# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c2m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 Cl2 K O24 Ru2 Zn2' _chemical_formula_sum 'C4 Cl2 K O24 Ru2 Zn2' _chemical_formula_weight 874.92 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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/m' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 15.771(2) _cell_length_b 15.374(2) _cell_length_c 10.6099(17) _cell_angle_alpha 90.00 _cell_angle_beta 104.882(2) _cell_angle_gamma 90.00 _cell_volume 2486.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 3.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3674 _exptl_absorpt_correction_T_max 0.5653 _exptl_absorpt_process_details sadab _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II CCD' _diffrn_measurement_method '\w-\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6760 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.98 _reflns_number_total 2521 _reflns_number_gt 2182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0726P)^2^+7.7865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2521 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Ru1 Ru 0.51044(3) 0.5000 0.89829(5) 0.01278(17) Uani 1 2 d S . . Ru2 Ru 0.95383(3) 0.5000 0.89844(5) 0.01249(17) Uani 1 2 d S . . Zn1 Zn 0.7500 0.7500 1.0000 0.0156(2) Uani 1 2 d S . . Zn2 Zn 0.2500 0.2500 0.5000 0.0228(2) Uani 1 2 d S . . K2 K 0.34087(13) 0.5000 0.5540(2) 0.0398(5) Uani 1 2 d S . . Cl2 Cl 0.54474(14) 0.5000 0.67648(19) 0.0302(5) Uani 1 2 d S . . Cl1 Cl 0.84355(14) 0.5000 0.6713(2) 0.0330(5) Uani 1 2 d S . . O1 O 0.6029(2) 0.5938(2) 0.9561(3) 0.0215(8) Uani 1 1 d . . . O4 O 0.8828(2) 0.5940(2) 0.9555(3) 0.0201(8) Uani 1 1 d . . . O3 O 0.4165(2) 0.4080(2) 0.8408(3) 0.0210(8) Uani 1 1 d . . . O6 O 1.0263(2) 0.4055(2) 0.8436(4) 0.0198(8) Uani 1 1 d . . . O5 O 0.8667(2) 0.6909(2) 1.1042(4) 0.0234(8) Uani 1 1 d . . . O2 O 0.6844(2) 0.6768(2) 1.1129(4) 0.0240(8) Uani 1 1 d . . . C2 C 0.9073(3) 0.6271(3) 1.0715(5) 0.0173(10) Uani 1 1 d . . . C1 C 0.6242(3) 0.6221(3) 1.0763(5) 0.0179(10) Uani 1 1 d . . . O8 O 0.1629(3) 0.1712(3) 0.5754(4) 0.0308(9) Uani 1 1 d . . . O9 O 0.2589(3) 0.1472(3) 0.3735(4) 0.0287(9) Uani 1 1 d . . . O10 O 0.3553(3) 0.2011(3) 0.6386(4) 0.0346(10) Uani 1 1 d . . . O11 O 0.4840(3) 0.2821(3) 0.3129(5) 0.0406(11) Uani 1 1 d . . . O12 O 0.5731(3) 0.9093(3) 0.6057(4) 0.0395(11) Uani 1 1 d . . . O7 O 0.7239(2) 0.6553(2) 0.8457(3) 0.0197(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0114(3) 0.0145(3) 0.0127(3) 0.000 0.0037(2) 0.000 Ru2 0.0107(3) 0.0123(3) 0.0141(3) 0.000 0.0024(2) 0.000 Zn1 0.0156(4) 0.0146(4) 0.0166(4) -0.0001(3) 0.0041(3) 0.0002(3) Zn2 0.0228(5) 0.0231(5) 0.0213(5) 0.0008(3) 0.0036(4) -0.0011(4) K2 0.0321(11) 0.0345(10) 0.0483(13) 0.000 0.0022(9) 0.000 Cl2 0.0336(11) 0.0410(11) 0.0197(9) 0.000 0.0134(8) 0.000 Cl1 0.0359(11) 0.0244(10) 0.0282(10) 0.000 -0.0109(9) 0.000 O1 0.0231(19) 0.0259(19) 0.0159(18) -0.0053(15) 0.0059(15) -0.0093(15) O4 0.0185(18) 0.0209(18) 0.0189(19) -0.0049(14) 0.0014(15) 0.0055(14) O3 0.024(2) 0.0264(19) 0.0141(18) -0.0025(15) 0.0078(15) -0.0085(15) O6 0.0201(19) 0.0202(18) 0.0186(18) -0.0022(15) 0.0042(15) 0.0067(14) O5 0.0220(19) 0.0204(18) 0.026(2) -0.0059(15) 0.0018(16) 0.0095(15) O2 0.027(2) 0.0245(19) 0.0213(19) -0.0019(15) 0.0067(16) -0.0151(16) C2 0.014(2) 0.018(2) 0.022(3) 0.001(2) 0.007(2) -0.0006(19) C1 0.015(2) 0.020(2) 0.018(2) 0.001(2) 0.002(2) 0.001(2) O8 0.031(2) 0.033(2) 0.031(2) 0.0044(18) 0.0125(18) -0.0035(18) O9 0.032(2) 0.029(2) 0.023(2) -0.0037(17) 0.0041(17) 0.0003(18) O10 0.031(2) 0.030(2) 0.037(2) 0.0062(19) -0.0016(19) 0.0025(18) O11 0.040(3) 0.033(2) 0.044(3) 0.002(2) 0.003(2) 0.0034(19) O12 0.037(3) 0.051(3) 0.032(2) 0.004(2) 0.012(2) 0.010(2) O7 0.0187(18) 0.0202(18) 0.0202(18) -0.0031(15) 0.0052(14) 0.0003(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 Ru1 O3 2.025(3) . ? Ru1 O3 2.025(3) 6_565 ? Ru1 O1 2.031(4) . ? Ru1 O1 2.031(3) 6_565 ? Ru1 Ru1 2.2652(11) 5_667 ? Ru1 Cl2 2.547(2) . ? Ru1 K2 3.934(2) . ? Ru2 O4 2.015(3) 6_565 ? Ru2 O4 2.015(3) . ? Ru2 O6 2.024(3) 6_565 ? Ru2 O6 2.024(3) . ? Ru2 Ru2 2.2701(11) 5_767 ? Ru2 Cl1 2.585(2) . ? Zn1 O5 2.095(4) . ? Zn1 O5 2.095(4) 7_667 ? Zn1 O2 2.100(4) . ? Zn1 O2 2.100(4) 7_667 ? Zn1 O7 2.150(3) 7_667 ? Zn1 O7 2.150(3) . ? Zn2 O10 2.057(4) . ? Zn2 O10 2.057(4) 7_556 ? Zn2 O9 2.101(4) 7_556 ? Zn2 O9 2.101(4) . ? Zn2 O8 2.134(4) . ? Zn2 O8 2.134(4) 7_556 ? Zn2 K2 4.0907(9) . ? Zn2 K2 4.0907(9) 7_556 ? K2 O8 2.963(4) 7_556 ? K2 O8 2.963(4) 4_556 ? K2 O9 2.968(4) 7_556 ? K2 O9 2.968(4) 4_556 ? K2 Cl2 3.143(3) . ? K2 Cl1 3.256(3) 5_666 ? K2 O3 3.289(4) 6_565 ? K2 O3 3.289(4) . ? K2 Cl2 3.391(3) 5_666 ? K2 Zn2 4.0907(9) 4_556 ? Cl2 K2 3.391(3) 5_666 ? Cl1 K2 3.256(3) 5_666 ? O1 C1 1.307(6) . ? O4 C2 1.295(6) . ? O3 C1 1.301(6) 5_667 ? O6 C2 1.295(6) 5_767 ? O5 C2 1.268(6) . ? O2 C1 1.252(6) . ? C2 O6 1.295(6) 5_767 ? C1 O3 1.301(6) 5_667 ? O8 K2 2.963(4) 7_556 ? O9 K2 2.968(4) 7_556 ? 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 Ru1 O3 88.6(2) . 6_565 ? O3 Ru1 O1 178.99(15) . . ? O3 Ru1 O1 90.46(16) 6_565 . ? O3 Ru1 O1 90.46(16) . 6_565 ? O3 Ru1 O1 178.99(15) 6_565 6_565 ? O1 Ru1 O1 90.5(2) . 6_565 ? O3 Ru1 Ru1 90.76(10) . 5_667 ? O3 Ru1 Ru1 90.76(10) 6_565 5_667 ? O1 Ru1 Ru1 88.91(10) . 5_667 ? O1 Ru1 Ru1 88.91(10) 6_565 5_667 ? O3 Ru1 Cl2 91.94(10) . . ? O3 Ru1 Cl2 91.94(10) 6_565 . ? O1 Ru1 Cl2 88.43(11) . . ? O1 Ru1 Cl2 88.43(11) 6_565 . ? Ru1 Ru1 Cl2 176.22(6) 5_667 . ? O3 Ru1 K2 56.64(10) . . ? O3 Ru1 K2 56.64(10) 6_565 . ? O1 Ru1 K2 123.01(11) . . ? O1 Ru1 K2 123.01(11) 6_565 . ? Ru1 Ru1 K2 130.86(5) 5_667 . ? Cl2 Ru1 K2 52.92(6) . . ? O4 Ru2 O4 91.7(2) 6_565 . ? O4 Ru2 O6 179.22(15) 6_565 6_565 ? O4 Ru2 O6 88.26(15) . 6_565 ? O4 Ru2 O6 88.26(15) 6_565 . ? O4 Ru2 O6 179.22(15) . . ? O6 Ru2 O6 91.8(2) 6_565 . ? O4 Ru2 Ru2 89.17(10) 6_565 5_767 ? O4 Ru2 Ru2 89.17(10) . 5_767 ? O6 Ru2 Ru2 90.06(11) 6_565 5_767 ? O6 Ru2 Ru2 90.06(11) . 5_767 ? O4 Ru2 Cl1 89.27(11) 6_565 . ? O4 Ru2 Cl1 89.27(11) . . ? O6 Ru2 Cl1 91.51(11) 6_565 . ? O6 Ru2 Cl1 91.51(11) . . ? Ru2 Ru2 Cl1 177.75(7) 5_767 . ? O5 Zn1 O5 180.000(1) . 7_667 ? O5 Zn1 O2 87.80(16) . . ? O5 Zn1 O2 92.20(16) 7_667 . ? O5 Zn1 O2 92.20(16) . 7_667 ? O5 Zn1 O2 87.80(16) 7_667 7_667 ? O2 Zn1 O2 180.000(1) . 7_667 ? O5 Zn1 O7 85.46(14) . 7_667 ? O5 Zn1 O7 94.54(14) 7_667 7_667 ? O2 Zn1 O7 87.39(14) . 7_667 ? O2 Zn1 O7 92.61(14) 7_667 7_667 ? O5 Zn1 O7 94.54(14) . . ? O5 Zn1 O7 85.46(14) 7_667 . ? O2 Zn1 O7 92.61(14) . . ? O2 Zn1 O7 87.39(14) 7_667 . ? O7 Zn1 O7 180.000(1) 7_667 . ? O10 Zn2 O10 180.000(1) . 7_556 ? O10 Zn2 O9 89.57(16) . 7_556 ? O10 Zn2 O9 90.43(16) 7_556 7_556 ? O10 Zn2 O9 90.43(16) . . ? O10 Zn2 O9 89.57(16) 7_556 . ? O9 Zn2 O9 180.0 7_556 . ? O10 Zn2 O8 90.22(17) . . ? O10 Zn2 O8 89.78(17) 7_556 . ? O9 Zn2 O8 91.86(16) 7_556 . ? O9 Zn2 O8 88.14(16) . . ? O10 Zn2 O8 89.78(17) . 7_556 ? O10 Zn2 O8 90.22(17) 7_556 7_556 ? O9 Zn2 O8 88.14(16) 7_556 7_556 ? O9 Zn2 O8 91.86(16) . 7_556 ? O8 Zn2 O8 180.00(18) . 7_556 ? O10 Zn2 K2 93.09(12) . . ? O10 Zn2 K2 86.91(12) 7_556 . ? O9 Zn2 K2 44.13(12) 7_556 . ? O9 Zn2 K2 135.87(12) . . ? O8 Zn2 K2 135.77(12) . . ? O8 Zn2 K2 44.23(12) 7_556 . ? O10 Zn2 K2 86.91(12) . 7_556 ? O10 Zn2 K2 93.09(12) 7_556 7_556 ? O9 Zn2 K2 135.87(12) 7_556 7_556 ? O9 Zn2 K2 44.13(12) . 7_556 ? O8 Zn2 K2 44.23(12) . 7_556 ? O8 Zn2 K2 135.77(12) 7_556 7_556 ? K2 Zn2 K2 180.0 . 7_556 ? O8 K2 O8 125.41(17) 7_556 4_556 ? O8 K2 O9 59.56(11) 7_556 7_556 ? O8 K2 O9 148.07(13) 4_556 7_556 ? O8 K2 O9 148.07(13) 7_556 4_556 ? O8 K2 O9 59.56(11) 4_556 4_556 ? O9 K2 O9 99.39(17) 7_556 4_556 ? O8 K2 Cl2 95.07(9) 7_556 . ? O8 K2 Cl2 95.07(9) 4_556 . ? O9 K2 Cl2 116.54(9) 7_556 . ? O9 K2 Cl2 116.54(9) 4_556 . ? O8 K2 Cl1 75.63(9) 7_556 5_666 ? O8 K2 Cl1 75.63(9) 4_556 5_666 ? O9 K2 Cl1 75.95(9) 7_556 5_666 ? O9 K2 Cl1 75.95(9) 4_556 5_666 ? Cl2 K2 Cl1 158.36(10) . 5_666 ? O8 K2 O3 140.37(11) 7_556 6_565 ? O8 K2 O3 90.33(10) 4_556 6_565 ? O9 K2 O3 100.30(12) 7_556 6_565 ? O9 K2 O3 61.50(10) 4_556 6_565 ? Cl2 K2 O3 61.83(8) . 6_565 ? Cl1 K2 O3 136.27(9) 5_666 6_565 ? O8 K2 O3 90.33(10) 7_556 . ? O8 K2 O3 140.37(11) 4_556 . ? O9 K2 O3 61.50(10) 7_556 . ? O9 K2 O3 100.30(12) 4_556 . ? Cl2 K2 O3 61.83(8) . . ? Cl1 K2 O3 136.27(9) 5_666 . ? O3 K2 O3 50.95(13) 6_565 . ? O8 K2 Cl2 67.48(9) 7_556 5_666 ? O8 K2 Cl2 67.48(9) 4_556 5_666 ? O9 K2 Cl2 127.03(9) 7_556 5_666 ? O9 K2 Cl2 127.03(9) 4_556 5_666 ? Cl2 K2 Cl2 67.73(7) . 5_666 ? Cl1 K2 Cl2 90.63(8) 5_666 5_666 ? O3 K2 Cl2 122.23(9) 6_565 5_666 ? O3 K2 Cl2 122.23(9) . 5_666 ? O8 K2 Ru1 110.99(9) 7_556 . ? O8 K2 Ru1 110.99(9) 4_556 . ? O9 K2 Ru1 92.21(9) 7_556 . ? O9 K2 Ru1 92.21(9) 4_556 . ? Cl2 K2 Ru1 40.27(4) . . ? Cl1 K2 Ru1 161.38(8) 5_666 . ? O3 K2 Ru1 30.96(6) 6_565 . ? O3 K2 Ru1 30.96(6) . . ? Cl2 K2 Ru1 107.99(7) 5_666 . ? O8 K2 Zn2 30.17(8) 7_556 . ? O8 K2 Zn2 143.65(11) 4_556 . ? O9 K2 Zn2 29.53(8) 7_556 . ? O9 K2 Zn2 124.26(10) 4_556 . ? Cl2 K2 Zn2 110.02(3) . . ? Cl1 K2 Zn2 71.48(3) 5_666 . ? O3 K2 Zn2 124.37(8) 6_565 . ? O3 K2 Zn2 75.90(6) . . ? Cl2 K2 Zn2 97.53(4) 5_666 . ? Ru1 K2 Zn2 105.08(3) . . ? O8 K2 Zn2 143.65(11) 7_556 4_556 ? O8 K2 Zn2 30.17(8) 4_556 4_556 ? O9 K2 Zn2 124.26(10) 7_556 4_556 ? O9 K2 Zn2 29.53(8) 4_556 4_556 ? Cl2 K2 Zn2 110.02(3) . 4_556 ? Cl1 K2 Zn2 71.48(3) 5_666 4_556 ? O3 K2 Zn2 75.90(6) 6_565 4_556 ? O3 K2 Zn2 124.37(8) . 4_556 ? Cl2 K2 Zn2 97.53(4) 5_666 4_556 ? Ru1 K2 Zn2 105.08(3) . 4_556 ? Zn2 K2 Zn2 139.97(5) . 4_556 ? Ru1 Cl2 K2 86.82(7) . . ? Ru1 Cl2 K2 160.91(9) . 5_666 ? K2 Cl2 K2 112.27(7) . 5_666 ? Ru2 Cl1 K2 160.87(11) . 5_666 ? C1 O1 Ru1 121.0(3) . . ? C2 O4 Ru2 120.9(3) . . ? C1 O3 Ru1 119.6(3) 5_667 . ? C1 O3 K2 130.8(3) 5_667 . ? Ru1 O3 K2 92.40(12) . . ? C2 O6 Ru2 119.6(3) 5_767 . ? C2 O5 Zn1 128.9(3) . . ? C1 O2 Zn1 128.9(3) . . ? O5 C2 O6 118.9(5) . 5_767 ? O5 C2 O4 121.1(5) . . ? O6 C2 O4 120.0(4) 5_767 . ? O2 C1 O3 119.7(5) . 5_667 ? O2 C1 O1 120.7(5) . . ? O3 C1 O1 119.6(4) 5_667 . ? Zn2 O8 K2 105.60(16) . 7_556 ? Zn2 O9 K2 106.34(16) . 7_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.917 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.246 _database_code_depnum_ccdc_archive 'CCDC 945135' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c2m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 Cl2 K O24 Ru2 Mn2' _chemical_formula_sum 'C4 Cl2 K Mn2 O24 Ru2' _chemical_formula_weight 854.06 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' 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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/m' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 15.943(3) _cell_length_b 15.564(3) _cell_length_c 10.689(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.867(3) _cell_angle_gamma 90.00 _cell_volume 2563.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 2.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6536 _exptl_absorpt_correction_T_max 0.7301 _exptl_absorpt_process_details sadab _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II CCD' _diffrn_measurement_method '\w-\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6334 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2307 _reflns_number_gt 2080 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1177P)^2^+12.8106P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2307 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1565 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.01108(4) 1.0000 0.39939(6) 0.0098(3) Uani 1 2 d S . . Ru2 Ru 0.45341(4) 1.0000 0.39981(6) 0.0098(3) Uani 1 2 d S . . Mn1 Mn 0.2500 1.2500 0.5000 0.0136(3) Uani 1 2 d S . . Mn2 Mn -0.2500 0.7500 0.0000 0.0204(4) Uani 1 2 d S . . K1 K -0.15725(16) 1.0000 0.0546(3) 0.0372(6) Uani 1 2 d S . . Cl1 Cl 0.04530(16) 1.0000 0.1790(2) 0.0265(5) Uani 1 2 d S . . Cl2 Cl 0.34117(17) 1.0000 0.1764(2) 0.0309(6) Uani 1 2 d S . . C1 C 0.1223(4) 1.1202(4) 0.5783(6) 0.0146(12) Uani 1 1 d . . . C2 C 0.4095(4) 1.1257(3) 0.5739(6) 0.0137(12) Uani 1 1 d . . . O1 O 0.1021(3) 1.0925(3) 0.4584(4) 0.0203(10) Uani 1 1 d . . . O2 O -0.0817(3) 0.9091(3) 0.3415(4) 0.0187(9) Uani 1 1 d . . . O3 O 0.1832(3) 1.1741(3) 0.6146(4) 0.0233(10) Uani 1 1 d . . . O4 O 0.3835(3) 1.0931(3) 0.4581(4) 0.0191(9) Uani 1 1 d . . . O5 O 0.5243(3) 0.9060(3) 0.3437(4) 0.0176(9) Uani 1 1 d . . . O6 O 0.3693(3) 1.1884(3) 0.6059(4) 0.0229(10) Uani 1 1 d . . . O7 O 0.2228(3) 1.1496(3) 0.3423(4) 0.0190(9) Uani 1 1 d . . . O8 O -0.2602(3) 0.8566(3) 0.1297(5) 0.0314(11) Uani 1 1 d . . . O9 O -0.3592(4) 0.8001(3) -0.1416(6) 0.0376(13) Uani 1 1 d . . . O10 O -0.1596(4) 0.8306(3) -0.0747(5) 0.0344(12) Uani 1 1 d . . . O11 O 0.5168(4) 0.2831(3) 0.1911(6) 0.0437(14) Uani 1 1 d . . . O12 O 0.4282(4) 0.0902(4) 0.8926(5) 0.0398(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0095(4) 0.0117(4) 0.0088(4) 0.000 0.0032(3) 0.000 Ru2 0.0078(4) 0.0094(4) 0.0111(4) 0.000 0.0005(3) 0.000 Mn1 0.0130(7) 0.0127(6) 0.0146(7) 0.0006(5) 0.0025(5) 0.0003(5) Mn2 0.0219(8) 0.0192(7) 0.0182(7) 0.0012(5) 0.0020(6) -0.0012(6) K1 0.0313(13) 0.0307(12) 0.0453(14) 0.000 0.0018(11) 0.000 Cl1 0.0309(13) 0.0354(12) 0.0161(11) 0.000 0.0114(9) 0.000 Cl2 0.0352(14) 0.0232(11) 0.0238(12) 0.000 -0.0118(10) 0.000 C1 0.015(3) 0.016(3) 0.013(3) 0.000(2) 0.003(2) 0.002(2) C2 0.011(3) 0.012(3) 0.018(3) -0.001(2) 0.004(2) 0.000(2) O1 0.019(2) 0.028(2) 0.015(2) -0.0044(18) 0.0066(18) -0.0129(19) O2 0.021(2) 0.021(2) 0.014(2) -0.0022(17) 0.0045(18) -0.0080(18) O3 0.023(2) 0.028(2) 0.019(2) -0.0045(19) 0.0056(19) -0.017(2) O4 0.015(2) 0.023(2) 0.018(2) -0.0038(17) 0.0008(18) 0.0087(17) O5 0.018(2) 0.020(2) 0.015(2) -0.0018(17) 0.0050(18) 0.0063(18) O6 0.020(2) 0.022(2) 0.024(2) -0.0093(18) 0.0009(19) 0.0102(19) O7 0.019(2) 0.017(2) 0.021(2) -0.0016(17) 0.0046(19) 0.0027(17) O8 0.033(3) 0.037(3) 0.022(2) -0.002(2) 0.003(2) 0.002(2) O9 0.032(3) 0.032(3) 0.041(3) 0.008(2) -0.006(3) 0.002(2) O10 0.035(3) 0.035(3) 0.036(3) 0.004(2) 0.014(2) -0.006(2) O11 0.038(3) 0.027(3) 0.058(4) 0.001(3) -0.001(3) 0.000(2) O12 0.037(3) 0.051(3) 0.034(3) 0.007(2) 0.014(3) 0.011(3) _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 Ru1 O2 2.026(4) 6_575 ? Ru1 O2 2.026(4) . ? Ru1 O1 2.027(4) . ? Ru1 O1 2.027(4) 6_575 ? Ru1 Ru1 2.2674(13) 5_576 ? Ru1 Cl1 2.551(2) . ? Ru1 K1 3.964(3) . ? Ru2 O4 2.021(4) 6_575 ? Ru2 O4 2.021(4) . ? Ru2 O5 2.030(4) 6_575 ? Ru2 O5 2.030(4) . ? Ru2 Ru2 2.2720(13) 5_676 ? Ru2 Cl2 2.591(2) . ? Mn1 O3 2.168(4) . ? Mn1 O3 2.168(4) 7_576 ? Mn1 O6 2.171(4) 7_576 ? Mn1 O6 2.171(4) . ? Mn1 O7 2.257(4) 7_576 ? Mn1 O7 2.257(4) . ? Mn2 O9 2.140(5) 7_465 ? Mn2 O9 2.140(5) . ? Mn2 O8 2.194(5) . ? Mn2 O8 2.194(5) 7_465 ? Mn2 O10 2.209(5) . ? Mn2 O10 2.209(5) 7_465 ? K1 O10 2.973(6) 6_575 ? K1 O10 2.973(6) . ? K1 O8 2.999(5) 6_575 ? K1 O8 2.999(5) . ? K1 Cl1 3.161(4) . ? K1 O2 3.311(5) 6_575 ? K1 O2 3.311(5) . ? K1 Cl2 3.313(3) 5_575 ? K1 Cl1 3.421(4) 5_575 ? Cl1 K1 3.421(4) 5_575 ? Cl2 K1 3.313(3) 5_575 ? C1 O3 1.267(8) . ? C1 O2 1.283(7) 5_576 ? C1 O1 1.312(7) . ? C2 O6 1.261(7) . ? C2 O5 1.288(7) 5_676 ? C2 O4 1.304(7) . ? O2 C1 1.283(7) 5_576 ? O5 C2 1.288(7) 5_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ru1 O2 88.6(3) 6_575 . ? O2 Ru1 O1 90.4(2) 6_575 . ? O2 Ru1 O1 178.85(17) . . ? O2 Ru1 O1 178.85(17) 6_575 6_575 ? O2 Ru1 O1 90.42(19) . 6_575 ? O1 Ru1 O1 90.5(3) . 6_575 ? O2 Ru1 Ru1 90.61(12) 6_575 5_576 ? O2 Ru1 Ru1 90.61(12) . 5_576 ? O1 Ru1 Ru1 88.76(12) . 5_576 ? O1 Ru1 Ru1 88.76(12) 6_575 5_576 ? O2 Ru1 Cl1 91.74(13) 6_575 . ? O2 Ru1 Cl1 91.74(13) . . ? O1 Ru1 Cl1 88.93(13) . . ? O1 Ru1 Cl1 88.93(12) 6_575 . ? Ru1 Ru1 Cl1 176.73(7) 5_576 . ? O2 Ru1 K1 56.56(12) 6_575 . ? O2 Ru1 K1 56.56(12) . . ? O1 Ru1 K1 123.31(13) . . ? O1 Ru1 K1 123.31(13) 6_575 . ? Ru1 Ru1 K1 130.47(6) 5_576 . ? Cl1 Ru1 K1 52.80(7) . . ? O4 Ru2 O4 91.6(3) 6_575 . ? O4 Ru2 O5 179.25(18) 6_575 6_575 ? O4 Ru2 O5 88.13(18) . 6_575 ? O4 Ru2 O5 88.13(18) 6_575 . ? O4 Ru2 O5 179.25(17) . . ? O5 Ru2 O5 92.2(2) 6_575 . ? O4 Ru2 Ru2 89.33(12) 6_575 5_676 ? O4 Ru2 Ru2 89.33(12) . 5_676 ? O5 Ru2 Ru2 89.98(13) 6_575 5_676 ? O5 Ru2 Ru2 89.98(13) . 5_676 ? O4 Ru2 Cl2 88.80(13) 6_575 . ? O4 Ru2 Cl2 88.80(13) . . ? O5 Ru2 Cl2 91.87(13) 6_575 . ? O5 Ru2 Cl2 91.87(13) . . ? Ru2 Ru2 Cl2 177.33(8) 5_676 . ? O3 Mn1 O3 180.0(2) . 7_576 ? O3 Mn1 O6 92.52(19) . 7_576 ? O3 Mn1 O6 87.48(19) 7_576 7_576 ? O3 Mn1 O6 87.48(19) . . ? O3 Mn1 O6 92.52(19) 7_576 . ? O6 Mn1 O6 180.000(1) 7_576 . ? O3 Mn1 O7 89.03(16) . 7_576 ? O3 Mn1 O7 90.97(16) 7_576 7_576 ? O6 Mn1 O7 93.35(15) 7_576 7_576 ? O6 Mn1 O7 86.65(15) . 7_576 ? O3 Mn1 O7 90.97(16) . . ? O3 Mn1 O7 89.03(16) 7_576 . ? O6 Mn1 O7 86.65(15) 7_576 . ? O6 Mn1 O7 93.35(15) . . ? O7 Mn1 O7 180.000(1) 7_576 . ? O9 Mn2 O9 180.000(1) 7_465 . ? O9 Mn2 O8 90.4(2) 7_465 . ? O9 Mn2 O8 89.6(2) . . ? O9 Mn2 O8 89.6(2) 7_465 7_465 ? O9 Mn2 O8 90.4(2) . 7_465 ? O8 Mn2 O8 180.0 . 7_465 ? O9 Mn2 O10 88.5(2) 7_465 . ? O9 Mn2 O10 91.5(2) . . ? O8 Mn2 O10 87.7(2) . . ? O8 Mn2 O10 92.3(2) 7_465 . ? O9 Mn2 O10 91.5(2) 7_465 7_465 ? O9 Mn2 O10 88.5(2) . 7_465 ? O8 Mn2 O10 92.3(2) . 7_465 ? O8 Mn2 O10 87.7(2) 7_465 7_465 ? O10 Mn2 O10 180.000(1) . 7_465 ? O10 K1 O10 125.0(2) 6_575 . ? O10 K1 O8 61.43(14) 6_575 6_575 ? O10 K1 O8 147.36(17) . 6_575 ? O10 K1 O8 147.36(17) 6_575 . ? O10 K1 O8 61.43(14) . . ? O8 K1 O8 96.2(2) 6_575 . ? O10 K1 Cl1 94.90(12) 6_575 . ? O10 K1 Cl1 94.90(12) . . ? O8 K1 Cl1 117.21(12) 6_575 . ? O8 K1 Cl1 117.21(12) . . ? O10 K1 O2 90.55(13) 6_575 6_575 ? O10 K1 O2 140.16(14) . 6_575 ? O8 K1 O2 61.83(13) 6_575 6_575 ? O8 K1 O2 99.44(14) . 6_575 ? Cl1 K1 O2 61.36(9) . 6_575 ? O10 K1 O2 140.16(14) 6_575 . ? O10 K1 O2 90.55(13) . . ? O8 K1 O2 99.44(14) 6_575 . ? O8 K1 O2 61.83(13) . . ? Cl1 K1 O2 61.36(9) . . ? O2 K1 O2 50.60(15) 6_575 . ? O10 K1 Cl2 75.55(12) 6_575 5_575 ? O10 K1 Cl2 75.55(12) . 5_575 ? O8 K1 Cl2 76.06(12) 6_575 5_575 ? O8 K1 Cl2 76.06(12) . 5_575 ? Cl1 K1 Cl2 157.94(11) . 5_575 ? O2 K1 Cl2 137.06(11) 6_575 5_575 ? O2 K1 Cl2 137.06(11) . 5_575 ? O10 K1 Cl1 66.89(11) 6_575 5_575 ? O10 K1 Cl1 66.89(11) . 5_575 ? O8 K1 Cl1 128.25(11) 6_575 5_575 ? O8 K1 Cl1 128.25(11) . 5_575 ? Cl1 K1 Cl1 68.85(8) . 5_575 ? O2 K1 Cl1 122.82(11) 6_575 5_575 ? O2 K1 Cl1 122.82(11) . 5_575 ? Cl2 K1 Cl1 89.09(9) 5_575 5_575 ? O10 K1 Ru1 110.92(12) 6_575 . ? O10 K1 Ru1 110.92(12) . . ? O8 K1 Ru1 92.14(11) 6_575 . ? O8 K1 Ru1 92.14(11) . . ? Cl1 K1 Ru1 40.00(5) . . ? O2 K1 Ru1 30.70(8) 6_575 . ? O2 K1 Ru1 30.70(8) . . ? Cl2 K1 Ru1 162.06(10) 5_575 . ? Cl1 K1 Ru1 108.85(8) 5_575 . ? Ru1 Cl1 K1 87.20(8) . . ? Ru1 Cl1 K1 161.65(11) . 5_575 ? K1 Cl1 K1 111.15(8) . 5_575 ? Ru2 Cl2 K1 163.06(12) . 5_575 ? O3 C1 O2 120.6(5) . 5_576 ? O3 C1 O1 119.6(5) . . ? O2 C1 O1 119.8(5) 5_576 . ? O6 C2 O5 119.7(5) . 5_676 ? O6 C2 O4 119.9(5) . . ? O5 C2 O4 120.3(5) 5_676 . ? C1 O1 Ru1 120.9(4) . . ? C1 O2 Ru1 119.9(4) 5_576 . ? C1 O2 K1 130.1(4) 5_576 . ? Ru1 O2 K1 92.75(15) . . ? C1 O3 Mn1 129.5(4) . . ? C2 O4 Ru2 120.4(4) . . ? C2 O5 Ru2 119.7(4) 5_676 . ? C2 O6 Mn1 129.6(4) . . ? Mn2 O8 K1 105.04(19) . . ? Mn2 O10 K1 105.5(2) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 4.691 _refine_diff_density_min -1.303 _refine_diff_density_rms 0.268 _database_code_depnum_ccdc_archive 'CCDC 945136'