Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 #'SHELXL-97 plus manual edit of cif file' _publ_contact_author_name 'Prof. Helgard G. Raubenheimer' _publ_contact_author_address ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; _publ_contact_author_phone '+27 21 808 3345' _publ_contact_author_fax '+27 21 808 3360' _publ_contact_author_email ce@maties.sun.ac.za _publ_requested_journal ; Journal of the Chemical Society, Dalton Transactions ; loop_ _publ_author_name 'An, Jin' 'Chen, Zhi-Da' 'Esterhuysen, Catherine' 'Gao, Song' 'Raubenheimer, Helgard G.' 'Xu, Guang-Xian' 'Zhang, Xi-Xiang' _publ_section_title ; Synthesis, X-ray characterization, and single molecule magnetic behaviour of [Mn~12~O~12~(O~2~CCH~2~X)~16~(H~2~O)~4~].mCH~2~Cl~2~.nH~2~O (X=Cl, m=2, n=6, 1; X=Br, m=4, n=0, 2) ; _publ_section_references ; Farrugia, L.J. (1997). J. Appl. Cryst. 30, 565. Farrugia, L. J. (1999) J. Appl. Cryst. 32, 837-838 Nonius BV (1998) COLLECT. Data collection software. Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997) Methods Enzymol., 276, 307. Sheldrick, G.M. (1997). SHELX-97. Program for crystal structure analysis. Univ. of G\"ottingen, Germany. ; #=== data_1 _database_code_CSD 165981 _audit_creation_method SHELXL-97 _chemical_name_systematic ; dodecakis(\m^3^-Oxo)-hexadecakis(\m^2^-chloro/bromoacetato)-tetra-aqua- tetra-manganese(iv)-octa-manganese(iii) hexahydrate di-dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 Cl16 Mn12 O48, 6(H2 O1), 2(C1 H2 Cl2)' _chemical_formula_sum 'C34 H48 Cl20 Mn12 O54' _chemical_formula_weight 2689.015 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' '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.132(2) _cell_length_b 13.195(2) _cell_length_c 26.068(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.255(2) _cell_angle_gamma 90.00 _cell_volume 8620.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17900 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5296 _exptl_absorpt_coefficient_mu 2.412 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.55 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 17900 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.0 _reflns_number_total 8453 _reflns_number_gt 6772 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'WINGX (Farrugia, 1999)' _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 'w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+82.1460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8453 _refine_ls_number_parameters 678 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1734 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.053 _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 0.02850(3) 0.71201(6) 0.20242(3) 0.01680(19) Uani 1 1 d . . . Mn2 Mn -0.05153(3) 0.56924(6) 0.21879(3) 0.01624(19) Uani 1 1 d . . . Mn3 Mn 0.08743(3) 0.70591(6) 0.11690(3) 0.0211(2) Uani 1 1 d . A . Mn4 Mn -0.14539(3) 0.57381(7) 0.15551(3) 0.0217(2) Uani 1 1 d . A . Mn5 Mn -0.16322(3) 0.66708(7) 0.27169(3) 0.0230(2) Uani 1 1 d . . . Mn6 Mn -0.03455(3) 0.61015(6) 0.09099(3) 0.0197(2) Uani 1 1 d . A . Cl1A Cl -0.14587(11) 0.19061(18) 0.19735(11) 0.0623(7) Uani 0.83 1 d PD A 1 Cl1B Cl -0.054(2) 0.227(3) 0.2591(16) 0.37(5) Uani 0.17 1 d PD . 2 Cl2A Cl -0.23224(17) 0.4907(6) -0.0040(2) 0.0681(17) Uani 0.55 1 d PD B 3 Cl2B Cl -0.2214(5) 0.5382(10) -0.0215(5) 0.154(6) Uani 0.45 1 d PD B 4 Cl3A Cl 0.0992(3) 0.7572(8) -0.0619(4) 0.0376(15) Uani 0.57 1 d PD C 5 Cl3B Cl 0.0941(6) 0.7717(14) -0.0615(7) 0.092(6) Uani 0.43 1 d PD C 6 Cl4A Cl 0.2418(4) 0.7993(10) 0.0427(2) 0.128(4) Uani 0.444 1 d PD D 7 Cl4B Cl 0.2219(8) 0.8884(16) 0.0633(7) 0.084(6) Uani 0.133 1 d PD D 8 Cl4C Cl 0.2816(4) 0.6739(8) 0.0908(5) 0.071(3) Uani 0.260 1 d PD D 9 Cl4D Cl 0.2696(7) 0.7219(15) 0.0642(8) 0.068(5) Uani 0.163 1 d PD D 10 Cl5A Cl -0.02527(17) 1.0438(3) 0.1322(2) 0.0711(13) Uani 0.53 1 d PD E 11 Cl5B Cl 0.0089(9) 1.0689(12) 0.2110(7) 0.063(6) Uani 0.19 1 d PD . 12 Cl5C Cl 0.0367(11) 1.069(2) 0.2194(9) 0.053(7) Uani 0.11 1 d PD E 13 Cl5D Cl -0.0164(9) 1.057(3) 0.1937(11) 0.050(8) Uani 0.10 1 d PD E 14 Cl5E Cl 0.0537(9) 1.1055(15) 0.1203(8) 0.039(5) Uani 0.07 1 d PD E 15 Cl6 Cl 0.04809(12) 0.28294(17) 0.15282(10) 0.0770(8) Uani 1 1 d . . . Cl7A Cl -0.32964(10) 0.5203(3) 0.13102(12) 0.0650(10) Uani 0.664 1 d PD F 16 Cl7B Cl -0.3338(5) 0.4782(11) 0.2098(6) 0.084(4) Uani 0.203 1 d PD F 17 Cl7C Cl -0.3480(8) 0.574(3) 0.2368(10) 0.119(10) Uani 0.133 1 d PD F 18 Cl8A Cl -0.1557(3) 0.9385(7) 0.0954(3) 0.0535(15) Uani 0.59 1 d PD G 19 Cl8B Cl -0.1351(6) 0.9481(11) 0.1016(5) 0.116(6) Uani 0.41 1 d PD G 20 C1 C -0.0948(2) 0.3734(4) 0.1959(2) 0.0243(12) Uani 1 1 d . A . C2 C -0.0869(3) 0.2609(5) 0.2020(3) 0.0398(16) Uani 1 1 d D . . C3 C -0.1352(2) 0.5206(5) 0.0475(2) 0.0262(12) Uani 1 1 d . A . C4 C -0.1630(2) 0.4724(6) 0.0001(3) 0.0448(18) Uani 1 1 d D . . C5 C 0.0366(2) 0.6905(4) 0.0134(2) 0.0247(12) Uani 1 1 d . A . C6 C 0.0359(2) 0.7131(5) -0.0435(2) 0.0339(14) Uani 1 1 d D . . C7 C 0.2014(2) 0.7553(5) 0.1345(2) 0.0296(13) Uani 1 1 d . . . C8 C 0.2493(3) 0.7961(6) 0.1095(3) 0.053(2) Uani 1 1 d D . . C9 C 0.0452(2) 0.9057(5) 0.1588(3) 0.0319(14) Uani 1 1 d . A . C10 C 0.0341(3) 1.0175(5) 0.1589(3) 0.058(2) Uani 1 1 d D . . C11 C 0.0632(2) 0.4727(5) 0.1121(3) 0.0392(16) Uani 1 1 d . . . C12A C 0.0871(6) 0.3663(11) 0.1086(12) 0.087(8) Uani 0.53 1 d P H 21 C12B C 0.0855(6) 0.3829(13) 0.1489(7) 0.039(4) Uani 0.47 1 d P H 22 C13 C -0.2490(2) 0.5859(6) 0.1976(3) 0.0447(18) Uani 1 1 d . A . C14 C -0.3075(3) 0.5693(11) 0.1896(4) 0.098(5) Uani 1 1 d D . . C15 C -0.1573(2) 0.8082(5) 0.1780(2) 0.0330(14) Uani 1 1 d . A . C16 C -0.1533(5) 0.9201(6) 0.1630(3) 0.067(3) Uani 1 1 d D . . O1 O -0.22046(15) 0.5559(4) 0.16277(16) 0.0359(11) Uani 1 1 d . . . O2 O -0.16288(15) 0.5507(3) 0.08267(15) 0.0296(9) Uani 1 1 d . . . O3 O -0.13468(16) 0.4076(3) 0.17054(16) 0.0296(9) Uani 1 1 d . . . O4 O -0.07134(13) 0.5787(3) 0.14872(14) 0.0193(8) Uani 1 1 d . . . O5 O -0.12526(14) 0.5854(3) 0.22730(14) 0.0210(8) Uani 1 1 d . . . O6 O -0.15198(16) 0.7392(3) 0.14619(16) 0.0296(9) Uani 1 1 d . . . O7 O -0.08482(15) 0.5238(3) 0.04737(15) 0.0288(9) Uani 1 1 d . . . O8 O -0.08580(16) 0.7354(3) 0.06826(16) 0.0336(10) Uani 1 1 d D . . H81 H -0.0681 0.7876 0.0681 0.040 Uiso 1 1 calc RD A . H82 H -0.1138 0.7627 0.0828 0.040 Uiso 1 1 d RD . . O9 O 0.01484(13) 0.6943(3) 0.13114(14) 0.0195(8) Uani 1 1 d . . . O10 O 0.01400(15) 0.4794(3) 0.10224(17) 0.0298(9) Uani 1 1 d . A . O11 O -0.00325(16) 0.6412(3) 0.02601(15) 0.0314(10) Uani 1 1 d . . . O12 O 0.02410(13) 0.5698(3) 0.21062(13) 0.0170(7) Uani 1 1 d . . . O13 O -0.04262(13) 0.7118(3) 0.22358(13) 0.0171(7) Uani 1 1 d . . . O14 O 0.02700(16) 0.8564(3) 0.19641(15) 0.0273(9) Uani 1 1 d . . . O15 O 0.10007(14) 0.7029(3) 0.18878(14) 0.0194(8) Uani 1 1 d . . . O16 O 0.07056(18) 0.8714(3) 0.12417(17) 0.0342(10) Uani 1 1 d . . . O17 O 0.09702(15) 0.5424(3) 0.10989(16) 0.0271(9) Uani 1 1 d . A . O18 O 0.16175(15) 0.7291(3) 0.10516(15) 0.0313(10) Uani 1 1 d . . . O19 O 0.07436(16) 0.7217(3) 0.04311(15) 0.0296(9) Uani 1 1 d . . . O20 O -0.16580(18) 0.7988(3) 0.22477(17) 0.0347(10) Uani 1 1 d . . . O21 O -0.23415(16) 0.6312(4) 0.23768(17) 0.0417(12) Uani 1 1 d . . . O22 O -0.20583(15) 0.7490(4) 0.31750(15) 0.0311(9) Uani 1 1 d . . . O23 O -0.05645(15) 0.4246(3) 0.21866(14) 0.0229(8) Uani 1 1 d . . . O24 O -0.18292(17) 0.5388(4) 0.32045(17) 0.0356(10) Uani 1 1 d . . . O25 O 0.0354(4) 0.1167(7) -0.0136(5) 0.134(4) Uani 1 1 d . . . O26 O 0.2193(3) 0.3825(5) 0.2432(2) 0.0723(19) Uani 1 1 d . . . O27 O 0.0828(5) -0.0456(7) 0.0244(4) 0.090(4) Uani 0.732(16) 1 d P . . O28 O 0.144(2) 0.094(2) 0.0378(11) 0.14(2) Uani 0.269(16) 1 d P . . C17 C 0.2333(4) 0.2345(12) 0.0708(4) 0.105(5) Uani 1 1 d D . . Cl9 Cl 0.17539(15) 0.2338(4) 0.02810(14) 0.1345(16) Uani 1 1 d D . . Cl10 Cl 0.21860(10) 0.2885(3) 0.13039(11) 0.0951(10) Uani 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 0.0169(4) 0.0142(4) 0.0195(4) 0.0011(3) 0.0023(3) -0.0014(3) Mn2 0.0150(4) 0.0152(4) 0.0185(4) -0.0002(3) 0.0014(3) -0.0010(3) Mn3 0.0191(4) 0.0252(5) 0.0193(4) 0.0017(3) 0.0031(3) -0.0057(3) Mn4 0.0150(4) 0.0294(5) 0.0205(4) -0.0017(3) 0.0011(3) -0.0022(3) Mn5 0.0155(4) 0.0309(5) 0.0227(4) -0.0027(4) 0.0020(3) 0.0034(3) Mn6 0.0172(4) 0.0230(4) 0.0189(4) 0.0003(3) 0.0017(3) -0.0032(3) Cl1A 0.0652(15) 0.0351(12) 0.0860(19) 0.0121(12) 0.0016(13) -0.0311(11) Cl1B 0.28(5) 0.11(3) 0.69(12) 0.10(5) -0.23(7) -0.08(3) Cl2A 0.0253(16) 0.125(6) 0.051(3) -0.017(3) -0.0138(17) -0.001(2) Cl2B 0.169(11) 0.158(12) 0.118(10) -0.054(7) -0.108(8) 0.077(9) Cl3A 0.041(3) 0.051(3) 0.023(3) 0.007(2) 0.014(2) -0.012(2) Cl3B 0.117(11) 0.123(12) 0.037(6) -0.009(7) 0.019(7) -0.076(9) Cl4A 0.123(7) 0.219(12) 0.046(3) -0.015(5) 0.030(4) -0.115(8) Cl4B 0.089(14) 0.115(17) 0.048(10) -0.008(11) 0.008(9) -0.046(13) Cl4C 0.055(5) 0.075(7) 0.091(8) -0.012(6) 0.056(6) -0.011(5) Cl4D 0.060(10) 0.075(12) 0.075(12) -0.024(9) 0.054(9) -0.028(8) Cl5A 0.055(2) 0.045(2) 0.112(4) 0.010(2) -0.007(2) 0.0113(18) Cl5B 0.084(16) 0.024(7) 0.085(14) 0.004(9) 0.036(13) 0.015(16) Cl5C 0.073(18) 0.016(9) 0.073(14) -0.010(8) 0.014(14) 0.001(14) Cl5D 0.054(15) 0.029(13) 0.074(18) 0.025(12) 0.038(13) 0.026(13) Cl5E 0.041(12) 0.029(11) 0.046(13) -0.003(9) 0.008(10) -0.009(9) Cl6 0.114(2) 0.0454(12) 0.0662(15) 0.0065(10) -0.0285(14) 0.0107(12) Cl7A 0.0236(12) 0.116(3) 0.0538(17) -0.0329(18) -0.0056(11) -0.0220(15) Cl7B 0.072(8) 0.087(9) 0.092(10) -0.010(8) 0.005(7) -0.009(7) Cl7C 0.053(11) 0.15(3) 0.15(2) -0.03(2) 0.035(13) -0.015(13) Cl8A 0.072(3) 0.047(3) 0.041(2) 0.0160(19) 0.000(2) 0.007(2) Cl8B 0.213(17) 0.037(4) 0.113(10) 0.021(6) 0.105(10) 0.019(9) C1 0.030(3) 0.020(3) 0.024(3) -0.002(2) 0.004(2) -0.008(2) C2 0.055(4) 0.019(3) 0.044(4) 0.001(3) -0.005(3) -0.008(3) C3 0.023(3) 0.031(3) 0.024(3) 0.001(2) 0.000(2) -0.005(2) C4 0.024(3) 0.078(5) 0.032(4) -0.018(4) -0.003(3) -0.008(3) C5 0.029(3) 0.027(3) 0.020(3) -0.001(2) 0.005(2) -0.002(2) C6 0.036(3) 0.041(4) 0.025(3) 0.001(3) 0.003(2) -0.014(3) C7 0.022(3) 0.034(3) 0.033(3) 0.006(3) 0.003(2) -0.008(2) C8 0.030(3) 0.094(6) 0.034(4) 0.008(4) 0.009(3) -0.026(4) C9 0.032(3) 0.020(3) 0.043(4) 0.005(3) 0.002(3) -0.003(2) C10 0.073(6) 0.024(4) 0.077(6) 0.014(4) 0.021(5) 0.010(4) C11 0.022(3) 0.022(3) 0.073(5) -0.008(3) 0.003(3) 0.002(2) C12A 0.033(8) 0.015(7) 0.22(3) 0.012(11) 0.052(13) -0.002(6) C12B 0.031(8) 0.041(9) 0.048(9) 0.014(8) 0.011(7) 0.014(6) C13 0.019(3) 0.076(5) 0.039(4) -0.016(4) 0.001(3) -0.003(3) C14 0.025(4) 0.197(14) 0.072(6) -0.057(8) 0.009(4) -0.029(6) C15 0.033(3) 0.033(3) 0.033(3) 0.004(3) 0.001(3) 0.004(3) C16 0.122(8) 0.035(4) 0.047(5) 0.009(4) 0.024(5) -0.002(5) O1 0.0161(19) 0.061(3) 0.032(2) -0.006(2) 0.0079(16) -0.0108(19) O2 0.0200(19) 0.047(3) 0.022(2) -0.0029(18) 0.0003(15) -0.0006(18) O3 0.028(2) 0.026(2) 0.034(2) -0.0002(18) 0.0013(17) -0.0093(17) O4 0.0154(17) 0.0216(19) 0.0209(19) 0.0008(15) 0.0012(14) -0.0016(14) O5 0.0181(17) 0.026(2) 0.0193(19) -0.0013(15) 0.0016(14) -0.0017(15) O6 0.030(2) 0.031(2) 0.029(2) 0.0033(19) 0.0033(17) 0.0056(18) O7 0.0223(19) 0.040(2) 0.024(2) -0.0042(18) 0.0026(15) -0.0062(18) O8 0.030(2) 0.034(2) 0.036(2) 0.0079(19) 0.0041(18) 0.0018(18) O9 0.0160(17) 0.0236(19) 0.0193(18) 0.0004(15) 0.0044(14) -0.0042(14) O10 0.025(2) 0.023(2) 0.041(2) -0.0075(18) 0.0038(17) -0.0014(16) O11 0.030(2) 0.043(3) 0.021(2) -0.0034(18) 0.0037(16) -0.0104(19) O12 0.0170(17) 0.0148(18) 0.0195(18) -0.0005(14) 0.0034(14) 0.0009(14) O13 0.0172(17) 0.0161(18) 0.0181(18) 0.0001(14) 0.0017(14) 0.0006(14) O14 0.033(2) 0.018(2) 0.031(2) 0.0023(17) 0.0068(17) -0.0013(16) O15 0.0179(17) 0.0197(19) 0.0209(19) 0.0003(15) 0.0045(14) -0.0030(14) O16 0.041(2) 0.026(2) 0.037(2) 0.0088(19) 0.011(2) -0.0068(19) O17 0.0205(19) 0.024(2) 0.038(2) -0.0041(18) 0.0091(16) -0.0032(16) O18 0.022(2) 0.047(3) 0.025(2) 0.0016(19) 0.0056(16) -0.0112(18) O19 0.028(2) 0.042(3) 0.019(2) 0.0039(18) 0.0038(16) -0.0123(18) O20 0.040(2) 0.034(2) 0.031(2) 0.0009(19) 0.0026(18) 0.0101(19) O21 0.019(2) 0.074(4) 0.033(2) -0.019(2) 0.0014(17) 0.003(2) O22 0.024(2) 0.045(3) 0.025(2) -0.0037(19) 0.0024(16) 0.0101(18) O23 0.0248(19) 0.0179(19) 0.026(2) -0.0007(15) 0.0033(15) -0.0041(15) O24 0.035(2) 0.039(3) 0.033(2) 0.000(2) 0.0064(18) -0.010(2) O25 0.145(9) 0.089(6) 0.182(11) 0.010(6) 0.100(8) -0.005(6) O26 0.095(5) 0.071(4) 0.052(4) 0.015(3) 0.012(3) 0.047(4) O27 0.158(11) 0.062(6) 0.053(6) 0.011(4) 0.022(6) 0.022(6) O28 0.29(5) 0.063(19) 0.057(18) 0.019(14) -0.03(2) -0.08(3) C17 0.074(7) 0.166(13) 0.070(7) -0.031(8) -0.029(6) 0.042(8) Cl9 0.098(2) 0.211(5) 0.087(2) -0.040(3) -0.0393(18) 0.035(3) Cl10 0.0596(14) 0.137(3) 0.0852(18) -0.0393(18) -0.0161(13) 0.0419(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O15 1.863(3) . ? Mn1 O9 1.879(4) . ? Mn1 O12 1.893(4) . ? Mn1 O13 1.909(3) . ? Mn1 O14 1.912(4) . ? Mn1 O13 1.935(4) 2 ? Mn1 Mn3 2.7677(11) . ? Mn1 Mn2 2.8113(11) . ? Mn1 Mn2 2.8154(11) 2 ? Mn1 Mn1 2.9552(15) 2 ? Mn2 O4 1.861(4) . ? Mn2 O5 1.895(4) . ? Mn2 O13 1.897(4) . ? Mn2 O23 1.912(4) . ? Mn2 O12 1.917(4) 2 ? Mn2 O12 1.928(3) . ? Mn2 Mn4 2.7770(11) . ? Mn2 Mn1 2.8154(11) 2 ? Mn2 Mn2 2.9548(15) 2 ? Mn3 O15 1.878(4) . ? Mn3 O9 1.895(3) . ? Mn3 O19 1.938(4) . ? Mn3 O18 1.939(4) . ? Mn3 O17 2.180(4) . ? Mn3 O16 2.235(4) . ? Mn4 O4 1.883(3) . ? Mn4 O5 1.908(4) . ? Mn4 O1 1.925(4) . ? Mn4 O2 1.941(4) . ? Mn4 O6 2.201(4) . ? Mn4 O3 2.240(4) . ? Mn5 O15 1.887(4) 2 ? Mn5 O5 1.891(4) . ? Mn5 O22 1.983(4) . ? Mn5 O21 1.988(4) . ? Mn5 O20 2.124(4) . ? Mn5 O24 2.195(5) . ? Mn6 O4 1.871(4) . ? Mn6 O9 1.918(4) . ? Mn6 O11 1.963(4) . ? Mn6 O7 1.993(4) . ? Mn6 O10 2.121(4) . ? Mn6 O8 2.151(4) . ? Cl1A C2 1.745(7) . ? Cl1B C2 1.71(2) . ? Cl1B Cl6 2.41(5) 2 ? Cl2A C4 1.752(7) . ? Cl2B C4 1.762(11) . ? Cl3A C6 1.793(10) . ? Cl3B C6 1.750(14) . ? Cl4A C8 1.738(9) . ? Cl4B C8 1.812(16) . ? Cl4C C8 1.886(12) . ? Cl4D C8 1.647(13) . ? Cl5A C10 1.636(9) . ? Cl5B C10 1.683(15) . ? Cl5B Cl5B 2.11(3) 2 ? Cl5C C10 1.713(18) . ? Cl5D C10 1.696(17) . ? Cl5E C10 1.636(16) . ? Cl6 C12B 1.627(17) . ? Cl6 C12A 1.915(19) . ? Cl6 Cl1B 2.41(5) 2 ? Cl7A C14 1.713(9) . ? Cl7B C14 1.486(14) . ? Cl7C C14 1.654(17) . ? Cl8A C16 1.776(10) . ? Cl8B C16 1.738(14) . ? C1 O3 1.244(7) . ? C1 O23 1.286(7) . ? C1 C2 1.504(8) . ? C3 O2 1.256(7) . ? C3 O7 1.267(7) . ? C3 C4 1.513(8) . ? C5 O19 1.248(7) . ? C5 O11 1.258(7) . ? C5 C6 1.512(8) . ? C7 O22 1.251(7) 2 ? C7 O18 1.259(7) . ? C7 C8 1.508(8) . ? C9 O16 1.229(8) . ? C9 O14 1.289(7) . ? C9 C10 1.501(9) . ? C11 O10 1.247(7) . ? C11 O17 1.257(7) . ? C11 C12A 1.533(16) . ? C11 C12B 1.601(17) . ? C13 O21 1.236(8) . ? C13 O1 1.263(8) . ? C13 C14 1.486(9) . ? C15 O6 1.246(8) . ? C15 O20 1.258(8) . ? C15 C16 1.533(10) . ? O8 H81 0.8200 . ? O8 H82 0.8994 . ? O12 Mn2 1.917(4) 2 ? O13 Mn1 1.935(4) 2 ? O15 Mn5 1.887(4) 2 ? O22 C7 1.251(7) 2 ? O28 Cl9 2.03(3) . ? C17 Cl9 1.766(9) . ? C17 Cl10 1.771(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O15 Mn1 O9 84.92(15) . . ? O15 Mn1 O12 91.32(15) . . ? O9 Mn1 O12 88.90(16) . . ? O15 Mn1 O13 173.12(15) . . ? O9 Mn1 O13 100.33(15) . . ? O12 Mn1 O13 84.38(15) . . ? O15 Mn1 O14 93.55(17) . . ? O9 Mn1 O14 92.38(17) . . ? O12 Mn1 O14 175.05(16) . . ? O13 Mn1 O14 90.69(16) . . ? O15 Mn1 O13 94.69(15) . 2 ? O9 Mn1 O13 172.79(16) . 2 ? O12 Mn1 O13 83.91(15) . 2 ? O13 Mn1 O13 79.54(15) . 2 ? O14 Mn1 O13 94.83(16) . 2 ? O15 Mn1 Mn3 42.48(11) . . ? O9 Mn1 Mn3 43.05(10) . . ? O12 Mn1 Mn3 95.82(11) . . ? O13 Mn1 Mn3 143.23(11) . . ? O14 Mn1 Mn3 88.36(12) . . ? O13 Mn1 Mn3 137.16(10) 2 . ? O15 Mn1 Mn2 134.23(12) . . ? O9 Mn1 Mn2 89.24(11) . . ? O12 Mn1 Mn2 43.12(10) . . ? O13 Mn1 Mn2 42.23(11) . . ? O14 Mn1 Mn2 132.09(12) . . ? O13 Mn1 Mn2 85.88(10) 2 . ? Mn3 Mn1 Mn2 122.30(4) . . ? O15 Mn1 Mn2 86.96(11) . 2 ? O9 Mn1 Mn2 130.62(12) . 2 ? O12 Mn1 Mn2 42.68(11) . 2 ? O13 Mn1 Mn2 86.24(11) . 2 ? O14 Mn1 Mn2 136.75(13) . 2 ? O13 Mn1 Mn2 42.20(10) 2 2 ? Mn3 Mn1 Mn2 118.35(4) . 2 ? Mn2 Mn1 Mn2 63.35(3) . 2 ? O15 Mn1 Mn1 134.04(12) . 2 ? O9 Mn1 Mn1 139.98(11) . 2 ? O12 Mn1 Mn1 82.48(11) . 2 ? O13 Mn1 Mn1 40.09(10) . 2 ? O14 Mn1 Mn1 93.50(12) . 2 ? O13 Mn1 Mn1 39.45(10) 2 2 ? Mn3 Mn1 Mn1 176.25(4) . 2 ? Mn2 Mn1 Mn1 58.38(2) . 2 ? Mn2 Mn1 Mn1 58.25(3) 2 2 ? O4 Mn2 O5 85.10(15) . . ? O4 Mn2 O13 91.14(16) . . ? O5 Mn2 O13 89.56(15) . . ? O4 Mn2 O23 93.01(16) . . ? O5 Mn2 O23 92.80(16) . . ? O13 Mn2 O23 175.39(16) . . ? O4 Mn2 O12 173.16(15) . 2 ? O5 Mn2 O12 99.93(15) . 2 ? O13 Mn2 O12 84.30(15) . 2 ? O23 Mn2 O12 91.39(16) . 2 ? O4 Mn2 O12 94.90(15) . . ? O5 Mn2 O12 173.30(16) . . ? O13 Mn2 O12 83.74(15) . . ? O23 Mn2 O12 93.89(16) . . ? O12 Mn2 O12 79.56(16) 2 . ? O4 Mn2 Mn4 42.44(11) . . ? O5 Mn2 Mn4 43.29(11) . . ? O13 Mn2 Mn4 96.22(11) . . ? O23 Mn2 Mn4 88.20(12) . . ? O12 Mn2 Mn4 143.08(11) 2 . ? O12 Mn2 Mn4 137.31(11) . . ? O4 Mn2 Mn1 87.05(11) . . ? O5 Mn2 Mn1 131.24(12) . . ? O13 Mn2 Mn1 42.56(10) . . ? O23 Mn2 Mn1 135.67(12) . . ? O12 Mn2 Mn1 86.14(10) 2 . ? O12 Mn2 Mn1 42.14(11) . . ? Mn4 Mn2 Mn1 118.75(4) . . ? O4 Mn2 Mn1 134.16(12) . 2 ? O5 Mn2 Mn1 89.38(11) . 2 ? O13 Mn2 Mn1 43.26(11) . 2 ? O23 Mn2 Mn1 132.75(12) . 2 ? O12 Mn2 Mn1 42.02(11) 2 2 ? O12 Mn2 Mn1 85.81(11) . 2 ? Mn4 Mn2 Mn1 122.58(4) . 2 ? Mn1 Mn2 Mn1 63.36(3) . 2 ? O4 Mn2 Mn2 134.44(11) . 2 ? O5 Mn2 Mn2 139.51(12) . 2 ? O13 Mn2 Mn2 82.50(10) . 2 ? O23 Mn2 Mn2 93.15(11) . 2 ? O12 Mn2 Mn2 39.92(10) 2 2 ? O12 Mn2 Mn2 39.64(10) . 2 ? Mn4 Mn2 Mn2 176.73(4) . 2 ? Mn1 Mn2 Mn2 58.39(2) . 2 ? Mn1 Mn2 Mn2 58.26(2) 2 2 ? O15 Mn3 O9 84.08(15) . . ? O15 Mn3 O19 175.04(18) . . ? O9 Mn3 O19 96.22(16) . . ? O15 Mn3 O18 93.86(16) . . ? O9 Mn3 O18 175.07(18) . . ? O19 Mn3 O18 85.45(17) . . ? O15 Mn3 O17 92.94(16) . . ? O9 Mn3 O17 92.91(15) . . ? O19 Mn3 O17 91.98(17) . . ? O18 Mn3 O17 91.67(17) . . ? O15 Mn3 O16 87.42(16) . . ? O9 Mn3 O16 82.56(16) . . ? O19 Mn3 O16 87.71(18) . . ? O18 Mn3 O16 92.89(18) . . ? O17 Mn3 O16 175.40(15) . . ? O15 Mn3 Mn1 42.08(11) . . ? O9 Mn3 Mn1 42.60(11) . . ? O19 Mn3 Mn1 137.29(13) . . ? O18 Mn3 Mn1 134.57(13) . . ? O17 Mn3 Mn1 99.52(11) . . ? O16 Mn3 Mn1 77.70(11) . . ? O4 Mn4 O5 84.12(15) . . ? O4 Mn4 O1 174.89(19) . . ? O5 Mn4 O1 95.96(17) . . ? O4 Mn4 O2 93.85(16) . . ? O5 Mn4 O2 175.08(18) . . ? O1 Mn4 O2 85.66(17) . . ? O4 Mn4 O6 91.30(16) . . ? O5 Mn4 O6 92.35(16) . . ? O1 Mn4 O6 93.80(19) . . ? O2 Mn4 O6 92.18(18) . . ? O4 Mn4 O3 86.74(15) . . ? O5 Mn4 O3 83.52(16) . . ? O1 Mn4 O3 88.19(18) . . ? O2 Mn4 O3 91.89(18) . . ? O6 Mn4 O3 175.59(16) . . ? O4 Mn4 Mn2 41.83(11) . . ? O5 Mn4 Mn2 42.90(11) . . ? O1 Mn4 Mn2 137.27(14) . . ? O2 Mn4 Mn2 134.31(12) . . ? O6 Mn4 Mn2 98.10(11) . . ? O3 Mn4 Mn2 77.82(11) . . ? O15 Mn5 O5 92.00(15) 2 . ? O15 Mn5 O22 90.25(16) 2 . ? O5 Mn5 O22 177.49(17) . . ? O15 Mn5 O21 173.20(17) 2 . ? O5 Mn5 O21 93.88(17) . . ? O22 Mn5 O21 83.81(18) . . ? O15 Mn5 O20 95.61(17) 2 . ? O5 Mn5 O20 96.28(17) . . ? O22 Mn5 O20 84.60(18) . . ? O21 Mn5 O20 87.1(2) . . ? O15 Mn5 O24 95.37(16) 2 . ? O5 Mn5 O24 93.47(17) . . ? O22 Mn5 O24 85.22(18) . . ? O21 Mn5 O24 80.9(2) . . ? O20 Mn5 O24 165.03(17) . . ? O4 Mn6 O9 91.61(15) . . ? O4 Mn6 O11 173.84(16) . . ? O9 Mn6 O11 93.76(16) . . ? O4 Mn6 O7 90.11(16) . . ? O9 Mn6 O7 178.28(16) . . ? O11 Mn6 O7 84.52(17) . . ? O4 Mn6 O10 91.25(16) . . ? O9 Mn6 O10 93.06(16) . . ? O11 Mn6 O10 91.47(18) . . ? O7 Mn6 O10 87.02(16) . . ? O4 Mn6 O8 94.04(16) . . ? O9 Mn6 O8 93.18(16) . . ? O11 Mn6 O8 82.67(18) . . ? O7 Mn6 O8 86.59(18) . . ? O10 Mn6 O8 171.71(17) . . ? C2 Cl1B Cl6 138(3) . 2 ? C10 Cl5B Cl5B 153.6(10) . 2 ? C12B Cl6 C12A 34.2(8) . . ? C12B Cl6 Cl1B 108.3(12) . 2 ? C12A Cl6 Cl1B 138.7(15) . 2 ? O3 C1 O23 126.9(5) . . ? O3 C1 C2 120.7(5) . . ? O23 C1 C2 112.4(5) . . ? C1 C2 Cl1B 113.9(15) . . ? C1 C2 Cl1A 114.3(5) . . ? Cl1B C2 Cl1A 105.7(15) . . ? O2 C3 O7 126.8(5) . . ? O2 C3 C4 118.8(5) . . ? O7 C3 C4 114.4(5) . . ? C3 C4 Cl2A 112.8(5) . . ? C3 C4 Cl2B 112.2(6) . . ? Cl2A C4 Cl2B 27.5(5) . . ? O19 C5 O11 126.3(5) . . ? O19 C5 C6 119.8(5) . . ? O11 C5 C6 113.9(5) . . ? C5 C6 Cl3B 113.7(8) . . ? C5 C6 Cl3A 112.4(5) . . ? Cl3B C6 Cl3A 7.3(9) . . ? O22 C7 O18 126.6(5) 2 . ? O22 C7 C8 116.2(5) 2 . ? O18 C7 C8 117.2(5) . . ? C7 C8 Cl4D 113.5(7) . . ? C7 C8 Cl4A 114.2(5) . . ? Cl4D C8 Cl4A 46.5(9) . . ? C7 C8 Cl4B 104.6(8) . . ? Cl4D C8 Cl4B 92.6(12) . . ? Cl4A C8 Cl4B 46.4(8) . . ? C7 C8 Cl4C 100.3(6) . . ? Cl4D C8 Cl4C 30.9(8) . . ? Cl4A C8 Cl4C 77.2(7) . . ? Cl4B C8 Cl4C 123.5(9) . . ? O16 C9 O14 127.2(6) . . ? O16 C9 C10 118.1(6) . . ? O14 C9 C10 114.7(6) . . ? C9 C10 Cl5A 111.8(6) . . ? C9 C10 Cl5E 129.2(10) . . ? Cl5A C10 Cl5E 84.0(9) . . ? C9 C10 Cl5B 118.6(8) . . ? Cl5A C10 Cl5B 82.6(9) . . ? Cl5E C10 Cl5B 111.0(11) . . ? C9 C10 Cl5D 116.7(13) . . ? Cl5A C10 Cl5D 57.8(11) . . ? Cl5E C10 Cl5D 112.4(14) . . ? Cl5B C10 Cl5D 26.3(10) . . ? C9 C10 Cl5C 113.2(13) . . ? Cl5A C10 Cl5C 106.3(11) . . ? Cl5E C10 Cl5C 107.1(15) . . ? Cl5B C10 Cl5C 24.4(8) . . ? Cl5D C10 Cl5C 50.6(13) . . ? O10 C11 O17 127.1(6) . . ? O10 C11 C12A 116.1(8) . . ? O17 C11 C12A 113.4(7) . . ? O10 C11 C12B 118.2(8) . . ? O17 C11 C12B 111.2(8) . . ? C12A C11 C12B 40.1(11) . . ? C11 C12A Cl6 105.7(11) . . ? C11 C12B Cl6 117.4(10) . . ? O21 C13 O1 127.4(6) . . ? O21 C13 C14 115.0(6) . . ? O1 C13 C14 117.5(6) . . ? Cl7B C14 C13 122.0(11) . . ? Cl7B C14 Cl7C 56.8(13) . . ? C13 C14 Cl7C 123.2(11) . . ? Cl7B C14 Cl7A 83.5(8) . . ? C13 C14 Cl7A 115.7(6) . . ? Cl7C C14 Cl7A 120.0(11) . . ? O6 C15 O20 127.5(6) . . ? O6 C15 C16 121.4(6) . . ? O20 C15 C16 111.1(6) . . ? C15 C16 Cl8B 117.8(7) . . ? C15 C16 Cl8A 112.8(6) . . ? Cl8B C16 Cl8A 17.8(6) . . ? C13 O1 Mn4 130.2(4) . . ? C3 O2 Mn4 131.8(4) . . ? C1 O3 Mn4 122.0(3) . . ? Mn2 O4 Mn6 133.80(19) . . ? Mn2 O4 Mn4 95.73(16) . . ? Mn6 O4 Mn4 129.4(2) . . ? Mn5 O5 Mn2 132.7(2) . . ? Mn5 O5 Mn4 122.47(19) . . ? Mn2 O5 Mn4 93.81(16) . . ? C15 O6 Mn4 131.4(4) . . ? C3 O7 Mn6 127.5(4) . . ? Mn6 O8 H81 109.5 . . ? Mn6 O8 H82 131.6 . . ? H81 O8 H82 96.1 . . ? Mn1 O9 Mn3 94.35(16) . . ? Mn1 O9 Mn6 132.46(19) . . ? Mn3 O9 Mn6 122.23(19) . . ? C11 O10 Mn6 129.6(4) . . ? C5 O11 Mn6 135.3(4) . . ? Mn1 O12 Mn2 95.31(16) . 2 ? Mn1 O12 Mn2 94.74(15) . . ? Mn2 O12 Mn2 100.44(16) 2 . ? Mn2 O13 Mn1 95.21(15) . . ? Mn2 O13 Mn1 94.54(15) . 2 ? Mn1 O13 Mn1 100.46(15) . 2 ? C9 O14 Mn1 124.0(4) . . ? Mn1 O15 Mn3 95.44(16) . . ? Mn1 O15 Mn5 134.2(2) . 2 ? Mn3 O15 Mn5 128.56(19) . 2 ? C9 O16 Mn3 122.3(4) . . ? C11 O17 Mn3 129.9(4) . . ? C7 O18 Mn3 132.5(4) . . ? C5 O19 Mn3 130.1(4) . . ? C15 O20 Mn5 129.6(4) . . ? C13 O21 Mn5 134.1(4) . . ? C7 O22 Mn5 128.8(4) 2 . ? C1 O23 Mn2 124.9(4) . . ? Cl9 C17 Cl10 109.9(6) . . ? C17 Cl9 O28 103.8(12) . . ? _diffrn_reflns_theta_full 25.00 _refine_diff_density_max 1.430 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.243 #===END data_2 _database_code_CSD 165982 _audit_creation_method SHELXL-97 _chemical_name_systematic ; dodecakis(\m^3^-Oxo)-hexadecakis(\m^2^-bromoacetato)-tetra-aqua- tetra-manganese(iv)-octa-manganese(iii) tetra-dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 Br16 Mn12 O48, 4(C1 H2 Cl2)' _chemical_formula_sum 'C36 H48 Br16 Cl8 Mn12 O48' _chemical_formula_weight 3470.18 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' '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' 'Br' 'Br' -0.2901 2.4595 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 26.647(4) _cell_length_b 26.647(4) _cell_length_c 12.850(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9124(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23936 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.6 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6576 _exptl_absorpt_coefficient_mu 8.929 _exptl_absorpt_correction_type cylinder _exptl_absorpt_correction_T_min 0.12 _exptl_absorpt_correction_T_max 0.16 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 23936 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5156 _reflns_number_gt 3607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'WINGX (Farrugia, 1999)' _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 'w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+165.7069P] 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 5156 _refine_ls_number_parameters 298 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2241 _refine_ls_wR_factor_gt 0.1992 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 0.53219(4) 0.90435(4) 0.10944(10) 0.0209(3) Uani 1 1 d . . . Mn2 Mn 0.63568(4) 0.83506(4) 0.05843(10) 0.0215(3) Uani 1 1 d . . . Mn3 Mn 0.54788(4) 0.77865(4) 0.05210(9) 0.0166(3) Uani 1 1 d . . . Br1A Br 0.62256(6) 0.73954(5) -0.30659(10) 0.0582(4) Uani 0.94 1 d PD A 1 Br1B Br 0.5325(15) 0.7573(18) -0.312(2) 0.128(16) Uani 0.06 1 d PD . 2 Br2 Br 0.39907(4) 1.06177(4) 0.26902(10) 0.0508(3) Uani 1 1 d . . . Br3A Br 0.71894(10) 0.98723(11) -0.0371(4) 0.1404(16) Uani 0.77 1 d PD B 3 Br3B Br 0.7000(4) 1.0131(3) 0.0692(8) 0.103(3) Uani 0.23 1 d PD B 4 Br4A Br 0.39235(9) 0.90596(8) -0.23104(14) 0.0652(5) Uani 0.81 1 d PD C 5 Br4B Br 0.3718(7) 0.8916(13) -0.2000(14) 0.31(2) Uani 0.19 1 d PD C 6 O1 O 0.56590(19) 0.84586(19) 0.0675(4) 0.0194(11) Uani 1 1 d . . . O2 O 0.48346(19) 0.86697(19) 0.1857(4) 0.0195(11) Uani 1 1 d . . . O5 O 0.6230(2) 0.8263(2) -0.1116(5) 0.0310(14) Uani 1 1 d . . . O12 O 0.4098(2) 0.8939(2) 0.0219(5) 0.0290(13) Uani 1 1 d . . . O10 O 0.6522(2) 0.9053(2) 0.0432(5) 0.0315(14) Uani 1 1 d . . . O9 O 0.5791(2) 0.9466(2) 0.0304(5) 0.0309(14) Uani 1 1 d . . . O8 O 0.4264(2) 0.9566(2) 0.2143(5) 0.0309(14) Uani 1 1 d . . . O6 O 0.5523(2) 0.7806(2) -0.0965(4) 0.0233(12) Uani 1 1 d . . . O3 O 0.5806(3) 0.9160(3) 0.2454(5) 0.0393(16) Uani 1 1 d . . . O11 O 0.4893(2) 0.9016(2) -0.0292(5) 0.0327(14) Uani 1 1 d . . . O7 O 0.5045(2) 0.9691(2) 0.1555(6) 0.0348(15) Uani 1 1 d . . . O4 O 0.5395(2) 0.77330(19) 0.1985(4) 0.0200(11) Uani 1 1 d . . . C7 C 0.4453(3) 0.8883(3) -0.0433(7) 0.032(2) Uani 1 1 d . C . C8 C 0.4344(4) 0.8626(4) -0.1486(9) 0.052(3) Uani 1 1 d D . . H4A H 0.4177 0.8307 -0.1371 0.063 Uiso 1 1 calc R C 5 H4B H 0.4657 0.8561 -0.1851 0.063 Uiso 1 1 calc R C 5 C5 C 0.6260(3) 0.9433(3) 0.0234(8) 0.031(2) Uani 1 1 d . B . C6 C 0.6506(3) 0.9902(3) -0.0135(10) 0.050(3) Uani 1 1 d D . . H6A H 0.6444 1.0163 0.0375 0.059 Uiso 1 1 calc R B 3 H6B H 0.6345 1.0004 -0.0778 0.059 Uiso 1 1 calc R B 3 C3 C 0.4640(3) 0.9829(3) 0.1956(7) 0.0263(18) Uani 1 1 d . . . C4 C 0.4632(4) 1.0376(3) 0.2216(8) 0.034(2) Uani 1 1 d . . . H8A H 0.4729 1.0565 0.1603 0.041 Uiso 1 1 calc R . . H8B H 0.4880 1.0440 0.2752 0.041 Uiso 1 1 calc R . . C1 C 0.5877(3) 0.8024(3) -0.1489(7) 0.0275(18) Uani 1 1 d . A . C2 C 0.5845(4) 0.7975(4) -0.2633(7) 0.043(2) Uani 1 1 d D . . H10A H 0.5978 0.8274 -0.2962 0.052 Uiso 1 1 calc R A 1 H10B H 0.5497 0.7937 -0.2841 0.052 Uiso 1 1 calc R A 1 Cl2 Cl 0.75875(18) 0.09107(18) 0.1554(5) 0.1056(16) Uani 1 1 d . . . Cl1 Cl 0.7483(4) 0.1875(4) 0.2199(10) 0.220(5) Uani 1 1 d . . . C11 C 0.7751(10) 0.1330(11) 0.2583(17) 0.145(11) Uani 1 1 d . . . H20A H 0.7614 0.1217 0.3243 0.174 Uiso 1 1 calc R . . H20B H 0.8112 0.1364 0.2646 0.174 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0156(6) 0.0116(6) 0.0357(7) -0.0003(5) 0.0022(5) -0.0009(4) Mn2 0.0127(6) 0.0159(6) 0.0358(7) 0.0031(5) 0.0016(5) -0.0003(4) Mn3 0.0122(5) 0.0129(5) 0.0246(6) -0.0001(4) 0.0009(4) -0.0005(4) Br1A 0.0714(9) 0.0495(7) 0.0537(7) -0.0191(6) 0.0195(6) -0.0063(6) Br1B 0.17(4) 0.17(4) 0.050(16) 0.001(19) -0.004(19) -0.06(3) Br2 0.0468(7) 0.0281(5) 0.0776(8) -0.0092(5) 0.0142(6) 0.0099(4) Br3A 0.0654(15) 0.0849(18) 0.271(5) 0.064(2) 0.047(2) -0.0054(12) Br3B 0.102(6) 0.083(5) 0.125(7) 0.008(5) -0.023(5) -0.044(5) Br4A 0.0833(14) 0.0761(12) 0.0363(8) 0.0027(7) -0.0173(8) 0.0147(10) Br4B 0.19(2) 0.64(6) 0.083(11) 0.09(2) -0.070(12) -0.15(3) O1 0.016(3) 0.012(2) 0.030(3) 0.000(2) 0.002(2) -0.002(2) O2 0.015(3) 0.010(2) 0.033(3) -0.002(2) 0.003(2) -0.001(2) O5 0.029(3) 0.028(3) 0.035(3) 0.006(3) 0.009(3) -0.003(3) O12 0.022(3) 0.029(3) 0.036(3) 0.007(3) -0.001(2) 0.003(2) O10 0.017(3) 0.021(3) 0.057(4) 0.003(3) -0.002(3) -0.003(2) O9 0.025(3) 0.017(3) 0.051(4) 0.007(3) 0.003(3) 0.000(2) O8 0.027(3) 0.011(3) 0.054(4) 0.000(3) 0.009(3) 0.001(2) O6 0.017(3) 0.026(3) 0.027(3) -0.001(2) 0.002(2) 0.001(2) O3 0.034(4) 0.039(4) 0.045(4) -0.010(3) -0.005(3) 0.000(3) O11 0.024(3) 0.037(4) 0.038(3) 0.008(3) -0.003(3) -0.003(3) O7 0.030(3) 0.014(3) 0.060(4) -0.002(3) 0.009(3) -0.001(2) O4 0.018(3) 0.015(3) 0.027(3) 0.003(2) 0.000(2) 0.001(2) C7 0.030(5) 0.026(5) 0.040(5) 0.010(4) -0.010(4) -0.003(4) C8 0.052(7) 0.044(6) 0.061(7) 0.000(5) -0.003(6) -0.009(5) C5 0.018(4) 0.024(4) 0.049(5) 0.004(4) 0.002(4) -0.002(3) C6 0.029(5) 0.015(4) 0.105(9) 0.013(5) -0.003(6) -0.008(4) C3 0.026(4) 0.021(4) 0.032(4) -0.007(3) 0.002(3) -0.001(3) C4 0.033(5) 0.020(4) 0.050(5) -0.008(4) 0.013(4) 0.000(4) C1 0.027(5) 0.019(4) 0.036(4) 0.003(3) 0.003(4) 0.006(4) C2 0.058(7) 0.042(6) 0.030(5) 0.005(4) 0.003(5) 0.005(5) Cl2 0.081(3) 0.076(3) 0.159(5) 0.021(3) 0.023(3) -0.006(2) Cl1 0.183(8) 0.166(8) 0.310(13) -0.066(8) 0.116(9) -0.040(7) C11 0.15(2) 0.19(3) 0.097(15) 0.014(16) 0.045(15) 0.08(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 O1 1.878(5) . ? Mn1 O2 1.907(5) . ? Mn1 O9 1.966(6) . ? Mn1 O7 1.968(6) . ? Mn1 O11 2.119(6) . ? Mn1 O3 2.193(7) . ? Mn2 O1 1.885(5) . ? Mn2 O2 1.894(5) 15_565 ? Mn2 O10 1.934(6) . ? Mn2 O8 1.938(6) 15_565 ? Mn2 O12 2.195(6) 15_565 ? Mn2 O5 2.222(6) . ? Mn2 Mn3 2.7821(16) . ? Mn3 O1 1.865(5) . ? Mn3 O2 1.876(5) 15_565 ? Mn3 O4 1.900(6) . ? Mn3 O6 1.914(6) . ? Mn3 O4 1.919(5) 12_766 ? Mn3 O4 1.931(5) 15_565 ? Mn3 Mn3 2.8162(19) 12_766 ? Mn3 Mn3 2.8162(19) 15_565 ? Mn3 Mn3 2.973(2) 6_564 ? Br1A C2 1.929(9) . ? Br1B Br1B 1.77(6) 6_564 ? Br1B C2 1.862(19) . ? Br1B Br1B 2.04(5) 15_564 ? Br1B Br1B 2.04(5) 12_765 ? Br2 C4 1.924(9) . ? Br3A C6 1.847(9) . ? Br3B C6 1.798(12) . ? Br4A C8 1.927(10) . ? Br4B C8 1.954(18) . ? O2 Mn3 1.876(5) 12_766 ? O2 Mn2 1.894(5) 12_766 ? O5 C1 1.234(11) . ? O12 C7 1.272(11) . ? O12 Mn2 2.195(6) 12_766 ? O10 C5 1.253(10) . ? O9 C5 1.256(10) . ? O8 C3 1.244(10) . ? O8 Mn2 1.938(6) 12_766 ? O6 C1 1.296(10) . ? O11 C7 1.237(11) . ? O7 C3 1.253(10) . ? O4 Mn3 1.919(5) 15_565 ? O4 Mn3 1.931(5) 12_766 ? C7 C8 1.545(15) . ? C8 H4A 0.9700 . ? C8 H4B 0.9700 . ? C5 C6 1.490(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C3 C4 1.496(12) . ? C4 H8A 0.9700 . ? C4 H8B 0.9700 . ? C1 C2 1.478(13) . ? C2 H10A 0.9700 . ? C2 H10B 0.9700 . ? Cl2 C11 1.78(3) . ? Cl1 C11 1.69(3) . ? C11 H20A 0.9700 . ? C11 H20B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 92.3(2) . . ? O1 Mn1 O9 91.3(2) . . ? O2 Mn1 O9 176.1(2) . . ? O1 Mn1 O7 173.4(3) . . ? O2 Mn1 O7 92.8(2) . . ? O9 Mn1 O7 83.8(3) . . ? O1 Mn1 O11 89.3(2) . . ? O2 Mn1 O11 92.7(2) . . ? O9 Mn1 O11 85.9(3) . . ? O7 Mn1 O11 94.6(3) . . ? O1 Mn1 O3 93.7(2) . . ? O2 Mn1 O3 93.7(3) . . ? O9 Mn1 O3 87.5(3) . . ? O7 Mn1 O3 81.7(3) . . ? O11 Mn1 O3 172.8(3) . . ? O1 Mn2 O2 83.4(2) . 15_565 ? O1 Mn2 O10 94.8(2) . . ? O2 Mn2 O10 175.9(3) 15_565 . ? O1 Mn2 O8 174.8(3) . 15_565 ? O2 Mn2 O8 96.3(2) 15_565 15_565 ? O10 Mn2 O8 85.2(3) . 15_565 ? O1 Mn2 O12 91.6(2) . 15_565 ? O2 Mn2 O12 92.7(2) 15_565 15_565 ? O10 Mn2 O12 91.0(3) . 15_565 ? O8 Mn2 O12 93.6(3) 15_565 15_565 ? O1 Mn2 O5 85.8(2) . . ? O2 Mn2 O5 84.2(2) 15_565 . ? O10 Mn2 O5 92.1(3) . . ? O8 Mn2 O5 89.0(3) 15_565 . ? O12 Mn2 O5 176.1(2) 15_565 . ? O1 Mn2 Mn3 41.83(15) . . ? O2 Mn2 Mn3 42.18(15) 15_565 . ? O10 Mn2 Mn3 135.38(18) . . ? O8 Mn2 Mn3 136.95(19) 15_565 . ? O12 Mn2 Mn3 98.42(16) 15_565 . ? O5 Mn2 Mn3 77.72(16) . . ? O1 Mn3 O2 84.5(2) . 15_565 ? O1 Mn3 O4 89.8(2) . . ? O2 Mn3 O4 91.1(2) 15_565 . ? O1 Mn3 O6 93.7(2) . . ? O2 Mn3 O6 91.6(2) 15_565 . ? O4 Mn3 O6 175.8(2) . . ? O1 Mn3 O4 96.3(2) . 12_766 ? O2 Mn3 O4 175.3(2) 15_565 12_766 ? O4 Mn3 O4 84.2(2) . 12_766 ? O6 Mn3 O4 93.0(2) . 12_766 ? O1 Mn3 O4 172.4(2) . 15_565 ? O2 Mn3 O4 99.9(2) 15_565 15_565 ? O4 Mn3 O4 83.9(3) . 15_565 ? O6 Mn3 O4 92.4(2) . 15_565 ? O4 Mn3 O4 78.9(2) 12_766 15_565 ? O1 Mn3 Mn2 42.38(16) . . ? O2 Mn3 Mn2 42.70(16) 15_565 . ? O4 Mn3 Mn2 96.32(17) . . ? O6 Mn3 Mn2 87.86(17) . . ? O4 Mn3 Mn2 138.57(16) 12_766 . ? O4 Mn3 Mn2 142.53(16) 15_565 . ? O1 Mn3 Mn3 86.63(17) . 12_766 ? O2 Mn3 Mn3 133.35(18) 15_565 12_766 ? O4 Mn3 Mn3 43.12(16) . 12_766 ? O6 Mn3 Mn3 134.71(17) . 12_766 ? O4 Mn3 Mn3 42.23(16) 12_766 12_766 ? O4 Mn3 Mn3 85.89(16) 15_565 12_766 ? Mn2 Mn3 Mn3 119.41(6) . 12_766 ? O1 Mn3 Mn3 132.21(18) . 15_565 ? O2 Mn3 Mn3 89.91(17) 15_565 15_565 ? O4 Mn3 Mn3 42.74(16) . 15_565 ? O6 Mn3 Mn3 134.00(18) . 15_565 ? O4 Mn3 Mn3 86.12(16) 12_766 15_565 ? O4 Mn3 Mn3 42.26(16) 15_565 15_565 ? Mn2 Mn3 Mn3 121.66(6) . 15_565 ? Mn3 Mn3 Mn3 63.73(5) 12_766 15_565 ? O1 Mn3 Mn3 135.57(17) . 6_564 ? O2 Mn3 Mn3 138.94(17) 15_565 6_564 ? O4 Mn3 Mn3 82.01(16) . 6_564 ? O6 Mn3 Mn3 93.83(17) . 6_564 ? O4 Mn3 Mn3 39.58(16) 12_766 6_564 ? O4 Mn3 Mn3 39.28(16) 15_565 6_564 ? Mn2 Mn3 Mn3 177.52(6) . 6_564 ? Mn3 Mn3 Mn3 58.13(2) 12_766 6_564 ? Mn3 Mn3 Mn3 58.13(2) 15_565 6_564 ? Br1B Br1B C2 148(4) 6_564 . ? Br1B Br1B Br1B 64.2(10) 6_564 15_564 ? C2 Br1B Br1B 144(3) . 15_564 ? Br1B Br1B Br1B 64.2(10) 6_564 12_765 ? C2 Br1B Br1B 118(3) . 12_765 ? Br1B Br1B Br1B 52(2) 15_564 12_765 ? Mn3 O1 Mn1 134.8(3) . . ? Mn3 O1 Mn2 95.8(2) . . ? Mn1 O1 Mn2 128.0(3) . . ? Mn3 O2 Mn2 95.1(2) 12_766 12_766 ? Mn3 O2 Mn1 132.3(3) 12_766 . ? Mn2 O2 Mn1 122.6(3) 12_766 . ? C1 O5 Mn2 123.5(6) . . ? C7 O12 Mn2 126.6(5) . 12_766 ? C5 O10 Mn2 132.4(6) . . ? C5 O9 Mn1 129.0(6) . . ? C3 O8 Mn2 130.3(6) . 12_766 ? C1 O6 Mn3 125.1(6) . . ? C7 O11 Mn1 130.1(6) . . ? C3 O7 Mn1 134.7(6) . . ? Mn3 O4 Mn3 95.0(2) . 15_565 ? Mn3 O4 Mn3 94.6(2) . 12_766 ? Mn3 O4 Mn3 101.1(2) 15_565 12_766 ? O11 C7 O12 125.0(9) . . ? O11 C7 C8 115.7(9) . . ? O12 C7 C8 119.3(8) . . ? C7 C8 Br4A 108.9(7) . . ? C7 C8 Br4B 106.3(10) . . ? Br4A C8 Br4B 23.1(7) . . ? C7 C8 H4A 109.9 . . ? Br4A C8 H4A 109.9 . . ? Br4B C8 H4A 90.3 . . ? C7 C8 H4B 109.9 . . ? Br4A C8 H4B 109.9 . . ? Br4B C8 H4B 129.8 . . ? H4A C8 H4B 108.3 . . ? O10 C5 O9 126.6(8) . . ? O10 C5 C6 119.8(8) . . ? O9 C5 C6 113.6(8) . . ? C5 C6 Br3B 114.7(8) . . ? C5 C6 Br3A 116.7(7) . . ? Br3B C6 Br3A 52.4(4) . . ? C5 C6 H6A 108.1 . . ? Br3B C6 H6A 58.9 . . ? Br3A C6 H6A 108.1 . . ? C5 C6 H6B 108.1 . . ? Br3B C6 H6B 137.2 . . ? Br3A C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? O8 C3 O7 127.5(8) . . ? O8 C3 C4 119.6(7) . . ? O7 C3 C4 112.9(7) . . ? C3 C4 Br2 114.2(6) . . ? C3 C4 H8A 108.7 . . ? Br2 C4 H8A 108.7 . . ? C3 C4 H8B 108.7 . . ? Br2 C4 H8B 108.7 . . ? H8A C4 H8B 107.6 . . ? O5 C1 O6 125.8(8) . . ? O5 C1 C2 118.5(8) . . ? O6 C1 C2 115.7(8) . . ? C1 C2 Br1B 115.6(12) . . ? C1 C2 Br1A 109.1(6) . . ? Br1B C2 Br1A 80.4(18) . . ? C1 C2 H10A 109.9 . . ? Br1B C2 H10A 126.7 . . ? Br1A C2 H10A 109.9 . . ? C1 C2 H10B 109.9 . . ? Br1B C2 H10B 30.1 . . ? Br1A C2 H10B 109.9 . . ? H10A C2 H10B 108.3 . . ? Cl1 C11 Cl2 102.6(14) . . ? Cl1 C11 H20A 111.2 . . ? Cl2 C11 H20A 111.2 . . ? Cl1 C11 H20B 111.2 . . ? Cl2 C11 H20B 111.2 . . ? H20A C11 H20B 109.2 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.810 _refine_diff_density_min -2.109 _refine_diff_density_rms 0.210