Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_complex_1 _database_code_CSD 156110 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H12 Co3 O11.50' _chemical_formula_weight 492.99 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7501(18) _cell_length_b 9.1116(18) _cell_length_c 10.350(2) _cell_angle_alpha 83.10(3) _cell_angle_beta 75.86(3) _cell_angle_gamma 68.69(3) _cell_volume 745.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour 'Deep Red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 490 _exptl_absorpt_coefficient_mu 3.362 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Siemens CAD4' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 3122 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.97 _reflns_number_total 2918 _reflns_number_gt 2547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V.5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0269P)^2^+0.4812P] 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 2918 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _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 Co1 Co 0.0000 0.0000 0.0000 0.01493(12) Uani 1 2 d S . . Co2 Co 0.0000 0.0000 0.5000 0.01406(12) Uani 1 2 d S . . Co3 Co -0.16462(4) -0.07713(5) 0.79555(4) 0.01458(10) Uani 1 1 d . . . Co4 Co -0.56175(5) 0.13982(5) 0.89823(4) 0.02157(11) Uani 1 1 d . . . O1 O -0.1796(2) 0.1204(2) -0.1072(2) 0.0192(4) Uani 1 1 d . . . O2 O -0.4433(3) 0.2833(3) -0.0726(3) 0.0340(6) Uani 1 1 d . . . C1 C -0.2920(3) 0.2560(4) -0.0806(3) 0.0205(6) Uani 1 1 d . . . C2 C -0.2403(4) 0.3898(4) -0.0582(4) 0.0296(8) Uani 1 1 d . . . H2A H -0.2544 0.3971 0.0370 0.036 Uiso 1 1 calc R . . H2B H -0.3165 0.4871 -0.0893 0.036 Uiso 1 1 calc R . . C3 C -0.0613(4) 0.3785(4) -0.1253(3) 0.0239(7) Uani 1 1 d . . . H3A H -0.0321 0.3291 -0.2102 0.029 Uiso 1 1 calc R . . H3B H -0.0591 0.4847 -0.1443 0.029 Uiso 1 1 calc R . . C4 C 0.0727(3) 0.2893(3) -0.0491(3) 0.0165(6) Uani 1 1 d . . . O3 O 0.2111(2) 0.3071(3) -0.0881(2) 0.0247(5) Uani 1 1 d . . . O4 O 0.0402(2) 0.1977(2) 0.0495(2) 0.0184(4) Uani 1 1 d . . . O5 O -0.1945(2) 0.0308(3) 0.1655(2) 0.0231(5) Uani 1 1 d . . . O6 O -0.0737(2) 0.0773(2) 0.3145(2) 0.0186(4) Uani 1 1 d . . . C5 C -0.1997(3) 0.0728(4) 0.2768(3) 0.0198(6) Uani 1 1 d . . . C6 C -0.3679(4) 0.1236(6) 0.3717(4) 0.0495(12) Uani 1 1 d . . . H6A H -0.3870 0.0297 0.4160 0.059 Uiso 1 1 calc R . . H6B H -0.4532 0.1723 0.3198 0.059 Uiso 1 1 calc R . . C7 C -0.3952(4) 0.2377(5) 0.4791(3) 0.0349(8) Uani 1 1 d . . . H7A H -0.3114 0.2882 0.4531 0.042 Uiso 1 1 calc R . . H7B H -0.5049 0.3192 0.4850 0.042 Uiso 1 1 calc R . . C8 C -0.3842(4) 0.1575(4) 0.6130(3) 0.0217(6) Uani 1 1 d . . . O7 O -0.2395(2) 0.0699(2) 0.6318(2) 0.0191(4) Uani 1 1 d . . . O8 O -0.5165(3) 0.1762(3) 0.6976(2) 0.0351(6) Uani 1 1 d . . . O9 O 0.1391(3) 0.2672(3) 0.3058(2) 0.0245(5) Uani 1 1 d . . . O10 O 0.0261(3) 0.2086(3) 0.5152(2) 0.0256(5) Uani 1 1 d . . . O1W O -0.3944(2) -0.0813(3) 0.8966(2) 0.0198(4) Uani 1 1 d . . . H1W H -0.403(5) -0.143(5) 0.861(4) 0.043(13) Uiso 1 1 d . . . C9 C 0.0855(3) 0.2933(4) 0.4287(3) 0.0192(6) Uani 1 1 d . . . C10 C 0.0891(4) 0.4421(4) 0.4768(3) 0.0227(7) Uani 1 1 d . . . H10A H 0.1507 0.4911 0.4051 0.027 Uiso 1 1 calc R . . H10B H 0.1468 0.4157 0.5499 0.027 Uiso 1 1 calc R . . O2W O -0.268(2) 0.4542(16) 0.2812(13) 0.187(6) Uani 0.50 1 d P . . H2WA H -0.3568 0.5167 0.2583 0.224 Uiso 0.50 1 d PR . . H2WB H -0.1938 0.4094 0.2143 0.224 Uiso 0.50 1 d PR . . 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 Co1 0.0161(2) 0.0176(3) 0.0122(3) -0.0025(2) -0.0029(2) -0.0067(2) Co2 0.0170(2) 0.0137(3) 0.0115(3) -0.0014(2) -0.00092(19) -0.0065(2) Co3 0.01490(17) 0.0175(2) 0.0110(2) -0.00271(15) -0.00058(14) -0.00610(15) Co4 0.01426(18) 0.0288(3) 0.0174(2) 0.00014(18) 0.00013(15) -0.00508(17) O1 0.0177(9) 0.0190(11) 0.0201(11) -0.0055(9) -0.0068(8) -0.0024(8) O2 0.0155(10) 0.0286(14) 0.0562(17) -0.0083(12) -0.0028(10) -0.0068(10) C1 0.0185(13) 0.0226(17) 0.0183(16) -0.0002(13) -0.0022(11) -0.0060(12) C2 0.0166(14) 0.0196(17) 0.052(2) -0.0084(16) -0.0101(14) -0.0012(12) C3 0.0218(14) 0.0197(16) 0.0314(18) 0.0065(14) -0.0097(13) -0.0085(12) C4 0.0183(13) 0.0133(14) 0.0166(15) -0.0065(12) -0.0017(11) -0.0034(11) O3 0.0159(10) 0.0260(12) 0.0309(13) 0.0055(10) -0.0038(9) -0.0087(9) O4 0.0227(10) 0.0191(11) 0.0159(11) 0.0007(9) -0.0057(8) -0.0095(8) O5 0.0231(10) 0.0359(13) 0.0123(11) -0.0062(9) -0.0005(8) -0.0130(9) O6 0.0172(9) 0.0241(12) 0.0135(10) -0.0011(9) -0.0009(8) -0.0076(8) C5 0.0185(13) 0.0252(17) 0.0140(15) 0.0002(13) -0.0009(11) -0.0077(12) C6 0.0231(16) 0.111(4) 0.0187(18) -0.021(2) 0.0026(14) -0.027(2) C7 0.0242(15) 0.049(2) 0.0151(17) 0.0026(16) -0.0033(13) 0.0053(15) C8 0.0210(13) 0.0263(17) 0.0156(15) -0.0054(13) -0.0019(11) -0.0055(12) O7 0.0174(9) 0.0221(11) 0.0150(11) -0.0003(9) -0.0019(8) -0.0046(8) O8 0.0197(10) 0.0556(17) 0.0191(12) 0.0030(12) -0.0001(9) -0.0041(11) O9 0.0357(11) 0.0196(12) 0.0173(12) -0.0034(9) 0.0005(9) -0.0119(10) O10 0.0389(12) 0.0194(12) 0.0203(12) -0.0043(9) 0.0016(9) -0.0161(10) O1W 0.0192(10) 0.0242(12) 0.0175(11) -0.0041(9) -0.0016(8) -0.0098(9) C9 0.0213(13) 0.0156(15) 0.0202(16) -0.0042(12) -0.0012(11) -0.0067(12) C10 0.0266(15) 0.0193(16) 0.0242(17) -0.0068(13) 0.0000(12) -0.0121(13) O2W 0.228(16) 0.142(12) 0.145(12) 0.034(10) 0.004(11) -0.051(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.052(2) 2 ? Co1 O1 2.052(2) . ? Co1 O5 2.063(2) . ? Co1 O5 2.063(2) 2 ? Co1 O4 2.0976(19) . ? Co1 O4 2.0976(19) 2 ? Co2 O10 2.023(2) . ? Co2 O10 2.023(2) 2_556 ? Co2 O7 2.121(2) . ? Co2 O7 2.121(2) 2_556 ? Co2 O6 2.133(2) . ? Co2 O6 2.133(2) 2_556 ? Co3 O1W 2.038(2) . ? Co3 O9 2.047(2) 2_556 ? Co3 O7 2.111(2) . ? Co3 O1 2.114(2) 1_556 ? Co3 O6 2.118(2) 2_556 ? Co3 O4 2.127(2) 2_556 ? Co4 O3 2.001(2) 1_456 ? Co4 O1W 2.014(2) . ? Co4 O8 2.026(2) . ? Co4 O2 2.027(2) 1_556 ? Co4 O1W 2.103(2) 2_457 ? O1 C1 1.279(4) . ? O1 Co3 2.114(2) 1_554 ? O2 C1 1.238(4) . ? O2 Co4 2.027(2) 1_554 ? C1 C2 1.506(4) . ? C2 C3 1.522(4) . ? C3 C4 1.504(4) . ? C4 O3 1.243(3) . ? C4 O4 1.282(4) . ? O3 Co4 2.001(2) 1_654 ? O4 Co3 2.127(2) 2_556 ? O5 C5 1.242(4) . ? O6 C5 1.272(3) . ? O6 Co3 2.118(2) 2_556 ? C5 C6 1.501(4) . ? C6 C7 1.529(5) . ? C7 C8 1.496(5) . ? C8 O8 1.238(4) . ? C8 O7 1.275(4) . ? O9 C9 1.263(4) . ? O9 Co3 2.047(2) 2_556 ? O10 C9 1.252(4) . ? O1W Co4 2.103(2) 2_457 ? C9 C10 1.512(4) . ? C10 C10 1.528(6) 2_566 ? 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 Co1 O1 180.00(18) 2 . ? O1 Co1 O5 93.16(8) 2 . ? O1 Co1 O5 86.84(8) . . ? O1 Co1 O5 86.84(8) 2 2 ? O1 Co1 O5 93.16(8) . 2 ? O5 Co1 O5 180.00(17) . 2 ? O1 Co1 O4 83.36(8) 2 . ? O1 Co1 O4 96.64(8) . . ? O5 Co1 O4 89.61(8) . . ? O5 Co1 O4 90.39(8) 2 . ? O1 Co1 O4 96.64(8) 2 2 ? O1 Co1 O4 83.36(8) . 2 ? O5 Co1 O4 90.39(8) . 2 ? O5 Co1 O4 89.61(8) 2 2 ? O4 Co1 O4 180.00(11) . 2 ? O10 Co2 O10 180.0 . 2_556 ? O10 Co2 O7 91.71(9) . . ? O10 Co2 O7 88.29(9) 2_556 . ? O10 Co2 O7 88.29(9) . 2_556 ? O10 Co2 O7 91.71(9) 2_556 2_556 ? O7 Co2 O7 180.0 . 2_556 ? O10 Co2 O6 90.73(9) . . ? O10 Co2 O6 89.27(9) 2_556 . ? O7 Co2 O6 99.76(8) . . ? O7 Co2 O6 80.24(8) 2_556 . ? O10 Co2 O6 89.27(9) . 2_556 ? O10 Co2 O6 90.73(9) 2_556 2_556 ? O7 Co2 O6 80.24(8) . 2_556 ? O7 Co2 O6 99.76(8) 2_556 2_556 ? O6 Co2 O6 180.00(4) . 2_556 ? O1W Co3 O9 88.04(9) . 2_556 ? O1W Co3 O7 98.49(8) . . ? O9 Co3 O7 88.78(9) 2_556 . ? O1W Co3 O1 94.96(9) . 1_556 ? O9 Co3 O1 176.93(8) 2_556 1_556 ? O7 Co3 O1 90.15(8) . 1_556 ? O1W Co3 O6 178.05(8) . 2_556 ? O9 Co3 O6 90.12(9) 2_556 2_556 ? O7 Co3 O6 80.81(8) . 2_556 ? O1 Co3 O6 86.87(8) 1_556 2_556 ? O1W Co3 O4 94.46(8) . 2_556 ? O9 Co3 O4 99.23(9) 2_556 2_556 ? O7 Co3 O4 165.00(7) . 2_556 ? O1 Co3 O4 81.19(8) 1_556 2_556 ? O6 Co3 O4 86.48(8) 2_556 2_556 ? O3 Co4 O1W 156.48(8) 1_456 . ? O3 Co4 O8 89.27(10) 1_456 . ? O1W Co4 O8 95.74(10) . . ? O3 Co4 O2 96.07(9) 1_456 1_556 ? O1W Co4 O2 106.45(9) . 1_556 ? O8 Co4 O2 93.93(11) . 1_556 ? O3 Co4 O1W 93.29(10) 1_456 2_457 ? O1W Co4 O1W 80.19(10) . 2_457 ? O8 Co4 O1W 174.92(10) . 2_457 ? O2 Co4 O1W 90.17(10) 1_556 2_457 ? C1 O1 Co1 125.65(18) . . ? C1 O1 Co3 134.22(17) . 1_554 ? Co1 O1 Co3 96.28(9) . 1_554 ? C1 O2 Co4 130.0(2) . 1_554 ? O2 C1 O1 122.9(3) . . ? O2 C1 C2 117.8(3) . . ? O1 C1 C2 119.3(2) . . ? C1 C2 C3 116.1(3) . . ? C4 C3 C2 116.6(3) . . ? O3 C4 O4 123.8(3) . . ? O3 C4 C3 117.1(3) . . ? O4 C4 C3 119.1(2) . . ? C4 O3 Co4 127.0(2) . 1_654 ? C4 O4 Co1 115.37(17) . . ? C4 O4 Co3 133.88(17) . 2_556 ? Co1 O4 Co3 94.51(9) . 2_556 ? C5 O5 Co1 126.88(18) . . ? C5 O6 Co3 131.13(19) . 2_556 ? C5 O6 Co2 129.21(19) . . ? Co3 O6 Co2 96.11(8) 2_556 . ? O5 C5 O6 124.6(3) . . ? O5 C5 C6 117.1(2) . . ? O6 C5 C6 118.3(3) . . ? C5 C6 C7 117.4(3) . . ? C8 C7 C6 112.6(3) . . ? O8 C8 O7 123.9(3) . . ? O8 C8 C7 118.1(3) . . ? O7 C8 C7 117.9(3) . . ? C8 O7 Co3 131.46(19) . . ? C8 O7 Co2 131.44(19) . . ? Co3 O7 Co2 96.64(8) . . ? C8 O8 Co4 131.8(2) . . ? C9 O9 Co3 129.40(19) . 2_556 ? C9 O10 Co2 130.59(19) . . ? Co4 O1W Co3 108.52(11) . . ? Co4 O1W Co4 99.81(10) . 2_457 ? Co3 O1W Co4 120.73(10) . 2_457 ? O10 C9 O9 126.0(3) . . ? O10 C9 C10 116.3(3) . . ? O9 C9 C10 117.7(3) . . ? C9 C10 C10 110.8(3) . 2_566 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.516 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.085