Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_Cuban-1 _database_code_CSD 162244 _journal_coden_Cambridge 182 _audit_creation_date january-22-2001 _audit_creation_method 'ct.exe (M. K\"ockerling, 1996)' _publ_contact_author_name 'Dr. Martin K\"ockerling' _publ_contact_author_address ; Gerhard-Mercator-Universit\"at Duisburg FB 6 - Festk\"orperchemie Lotharstr. 1 47057 Duisburg Germany ; _publ_contact_author_phone 'intl-code-(0)203-379-1715' _publ_contact_author_fax 'intl-code-(0)203-379-2110' _publ_contact_author_email 'hi356ko@uni-duisburg.de' loop_ _publ_author_name _publ_author_address 'Martin K\"ockerling' ; Gerhard-Mercator-Universit\"at Duisburg FB 6 - Festk\"orperchemie Lotharstr. 1 47057 Duisburg Germany ; 'Johannes B. Willems' ; Gerhard-Mercator-Universit\"at Duisburg FB 6 - Festk\"orperchemie Lotharstr. 1 47057 Duisburg Germany ; _publ_requested_journal 'Chemical Communications' _chemical_formula_sum 'C48 H96 CL8 Fe5 K4 O24 S4' _chemical_formula_moiety '[(C12 H24 O6)4 K4 (Fe Cl4)] [Fe4 S4 Cl4]' _chemical_formula_weight 1904.740 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' 'S' 'S' 0.1246 0.1234 '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' 'K' 'K' 0.2009 0.2494 'INTERNATIONAL TABLES VOL C TABLES 4.2.6.8 AND 6.1.1.4' 'FE' 'FE' 0.3463 0.8444 'INTERNATIONAL TABLES VOL C TABLES 4.2.6.8 AND 6.1.1.4' _symmetry_cell_setting 'cubic' _symmetry_space_group_name_H-M 'F 2 3' loop_ _symmetry_equiv_pos_as_xyz 'X, Y, Z' '-X, -Y, Z' '-X, Y, -Z' 'X, -Y, -Z' 'Z, X, Y' 'Z, -X, -Y' '-Z, -X, Y' '-Z, X, -Y' 'Y, Z, X' '-Y, Z, -X' 'Y, -Z, -X' '-Y, -Z, X' 'X, Y+1/2, Z+1/2' '-X, -Y+1/2, Z+1/2' '-X, Y+1/2, -Z+1/2' 'X, -Y+1/2, -Z+1/2' 'Z, X+1/2, Y+1/2' 'Z, -X+1/2, -Y+1/2' '-Z, -X+1/2, Y+1/2' '-Z, X+1/2, -Y+1/2' 'Y, Z+1/2, X+1/2' '-Y, Z+1/2, -X+1/2' 'Y, -Z+1/2, -X+1/2' '-Y, -Z+1/2, X+1/2' 'X+1/2, Y, Z+1/2' '-X+1/2, -Y, Z+1/2' '-X+1/2, Y, -Z+1/2' 'X+1/2, -Y, -Z+1/2' 'Z+1/2, X, Y+1/2' 'Z+1/2, -X, -Y+1/2' '-Z+1/2, -X, Y+1/2' '-Z+1/2, X, -Y+1/2' 'Y+1/2, Z, X+1/2' '-Y+1/2, Z, -X+1/2' 'Y+1/2, -Z, -X+1/2' '-Y+1/2, -Z, X+1/2' 'X+1/2, Y+1/2, Z' '-X+1/2, -Y+1/2, Z' '-X+1/2, Y+1/2, -Z' 'X+1/2, -Y+1/2, -Z' 'Z+1/2, X+1/2, Y' 'Z+1/2, -X+1/2, -Y' '-Z+1/2, -X+1/2, Y' '-Z+1/2, X+1/2, -Y' 'Y+1/2, Z+1/2, X' '-Y+1/2, Z+1/2, -X' 'Y+1/2, -Z+1/2, -X' '-Y+1/2, -Z+1/2, X' _cell_length_a 21.241(2) _cell_length_b 21.241(2) _cell_length_c 21.241(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9583(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 56 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 22.7 _exptl_crystal_description 'small cylinder' _exptl_crystal_colour black _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.32 _exptl_crystal_F_000 3928 _exptl_absorpt_coefficient_mu 1.277 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tune' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Stoe IPDS' _computing_structure_solution 'SHELXL (Sheldrick, 1990' _computing_molecular_graphics 'Siemens SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_reflns_number 23259 _diffrn_reflns_av_R_equivalents 0.093 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.15 _reflns_number_total 1973 _reflns_number_gt 1182 _reflns_threshold_expression '> 2.0sigma(I)' _refine_ls_structure_factor_coef 'Fsqd' _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme 'CALC W=1/[\S^2^(FO^2^)+(0.1021P)^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 0.0006(1) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1973 _refine_ls_number_parameters 72 _refine_ls_number_restraints 4 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.175 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.57 _refine_diff_density_min -0.3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Fe1 0.79644(4) 0.70356(4) 0.79644(4) 0.0513(4) S1 0.80986(7) 0.80986(7) 0.80986(7) 0.0551(6) Cl1 0.85683(8) 0.64317(8) 0.85683(8) 0.0719(8) Fe2 0.25 0.75 0.75 0.0532(7) Cl2 0.3114(1) 0.8114(1) 0.8114(1) 0.151(2) K1 0.14733(8) 0.85267(8) 0.85267(8) 0.0693(7) C1 0.1750(8) 0.8052(9) 1.0183(6) 0.18(1) C2 0.054(1) 0.7289(6) 0.9265(9) 0.20(1) O1 0.2075(5) 0.8420(4) 0.9723(3) 0.127(3) O2 0.0937(5) 0.7765(4) 0.9541(4) 0.132(4) C3 0.0036(8) 0.7585(8) 0.896(1) 0.19(1) C4 0.1463(9) 0.7529(9) 0.9896(7) 0.23(2) H1A 0.20496 0.78334 1.04412 0.27235 H1B 0.1486 0.82953 1.04578 0.27235 H2A 0.07718 0.70645 0.89475 0.29762 H2B 0.0398 0.69909 0.95726 0.29762 H3A -0.02752 0.72822 0.88353 0.29221 H3B -0.01517 0.78735 0.92526 0.29221 H4A 0.17026 0.72733 0.96104 0.34198 H4B 0.12418 0.72645 1.0188 0.34198 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 Fe1 0.0513(4) 0.0513(4) 0.0513(4) 0.0012(3) -0.0012(3) 0.0012(3) S1 0.0551(6) 0.0551(6) 0.0551(6) -0.0044(5) -0.0044(5) -0.0044(5) Cl1 0.0719(8) 0.0719(8) 0.0719(8) 0.0110(7) -0.0110(7) 0.0110(7) Fe2 0.0532(7) 0.0532(7) 0.0532(7) 0 0 0 Cl2 0.151(2) 0.151(2) 0.151(2) -0.053(2) -0.053(2) -0.053(2) K1 0.0693(7) 0.0693(7) 0.0693(7) 0.0035(7) -0.0035(7) -0.0035(7) C1 0.20(2) 0.29(3) 0.062(6) 0.03(1) 0.019(8) 0.16(2) C2 0.27(2) 0.064(7) 0.26(2) -0.013(10) 0.19(2) -0.03(1) O1 0.135(6) 0.186(8) 0.061(3) -0.025(4) -0.019(4) 0.063(6) O2 0.184(9) 0.086(5) 0.127(6) 0.027(4) 0.081(6) 0.023(5) C3 0.14(1) 0.15(1) 0.29(3) -0.12(2) 0.14(2) -0.09(1) C4 0.32(3) 0.20(2) 0.15(2) 0.14(2) 0.13(2) 0.14(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 Cl1 2.222(3) Fe1 S1 2.294(2) Fe1 Fe1 2.790(2) Fe2 Cl2 2.260(4) Fe2 K1 3.777(3) Cl2 K1 3.699(3) K1 O1 2.854(6) K1 O2 2.925(7) C1 C4 1.41(2) C1 O1 1.43(2) C2 C3 1.40(2) C2 O2 1.44(2) O1 C3 1.45(2) O2 C4 1.44(2) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle S1 Fe1 Cl1 115.14(5) S1 Fe1 S1 103.25(6) S1 Fe1 S1 103.25(6) Fe1 Fe1 Cl1 144.7 Fe1 Fe1 S1 52.54(4) Fe1 Fe1 S1 100.12(5) Fe1 Fe1 S1 52.54(4) Fe1 Fe1 Fe1 60 Fe1 Fe1 Fe1 60 Fe1 S1 Fe1 74.92(8) Fe1 S1 Fe1 74.92(8) Cl2 Fe2 Cl2 109.5 Cl2 Fe2 Cl2 109.5 Cl2 Fe2 Cl2 109.471(1) Cl2 Fe2 K1 180.0(2) Cl2 Fe2 K1 70.5 Cl2 Fe2 K1 70.5 K1 Fe2 K1 109.5 K1 Fe2 K1 109.5 Fe2 Cl2 K1 74.30(6) K1 Cl2 K1 112.96(5) K1 Cl2 K1 112.96(5) O1 K1 O1 115.7(1) O1 K1 O1 115.7(1) O1 K1 O2 148.6(2) O1 K1 O2 57.6(3) O1 K1 O2 58.3(3) O2 K1 O2 109.7(1) O2 K1 O2 109.7(1) Cl2 K1 O1 76.7(2) Cl2 K1 O1 91.7(2) Cl2 K1 O1 135.6(2) Cl2 K1 O2 130.9(2) Cl2 K1 O2 75.2(2) Cl2 K1 O2 114.2(2) Cl2 K1 Cl2 59.8(1) Cl2 K1 Cl2 59.8(1) Fe2 K1 O1 102.1(2) Fe2 K1 O1 102.1(2) Fe2 K1 O2 109.3(2) Fe2 K1 O2 109.3(2) Fe2 K1 Cl2 35.17(6) Fe2 K1 Cl2 35.17(6) O1 C1 C4 110(1) O2 C2 C3 109(1) C1 O1 C3 116(1) K1 O1 C1 115.8(8) K1 O1 C3 118.4(9) C2 O2 C4 115(1) K1 O2 C4 106.1(7) K1 O2 C2 108.4(7) C2 C3 O1 109(1)