0.062(6) 0.036(4) 0.015(4) 0.021(5) 0.002(5) C14 0.039(5) 0.127(12) 0.038(5) 0.016(6) -0.001(4) 0.009(6) C15 0.040(4) 0.070(6) 0.047(5) 0.020(5) 0.012(4) 0.006(5) S2 0.073(2) 0.130(3) 0.0531(14) 0.0188(18) 0.0211(15) -0.018(2) C16 0.149(16) 0.107(11) 0.044(6) 0.035(7) 0.038(8) 0.001(12) C17 0.026(4) 0.036(4) 0.028(3) -0.004(3) -0.002(3) 0.006(3) C18 0.032(4) 0.036(4) 0.044(4) -0.002(4) -0.008(4) -0.009(3) C19 0.031(5) 0.049(6) 0.138(12) -0.005(7) -0.005(6) -0.002(4) C20 0.034(5) 0.074(7) 0.125(12) -0.015(8) 0.000(6) -0.019(5) C21 0.033(5) 0.080(8) 0.092(7) -0.012(7) -0.004(6) -0.027(5) C22 0.023(5) 0.088(8) 0.128(10) -0.026(8) -0.024(6) 0.008(5) C23 0.023(4) 0.054(5) 0.082(7) -0.027(5) -0.016(4) 0.001(4) S3 0.0386(17) 0.138(5) 0.236(8) -0.011(5) -0.032(3) -0.041(2) C24 0.057(9) 0.34(4) 0.076(10) -0.030(18) -0.002(8) -0.041(17) C25 0.026(3) 0.014(3) 0.034(4) 0.001(3) -0.002(3) -0.006(3) C26 0.031(3) 0.017(3) 0.045(3) -0.009(3) -0.002(3) -0.005(3) C27 0.057(6) 0.021(4) 0.084(7) -0.007(4) -0.038(6) 0.008(4) C28 0.067(7) 0.036(5) 0.127(12) -0.026(6) -0.054(8) 0.000(5) C29 0.073(7) 0.028(4) 0.065(6) -0.013(4) -0.020(6) -0.007(5) C30 0.067(7) 0.034(5) 0.087(8) -0.010(5) -0.034(7) 0.007(5) C31 0.056(6) 0.033(4) 0.065(7) 0.010(4) -0.024(5) 0.007(4) S4 0.128(4) 0.0324(14) 0.199(6) -0.048(2) -0.076(4) 0.0037(18) C32 0.159(17) 0.023(5) 0.122(13) -0.019(7) -0.072(13) 0.023(7) Cl1 0.099(4) 0.144(7) 0.134(6) 0.054(5) -0.008(4) -0.026(5) Cl2 0.104(4) 0.120(5) 0.083(3) 0.013(3) -0.021(3) -0.036(4) Cl3 0.071(3) 0.291(14) 0.078(3) -0.031(5) -0.010(3) 0.006(5) Cl4 0.73(4) 0.167(10) 0.222(12) 0.084(10) -0.32(2) -0.187(18) Cl5 0.299(18) 0.258(14) 0.099(5) -0.033(8) -0.003(8) -0.007(13) Cl6 0.45(3) 0.147(9) 0.213(12) 0.060(9) 0.205(17) 0.100(14) Cl7 0.122(7) 0.104(6) 0.083(4) 0.025(5) 0.030(5) 0.041(6) Cl8 0.113(10) 0.34(3) 0.181(15) -0.110(19) -0.025(10) 0.041(15) Cl9A 0.117(15) 0.126(16) 0.127(17) -0.059(14) 0.025(13) 0.003(13) Cl9B 0.091(10) 0.100(11) 0.079(8) -0.024(8) 0.015(8) 0.018(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. ; # MOLECULAR GEOMETRY 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 O3 1.858(5) . ? Mn1 O2 1.890(5) 4_757 ? Mn1 O4 1.902(4) . ? Mn1 O1 1.911(4) . ? Mn1 O1 1.915(5) 3_577 ? Mn1 O1 1.923(5) 4_757 ? Mn1 Mn2 2.7842(12) . ? Mn1 Mn1 2.8281(15) 4_757 ? Mn1 Mn1 2.8281(15) 3_577 ? Mn1 Mn1 2.9307(17) 2_775 ? Mn2 O3 1.903(5) . ? Mn2 O2 1.903(6) 4_757 ? Mn2 O8 1.946(5) . ? Mn2 O10 1.955(5) . ? Mn2 O6 2.177(5) . ? Mn2 O5 2.230(5) . ? Mn3 O3 1.880(5) . ? Mn3 O2 1.891(5) . ? Mn3 O11 1.953(5) 3_577 ? Mn3 O9 1.965(5) . ? Mn3 O7 2.098(6) 3_577 ? Mn3 O12 2.268(6) . ? O4 C1 1.286(9) . ? O5 C1 1.231(10) . ? O6 C9 1.288(10) . ? O7 C9 1.264(10) . ? O8 C17 1.263(10) . ? O9 C17 1.246(11) . ? O10 C25 1.270(10) . ? O11 C25 1.248(9) . ? C1 C2 1.509(9) . ? C2 C7 1.387(12) . ? C2 C3 1.389(14) . ? C3 C4 1.366(14) . ? C4 C5 1.393(16) . ? C5 C6 1.39(2) . ? C5 S1 1.747(10) . ? C6 C7 1.400(14) . ? S1 C8 1.66(2) . ? C9 C10 1.515(11) . ? C10 C15 1.376(13) . ? C10 C11 1.382(13) . ? C11 C12 1.442(13) . ? C12 C13 1.337(17) . ? C13 C14 1.394(15) . ? C13 S2 1.783(9) . ? C14 C15 1.396(14) . ? S2 C16 1.776(19) . ? C17 C18 1.468(12) . ? C18 C19 1.356(15) . ? C18 C23 1.390(15) . ? C19 C20 1.354(15) . ? C20 C21 1.38(2) . ? C21 C22 1.34(2) . ? C21 S3 1.744(11) . ? C22 C23 1.403(14) . ? S3 C24 1.72(2) . ? C25 C26 1.531(9) . ? C26 C31 1.366(13) . ? C26 C27 1.373(13) . ? C27 C28 1.390(14) . ? C28 C29 1.403(17) . ? C29 C30 1.379(16) . ? C29 S4 1.758(10) . ? C30 C31 1.345(16) . ? S4 C32 1.750(16) . ? Cl1 C33 1.71(3) . ? Cl2 C33 1.78(2) . ? Cl3 C33 1.66(2) . ? Cl4 C34 1.70(4) . ? Cl5 C34 1.56(4) . ? Cl6 C34 1.47(4) . ? Cl7 C35 1.71(3) . ? Cl8 C35 1.68(3) . ? Cl9A C35 1.69(3) . ? Cl9B C35 1.64(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 Mn1 O2 84.82(18) . 4_757 ? O3 Mn1 O4 91.7(2) . . ? O2 Mn1 O4 93.7(2) 4_757 . ? O3 Mn1 O1 89.8(2) . . ? O2 Mn1 O1 92.2(2) 4_757 . ? O4 Mn1 O1 174.0(2) . . ? O3 Mn1 O1 97.3(2) . 3_577 ? O2 Mn1 O1 175.7(2) 4_757 3_577 ? O4 Mn1 O1 90.0(2) . 3_577 ? O1 Mn1 O1 84.1(2) . 3_577 ? O3 Mn1 O1 173.4(2) . 4_757 ? O2 Mn1 O1 97.1(2) 4_757 4_757 ? O4 Mn1 O1 94.4(2) . 4_757 ? O1 Mn1 O1 83.9(2) . 4_757 ? O1 Mn1 O1 80.39(19) 3_577 4_757 ? Mn2 Mn1 Mn1 122.62(6) . 4_757 ? Mn2 Mn1 Mn1 122.61(6) . 3_577 ? Mn1 Mn1 Mn1 62.41(3) 4_757 3_577 ? Mn2 Mn1 Mn1 178.22(3) . 2_775 ? Mn1 Mn1 Mn1 58.793(17) 4_757 2_775 ? Mn1 Mn1 Mn1 58.793(17) 3_577 2_775 ? O3 Mn2 O2 83.24(17) . 4_757 ? O3 Mn2 O8 94.7(2) . . ? O2 Mn2 O8 177.8(2) 4_757 . ? O3 Mn2 O10 173.1(2) . . ? O2 Mn2 O10 95.7(2) 4_757 . ? O8 Mn2 O10 86.5(2) . . ? O3 Mn2 O6 94.6(2) . . ? O2 Mn2 O6 93.3(2) 4_757 . ? O8 Mn2 O6 86.1(2) . . ? O10 Mn2 O6 92.3(3) . . ? O3 Mn2 O5 84.0(2) . . ? O2 Mn2 O5 89.6(2) 4_757 . ? O8 Mn2 O5 91.0(2) . . ? O10 Mn2 O5 89.2(2) . . ? O6 Mn2 O5 176.7(2) . . ? O3 Mn3 O2 95.11(18) . . ? O3 Mn3 O11 172.6(2) . 3_577 ? O2 Mn3 O11 90.9(2) . 3_577 ? O3 Mn3 O9 90.7(2) . . ? O2 Mn3 O9 171.2(2) . . ? O11 Mn3 O9 82.8(2) 3_577 . ? O3 Mn3 O7 93.2(2) . 3_577 ? O2 Mn3 O7 97.9(2) . 3_577 ? O11 Mn3 O7 90.1(3) 3_577 3_577 ? O9 Mn3 O7 88.3(3) . 3_577 ? O3 Mn3 O12 89.8(2) . . ? O2 Mn3 O12 86.8(2) . . ? O11 Mn3 O12 86.3(3) 3_577 . ? O9 Mn3 O12 86.6(3) . . ? O7 Mn3 O12 174.1(3) 3_577 . ? Mn1 O1 Mn1 95.3(2) . 4_757 ? Mn1 O1 Mn1 95.1(2) . 3_577 ? Mn1 O1 Mn1 99.59(18) 4_757 3_577 ? Mn1 O2 Mn3 130.8(3) 3_577 . ? Mn1 O2 Mn2 94.4(2) 3_577 3_577 ? Mn3 O2 Mn2 122.7(3) . 3_577 ? Mn1 O3 Mn3 131.9(3) . . ? Mn1 O3 Mn2 95.5(2) . . ? Mn3 O3 Mn2 131.3(3) . . ? C1 O4 Mn1 125.8(5) . . ? C1 O5 Mn2 120.5(4) . . ? C9 O6 Mn2 133.9(5) . . ? C9 O7 Mn3 127.3(5) . 4_757 ? C17 O8 Mn2 132.7(5) . . ? C17 O9 Mn3 134.1(5) . . ? C25 O10 Mn2 125.7(5) . . ? C25 O11 Mn3 137.8(5) . 4_757 ? O5 C1 O4 126.3(6) . . ? O5 C1 C2 120.4(7) . . ? O4 C1 C2 113.3(7) . . ? C7 C2 C3 119.4(8) . . ? C7 C2 C1 120.3(8) . . ? C3 C2 C1 120.3(7) . . ? C4 C3 C2 121.8(9) . . ? C3 C4 C5 120.1(11) . . ? C6 C5 C4 118.1(9) . . ? C6 C5 S1 118.5(9) . . ? C4 C5 S1 123.3(11) . . ? C5 C6 C7 122.0(10) . . ? C2 C7 C6 118.4(10) . . ? C8 S1 C5 103.0(9) . . ? O7 C9 O6 126.2(7) . . ? O7 C9 C10 119.0(7) . . ? O6 C9 C10 114.8(7) . . ? C15 C10 C11 119.3(9) . . ? C15 C10 C9 121.3(8) . . ? C11 C10 C9 119.3(7) . . ? C10 C11 C12 120.0(9) . . ? C13 C12 C11 119.0(9) . . ? C12 C13 C14 121.8(9) . . ? C12 C13 S2 124.7(8) . . ? C14 C13 S2 113.4(9) . . ? C13 C14 C15 119.0(10) . . ? C10 C15 C14 121.0(10) . . ? C16 S2 C13 105.1(7) . . ? O9 C17 O8 126.1(8) . . ? O9 C17 C18 117.4(7) . . ? O8 C17 C18 116.4(8) . . ? C19 C18 C23 116.5(9) . . ? C19 C18 C17 122.8(9) . . ? C23 C18 C17 120.7(9) . . ? C20 C19 C18 122.2(12) . . ? C19 C20 C21 121.6(13) . . ? C22 C21 C20 115.6(11) . . ? C22 C21 S3 125.3(11) . . ? C20 C21 S3 118.6(10) . . ? C21 C22 C23 122.2(13) . . ? C18 C23 C22 119.7(12) . . ? C24 S3 C21 102.4(10) . . ? O11 C25 O10 127.1(7) . . ? O11 C25 C26 115.4(7) . . ? O10 C25 C26 117.5(7) . . ? C31 C26 C27 121.7(8) . . ? C31 C26 C25 119.1(8) . . ? C27 C26 C25 119.2(7) . . ? C26 C27 C28 117.5(9) . . ? C27 C28 C29 120.4(10) . . ? C30 C29 C28 117.4(9) . . ? C30 C29 S4 125.0(9) . . ? C28 C29 S4 117.3(8) . . ? C31 C30 C29 121.7(11) . . ? C30 C31 C26 119.8(10) . . ? C32 S4 C29 105.4(7) . . ? Cl3 C33 Cl1 119.7(15) . . ? Cl3 C33 Cl2 108.5(14) . . ? Cl1 C33 Cl2 109.5(13) . . ? Cl6 C34 Cl5 123(3) . . ? Cl6 C34 Cl4 118(3) . . ? Cl5 C34 Cl4 113(3) . . ? Cl9B C35 Cl8 109(2) . . ? Cl8 C35 Cl9A 118(3) . . ? Cl9B C35 Cl7 118(2) . . ? Cl8 C35 Cl7 121.2(19) . . ? Cl9A C35 Cl7 110(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.014 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.105