# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jonathan Steed' _publ_contact_author_email JON.STEED@DUR.AC.UK _publ_section_title ; A Catenated Imidazole-Based Coordination Polymer Exhibiting Significant CO2 Sorption at Low Pressure ; _publ_author_name 'Jonathan Steed' # Attachment 'TIF1.CIF' data_z:\xraydata\sarafr~1\08srv1~1\work\squeeze\squf _database_code_depnum_ccdc_archive 'CCDC 721169' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 Cl6 Co3 N12' _chemical_formula_sum 'C48 H60 Cl6 Co3 N12' _chemical_formula_weight 1194.57 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' N N 0.0061 0.0033 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ima2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y, z' 'x+1/2, -y, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' _cell_length_a 40.116(4) _cell_length_b 15.0126(13) _cell_length_c 11.1975(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6743.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2003 _cell_measurement_theta_min 2.269 _cell_measurement_theta_max 32.989 _exptl_crystal_description Needle _exptl_crystal_colour Blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2906 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8412 _exptl_absorpt_correction_T_max 0.9610 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Smart-6K _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20034 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.1038 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6029 _reflns_number_gt 4640 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Xseed _computing_publication_material Xseed _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. Structure is run through the Squeeze routine in Platon as there are large voids that contain some unmodelled electron density from disordered solvent molecules. ; _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^)+(0.0686P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 6029 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _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 Co1 Co 0.941218(18) 0.37155(5) 0.48583(7) 0.01533(18) Uani 1 1 d . . . Co2 Co 0.7500 -0.19039(8) -0.04875(8) 0.0201(3) Uani 1 2 d S . . Cl1 Cl 0.90249(4) 0.45573(10) 0.57469(14) 0.0264(4) Uani 1 1 d . . . Cl2 Cl 0.95812(4) 0.41757(10) 0.30307(12) 0.0246(3) Uani 1 1 d . . . Cl3 Cl 0.7500 -0.33789(15) -0.08518(19) 0.0262(5) Uani 1 2 d S . . Cl4 Cl 0.7500 -0.10256(18) -0.2088(2) 0.0413(6) Uani 1 2 d S . . N1 N 0.78983(13) -0.1658(4) 0.0533(4) 0.0242(12) Uani 1 1 d . . . N2 N 0.82373(11) -0.1768(3) 0.2084(4) 0.0126(10) Uani 1 1 d . . . N3 N 0.97763(11) -0.1775(3) 0.2117(4) 0.0139(10) Uani 1 1 d . . . N4 N 1.01612(12) -0.1417(3) 0.0802(4) 0.0191(11) Uani 1 1 d . . . N5 N 0.90974(11) 0.1070(3) 0.4804(5) 0.0175(10) Uani 1 1 d . . . N6 N 0.92376(11) 0.2484(3) 0.4573(4) 0.0198(11) Uani 1 1 d . . . C1 C 0.79594(14) -0.2081(4) 0.1564(5) 0.0179(13) Uani 1 1 d . . . H1 H 0.7824 -0.2541 0.1885 0.021 Uiso 1 1 calc R . . C2 C 0.81546(17) -0.1035(5) 0.0404(6) 0.0302(16) Uani 1 1 d . . . H2 H 0.8176 -0.0622 -0.0234 0.036 Uiso 1 1 calc R . . C3 C 0.83659(16) -0.1114(4) 0.1330(5) 0.0287(16) Uani 1 1 d . . . H3 H 0.8566 -0.0785 0.1449 0.034 Uiso 1 1 calc R . . C4 C 0.83600(14) -0.2087(4) 0.3249(5) 0.0166(13) Uani 1 1 d . . . H4A H 0.8382 -0.2743 0.3226 0.020 Uiso 1 1 calc R . . H4B H 0.8195 -0.1935 0.3875 0.020 Uiso 1 1 calc R . . C5 C 0.86926(13) -0.1681(4) 0.3569(5) 0.0138(12) Uani 1 1 d . . . C6 C 0.89946(13) -0.2118(4) 0.3185(5) 0.0140(12) Uani 1 1 d . . . C7 C 0.92979(14) -0.1759(4) 0.3537(5) 0.0149(12) Uani 1 1 d . . . C8 C 0.93170(14) -0.0980(4) 0.4248(5) 0.0148(12) Uani 1 1 d . . . C9 C 0.90194(13) -0.0568(3) 0.4598(5) 0.0136(12) Uani 1 1 d . . . C10 C 0.87097(14) -0.0899(4) 0.4257(5) 0.0140(12) Uani 1 1 d . . . C11 C 0.89730(16) -0.2930(4) 0.2439(5) 0.0211(14) Uani 1 1 d . . . H11A H 0.9164 -0.2946 0.1881 0.025 Uiso 1 1 calc R . . H11B H 0.8766 -0.2911 0.1959 0.025 Uiso 1 1 calc R . . C12 C 0.89742(16) -0.3784(4) 0.3213(6) 0.0268(15) Uani 1 1 d . . . H12A H 0.8951 -0.4307 0.2696 0.040 Uiso 1 1 calc R . . H12B H 0.8788 -0.3764 0.3777 0.040 Uiso 1 1 calc R . . H12C H 0.9184 -0.3822 0.3655 0.040 Uiso 1 1 calc R . . C13 C 0.96196(14) -0.2213(4) 0.3172(5) 0.0195(13) Uani 1 1 d . . . H13A H 0.9778 -0.2200 0.3851 0.023 Uiso 1 1 calc R . . H13B H 0.9573 -0.2845 0.2979 0.023 Uiso 1 1 calc R . . C14 C 0.96176(14) -0.1331(4) 0.1212(5) 0.0185(13) Uani 1 1 d . . . H14 H 0.9386 -0.1206 0.1167 0.022 Uiso 1 1 calc R . . C15 C 0.98503(14) -0.1100(4) 0.0395(5) 0.0181(13) Uani 1 1 d . . . H15 H 0.9811 -0.0782 -0.0324 0.022 Uiso 1 1 calc R . . C16 C 1.00967(14) -0.1820(4) 0.1843(5) 0.0179(12) Uani 1 1 d . . . H16 H 1.0260 -0.2103 0.2325 0.022 Uiso 1 1 calc R . . C17 C 0.96471(13) -0.0624(4) 0.4629(5) 0.0166(12) Uani 1 1 d . . . H17A H 0.9630 0.0028 0.4745 0.020 Uiso 1 1 calc R . . H17B H 0.9814 -0.0738 0.3994 0.020 Uiso 1 1 calc R . . C18 C 0.97649(15) -0.1065(4) 0.5807(5) 0.0228(14) Uani 1 1 d . . . H18A H 0.9981 -0.0817 0.6039 0.034 Uiso 1 1 calc R . . H18B H 0.9786 -0.1709 0.5688 0.034 Uiso 1 1 calc R . . H18C H 0.9601 -0.0948 0.6438 0.034 Uiso 1 1 calc R . . C19 C 0.90374(15) 0.0223(3) 0.5422(5) 0.0172(13) Uani 1 1 d . . . H19A H 0.8825 0.0267 0.5871 0.021 Uiso 1 1 calc R . . H19B H 0.9218 0.0124 0.6008 0.021 Uiso 1 1 calc R . . C20 C 0.89912(17) 0.1319(4) 0.3672(5) 0.0273(15) Uani 1 1 d . . . H20 H 0.8882 0.0956 0.3097 0.033 Uiso 1 1 calc R . . C21 C 0.90758(17) 0.2193(4) 0.3558(6) 0.0295(16) Uani 1 1 d . . . H21 H 0.9030 0.2551 0.2878 0.035 Uiso 1 1 calc R . . C22 C 0.92463(14) 0.1794(4) 0.5290(5) 0.0199(14) Uani 1 1 d . . . H22 H 0.9345 0.1801 0.6061 0.024 Uiso 1 1 calc R . . C23 C 0.83869(13) -0.0416(4) 0.4604(5) 0.0186(13) Uani 1 1 d . . . H23A H 0.8216 -0.0524 0.3983 0.022 Uiso 1 1 calc R . . H23B H 0.8429 0.0233 0.4640 0.022 Uiso 1 1 calc R . . C24 C 0.82506(16) -0.0740(5) 0.5842(6) 0.0310(16) Uani 1 1 d . . . H24A H 0.8049 -0.0403 0.6045 0.047 Uiso 1 1 calc R . . H24B H 0.8421 -0.0644 0.6457 0.047 Uiso 1 1 calc R . . H24C H 0.8197 -0.1376 0.5797 0.047 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 Co1 0.0138(4) 0.0163(3) 0.0159(3) 0.0002(4) -0.0013(3) 0.0016(3) Co2 0.0110(6) 0.0349(6) 0.0143(6) -0.0006(5) 0.000 0.000 Cl1 0.0251(9) 0.0236(7) 0.0306(8) -0.0014(7) 0.0070(7) 0.0077(7) Cl2 0.0243(8) 0.0334(8) 0.0163(7) 0.0029(7) 0.0019(6) -0.0028(7) Cl3 0.0145(11) 0.0287(11) 0.0353(12) 0.0041(10) 0.000 0.000 Cl4 0.0378(15) 0.0547(16) 0.0314(13) 0.0045(13) 0.000 0.000 N1 0.023(3) 0.034(3) 0.016(3) 0.005(2) 0.003(2) 0.004(2) N2 0.009(2) 0.020(2) 0.010(2) -0.003(2) -0.0043(17) -0.004(2) N3 0.012(3) 0.019(2) 0.011(2) 0.001(2) 0.0068(18) 0.001(2) N4 0.020(3) 0.019(2) 0.018(2) 0.003(2) 0.003(2) 0.001(2) N5 0.015(2) 0.018(2) 0.020(2) 0.004(2) 0.000(2) -0.0027(19) N6 0.016(3) 0.026(3) 0.017(3) -0.001(2) -0.006(2) -0.004(2) C1 0.008(3) 0.028(3) 0.018(3) 0.001(3) 0.001(2) -0.002(3) C2 0.023(4) 0.043(4) 0.024(3) 0.007(3) -0.005(3) -0.002(3) C3 0.023(4) 0.041(4) 0.022(3) 0.008(3) -0.004(3) -0.019(3) C4 0.011(3) 0.018(3) 0.021(3) 0.000(3) -0.002(2) -0.005(3) C5 0.003(3) 0.024(3) 0.014(3) 0.001(3) 0.002(2) 0.000(2) C6 0.009(3) 0.016(3) 0.018(3) 0.004(2) 0.006(2) 0.005(2) C7 0.018(3) 0.013(3) 0.013(3) 0.000(2) -0.001(2) 0.001(2) C8 0.016(3) 0.017(3) 0.012(3) 0.008(2) -0.006(2) -0.004(2) C9 0.013(3) 0.011(3) 0.017(3) -0.004(2) -0.005(2) -0.003(2) C10 0.012(3) 0.013(3) 0.017(3) -0.008(2) 0.002(2) 0.000(2) C11 0.026(4) 0.021(3) 0.017(3) -0.004(3) 0.001(2) -0.008(3) C12 0.022(4) 0.018(3) 0.041(4) -0.005(3) 0.002(3) 0.004(3) C13 0.017(3) 0.016(3) 0.025(3) 0.005(3) 0.003(3) -0.005(3) C14 0.008(3) 0.021(3) 0.026(3) 0.005(3) -0.003(2) 0.004(3) C15 0.010(3) 0.020(3) 0.025(3) 0.003(3) 0.002(2) 0.008(2) C16 0.016(3) 0.020(3) 0.018(3) 0.003(3) 0.000(3) 0.005(3) C17 0.011(3) 0.025(3) 0.014(3) 0.004(2) -0.001(2) -0.001(2) C18 0.019(3) 0.033(4) 0.016(3) 0.004(3) -0.011(3) -0.004(3) C19 0.021(3) 0.017(3) 0.013(3) -0.001(2) 0.001(2) -0.004(3) C20 0.039(4) 0.026(3) 0.017(3) 0.003(3) -0.006(3) -0.010(3) C21 0.039(4) 0.031(3) 0.019(3) -0.001(3) -0.004(3) -0.006(3) C22 0.013(3) 0.025(3) 0.022(3) -0.002(3) -0.001(2) 0.005(3) C23 0.011(3) 0.019(3) 0.026(3) 0.001(3) 0.003(2) -0.001(2) C24 0.017(4) 0.043(4) 0.033(4) -0.002(3) 0.009(3) 0.000(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 Co1 N6 2.003(5) . ? Co1 N4 2.021(5) 7_655 ? Co1 Cl1 2.2363(16) . ? Co1 Cl2 2.2639(16) . ? Co2 N1 1.998(5) . ? Co2 N1 1.998(5) 3_655 ? Co2 Cl4 2.225(3) . ? Co2 Cl3 2.252(3) . ? N1 C1 1.341(7) . ? N1 C2 1.397(8) . ? N2 C1 1.343(7) . ? N2 C3 1.395(8) . ? N2 C4 1.474(7) . ? N3 C16 1.323(7) . ? N3 C14 1.370(7) . ? N3 C13 1.491(7) . ? N4 C16 1.340(7) . ? N4 C15 1.410(7) . ? N4 Co1 2.021(5) 7_644 ? N5 C22 1.354(7) . ? N5 C20 1.389(8) . ? N5 C19 1.467(7) . ? N6 C22 1.312(7) . ? N6 C21 1.379(8) . ? C1 H1 0.9500 . ? C2 C3 1.345(9) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.510(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.406(8) . ? C5 C6 1.443(7) . ? C6 C7 1.388(8) . ? C6 C11 1.480(8) . ? C7 C8 1.416(8) . ? C7 C13 1.516(8) . ? C8 C9 1.401(8) . ? C8 C17 1.490(7) . ? C9 C10 1.392(7) . ? C9 C19 1.506(7) . ? C10 C23 1.534(7) . ? C11 C12 1.547(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.352(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.549(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.361(9) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.567(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 N6 Co1 N4 106.79(19) . 7_655 ? N6 Co1 Cl1 110.47(14) . . ? N4 Co1 Cl1 114.29(14) 7_655 . ? N6 Co1 Cl2 104.01(14) . . ? N4 Co1 Cl2 104.41(14) 7_655 . ? Cl1 Co1 Cl2 115.97(6) . . ? N1 Co2 N1 106.2(3) . 3_655 ? N1 Co2 Cl4 110.53(15) . . ? N1 Co2 Cl4 110.53(15) 3_655 . ? N1 Co2 Cl3 106.58(16) . . ? N1 Co2 Cl3 106.58(16) 3_655 . ? Cl4 Co2 Cl3 115.90(10) . . ? C1 N1 C2 105.7(5) . . ? C1 N1 Co2 123.4(4) . . ? C2 N1 Co2 130.8(4) . . ? C1 N2 C3 106.9(5) . . ? C1 N2 C4 123.2(5) . . ? C3 N2 C4 129.9(5) . . ? C16 N3 C14 107.7(5) . . ? C16 N3 C13 124.8(5) . . ? C14 N3 C13 127.2(5) . . ? C16 N4 C15 105.2(5) . . ? C16 N4 Co1 131.5(4) . 7_644 ? C15 N4 Co1 123.2(4) . 7_644 ? C22 N5 C20 106.6(5) . . ? C22 N5 C19 125.3(5) . . ? C20 N5 C19 127.9(5) . . ? C22 N6 C21 105.5(5) . . ? C22 N6 Co1 128.5(4) . . ? C21 N6 Co1 126.0(4) . . ? N1 C1 N2 111.1(5) . . ? N1 C1 H1 124.4 . . ? N2 C1 H1 124.4 . . ? C3 C2 N1 109.0(6) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N2 107.2(6) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? N2 C4 C5 112.0(4) . . ? N2 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C10 C5 C6 120.1(5) . . ? C10 C5 C4 120.6(5) . . ? C6 C5 C4 119.2(5) . . ? C7 C6 C5 118.4(5) . . ? C7 C6 C11 122.1(5) . . ? C5 C6 C11 119.5(5) . . ? C6 C7 C8 121.8(5) . . ? C6 C7 C13 119.7(5) . . ? C8 C7 C13 118.5(5) . . ? C9 C8 C7 118.4(5) . . ? C9 C8 C17 121.3(5) . . ? C7 C8 C17 120.3(5) . . ? C10 C9 C8 121.7(5) . . ? C10 C9 C19 119.5(5) . . ? C8 C9 C19 118.6(5) . . ? C9 C10 C5 119.5(5) . . ? C9 C10 C23 121.0(5) . . ? C5 C10 C23 119.5(5) . . ? C6 C11 C12 111.5(5) . . ? C6 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C6 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C7 112.0(4) . . ? N3 C13 H13A 109.2 . . ? C7 C13 H13A 109.2 . . ? N3 C13 H13B 109.2 . . ? C7 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C15 C14 N3 107.7(5) . . ? C15 C14 H14 126.1 . . ? N3 C14 H14 126.1 . . ? C14 C15 N4 107.8(5) . . ? C14 C15 H15 126.1 . . ? N4 C15 H15 126.1 . . ? N3 C16 N4 111.5(5) . . ? N3 C16 H16 124.3 . . ? N4 C16 H16 124.3 . . ? C8 C17 C18 111.2(4) . . ? C8 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? C8 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C9 113.7(5) . . ? N5 C19 H19A 108.8 . . ? C9 C19 H19A 108.8 . . ? N5 C19 H19B 108.8 . . ? C9 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C21 C20 N5 105.6(5) . . ? C21 C20 H20 127.2 . . ? N5 C20 H20 127.2 . . ? C20 C21 N6 110.2(6) . . ? C20 C21 H21 124.9 . . ? N6 C21 H21 124.9 . . ? N6 C22 N5 112.1(5) . . ? N6 C22 H22 123.9 . . ? N5 C22 H22 123.9 . . ? C10 C23 C24 111.9(5) . . ? C10 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? C10 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co2 N1 C1 59.1(6) 3_655 . . . ? Cl4 Co2 N1 C1 179.0(4) . . . . ? Cl3 Co2 N1 C1 -54.3(5) . . . . ? N1 Co2 N1 C2 -118.0(5) 3_655 . . . ? Cl4 Co2 N1 C2 1.9(6) . . . . ? Cl3 Co2 N1 C2 128.6(5) . . . . ? N4 Co1 N6 C22 36.8(5) 7_655 . . . ? Cl1 Co1 N6 C22 -88.0(5) . . . . ? Cl2 Co1 N6 C22 146.9(5) . . . . ? N4 Co1 N6 C21 -144.2(5) 7_655 . . . ? Cl1 Co1 N6 C21 91.0(5) . . . . ? Cl2 Co1 N6 C21 -34.1(5) . . . . ? C2 N1 C1 N2 -0.4(7) . . . . ? Co2 N1 C1 N2 -178.1(4) . . . . ? C3 N2 C1 N1 -1.0(7) . . . . ? C4 N2 C1 N1 177.8(5) . . . . ? C1 N1 C2 C3 1.7(7) . . . . ? Co2 N1 C2 C3 179.2(5) . . . . ? N1 C2 C3 N2 -2.3(8) . . . . ? C1 N2 C3 C2 2.1(7) . . . . ? C4 N2 C3 C2 -176.7(6) . . . . ? C1 N2 C4 C5 174.9(5) . . . . ? C3 N2 C4 C5 -6.5(8) . . . . ? N2 C4 C5 C10 92.8(6) . . . . ? N2 C4 C5 C6 -88.7(6) . . . . ? C10 C5 C6 C7 1.6(8) . . . . ? C4 C5 C6 C7 -176.9(5) . . . . ? C10 C5 C6 C11 -178.7(5) . . . . ? C4 C5 C6 C11 2.8(8) . . . . ? C5 C6 C7 C8 -0.5(8) . . . . ? C11 C6 C7 C8 179.8(5) . . . . ? C5 C6 C7 C13 178.6(5) . . . . ? C11 C6 C7 C13 -1.1(8) . . . . ? C6 C7 C8 C9 -0.1(8) . . . . ? C13 C7 C8 C9 -179.2(5) . . . . ? C6 C7 C8 C17 178.8(5) . . . . ? C13 C7 C8 C17 -0.3(7) . . . . ? C7 C8 C9 C10 -0.5(8) . . . . ? C17 C8 C9 C10 -179.4(5) . . . . ? C7 C8 C9 C19 175.9(5) . . . . ? C17 C8 C9 C19 -2.9(8) . . . . ? C8 C9 C10 C5 1.7(8) . . . . ? C19 C9 C10 C5 -174.7(5) . . . . ? C8 C9 C10 C23 -177.4(5) . . . . ? C19 C9 C10 C23 6.2(8) . . . . ? C6 C5 C10 C9 -2.2(8) . . . . ? C4 C5 C10 C9 176.3(5) . . . . ? C6 C5 C10 C23 176.9(5) . . . . ? C4 C5 C10 C23 -4.6(8) . . . . ? C7 C6 C11 C12 87.5(7) . . . . ? C5 C6 C11 C12 -92.2(7) . . . . ? C16 N3 C13 C7 156.6(5) . . . . ? C14 N3 C13 C7 -29.7(7) . . . . ? C6 C7 C13 N3 99.3(6) . . . . ? C8 C7 C13 N3 -81.5(6) . . . . ? C16 N3 C14 C15 -0.7(6) . . . . ? C13 N3 C14 C15 -175.3(5) . . . . ? N3 C14 C15 N4 0.4(6) . . . . ? C16 N4 C15 C14 0.0(6) . . . . ? Co1 N4 C15 C14 177.4(4) 7_644 . . . ? C14 N3 C16 N4 0.7(7) . . . . ? C13 N3 C16 N4 175.5(5) . . . . ? C15 N4 C16 N3 -0.4(6) . . . . ? Co1 N4 C16 N3 -177.6(4) 7_644 . . . ? C9 C8 C17 C18 91.7(6) . . . . ? C7 C8 C17 C18 -87.1(6) . . . . ? C22 N5 C19 C9 -153.4(5) . . . . ? C20 N5 C19 C9 32.7(8) . . . . ? C10 C9 C19 N5 -99.3(6) . . . . ? C8 C9 C19 N5 84.2(6) . . . . ? C22 N5 C20 C21 -1.5(7) . . . . ? C19 N5 C20 C21 173.2(6) . . . . ? N5 C20 C21 N6 1.4(8) . . . . ? C22 N6 C21 C20 -0.7(7) . . . . ? Co1 N6 C21 C20 -179.8(4) . . . . ? C21 N6 C22 N5 -0.4(7) . . . . ? Co1 N6 C22 N5 178.8(4) . . . . ? C20 N5 C22 N6 1.2(6) . . . . ? C19 N5 C22 N6 -173.7(5) . . . . ? C9 C10 C23 C24 -89.1(6) . . . . ? C5 C10 C23 C24 91.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.759 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.094 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.750 -0.020 880 446 ' ' 2 0.750 0.250 -0.021 880 446 ' ' _platon_squeeze_details ; ; # Attachment 'emptyTIF1.CIF' data_z:\xraydata\sarafr~1\08srv4~1\work\422s _database_code_depnum_ccdc_archive 'CCDC 735247' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 Cl6 Co3 N12' _chemical_formula_sum 'C48 H60 Cl6 Co3 N12' _chemical_formula_weight 1194.57 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' N N 0.0061 0.0033 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ima2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y, z' 'x+1/2, -y, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' _cell_length_a 40.1816(8) _cell_length_b 15.0535(3) _cell_length_c 11.1487(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6743.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5717 _cell_measurement_theta_min 2.275 _cell_measurement_theta_max 29.583 _exptl_crystal_description Needle _exptl_crystal_colour Blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2577 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6642 _exptl_absorpt_correction_T_max 0.9610 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Smart-6K _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31768 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 30.52 _reflns_number_total 10335 _reflns_number_gt 8584 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Xseed _computing_publication_material Xseed _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. Structure is run through the Squeeze routine in Platon as there are large voids that may contain some unmodelled electron density. ; _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^)+(0.0670P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(10) _refine_ls_number_reflns 10335 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.817 _refine_ls_shift/su_max 0.003 _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 0.941728(7) 0.628353(16) 0.37357(3) 0.01809(6) Uani 1 1 d . . . Co2 Co 1.2500 0.69094(3) 0.41253(4) 0.02320(9) Uani 1 2 d S . . Cl3 Cl 0.957997(14) 0.58290(4) 0.55712(5) 0.02697(11) Uani 1 1 d . . . Cl4 Cl 1.2500 0.83802(6) 0.44948(8) 0.02848(16) Uani 1 2 d S . . Cl5 Cl 0.903547(15) 0.54407(4) 0.28255(6) 0.03055(12) Uani 1 1 d . . . Cl6 Cl 1.2500 0.60438(6) 0.57491(7) 0.03257(17) Uani 1 2 d S . . C2 C 1.09878(5) 0.55533(12) -0.10152(17) 0.0186(4) Uani 1 1 d . . . N3 N 1.17654(4) 0.67499(12) 0.15458(16) 0.0204(3) Uani 1 1 d . . . N5 N 1.09074(5) 0.39141(10) -0.12140(17) 0.0208(3) Uani 1 1 d . . . N6 N 1.07585(5) 0.25167(12) -0.09808(17) 0.0242(4) Uani 1 1 d . . . N7 N 0.98476(4) 0.64159(11) 0.27987(17) 0.0203(3) Uani 1 1 d . . . C8 C 1.03887(5) 0.71954(13) 0.04217(19) 0.0191(4) Uani 1 1 d . . . H8A H 1.0437 0.7824 0.0616 0.023 Uiso 1 1 calc R . . H8B H 1.0231 0.7185 -0.0260 0.023 Uiso 1 1 calc R . . C9 C 1.12998(5) 0.58800(13) -0.06484(19) 0.0192(4) Uani 1 1 d . . . C10 C 1.09727(6) 0.47546(13) -0.18494(19) 0.0211(4) Uani 1 1 d . . . H10A H 1.0795 0.4853 -0.2451 0.025 Uiso 1 1 calc R . . H10B H 1.1187 0.4705 -0.2285 0.025 Uiso 1 1 calc R . . C12 C 1.09299(7) 0.27902(15) 0.0026(2) 0.0297(5) Uani 1 1 d . . . H12 H 1.0977 0.2432 0.0707 0.036 Uiso 1 1 calc R . . C13 C 1.03592(5) 0.56159(13) -0.10546(19) 0.0208(4) Uani 1 1 d . . . H13A H 1.0193 0.5725 -0.0416 0.025 Uiso 1 1 calc R . . H13B H 1.0376 0.4966 -0.1175 0.025 Uiso 1 1 calc R . . C14 C 1.16172(5) 0.54047(14) -0.0999(2) 0.0227(4) Uani 1 1 d . . . H14A H 1.1572 0.4759 -0.1041 0.027 Uiso 1 1 calc R . . H14B H 1.1786 0.5502 -0.0366 0.027 Uiso 1 1 calc R . . N15 N 1.02318(5) 0.67661(11) 0.14717(16) 0.0196(3) Uani 1 1 d . . . C16 C 1.20382(5) 0.70731(14) 0.2075(2) 0.0218(4) Uani 1 1 d . . . H16 H 1.2170 0.7543 0.1762 0.026 Uiso 1 1 calc R . . C17 C 1.10352(6) 0.79259(14) 0.1161(2) 0.0225(4) Uani 1 1 d . . . H17A H 1.1242 0.7915 0.1646 0.027 Uiso 1 1 calc R . . H17B H 1.0844 0.7943 0.1719 0.027 Uiso 1 1 calc R . . C18 C 1.06933(5) 0.59703(13) -0.06543(19) 0.0188(4) Uani 1 1 d . . . C19 C 1.01523(6) 0.61073(14) 0.3198(2) 0.0223(4) Uani 1 1 d . . . H19 H 1.0189 0.5795 0.3927 0.027 Uiso 1 1 calc R . . C20 C 1.07076(5) 0.67398(13) 0.00548(18) 0.0187(4) Uani 1 1 d . . . C21 C 1.16453(5) 0.70574(14) 0.0364(2) 0.0210(4) Uani 1 1 d . . . H21A H 1.1811 0.6894 -0.0257 0.025 Uiso 1 1 calc R . . H21B H 1.1627 0.7713 0.0374 0.025 Uiso 1 1 calc R . . C22 C 0.99071(5) 0.68105(14) 0.1749(2) 0.0217(4) Uani 1 1 d . . . H22 H 0.9742 0.7085 0.1264 0.026 Uiso 1 1 calc R . . C23 C 1.13106(5) 0.66620(13) 0.00320(19) 0.0191(4) Uani 1 1 d . . . C24 C 1.17604(6) 0.57124(18) -0.2205(2) 0.0312(5) Uani 1 1 d . . . H24A H 1.1961 0.5368 -0.2390 0.047 Uiso 1 1 calc R . . H24B H 1.1817 0.6345 -0.2158 0.047 Uiso 1 1 calc R . . H24C H 1.1595 0.5621 -0.2838 0.047 Uiso 1 1 calc R . . C25 C 1.03912(6) 0.63201(14) 0.2385(2) 0.0232(4) Uani 1 1 d . . . H25 H 1.0622 0.6188 0.2436 0.028 Uiso 1 1 calc R . . C26 C 1.10162(5) 0.70932(13) 0.04086(19) 0.0192(4) Uani 1 1 d . . . N27 N 1.21005(5) 0.66521(13) 0.30951(17) 0.0243(4) Uani 1 1 d . . . C28 C 1.10325(6) 0.87623(15) 0.0377(2) 0.0289(5) Uani 1 1 d . . . H28A H 1.1047 0.9290 0.0889 0.043 Uiso 1 1 calc R . . H28B H 1.0826 0.8782 -0.0089 0.043 Uiso 1 1 calc R . . H28C H 1.1223 0.8749 -0.0171 0.043 Uiso 1 1 calc R . . C29 C 1.07492(5) 0.32143(13) -0.1708(2) 0.0210(4) Uani 1 1 d . . . H29 H 1.0645 0.3220 -0.2474 0.025 Uiso 1 1 calc R . . C30 C 1.02395(6) 0.60499(16) -0.2221(2) 0.0268(4) Uani 1 1 d . . . H30A H 1.0028 0.5783 -0.2465 0.040 Uiso 1 1 calc R . . H30B H 1.0406 0.5956 -0.2852 0.040 Uiso 1 1 calc R . . H30C H 1.0209 0.6689 -0.2092 0.040 Uiso 1 1 calc R . . C31 C 1.10221(7) 0.36580(16) -0.0110(2) 0.0298(5) Uani 1 1 d . . . H31 H 1.1142 0.4012 0.0448 0.036 Uiso 1 1 calc R . . C32 C 1.18531(6) 0.60209(17) 0.3208(2) 0.0312(5) Uani 1 1 d . . . H32 H 1.1832 0.5611 0.3851 0.037 Uiso 1 1 calc R . . C33 C 1.16449(6) 0.60794(17) 0.2255(2) 0.0296(5) Uani 1 1 d . . . H33 H 1.1453 0.5726 0.2108 0.036 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 Co1 0.01968(12) 0.01681(11) 0.01778(12) 0.00068(11) 0.00125(12) -0.00027(9) Co2 0.01623(18) 0.0360(2) 0.01741(18) -0.00019(16) 0.000 0.000 Cl3 0.0301(3) 0.0327(3) 0.0181(2) 0.0036(2) -0.0001(2) 0.0023(2) Cl4 0.0205(3) 0.0328(4) 0.0321(4) 0.0030(3) 0.000 0.000 Cl5 0.0303(3) 0.0269(2) 0.0344(3) -0.0019(2) -0.0064(2) -0.0060(2) Cl6 0.0372(4) 0.0367(4) 0.0238(4) 0.0039(3) 0.000 0.000 C2 0.0228(9) 0.0173(8) 0.0158(9) 0.0008(7) 0.0000(7) -0.0029(7) N3 0.0172(8) 0.0244(8) 0.0196(8) 0.0009(7) -0.0013(7) -0.0024(7) N5 0.0269(8) 0.0184(7) 0.0171(8) -0.0015(7) 0.0001(8) -0.0022(6) N6 0.0291(9) 0.0213(8) 0.0221(9) 0.0002(7) -0.0024(8) -0.0011(7) N7 0.0185(8) 0.0206(8) 0.0217(8) 0.0014(7) 0.0026(7) 0.0008(6) C8 0.0183(9) 0.0197(8) 0.0192(9) 0.0017(7) 0.0017(8) 0.0010(7) C9 0.0168(9) 0.0212(9) 0.0197(10) 0.0039(7) 0.0016(8) -0.0001(7) C10 0.0262(10) 0.0184(9) 0.0187(9) -0.0011(7) -0.0004(8) -0.0023(8) C12 0.0395(13) 0.0272(11) 0.0224(11) 0.0063(9) -0.0061(10) -0.0103(10) C13 0.0168(9) 0.0219(9) 0.0238(11) 0.0009(7) -0.0019(8) -0.0047(7) C14 0.0195(9) 0.0245(9) 0.0240(11) -0.0009(8) 0.0007(8) 0.0022(7) N15 0.0191(8) 0.0226(8) 0.0170(8) 0.0009(7) 0.0003(7) -0.0001(6) C16 0.0174(10) 0.0261(10) 0.0220(10) -0.0015(8) -0.0018(8) -0.0042(8) C17 0.0215(10) 0.0240(10) 0.0221(10) -0.0045(8) -0.0014(8) -0.0005(8) C18 0.0168(9) 0.0197(9) 0.0200(9) 0.0032(7) -0.0013(8) -0.0042(7) C19 0.0255(10) 0.0216(9) 0.0197(9) 0.0021(8) -0.0008(9) 0.0016(8) C20 0.0172(9) 0.0201(9) 0.0188(9) 0.0023(7) 0.0001(8) 0.0003(7) C21 0.0159(9) 0.0260(10) 0.0209(10) 0.0030(8) -0.0016(8) -0.0019(7) C22 0.0180(9) 0.0252(10) 0.0219(10) 0.0013(8) -0.0017(8) 0.0014(8) C23 0.0162(9) 0.0210(9) 0.0201(9) 0.0012(8) -0.0021(8) -0.0027(7) C24 0.0261(12) 0.0403(13) 0.0271(11) -0.0023(10) 0.0053(10) 0.0001(10) C25 0.0214(10) 0.0238(10) 0.0242(10) 0.0037(8) -0.0033(9) 0.0024(8) C26 0.0193(9) 0.0196(9) 0.0185(9) 0.0021(7) 0.0012(8) -0.0002(7) N27 0.0191(9) 0.0333(10) 0.0206(9) -0.0004(7) -0.0023(7) -0.0001(7) C28 0.0311(12) 0.0238(10) 0.0319(12) -0.0034(9) 0.0010(10) -0.0001(8) C29 0.0240(10) 0.0197(9) 0.0194(9) -0.0021(7) -0.0038(8) -0.0038(7) C30 0.0251(11) 0.0303(11) 0.0249(10) 0.0001(9) -0.0040(9) -0.0046(9) C31 0.0390(13) 0.0300(11) 0.0205(10) 0.0017(9) -0.0073(10) -0.0092(9) C32 0.0279(12) 0.0388(12) 0.0270(11) 0.0099(10) -0.0007(10) -0.0072(10) C33 0.0229(11) 0.0364(12) 0.0296(12) 0.0052(10) -0.0024(10) -0.0105(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N6 2.0112(18) 7_655 ? Co1 N7 2.0298(18) . ? Co1 Cl5 2.2345(6) . ? Co1 Cl3 2.2546(6) . ? Co2 N27 2.0115(19) . ? Co2 N27 2.0115(19) 3_755 ? Co2 Cl6 2.2305(9) . ? Co2 Cl4 2.2519(10) . ? C2 C18 1.399(3) . ? C2 C9 1.407(3) . ? C2 C10 1.521(3) . ? N3 C16 1.337(3) . ? N3 C33 1.371(3) . ? N3 C21 1.478(3) . ? N5 C29 1.348(3) . ? N5 C31 1.370(3) . ? N5 C10 1.474(3) . ? N6 C29 1.327(3) . ? N6 C12 1.380(3) . ? N6 Co1 2.0112(18) 7_644 ? N7 C22 1.334(3) . ? N7 C19 1.383(3) . ? C8 N15 1.478(3) . ? C8 C20 1.510(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C23 1.401(3) . ? C9 C14 1.514(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 C31 1.366(3) . ? C12 H12 0.9500 . ? C13 C18 1.512(3) . ? C13 C30 1.532(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C24 1.534(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N15 C22 1.343(3) . ? N15 C25 1.377(3) . ? C16 N27 1.325(3) . ? C16 H16 0.9500 . ? C17 C26 1.511(3) . ? C17 C28 1.533(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C20 1.404(3) . ? C19 C25 1.358(3) . ? C19 H19 0.9500 . ? C20 C26 1.406(3) . ? C21 C23 1.517(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22 0.9500 . ? C23 C26 1.413(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25 0.9500 . ? N27 C32 1.381(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C32 C33 1.355(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? 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 N6 Co1 N7 106.82(7) 7_655 . ? N6 Co1 Cl5 110.75(6) 7_655 . ? N7 Co1 Cl5 114.01(6) . . ? N6 Co1 Cl3 103.84(6) 7_655 . ? N7 Co1 Cl3 104.47(6) . . ? Cl5 Co1 Cl3 116.04(2) . . ? N27 Co2 N27 105.89(11) . 3_755 ? N27 Co2 Cl6 110.54(6) . . ? N27 Co2 Cl6 110.54(6) 3_755 . ? N27 Co2 Cl4 107.09(6) . . ? N27 Co2 Cl4 107.09(6) 3_755 . ? Cl6 Co2 Cl4 115.20(4) . . ? C18 C2 C9 120.87(18) . . ? C18 C2 C10 119.78(18) . . ? C9 C2 C10 119.32(19) . . ? C16 N3 C33 107.63(19) . . ? C16 N3 C21 123.20(18) . . ? C33 N3 C21 129.04(19) . . ? C29 N5 C31 107.82(18) . . ? C29 N5 C10 123.94(19) . . ? C31 N5 C10 127.87(18) . . ? C29 N6 C12 105.97(18) . . ? C29 N6 Co1 128.63(15) . 7_644 ? C12 N6 Co1 125.35(15) . 7_644 ? C22 N7 C19 105.85(18) . . ? C22 N7 Co1 130.38(15) . . ? C19 N7 Co1 123.74(15) . . ? N15 C8 C20 112.20(16) . . ? N15 C8 H8A 109.2 . . ? C20 C8 H8A 109.2 . . ? N15 C8 H8B 109.2 . . ? C20 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C23 C9 C2 118.59(18) . . ? C23 C9 C14 120.72(18) . . ? C2 C9 C14 120.68(18) . . ? N5 C10 C2 113.07(17) . . ? N5 C10 H10A 109.0 . . ? C2 C10 H10A 109.0 . . ? N5 C10 H10B 109.0 . . ? C2 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C31 C12 N6 109.3(2) . . ? C31 C12 H12 125.4 . . ? N6 C12 H12 125.4 . . ? C18 C13 C30 112.25(17) . . ? C18 C13 H13A 109.2 . . ? C30 C13 H13A 109.2 . . ? C18 C13 H13B 109.2 . . ? C30 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C9 C14 C24 113.55(18) . . ? C9 C14 H14A 108.9 . . ? C24 C14 H14A 108.9 . . ? C9 C14 H14B 108.9 . . ? C24 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C22 N15 C25 107.81(18) . . ? C22 N15 C8 125.11(18) . . ? C25 N15 C8 126.87(18) . . ? N27 C16 N3 111.07(19) . . ? N27 C16 H16 124.5 . . ? N3 C16 H16 124.5 . . ? C26 C17 C28 111.36(18) . . ? C26 C17 H17A 109.4 . . ? C28 C17 H17A 109.4 . . ? C26 C17 H17B 109.4 . . ? C28 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C2 C18 C20 119.85(18) . . ? C2 C18 C13 120.53(18) . . ? C20 C18 C13 119.59(19) . . ? C25 C19 N7 109.36(19) . . ? C25 C19 H19 125.3 . . ? N7 C19 H19 125.3 . . ? C18 C20 C26 120.43(19) . . ? C18 C20 C8 119.52(18) . . ? C26 C20 C8 120.05(18) . . ? N3 C21 C23 112.60(17) . . ? N3 C21 H21A 109.1 . . ? C23 C21 H21A 109.1 . . ? N3 C21 H21B 109.1 . . ? C23 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? N7 C22 N15 110.74(19) . . ? N7 C22 H22 124.6 . . ? N15 C22 H22 124.6 . . ? C9 C23 C26 121.40(18) . . ? C9 C23 C21 119.29(18) . . ? C26 C23 C21 119.31(18) . . ? C14 C24 H24A 109.5 . . ? C14 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C14 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 N15 106.25(19) . . ? C19 C25 H25 126.9 . . ? N15 C25 H25 126.9 . . ? C20 C26 C23 118.76(18) . . ? C20 C26 C17 120.98(19) . . ? C23 C26 C17 120.26(19) . . ? C16 N27 C32 105.72(19) . . ? C16 N27 Co2 123.25(16) . . ? C32 N27 Co2 130.94(16) . . ? C17 C28 H28A 109.5 . . ? C17 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C17 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C29 N5 110.80(19) . . ? N6 C29 H29 124.6 . . ? N5 C29 H29 124.6 . . ? C13 C30 H30A 109.5 . . ? C13 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C13 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C12 C31 N5 106.1(2) . . ? C12 C31 H31 126.9 . . ? N5 C31 H31 126.9 . . ? C33 C32 N27 109.2(2) . . ? C33 C32 H32 125.4 . . ? N27 C32 H32 125.4 . . ? C32 C33 N3 106.4(2) . . ? C32 C33 H33 126.8 . . ? N3 C33 H33 126.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Co1 N7 C22 -56.9(2) 7_655 . . . ? Cl5 Co1 N7 C22 65.73(19) . . . . ? Cl3 Co1 N7 C22 -166.59(18) . . . . ? N6 Co1 N7 C19 120.97(17) 7_655 . . . ? Cl5 Co1 N7 C19 -116.36(16) . . . . ? Cl3 Co1 N7 C19 11.32(17) . . . . ? C18 C2 C9 C23 -3.5(3) . . . . ? C10 C2 C9 C23 174.40(18) . . . . ? C18 C2 C9 C14 177.46(19) . . . . ? C10 C2 C9 C14 -4.6(3) . . . . ? C29 N5 C10 C2 151.0(2) . . . . ? C31 N5 C10 C2 -36.9(3) . . . . ? C18 C2 C10 N5 -82.9(2) . . . . ? C9 C2 C10 N5 99.1(2) . . . . ? C29 N6 C12 C31 0.1(3) . . . . ? Co1 N6 C12 C31 177.61(18) 7_644 . . . ? C23 C9 C14 C24 -90.4(2) . . . . ? C2 C9 C14 C24 88.6(2) . . . . ? C20 C8 N15 C22 -156.10(19) . . . . ? C20 C8 N15 C25 29.8(3) . . . . ? C33 N3 C16 N27 -0.4(3) . . . . ? C21 N3 C16 N27 -176.64(19) . . . . ? C9 C2 C18 C20 1.8(3) . . . . ? C10 C2 C18 C20 -176.07(18) . . . . ? C9 C2 C18 C13 179.87(18) . . . . ? C10 C2 C18 C13 2.0(3) . . . . ? C30 C13 C18 C2 -91.5(2) . . . . ? C30 C13 C18 C20 86.6(2) . . . . ? C22 N7 C19 C25 0.0(2) . . . . ? Co1 N7 C19 C25 -178.32(14) . . . . ? C2 C18 C20 C26 -0.2(3) . . . . ? C13 C18 C20 C26 -178.27(18) . . . . ? C2 C18 C20 C8 178.89(18) . . . . ? C13 C18 C20 C8 0.8(3) . . . . ? N15 C8 C20 C18 81.5(2) . . . . ? N15 C8 C20 C26 -99.3(2) . . . . ? C16 N3 C21 C23 -173.42(19) . . . . ? C33 N3 C21 C23 11.2(3) . . . . ? C19 N7 C22 N15 -0.1(2) . . . . ? Co1 N7 C22 N15 178.14(14) . . . . ? C25 N15 C22 N7 0.1(2) . . . . ? C8 N15 C22 N7 -174.95(18) . . . . ? C2 C9 C23 C26 3.7(3) . . . . ? C14 C9 C23 C26 -177.33(19) . . . . ? C2 C9 C23 C21 -175.93(18) . . . . ? C14 C9 C23 C21 3.1(3) . . . . ? N3 C21 C23 C9 -93.0(2) . . . . ? N3 C21 C23 C26 87.4(2) . . . . ? N7 C19 C25 N15 0.0(2) . . . . ? C22 N15 C25 C19 0.0(2) . . . . ? C8 N15 C25 C19 174.86(18) . . . . ? C18 C20 C26 C23 0.3(3) . . . . ? C8 C20 C26 C23 -178.77(18) . . . . ? C18 C20 C26 C17 179.40(19) . . . . ? C8 C20 C26 C17 0.3(3) . . . . ? C9 C23 C26 C20 -2.1(3) . . . . ? C21 C23 C26 C20 177.49(18) . . . . ? C9 C23 C26 C17 178.83(19) . . . . ? C21 C23 C26 C17 -1.6(3) . . . . ? C28 C17 C26 C20 -86.9(2) . . . . ? C28 C17 C26 C23 92.1(2) . . . . ? N3 C16 N27 C32 0.5(3) . . . . ? N3 C16 N27 Co2 177.42(14) . . . . ? N27 Co2 N27 C16 -60.4(2) 3_755 . . . ? Cl6 Co2 N27 C16 179.82(16) . . . . ? Cl4 Co2 N27 C16 53.60(19) . . . . ? N27 Co2 N27 C32 115.6(2) 3_755 . . . ? Cl6 Co2 N27 C32 -4.1(2) . . . . ? Cl4 Co2 N27 C32 -130.3(2) . . . . ? C12 N6 C29 N5 0.2(3) . . . . ? Co1 N6 C29 N5 -177.17(15) 7_644 . . . ? C31 N5 C29 N6 -0.5(3) . . . . ? C10 N5 C29 N6 172.97(19) . . . . ? N6 C12 C31 N5 -0.4(3) . . . . ? C29 N5 C31 C12 0.5(3) . . . . ? C10 N5 C31 C12 -172.6(2) . . . . ? C16 N27 C32 C33 -0.5(3) . . . . ? Co2 N27 C32 C33 -177.04(18) . . . . ? N27 C32 C33 N3 0.2(3) . . . . ? C16 N3 C33 C32 0.1(3) . . . . ? C21 N3 C33 C32 176.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.630 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.057 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.250 -0.010 866 117 ' ' 2 0.750 0.750 -0.009 866 117 ' ' _platon_squeeze_details ; ;