# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Steed, Jonathan' _publ_contact_author_email jon.steed@durham.ac.uk _publ_section_title ; Tripodal Imidazole Frameworks: Reversible Vapour Sorption Both With and Without Significant Structural Changes ; loop_ _publ_author_name C.Willans S.French K.Anderson L.Barbour J.Gertenbach G.Lloyd ; R.Dyer ; P.Junk J.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 ; ; # Attachment '- Ligand 1.cif' data_c:\kirsty~1\crysta~1\charlo~1\06srv3~1\jan08dis _database_code_depnum_ccdc_archive 'CCDC 781848' #TrackingRef '- Ligand 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 N6 (H2 O)2' _chemical_formula_sum 'C24 H34 N6 O2' _chemical_formula_weight 438.57 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.913(2) _cell_length_b 12.452(3) _cell_length_c 19.873(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2453.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687715 _exptl_absorpt_correction_T_max 1.000000 _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 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21659 _diffrn_reflns_av_R_equivalents 0.2359 _diffrn_reflns_av_sigmaI/netI 0.1019 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 23.46 _reflns_number_total 2010 _reflns_number_gt 1260 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _refine_special_details ; The crystals were very small and poorly diffracting, hence poor resolution and Rint. There is disorder of one water molecule and it is likely that there is some disorder of the N positions in the imidazole rings, however no suitable solution could be found which incorporated the disorder. No hydrogens were located for the water molecules. Equivalents have been merged (MERG 4) 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^)+(0.1537P)^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 . _refine_ls_number_reflns 2010 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1623 _refine_ls_R_factor_gt 0.1007 _refine_ls_wR_factor_ref 0.2662 _refine_ls_wR_factor_gt 0.2345 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 O1W O 1.6067(11) 0.2679(14) 0.0583(6) 0.171(7) Uani 1 1 d . . . O2W O 1.369(2) 0.7872(18) 0.2774(14) 0.169(12) Uani 0.601(18) 1 d P A 1 O2W' O 1.5268(17) 0.6291(19) 0.2564(10) 0.079(9) Uani 0.399(18) 1 d P A 2 N1 N 0.9460(12) 0.7376(8) 0.4096(5) 0.066(3) Uani 1 1 d . . . N2 N 0.8975(9) 0.7693(6) 0.3020(4) 0.040(2) Uani 1 1 d . . . N3 N 1.3767(11) 0.5117(11) 0.1616(7) 0.088(4) Uani 1 1 d . . . N4 N 1.1940(9) 0.5285(7) 0.0937(4) 0.041(2) Uani 1 1 d . . . N5 N 1.3827(11) 1.0162(9) 0.1363(7) 0.079(4) Uani 1 1 d . . . N6 N 1.2069(9) 0.9887(7) 0.0710(5) 0.042(2) Uani 1 1 d . . . C1 C 0.8495(12) 0.7391(9) 0.3635(5) 0.053(3) Uani 1 1 d . . . H1 H 0.7579 0.7214 0.3722 0.064 Uiso 1 1 calc R . . C2 C 1.0652(13) 0.7669(9) 0.3749(6) 0.056(3) Uani 1 1 d . . . H2 H 1.1523 0.7723 0.3946 0.067 Uiso 1 1 calc R . . C3 C 1.0359(11) 0.7861(7) 0.3093(5) 0.038(3) Uani 1 1 d . . . H3 H 1.0975 0.8069 0.2751 0.045 Uiso 1 1 calc R . . C4 C 0.8155(10) 0.7837(8) 0.2398(4) 0.037(3) Uani 1 1 d . . . H4A H 0.7718 0.8552 0.2413 0.044 Uiso 1 1 calc R . . H4B H 0.7433 0.7288 0.2391 0.044 Uiso 1 1 calc R . . C5 C 0.8969(9) 0.7748(8) 0.1752(5) 0.037(3) Uani 1 1 d . . . C6 C 0.9363(9) 0.6730(8) 0.1509(5) 0.032(3) Uani 1 1 d . . . C7 C 0.8869(11) 0.5735(9) 0.1859(5) 0.042(3) Uani 1 1 d . . . H7A H 0.8777 0.5886 0.2346 0.051 Uiso 1 1 calc R . . H7B H 0.9549 0.5159 0.1806 0.051 Uiso 1 1 calc R . . C8 C 0.7512(11) 0.5338(8) 0.1587(6) 0.045(3) Uani 1 1 d . . . H8A H 0.6876 0.5940 0.1566 0.068 Uiso 1 1 calc R . . H8B H 0.7153 0.4781 0.1885 0.068 Uiso 1 1 calc R . . H8C H 0.7639 0.5041 0.1134 0.068 Uiso 1 1 calc R . . C9 C 1.2552(12) 0.5632(10) 0.1530(6) 0.053(3) Uani 1 1 d . . . H9 H 1.2183 0.6147 0.1831 0.063 Uiso 1 1 calc R . . C10 C 1.3886(14) 0.4427(10) 0.1047(8) 0.064(4) Uani 1 1 d . . . H10 H 1.4622 0.3964 0.0948 0.076 Uiso 1 1 calc R . . C11 C 1.2784(12) 0.4552(9) 0.0683(6) 0.053(3) Uani 1 1 d . . . H11 H 1.2609 0.4162 0.0281 0.064 Uiso 1 1 calc R . . C12 C 1.0608(11) 0.5589(8) 0.0666(6) 0.045(3) Uani 1 1 d . . . H12A H 0.9935 0.5042 0.0800 0.054 Uiso 1 1 calc R . . H12B H 1.0652 0.5598 0.0168 0.054 Uiso 1 1 calc R . . C13 C 1.0163(9) 0.6656(7) 0.0908(5) 0.030(3) Uani 1 1 d . . . C14 C 1.0590(9) 0.7584(7) 0.0559(4) 0.030(2) Uani 1 1 d . . . C15 C 1.1435(10) 0.7488(9) -0.0082(5) 0.040(3) Uani 1 1 d . . . H15A H 1.2014 0.6842 -0.0054 0.048 Uiso 1 1 calc R . . H15B H 1.2027 0.8124 -0.0125 0.048 Uiso 1 1 calc R . . C16 C 1.0494(11) 0.7404(10) -0.0721(5) 0.055(3) Uani 1 1 d . . . H16A H 0.9995 0.6725 -0.0707 0.083 Uiso 1 1 calc R . . H16B H 1.1046 0.7429 -0.1129 0.083 Uiso 1 1 calc R . . H16C H 0.9855 0.8005 -0.0722 0.083 Uiso 1 1 calc R . . C17 C 1.2654(12) 0.9642(9) 0.1338(7) 0.059(4) Uani 1 1 d . . . H17 H 1.2283 0.9193 0.1677 0.070 Uiso 1 1 calc R . . C18 C 1.4039(13) 1.0706(9) 0.0778(7) 0.056(3) Uani 1 1 d . . . H18 H 1.4825 1.1103 0.0664 0.068 Uiso 1 1 calc R . . C19 C 1.2928(14) 1.0583(9) 0.0385(7) 0.064(4) Uani 1 1 d . . . H19 H 1.2773 1.0916 -0.0038 0.077 Uiso 1 1 calc R . . C20 C 1.0685(11) 0.9604(8) 0.0474(6) 0.047(3) Uani 1 1 d . . . H20A H 1.0691 0.9498 -0.0020 0.057 Uiso 1 1 calc R . . H20B H 1.0056 1.0198 0.0579 0.057 Uiso 1 1 calc R . . C21 C 1.0210(11) 0.8576(7) 0.0819(5) 0.035(3) Uani 1 1 d . . . C22 C 0.9426(9) 0.8668(8) 0.1406(5) 0.033(3) Uani 1 1 d . . . C23 C 0.9020(10) 0.9763(8) 0.1681(5) 0.036(3) Uani 1 1 d . . . H23A H 0.9712 1.0300 0.1556 0.043 Uiso 1 1 calc R . . H23B H 0.8978 0.9729 0.2178 0.043 Uiso 1 1 calc R . . C24 C 0.7632(10) 1.0122(8) 0.1403(5) 0.041(3) Uani 1 1 d . . . H24A H 0.7648 1.0099 0.0910 0.061 Uiso 1 1 calc R . . H24B H 0.7441 1.0857 0.1553 0.061 Uiso 1 1 calc R . . H24C H 0.6929 0.9638 0.1571 0.061 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 O1W 0.064(7) 0.33(2) 0.119(9) 0.074(12) -0.022(7) 0.011(12) O2W 0.125(18) 0.14(2) 0.24(3) -0.030(18) -0.02(2) 0.018(15) O2W' 0.022(12) 0.13(2) 0.082(16) -0.014(14) 0.023(11) -0.006(12) N1 0.094(8) 0.053(6) 0.050(6) -0.011(5) -0.017(7) 0.013(7) N2 0.053(6) 0.032(5) 0.035(5) 0.000(4) -0.010(5) -0.014(5) N3 0.040(7) 0.105(10) 0.120(11) 0.073(9) -0.004(7) -0.007(7) N4 0.050(6) 0.034(5) 0.038(6) 0.008(4) 0.002(5) 0.004(5) N5 0.050(7) 0.074(8) 0.113(11) -0.019(8) 0.004(8) -0.019(7) N6 0.026(5) 0.040(5) 0.060(7) -0.008(5) 0.017(5) -0.021(4) C1 0.065(8) 0.056(8) 0.038(7) -0.024(7) 0.005(7) -0.006(7) C2 0.068(8) 0.035(7) 0.066(9) -0.007(6) -0.028(7) -0.014(7) C3 0.049(7) 0.032(6) 0.033(6) 0.000(5) -0.018(5) -0.003(5) C4 0.036(6) 0.033(6) 0.041(6) -0.008(5) -0.012(5) 0.009(5) C5 0.018(5) 0.054(7) 0.038(6) 0.008(6) 0.003(5) -0.005(5) C6 0.019(6) 0.043(7) 0.034(6) 0.002(5) 0.008(5) -0.008(5) C7 0.049(7) 0.056(7) 0.022(6) 0.010(5) -0.003(6) -0.003(6) C8 0.051(7) 0.036(7) 0.048(7) 0.009(6) -0.005(6) -0.002(6) C9 0.036(7) 0.076(9) 0.047(7) 0.012(7) 0.002(6) 0.006(6) C10 0.038(8) 0.054(8) 0.099(11) 0.018(8) 0.027(8) 0.023(7) C11 0.042(8) 0.050(7) 0.067(8) 0.018(7) 0.012(7) 0.016(7) C12 0.041(7) 0.036(6) 0.058(7) 0.014(5) -0.015(6) 0.004(6) C13 0.018(6) 0.028(6) 0.046(6) 0.001(5) -0.023(5) -0.006(4) C14 0.027(5) 0.029(6) 0.034(6) 0.006(5) -0.014(5) -0.007(5) C15 0.049(6) 0.026(5) 0.044(6) 0.006(5) 0.001(5) -0.024(5) C16 0.059(7) 0.069(8) 0.038(6) 0.008(6) 0.007(6) 0.014(7) C17 0.039(8) 0.041(7) 0.096(11) -0.011(7) 0.001(8) -0.008(6) C18 0.043(8) 0.049(7) 0.077(10) -0.018(7) 0.025(8) -0.023(6) C19 0.078(10) 0.043(7) 0.071(9) -0.026(6) 0.047(9) -0.028(7) C20 0.038(7) 0.047(7) 0.058(7) -0.003(6) 0.005(6) -0.019(6) C21 0.048(7) 0.021(6) 0.037(6) -0.002(5) -0.005(6) -0.001(5) C22 0.024(6) 0.040(7) 0.034(6) -0.007(5) -0.007(5) -0.001(5) C23 0.034(6) 0.044(6) 0.029(6) -0.005(5) 0.004(5) -0.015(5) C24 0.039(6) 0.024(6) 0.059(8) 0.009(5) 0.002(6) 0.004(5) _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 N1 C1 1.325(13) . ? N1 C2 1.416(15) . ? N2 C1 1.364(13) . ? N2 C3 1.396(13) . ? N2 C4 1.490(11) . ? N3 C9 1.375(15) . ? N3 C10 1.425(17) . ? N4 C11 1.337(13) . ? N4 C9 1.394(14) . ? N4 C12 1.475(14) . ? N5 C17 1.332(15) . ? N5 C18 1.362(15) . ? N6 C19 1.375(13) . ? N6 C17 1.409(16) . ? N6 C20 1.492(14) . ? C2 C3 1.357(14) . ? C4 C5 1.520(13) . ? C5 C22 1.411(13) . ? C5 C6 1.412(13) . ? C6 C13 1.436(13) . ? C6 C7 1.503(13) . ? C7 C8 1.533(15) . ? C10 C11 1.320(17) . ? C12 C13 1.480(14) . ? C13 C14 1.413(12) . ? C14 C21 1.391(13) . ? C14 C15 1.529(13) . ? C15 C16 1.579(13) . ? C18 C19 1.359(17) . ? C20 C21 1.526(13) . ? C21 C22 1.406(13) . ? C22 C23 1.523(13) . ? C23 C24 1.548(14) . ? 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 C1 N1 C2 105.2(9) . . ? C1 N2 C3 106.9(9) . . ? C1 N2 C4 125.9(9) . . ? C3 N2 C4 127.2(8) . . ? C9 N3 C10 104.7(12) . . ? C11 N4 C9 105.0(10) . . ? C11 N4 C12 126.7(10) . . ? C9 N4 C12 128.2(10) . . ? C17 N5 C18 110.1(12) . . ? C19 N6 C17 107.3(10) . . ? C19 N6 C20 124.8(11) . . ? C17 N6 C20 127.2(9) . . ? N1 C1 N2 111.8(10) . . ? C3 C2 N1 109.6(10) . . ? C2 C3 N2 106.5(10) . . ? N2 C4 C5 113.7(8) . . ? C22 C5 C6 118.2(9) . . ? C22 C5 C4 121.5(9) . . ? C6 C5 C4 120.1(8) . . ? C5 C6 C13 119.7(8) . . ? C5 C6 C7 119.4(8) . . ? C13 C6 C7 120.8(9) . . ? C6 C7 C8 112.8(8) . . ? N3 C9 N4 110.0(12) . . ? C11 C10 N3 107.2(12) . . ? C10 C11 N4 113.0(12) . . ? N4 C12 C13 112.2(9) . . ? C14 C13 C6 121.4(9) . . ? C14 C13 C12 119.0(9) . . ? C6 C13 C12 119.5(9) . . ? C21 C14 C13 117.6(9) . . ? C21 C14 C15 121.8(8) . . ? C13 C14 C15 120.6(9) . . ? C14 C15 C16 110.6(8) . . ? N5 C17 N6 106.7(12) . . ? C19 C18 N5 108.0(11) . . ? C18 C19 N6 107.7(12) . . ? N6 C20 C21 110.0(9) . . ? C14 C21 C22 122.0(9) . . ? C14 C21 C20 119.6(9) . . ? C22 C21 C20 118.4(9) . . ? C21 C22 C5 121.1(9) . . ? C21 C22 C23 121.1(9) . . ? C5 C22 C23 117.8(9) . . ? C22 C23 C24 111.5(8) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 23.46 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.537 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.075 # Attachment '- TIF2.cif' data_c:\kirsty~1\crysta~1\charlo~1\06kma0~1\all _database_code_depnum_ccdc_archive 'CCDC 781849' #TrackingRef '- TIF2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H64 Co N12 O2, 4(H2 O), 2(Cl)' _chemical_formula_sum 'C48 H72 Cl2 Co N12 O6' _chemical_formula_weight 1043.01 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2994(15) _cell_length_b 22.066(4) _cell_length_c 13.8764(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.412(6) _cell_angle_gamma 90.00 _cell_volume 2847.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1106 _exptl_absorpt_coefficient_mu 0.449 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21493 _diffrn_reflns_av_R_equivalents 0.2957 _diffrn_reflns_av_sigmaI/netI 0.6434 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.18 _reflns_number_total 7630 _reflns_number_gt 1558 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _refine_special_details ; The crystal decomposed/fell off in the middle of the data collection therefore only a small amount of data was collected. The connectivity is not in doubt though. Water hydrogens located in difference map and then DFIX'ed in position. 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^)+(0.0000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7630 _refine_ls_number_parameters 340 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2960 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 0.609 _refine_ls_restrained_S_all 0.609 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.0000 0.5000 0.0220(3) Uani 1 2 d S . . Cl1 Cl 0.42832(16) 0.06656(7) 0.34222(11) 0.0370(4) Uani 1 1 d . . . O1 O 0.2226(4) -0.01173(19) 0.4664(3) 0.0271(10) Uani 1 1 d D . . O2 O 0.5120(6) -0.0704(2) 0.3165(4) 0.0522(13) Uani 1 1 d D . . O3 O 0.3961(5) -0.1141(2) 0.4799(3) 0.0364(11) Uani 1 1 d D . . N1 N -0.0498(5) 0.02748(17) 0.3560(3) 0.0206(11) Uani 1 1 d . . . N2 N -0.1697(5) 0.05182(18) 0.2242(3) 0.0214(11) Uani 1 1 d . . . N3 N -0.3316(5) 0.3276(2) 0.0820(3) 0.0241(12) Uani 1 1 d . . . N4 N -0.4541(5) 0.40735(19) 0.0354(3) 0.0224(11) Uani 1 1 d . . . N5 N 0.0485(5) 0.1333(2) -0.1487(3) 0.0292(13) Uani 1 1 d . . . N7 N 0.2648(6) 0.0982(2) -0.1893(4) 0.0396(14) Uani 1 1 d . . . C1 C -0.1789(6) 0.0345(2) 0.3165(4) 0.0223(14) Uani 1 1 d . . . H1 H -0.2667 0.0280 0.3494 0.027 Uiso 1 1 calc R . . C2 C 0.0474(6) 0.0410(2) 0.2834(4) 0.0257(14) Uani 1 1 d . . . H2 H 0.1492 0.0398 0.2893 0.031 Uiso 1 1 calc R . . C3 C -0.0273(6) 0.0562(2) 0.2029(4) 0.0240(14) Uani 1 1 d . . . H3 H 0.0122 0.0678 0.1427 0.029 Uiso 1 1 calc R . . C4 C -0.2912(5) 0.0648(2) 0.1589(3) 0.0234(14) Uani 1 1 d . . . H4A H -0.3777 0.0746 0.1970 0.028 Uiso 1 1 calc R . . H4B H -0.3126 0.0287 0.1190 0.028 Uiso 1 1 calc R . . C5 C -0.2535(6) 0.1181(2) 0.0942(4) 0.0192(13) Uani 1 1 d . . . C6 C -0.2574(6) 0.1781(2) 0.1322(4) 0.0218(14) Uani 1 1 d . . . C7 C -0.2154(6) 0.2254(2) 0.0731(4) 0.0231(14) Uani 1 1 d . . . C8 C -0.1770(6) 0.2167(2) -0.0230(4) 0.0223(14) Uani 1 1 d . . . C9 C -0.1672(6) 0.1570(2) -0.0573(4) 0.0227(14) Uani 1 1 d . . . C10 C -0.2035(6) 0.1073(2) 0.0010(4) 0.0198(13) Uani 1 1 d . . . C11 C -0.3054(6) 0.1886(2) 0.2365(4) 0.0324(16) Uani 1 1 d . . . H11A H -0.3676 0.1544 0.2563 0.039 Uiso 1 1 calc R . . H11B H -0.3641 0.2260 0.2388 0.039 Uiso 1 1 calc R . . C12 C -0.1809(6) 0.1945(2) 0.3091(3) 0.0413(18) Uani 1 1 d . . . H12A H -0.1242 0.1570 0.3093 0.062 Uiso 1 1 calc R . . H12B H -0.2195 0.2016 0.3737 0.062 Uiso 1 1 calc R . . H12C H -0.1194 0.2286 0.2908 0.062 Uiso 1 1 calc R . . C13 C -0.2100(6) 0.2903(2) 0.1156(4) 0.0311(16) Uani 1 1 d . . . H13A H -0.2116 0.2879 0.1868 0.037 Uiso 1 1 calc R . . H13B H -0.1188 0.3099 0.0966 0.037 Uiso 1 1 calc R . . C14 C -0.3245(6) 0.3860(2) 0.0555(3) 0.0208(13) Uani 1 1 d . . . H14 H -0.2381 0.4089 0.0517 0.025 Uiso 1 1 calc R . . C15 C -0.4744(6) 0.3107(3) 0.0786(4) 0.0299(15) Uani 1 1 d . . . H15 H -0.5123 0.2718 0.0933 0.036 Uiso 1 1 calc R . . C16 C -0.5507(6) 0.3602(2) 0.0502(4) 0.0265(15) Uani 1 1 d . . . H16 H -0.6521 0.3622 0.0419 0.032 Uiso 1 1 calc R . . C17 C -0.1442(6) 0.2694(2) -0.0898(4) 0.0317(16) Uani 1 1 d . . . H17A H -0.0624 0.2584 -0.1316 0.038 Uiso 1 1 calc R . . H17B H -0.1154 0.3050 -0.0508 0.038 Uiso 1 1 calc R . . C18 C -0.2737(6) 0.2861(2) -0.1528(4) 0.0406(18) Uani 1 1 d . . . H18A H -0.3015 0.2511 -0.1923 0.061 Uiso 1 1 calc R . . H18B H -0.2484 0.3201 -0.1948 0.061 Uiso 1 1 calc R . . H18C H -0.3543 0.2978 -0.1117 0.061 Uiso 1 1 calc R . . C19 C -0.1054(6) 0.1460(2) -0.1567(4) 0.0312(15) Uani 1 1 d . . . H19A H -0.1549 0.1112 -0.1874 0.037 Uiso 1 1 calc R . . H19B H -0.1210 0.1822 -0.1976 0.037 Uiso 1 1 calc R . . C20 C 0.1250(7) 0.0993(2) -0.2105(4) 0.0342(16) Uani 1 1 d . . . H20 H 0.0835 0.0783 -0.2636 0.041 Uiso 1 1 calc R . . C21 C 0.1481(7) 0.1554(3) -0.0833(4) 0.0464(19) Uani 1 1 d . . . H21 H 0.1284 0.1811 -0.0300 0.056 Uiso 1 1 calc R . . C22 C 0.2770(7) 0.1341(3) -0.1084(5) 0.052(2) Uani 1 1 d . . . H22 H 0.3645 0.1426 -0.0753 0.063 Uiso 1 1 calc R . . C23 C -0.1877(6) 0.0432(2) -0.0382(4) 0.0295(15) Uani 1 1 d . . . H23A H -0.1641 0.0153 0.0155 0.035 Uiso 1 1 calc R . . H23B H -0.1071 0.0421 -0.0844 0.035 Uiso 1 1 calc R . . C24 C -0.3252(6) 0.0215(2) -0.0886(4) 0.0452(19) Uani 1 1 d . . . H24A H -0.4062 0.0248 -0.0442 0.068 Uiso 1 1 calc R . . H24B H -0.3136 -0.0208 -0.1085 0.068 Uiso 1 1 calc R . . H24C H -0.3438 0.0467 -0.1455 0.068 Uiso 1 1 calc R . . H1W1 H 0.294(5) 0.012(3) 0.440(4) 0.10(3) Uiso 1 1 d D . . H2W1 H 0.499(6) -0.0303(9) 0.313(3) 0.029(18) Uiso 1 1 d D . . H3W1 H 0.449(4) -0.106(2) 0.429(2) 0.029(18) Uiso 1 1 d D . . H1W2 H 0.296(6) -0.041(3) 0.473(5) 0.14(4) Uiso 1 1 d D . . H2W2 H 0.576(4) -0.080(3) 0.272(3) 0.06(2) Uiso 1 1 d D . . H3W2 H 0.400(6) -0.104(2) 0.5378(17) 0.028(19) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0235(7) 0.0193(6) 0.0232(6) 0.0006(6) 0.0023(5) -0.0002(6) Cl1 0.0320(10) 0.0355(10) 0.0437(10) 0.0007(8) 0.0096(8) -0.0010(8) O1 0.021(3) 0.031(3) 0.030(2) -0.002(2) 0.0000(19) -0.001(2) O2 0.052(4) 0.049(4) 0.055(4) 0.001(3) 0.023(3) 0.013(3) O3 0.036(3) 0.040(3) 0.033(3) 0.005(3) 0.007(3) 0.007(2) N1 0.026(3) 0.016(3) 0.020(3) -0.001(2) 0.000(2) 0.002(2) N2 0.024(3) 0.022(3) 0.019(3) 0.003(2) 0.000(2) 0.002(2) N3 0.029(3) 0.022(3) 0.021(3) -0.001(2) 0.007(2) 0.006(2) N4 0.032(3) 0.017(3) 0.019(3) -0.001(2) 0.005(2) 0.003(2) N5 0.034(3) 0.026(3) 0.028(3) 0.000(2) 0.011(3) 0.003(3) N7 0.044(4) 0.030(3) 0.045(4) -0.003(3) 0.012(3) 0.005(3) C1 0.021(4) 0.020(3) 0.026(4) 0.005(3) -0.004(3) 0.007(3) C2 0.023(4) 0.026(3) 0.029(4) 0.006(3) 0.008(3) 0.003(3) C3 0.031(4) 0.018(3) 0.023(3) 0.006(3) 0.008(3) -0.001(3) C4 0.027(4) 0.024(3) 0.018(3) -0.001(3) -0.005(3) 0.001(3) C5 0.016(3) 0.021(3) 0.021(3) 0.003(3) 0.000(3) 0.003(3) C6 0.024(4) 0.020(3) 0.022(3) 0.006(3) 0.003(3) 0.010(3) C7 0.020(4) 0.017(3) 0.031(4) 0.001(3) 0.000(3) 0.009(3) C8 0.025(4) 0.022(3) 0.019(3) 0.007(3) 0.002(3) -0.004(3) C9 0.015(3) 0.029(4) 0.024(4) 0.007(3) 0.000(3) 0.002(3) C10 0.018(3) 0.017(3) 0.024(3) -0.003(3) 0.002(3) 0.012(3) C11 0.041(4) 0.025(4) 0.030(4) 0.005(3) 0.005(3) 0.001(3) C12 0.071(5) 0.029(4) 0.025(4) 0.008(3) -0.002(4) 0.007(4) C13 0.033(4) 0.023(4) 0.037(4) 0.006(3) -0.006(3) -0.002(3) C14 0.025(4) 0.016(3) 0.021(3) -0.005(3) 0.004(3) 0.003(3) C15 0.029(4) 0.025(4) 0.036(4) -0.005(3) 0.005(3) -0.004(3) C16 0.030(4) 0.014(3) 0.035(4) -0.003(3) 0.002(3) 0.000(3) C17 0.047(5) 0.026(4) 0.022(3) 0.003(3) 0.009(3) 0.004(3) C18 0.054(5) 0.033(4) 0.034(4) 0.007(3) 0.001(4) 0.003(4) C19 0.029(4) 0.030(4) 0.035(4) 0.003(3) 0.004(3) -0.009(3) C20 0.044(5) 0.023(4) 0.036(4) 0.001(3) 0.010(3) 0.000(3) C21 0.052(5) 0.051(5) 0.036(4) -0.025(4) 0.007(4) 0.005(4) C22 0.051(6) 0.054(5) 0.052(5) -0.017(4) 0.008(4) 0.012(4) C23 0.033(4) 0.029(4) 0.026(3) -0.001(3) 0.002(3) 0.002(3) C24 0.053(5) 0.038(4) 0.044(4) -0.010(3) 0.005(4) -0.006(4) _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 N1 2.136(4) . ? Co1 N1 2.136(4) 3_556 ? Co1 O1 2.141(4) 3_556 ? Co1 O1 2.141(4) . ? Co1 N4 2.145(4) 2_445 ? Co1 N4 2.145(4) 4_666 ? N1 C1 1.325(5) . ? N1 C2 1.391(6) . ? N2 C1 1.340(6) . ? N2 C3 1.362(6) . ? N2 C4 1.470(5) . ? N3 C14 1.343(6) . ? N3 C15 1.380(6) . ? N3 C13 1.471(6) . ? N4 C14 1.322(6) . ? N4 C16 1.390(6) . ? N4 Co1 2.145(4) 2_455 ? N5 C20 1.346(7) . ? N5 C21 1.381(6) . ? N5 C19 1.462(6) . ? N7 C20 1.331(7) . ? N7 C22 1.378(7) . ? C2 C3 1.353(6) . ? C4 C5 1.521(6) . ? C5 C10 1.398(6) . ? C5 C6 1.425(6) . ? C6 C7 1.385(7) . ? C6 C11 1.536(7) . ? C7 C8 1.397(7) . ? C7 C13 1.549(7) . ? C8 C9 1.405(7) . ? C8 C17 1.518(6) . ? C9 C10 1.404(7) . ? C9 C19 1.518(7) . ? C10 C23 1.523(6) . ? C11 C12 1.536(6) . ? C15 C16 1.360(6) . ? C17 C18 1.529(6) . ? C21 C22 1.336(8) . ? C23 C24 1.530(6) . ? 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 N1 Co1 N1 180.0(2) . 3_556 ? N1 Co1 O1 88.05(16) . 3_556 ? N1 Co1 O1 91.95(16) 3_556 3_556 ? N1 Co1 O1 91.95(16) . . ? N1 Co1 O1 88.05(16) 3_556 . ? O1 Co1 O1 180.0(2) 3_556 . ? N1 Co1 N4 90.84(14) . 2_445 ? N1 Co1 N4 89.16(14) 3_556 2_445 ? O1 Co1 N4 88.52(16) 3_556 2_445 ? O1 Co1 N4 91.48(16) . 2_445 ? N1 Co1 N4 89.16(14) . 4_666 ? N1 Co1 N4 90.84(14) 3_556 4_666 ? O1 Co1 N4 91.48(16) 3_556 4_666 ? O1 Co1 N4 88.52(16) . 4_666 ? N4 Co1 N4 180.00(7) 2_445 4_666 ? C1 N1 C2 105.5(4) . . ? C1 N1 Co1 127.6(4) . . ? C2 N1 Co1 127.0(4) . . ? C1 N2 C3 107.2(4) . . ? C1 N2 C4 126.2(5) . . ? C3 N2 C4 126.6(4) . . ? C14 N3 C15 107.5(5) . . ? C14 N3 C13 125.8(5) . . ? C15 N3 C13 126.6(5) . . ? C14 N4 C16 107.0(4) . . ? C14 N4 Co1 124.5(4) . 2_455 ? C16 N4 Co1 128.3(4) . 2_455 ? C20 N5 C21 105.1(5) . . ? C20 N5 C19 125.4(5) . . ? C21 N5 C19 129.3(5) . . ? C20 N7 C22 104.1(5) . . ? N1 C1 N2 111.4(5) . . ? C3 C2 N1 108.5(5) . . ? C2 C3 N2 107.4(5) . . ? N2 C4 C5 109.6(4) . . ? C10 C5 C6 120.6(5) . . ? C10 C5 C4 119.6(5) . . ? C6 C5 C4 119.5(5) . . ? C7 C6 C5 118.3(5) . . ? C7 C6 C11 121.9(5) . . ? C5 C6 C11 119.8(5) . . ? C6 C7 C8 122.5(5) . . ? C6 C7 C13 118.7(5) . . ? C8 C7 C13 118.8(5) . . ? C7 C8 C9 118.0(5) . . ? C7 C8 C17 122.1(5) . . ? C9 C8 C17 119.9(5) . . ? C10 C9 C8 121.4(5) . . ? C10 C9 C19 119.5(5) . . ? C8 C9 C19 118.9(5) . . ? C5 C10 C9 118.9(5) . . ? C5 C10 C23 121.5(5) . . ? C9 C10 C23 119.6(5) . . ? C6 C11 C12 114.1(5) . . ? N3 C13 C7 112.0(4) . . ? N4 C14 N3 110.6(5) . . ? C16 C15 N3 107.0(5) . . ? C15 C16 N4 107.9(5) . . ? C8 C17 C18 111.9(5) . . ? N5 C19 C9 109.8(4) . . ? N7 C20 N5 112.9(6) . . ? C22 C21 N5 107.6(5) . . ? C21 C22 N7 110.2(6) . . ? C10 C23 C24 111.8(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.488 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.069 # Attachment '- TIF3.cif' data_06kma039 _database_code_depnum_ccdc_archive 'CCDC 781850' #TrackingRef '- TIF3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 Co N12, 2(Cl) 22(H2O)' _chemical_formula_sum 'C48 H104 Cl2 Co N12 O22' _chemical_formula_weight 1331.27 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' _cell_length_a 11.8951(6) _cell_length_b 11.8951(6) _cell_length_c 39.232(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4807.3(6) _cell_formula_units_Z 3 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2139 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9185 _exptl_absorpt_correction_T_max 0.9580 _exptl_absorpt_process_details 'SADABS Blessing, Acta Cryst. A51 (1995) 33-38' _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 1k' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12154 _diffrn_reflns_av_R_equivalents 0.1420 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 29.14 _reflns_number_total 1630 _reflns_number_gt 1082 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _refine_special_details ; Refinement also possible in R-3 with similar R value but higher symmetry preferred. Some trouble with data collection as xtal moved part way through therefore only a limited number of frames were collected. Carbons 2 and 3 in the imidazole ring are almost certainly disordered over two sites however this disorder could not be modelled. In the X-ray structure six unique atom positions represent the 22 water molecules and two chloride anions per formula unit and hence it is not possible to uniquely identify the positions of the chloride anions which necessarily share sites with water molecules. However elemental analysis firmly establishes the fact that this is a chloride salt and not a hydroxide salt. 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^)+(0.1281P)^2^+13.9621P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1630 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.2307 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.0000 0.0000 0.5000 0.0105(4) Uani 1 12 d S . . O1 O 0.13506(16) 0.2701(3) 0.36873(8) 0.0204(8) Uani 1 2 d S . . O2 O 0.0000 0.0000 0.35017(19) 0.0364(17) Uani 1 6 d S . . O3 O 0.2120(2) 0.4241(4) 0.42938(9) 0.0337(10) Uani 1 2 d S . . O4 O 0.3333 0.6667 0.50429(19) 0.0411(18) Uani 1 6 d S . . O5 O 0.4508(2) 0.5492(2) 0.47475(11) 0.0426(11) Uani 1 2 d S . . O6 O 0.3333 0.6667 0.39283(18) 0.0364(17) Uani 1 6 d S . . N1 N 0.1747(4) 0.08733(19) 0.46941(9) 0.0219(9) Uani 1 2 d S . . N2 N 0.3260(4) 0.16300(19) 0.42937(9) 0.0175(9) Uani 1 2 d S . . C1 C 0.1994(5) 0.0997(2) 0.43702(10) 0.0172(9) Uani 1 2 d S . . H1 H 0.1332 0.0666 0.4201 0.021 Uiso 1 2 calc SR . . C2 C 0.2931(7) 0.1465(3) 0.48373(15) 0.127(6) Uani 1 2 d S . . H2 H 0.3086 0.1543 0.5076 0.152 Uiso 1 2 calc SR . . C3 C 0.3891(7) 0.1946(3) 0.45925(15) 0.111(5) Uani 1 2 d S . . H3 H 0.4803 0.2402 0.4628 0.133 Uiso 1 2 calc SR . . C4 C 0.3831(4) 0.1916(2) 0.39497(10) 0.0170(9) Uani 1 2 d S . . H4A H 0.3524 0.2435 0.3825 0.020 Uiso 0.50 1 calc PR . . H4B H 0.3524 0.1090 0.3825 0.020 Uiso 0.50 1 calc PR . . C5 C 0.5310(4) 0.2655(2) 0.39551(10) 0.0145(9) Uani 1 2 d S . . C6 C 0.5985(2) 0.1969(4) 0.39576(10) 0.0145(9) Uani 1 2 d S . . C7 C 0.5246(2) 0.0493(4) 0.39669(11) 0.0191(10) Uani 1 2 d S . . H7A H 0.4423 0.0191 0.4093 0.023 Uiso 0.50 1 calc PR . . H7B H 0.5768 0.0191 0.4093 0.023 Uiso 0.50 1 calc PR . . C8 C 0.4944(3) -0.0112(5) 0.36117(13) 0.0272(12) Uani 1 2 d S . . H8A H 0.4208 -0.0067 0.3515 0.041 Uiso 0.50 1 calc PR . . H8B H 0.4725 -0.1022 0.3627 0.041 Uiso 0.50 1 calc PR . . H8C H 0.5705 0.0364 0.3465 0.041 Uiso 0.50 1 calc 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 0.0112(5) 0.0112(5) 0.0091(7) 0.000 0.000 0.0056(3) O1 0.0136(12) 0.0182(18) 0.0311(17) -0.0055(13) -0.0028(7) 0.0091(9) O2 0.025(2) 0.025(2) 0.059(5) 0.000 0.000 0.0127(12) O3 0.0287(16) 0.046(3) 0.032(2) 0.0103(17) 0.0051(9) 0.0229(13) O4 0.041(3) 0.041(3) 0.042(4) 0.000 0.000 0.0203(14) O5 0.045(2) 0.045(2) 0.043(2) 0.0009(10) -0.0009(10) 0.026(2) O6 0.033(3) 0.033(3) 0.043(4) 0.000 0.000 0.0165(13) N1 0.011(2) 0.0316(19) 0.0163(18) -0.0002(7) -0.0004(14) 0.0054(10) N2 0.015(2) 0.0204(16) 0.0155(18) 0.0010(7) 0.0020(14) 0.0074(10) C1 0.011(2) 0.0216(19) 0.0154(19) -0.0006(8) -0.0012(16) 0.0056(11) C2 0.014(3) 0.269(14) 0.011(3) -0.0004(11) -0.001(2) 0.0072(16) C3 0.014(3) 0.231(13) 0.016(3) -0.0025(11) -0.005(2) 0.0068(16) C4 0.015(2) 0.0210(18) 0.0130(19) 0.0006(8) 0.0012(15) 0.0074(12) C5 0.013(2) 0.0175(17) 0.0113(18) 0.0000(7) 0.0000(15) 0.0067(11) C6 0.0176(17) 0.013(2) 0.0112(18) 0.0008(15) 0.0004(7) 0.0066(11) C7 0.0196(18) 0.010(2) 0.024(2) 0.0020(16) 0.0010(8) 0.0052(11) C8 0.028(2) 0.017(3) 0.033(3) -0.009(2) -0.0043(10) 0.0084(13) _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 N1 2.163(4) 21_556 ? Co1 N1 2.163(4) 19_556 ? Co1 N1 2.163(4) 20_556 ? Co1 N1 2.163(4) 3 ? Co1 N1 2.163(4) . ? Co1 N1 2.163(4) 2 ? N1 C1 1.296(5) . ? N1 C2 1.343(8) . ? N2 C1 1.338(6) . ? N2 C3 1.341(7) . ? N2 C4 1.472(5) . ? C2 C3 1.379(9) . ? C4 C5 1.523(6) . ? C5 C6 1.401(3) 3_665 ? C5 C6 1.401(3) . ? C6 C5 1.401(3) 2_655 ? C6 C7 1.522(6) . ? C7 C8 1.526(7) . ? 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 N1 Co1 N1 92.19(14) 21_556 19_556 ? N1 Co1 N1 92.19(14) 21_556 20_556 ? N1 Co1 N1 92.19(14) 19_556 20_556 ? N1 Co1 N1 180.000(1) 21_556 3 ? N1 Co1 N1 87.81(14) 19_556 3 ? N1 Co1 N1 87.81(14) 20_556 3 ? N1 Co1 N1 87.81(14) 21_556 . ? N1 Co1 N1 180.00(16) 19_556 . ? N1 Co1 N1 87.81(14) 20_556 . ? N1 Co1 N1 92.19(14) 3 . ? N1 Co1 N1 87.81(14) 21_556 2 ? N1 Co1 N1 87.81(14) 19_556 2 ? N1 Co1 N1 180.00(16) 20_556 2 ? N1 Co1 N1 92.19(14) 3 2 ? N1 Co1 N1 92.19(14) . 2 ? C1 N1 C2 103.4(4) . . ? C1 N1 Co1 135.0(3) . . ? C2 N1 Co1 121.6(3) . . ? C1 N2 C3 106.1(4) . . ? C1 N2 C4 126.5(4) . . ? C3 N2 C4 127.4(5) . . ? N1 C1 N2 114.3(4) . . ? N1 C2 C3 111.1(5) . . ? N2 C3 C2 105.1(5) . . ? N2 C4 C5 112.8(3) . . ? C6 C5 C6 120.5(4) 3_665 . ? C6 C5 C4 119.8(2) 3_665 . ? C6 C5 C4 119.8(2) . . ? C5 C6 C5 119.5(4) 2_655 . ? C5 C6 C7 120.3(2) 2_655 . ? C5 C6 C7 120.3(2) . . ? C6 C7 C8 112.7(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.138 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.113 # Attachment '- TIF4.cif' data_07srv139 _database_code_depnum_ccdc_archive 'CCDC 781851' #TrackingRef '- TIF4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 Co N12, Cl2, H2O ' _chemical_formula_sum 'C48 H62 Cl2 Co N12 O' _chemical_formula_weight 952.94 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' _cell_length_a 10.4800(3) _cell_length_b 10.4800(3) _cell_length_c 17.8377(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1696.65(13) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue-pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.9325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 485 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.446063 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS Blessing, Acta Cryst. A51 (1995) 33-38' _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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8737 _diffrn_reflns_av_R_equivalents 0.2153 _diffrn_reflns_av_sigmaI/netI 0.1814 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 24.97 _reflns_number_total 997 _reflns_number_gt 450 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _refine_special_details ; The compound is completely disordered over a mirror plane. CH2 and H2O hydrogens have been omitted from the refinement but are included in the molecular formula. The disorder does not disappear on attempting refinement in P63 The high R value arises from a combination of the difficulties in modlling the disorder and poor crystal quality. ISOR restraints used on most atoms to guide the refinement of the disorder. PLATON suggests space group P63/mmc however no solution in this space group could be found. 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^)+(0.2000P)^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_number_reflns 997 _refine_ls_number_parameters 87 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.2316 _refine_ls_R_factor_gt 0.1289 _refine_ls_wR_factor_ref 0.3939 _refine_ls_wR_factor_gt 0.3595 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.161 _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 Co1 Co 0.0000 0.0000 0.0000 0.0348(13) Uani 0.50 6 d SPU . 1 Cl1 Cl 0.0000 0.0000 0.3073(3) 0.068(2) Uani 0.50 3 d SPU . 2 O1 O 0.3333 -0.3333 0.2500 0.117(11) Uani 0.50 6 d SPU . . N1 N 0.1819(11) 0.1628(11) 0.0670(5) 0.035(2) Uani 0.50 1 d PU . 1 C1 C 0.1922(15) 0.1753(15) 0.1400(8) 0.045(3) Uani 0.50 1 d PU . 1 H1 H 0.1154 0.1173 0.1743 0.054 Uiso 0.50 1 calc PR . 1 N2 N 0.3315(12) 0.2857(11) 0.1596(5) 0.040(3) Uani 0.50 1 d PU . 1 C2 C 0.3142(15) 0.2602(14) 0.0403(7) 0.041(3) Uani 0.50 1 d PU . 1 H2 H 0.3383 0.2709 -0.0116 0.050 Uiso 0.50 1 calc PR . 1 C3 C 0.4108(16) 0.3421(17) 0.0947(7) 0.051(4) Uani 0.50 1 d PU . 1 H3 H 0.5096 0.4200 0.0893 0.061 Uiso 0.50 1 calc PR . 1 C4 C 0.3851(13) 0.3228(14) 0.2500 0.066(3) Uani 1 2 d SU . 1 C5 C 0.5288(12) 0.3285(12) 0.2500 0.050(3) Uani 1 2 d SU . 1 C6 C 0.5328(10) 0.1970(10) 0.2500 0.044(2) Uani 1 2 d SU . 1 C7 C 0.3909(13) 0.0492(14) 0.2500 0.066(3) Uani 1 2 d SU . 1 C8 C 0.364(3) -0.025(2) 0.1684(10) 0.087(6) Uani 0.50 1 d PU . 1 H8A H 0.3488 0.0361 0.1318 0.131 Uiso 0.50 1 calc PR . 1 H8B H 0.2759 -0.1235 0.1697 0.131 Uiso 0.50 1 calc PR . 1 H8C H 0.4494 -0.0333 0.1538 0.131 Uiso 0.50 1 calc PR . 1 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 0.0393(17) 0.0393(17) 0.026(2) 0.000 0.000 0.0197(9) Cl1 0.083(3) 0.083(3) 0.037(3) 0.000 0.000 0.0417(16) O1 0.104(13) 0.104(13) 0.14(2) 0.000 0.000 0.052(7) N1 0.037(6) 0.037(6) 0.031(5) 0.006(4) -0.001(4) 0.018(5) C1 0.042(8) 0.042(8) 0.059(9) -0.012(6) 0.001(6) 0.026(7) N2 0.038(6) 0.039(6) 0.038(5) -0.012(5) -0.008(5) 0.017(5) C2 0.046(8) 0.041(8) 0.023(6) 0.002(5) -0.005(6) 0.011(6) C3 0.043(8) 0.061(9) 0.047(8) -0.006(7) -0.003(7) 0.026(7) C4 0.049(7) 0.076(8) 0.087(8) 0.000 0.000 0.041(6) C5 0.062(7) 0.055(7) 0.038(5) 0.000 0.000 0.034(6) C6 0.048(6) 0.038(6) 0.038(5) 0.000 0.000 0.016(5) C7 0.057(7) 0.074(8) 0.067(7) 0.000 0.000 0.032(7) C8 0.119(15) 0.067(11) 0.100(12) -0.039(9) -0.059(11) 0.064(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 N1 2.173(10) 7 ? Co1 N1 2.173(10) . ? Co1 N1 2.173(10) 5 ? Co1 N1 2.173(10) 9 ? Co1 N1 2.173(10) 11 ? Co1 N1 2.173(10) 3 ? Cl1 Cl1 2.043(12) 8_556 ? N1 C1 1.307(16) . ? N1 C2 1.332(16) . ? C1 N2 1.380(17) . ? N2 C3 1.374(17) . ? N2 C4 1.689(10) . ? C2 C3 1.355(18) . ? C4 C5 1.477(15) . ? C4 N2 1.689(10) 10_556 ? C5 C6 1.400(14) . ? C5 C6 1.436(14) 8_666 ? C6 C5 1.436(14) 3_655 ? C6 C7 1.519(15) . ? C7 C8 1.609(17) . ? C7 C8 1.609(17) 10_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 N1 Co1 N1 180.0(4) 7 . ? N1 Co1 N1 87.3(3) 7 5 ? N1 Co1 N1 92.7(3) . 5 ? N1 Co1 N1 92.7(3) 7 9 ? N1 Co1 N1 87.3(3) . 9 ? N1 Co1 N1 87.3(3) 5 9 ? N1 Co1 N1 92.7(3) 7 11 ? N1 Co1 N1 87.3(3) . 11 ? N1 Co1 N1 180.0(7) 5 11 ? N1 Co1 N1 92.7(3) 9 11 ? N1 Co1 N1 87.3(3) 7 3 ? N1 Co1 N1 92.7(3) . 3 ? N1 Co1 N1 92.7(3) 5 3 ? N1 Co1 N1 180.0(6) 9 3 ? N1 Co1 N1 87.3(3) 11 3 ? C1 N1 C2 106.1(11) . . ? C1 N1 Co1 128.5(9) . . ? C2 N1 Co1 125.0(8) . . ? N1 C1 N2 109.6(12) . . ? C3 N2 C1 107.9(10) . . ? C3 N2 C4 130.2(11) . . ? C1 N2 C4 121.7(10) . . ? N1 C2 C3 113.0(12) . . ? C2 C3 N2 103.4(12) . . ? C5 C4 N2 102.9(5) . . ? C5 C4 N2 102.9(5) . 10_556 ? N2 C4 N2 145.7(11) . 10_556 ? C6 C5 C6 119.7(10) . 8_666 ? C6 C5 C4 119.5(10) . . ? C6 C5 C4 120.8(9) 8_666 . ? C5 C6 C5 120.3(10) . 3_655 ? C5 C6 C7 120.5(9) . . ? C5 C6 C7 119.2(9) 3_655 . ? C6 C7 C8 109.9(9) . . ? C6 C7 C8 109.9(9) . 10_556 ? C8 C7 C8 129.7(16) . 10_556 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.610 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.104 # Attachment '- TIF5.CIF' data_RBAR3M.CIF _database_code_depnum_ccdc_archive 'CCDC 781852' #TrackingRef '- TIF5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ni complex' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H104 Cl2 N12 Ni O22' _chemical_formula_weight 1331.04 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' _cell_length_a 11.8538(5) _cell_length_b 11.8538(5) _cell_length_c 38.991(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4744.7(6) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2142 _exptl_absorpt_coefficient_mu 0.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8907 _exptl_absorpt_correction_T_max 0.9323 _exptl_absorpt_process_details 'SADABS Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 1k' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8640 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.1047 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1350 _reflns_number_gt 964 _reflns_threshold_expression >2s(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material ? _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^)+(0.1011P)^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_number_reflns 1350 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Ni1 Ni 0.0000 0.0000 0.0000 0.0075(4) Uani 1 12 d S . . N2 N 0.16231(18) 0.3246(4) 0.07002(8) 0.0153(8) Uani 1 2 d S . . N1 N 0.08572(19) 0.1714(4) 0.03009(9) 0.0228(10) Uani 1 2 d S . . C7 C 0.0488(4) 0.5244(2) 0.10304(11) 0.0170(10) Uani 1 2 d S . . H7A H 0.0180 0.4415 0.0905 0.020 Uiso 0.50 1 calc PR . . H7B H 0.0180 0.5765 0.0905 0.020 Uiso 0.50 1 calc PR . . C1 C 0.0988(2) 0.1975(4) 0.06246(10) 0.0140(9) Uani 1 2 d S . . H1 H 0.0658 0.1317 0.0796 0.017 Uiso 1 2 calc SR . . C6 C 0.1958(4) 0.5979(2) 0.10358(9) 0.0116(9) Uani 1 2 d S . . C8 C -0.0102(5) 0.4949(2) 0.13870(12) 0.0238(11) Uani 1 2 d S . . H8A H 0.0282 0.4530 0.1523 0.036 Uiso 0.50 1 calc PR . . H8B H -0.1046 0.4364 0.1370 0.036 Uiso 0.50 1 calc PR . . H8C H 0.0076 0.5762 0.1499 0.036 Uiso 0.50 1 calc PR . . C4 C 0.1912(2) 0.3823(4) 0.10464(10) 0.0145(9) Uani 1 2 d S . . H4A H 0.2434 0.3518 0.1172 0.017 Uiso 0.50 1 calc PR . . H4B H 0.1084 0.3518 0.1172 0.017 Uiso 0.50 1 calc PR . . C5 C 0.2652(2) 0.5304(4) 0.10386(10) 0.0108(9) Uani 1 2 d S . . O1 O -0.13497(14) 0.13497(14) 0.13089(7) 0.0125(7) Uani 1 2 d S . . O2 O -0.3333 0.3333 0.18274(17) 0.0331(16) Uani 1 6 d S . . O3 O -0.21267(19) 0.21267(19) 0.07003(9) 0.0306(9) Uani 1 2 d S . . O4 O -0.1008(4) 0.4496(2) 0.02431(9) 0.0398(11) Uani 1 2 d S . . O5 O -0.3333 0.3333 0.10681(16) 0.0328(16) Uani 1 6 d S . . O6 O 0.3333 0.6667 0.00579(18) 0.049(2) Uani 1 6 d S . . C3 C 0.2336(6) 0.3859(6) 0.03995(15) 0.0208(15) Uani 0.50 1 d P . 1 C2 C 0.1890(6) 0.2910(6) 0.01552(14) 0.0205(14) Uani 0.50 1 d P . 1 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 Ni1 0.0081(5) 0.0081(5) 0.0063(6) 0.000 0.000 0.0041(2) N2 0.0183(16) 0.012(2) 0.0132(16) -0.0017(14) -0.0009(7) 0.0062(10) N1 0.036(2) 0.010(2) 0.0132(18) 0.0000(14) 0.0000(7) 0.0050(10) C7 0.011(2) 0.0177(18) 0.020(2) -0.0011(8) -0.0022(17) 0.0055(11) C1 0.0157(17) 0.009(2) 0.0151(19) 0.0024(16) 0.0012(8) 0.0044(11) C6 0.010(2) 0.0161(17) 0.0065(17) 0.0001(7) 0.0002(14) 0.0052(11) C8 0.016(3) 0.024(2) 0.029(2) 0.0038(10) 0.0076(19) 0.0079(13) C4 0.0188(17) 0.015(2) 0.0087(18) -0.0004(16) -0.0002(8) 0.0074(12) C5 0.0140(17) 0.008(2) 0.0085(17) -0.0003(15) -0.0002(7) 0.0040(10) O1 0.0057(11) 0.0057(11) 0.0234(15) 0.0024(6) -0.0024(6) 0.0008(12) O2 0.023(2) 0.023(2) 0.054(4) 0.000 0.000 0.0115(11) O3 0.0230(14) 0.0230(14) 0.0337(19) -0.0068(8) 0.0068(8) 0.0024(17) O4 0.040(3) 0.0407(19) 0.038(2) 0.0037(9) 0.0073(18) 0.0202(13) O5 0.032(2) 0.032(2) 0.035(3) 0.000 0.000 0.0158(12) O6 0.050(3) 0.050(3) 0.048(4) 0.000 0.000 0.0252(16) C3 0.025(4) 0.009(3) 0.016(3) 0.003(2) 0.001(2) -0.001(3) C2 0.024(3) 0.013(3) 0.017(3) 0.000(2) 0.001(2) 0.003(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 Ni1 N1 2.115(4) . ? Ni1 N1 2.115(4) 2 ? Ni1 N1 2.115(4) 3 ? Ni1 N1 2.115(4) 19 ? Ni1 N1 2.115(4) 21 ? Ni1 N1 2.115(4) 20 ? N2 C1 1.338(6) . ? N2 C3 1.415(6) 22 ? N2 C3 1.415(6) . ? N2 C4 1.474(5) . ? N1 C1 1.290(5) . ? N1 C2 1.447(7) . ? N1 C2 1.447(7) 22 ? C7 C6 1.509(6) . ? C7 C8 1.517(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C1 H1 0.9500 . ? C6 C5 1.406(3) 3_565 ? C6 C5 1.406(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C4 C5 1.520(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.406(3) 2_665 ? C3 C3 0.964(14) 22 ? C3 C2 1.363(8) . ? C3 C2 1.688(9) 22 ? C2 C2 1.030(14) 22 ? C2 C3 1.688(9) 22 ? 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 N1 Ni1 N1 92.20(14) . 2 ? N1 Ni1 N1 92.20(14) . 3 ? N1 Ni1 N1 92.20(14) 2 3 ? N1 Ni1 N1 180.0(2) . 19 ? N1 Ni1 N1 87.80(14) 2 19 ? N1 Ni1 N1 87.80(14) 3 19 ? N1 Ni1 N1 87.80(14) . 21 ? N1 Ni1 N1 87.80(14) 2 21 ? N1 Ni1 N1 180.00(18) 3 21 ? N1 Ni1 N1 92.20(14) 19 21 ? N1 Ni1 N1 87.80(14) . 20 ? N1 Ni1 N1 180.0(2) 2 20 ? N1 Ni1 N1 87.80(14) 3 20 ? N1 Ni1 N1 92.20(14) 19 20 ? N1 Ni1 N1 92.20(14) 21 20 ? C1 N2 C3 104.5(4) . 22 ? C1 N2 C3 104.5(4) . . ? C3 N2 C3 39.8(6) 22 . ? C1 N2 C4 126.4(4) . . ? C3 N2 C4 125.5(4) 22 . ? C3 N2 C4 125.5(4) . . ? C1 N1 C2 102.0(4) . . ? C1 N1 C2 102.0(4) . 22 ? C2 N1 C2 41.7(5) . 22 ? C1 N1 Ni1 135.7(3) . . ? C2 N1 Ni1 119.2(3) . . ? C2 N1 Ni1 119.2(3) 22 . ? C6 C7 C8 112.8(4) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N1 C1 N2 114.7(4) . . ? N1 C1 H1 122.6 . . ? N2 C1 H1 122.6 . . ? C5 C6 C5 119.1(4) 3_565 . ? C5 C6 C7 120.5(2) 3_565 . ? C5 C6 C7 120.5(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C4 C5 112.5(3) . . ? N2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C6 120.9(4) 2_665 . ? C6 C5 C4 119.5(2) 2_665 . ? C6 C5 C4 119.5(2) . . ? C3 C3 C2 91.4(4) 22 . ? C3 C3 N2 70.1(3) 22 . ? C2 C3 N2 105.7(5) . . ? C3 C3 C2 53.8(3) 22 22 ? C2 C3 C2 37.6(5) . 22 ? N2 C3 C2 90.6(4) . 22 ? C2 C2 C3 88.6(4) 22 . ? C2 C2 N1 69.1(3) 22 . ? C3 C2 N1 108.8(5) . . ? C2 C2 C3 53.8(3) 22 22 ? C3 C2 C3 34.8(5) . 22 ? N1 C2 C3 93.3(4) . 22 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.283 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.103 # Attachment '- TIF6.CIF' data_08srv077 _database_code_depnum_ccdc_archive 'CCDC 781853' #TrackingRef '- TIF6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 08srv077 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Cl2 Mn N6' _chemical_formula_weight 528.38 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.675(4) _cell_length_b 20.932(7) _cell_length_c 9.027(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.544(14) _cell_angle_gamma 90.00 _cell_volume 2392.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8499 _exptl_absorpt_correction_T_max 0.9314 _exptl_absorpt_process_details 'SADABS Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; Multiple crystals resulting in some poor ADPs and high R-factor ISOR restraints used for N6 C15 which displayed a tendency to become NPD ; _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 1K' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12562 _diffrn_reflns_av_R_equivalents 0.1211 _diffrn_reflns_av_sigmaI/netI 0.1521 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4178 _reflns_number_gt 2798 _reflns_threshold_expression >2s(I) _computing_data_collection 'Bruker Software' _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 X-Seed _computing_publication_material ? _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. The high residuals are due to crystal twinning and no suitable twin law was found using Gemini. The large residual peaks near the heavy atoms arise from the twinning While precision i spoor, the structural details are unambiguous. ; _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^)+(0.0625P)^2^+97.8626P] 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 SHELXL _refine_ls_extinction_coef 0.0046(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4178 _refine_ls_number_parameters 299 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1894 _refine_ls_R_factor_gt 0.1509 _refine_ls_wR_factor_ref 0.3696 _refine_ls_wR_factor_gt 0.3500 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.097 _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 Mn1 Mn 0.74908(15) 0.11299(9) 0.4320(2) 0.0144(6) Uani 1 1 d . . . Cl1 Cl 0.7376(3) 0.22783(15) 0.3757(4) 0.0258(9) Uani 1 1 d . . . N1 N 0.7486(8) 0.0891(5) 0.1916(12) 0.019(2) Uani 1 1 d . . . C1 C 0.7509(10) 0.0311(6) 0.1284(16) 0.018(3) Uani 1 1 d . . . H1 H 0.7530 -0.0077 0.1832 0.021 Uiso 1 1 calc R . . Cl2 Cl 0.7572(3) -0.00440(15) 0.4826(4) 0.0214(8) Uani 1 1 d . . . N2 N 0.7499(8) 0.0334(5) -0.0171(12) 0.015(2) Uani 1 1 d . . . C2 C 0.7439(11) 0.1300(7) 0.0746(17) 0.024(3) Uani 1 1 d . . . H2 H 0.7405 0.1752 0.0832 0.029 Uiso 1 1 calc R . . N3 N 1.1051(9) -0.1289(5) 0.4352(14) 0.024(3) Uani 1 1 d . . . C3 C 0.7448(11) 0.0975(6) -0.0577(19) 0.027(3) Uani 1 1 d . . . H3 H 0.7425 0.1149 -0.1550 0.032 Uiso 1 1 calc R . . N4 N 0.9847(9) -0.1666(6) 0.2759(12) 0.022(3) Uani 1 1 d . . . C4 C 0.7517(11) -0.0205(6) -0.1257(16) 0.021(3) Uani 1 1 d . . . H4A H 0.8177 -0.0189 -0.1802 0.025 Uiso 1 1 calc R . . H4B H 0.6913 -0.0166 -0.1985 0.025 Uiso 1 1 calc R . . N5 N 0.3874(9) -0.1221(5) 0.4218(13) 0.023(3) Uani 1 1 d . . . C5 C 0.7450(11) -0.0840(6) -0.0423(15) 0.019(3) Uani 1 1 d . . . N6 N 0.4953(9) -0.1530(5) 0.2511(12) 0.018(2) Uani 1 1 d U . . C6 C 0.8406(11) -0.1143(6) 0.0087(17) 0.023(3) Uani 1 1 d . . . C7 C 0.9435(11) -0.0871(7) -0.0323(17) 0.028(3) Uani 1 1 d . . . H7A H 0.9985 -0.0996 0.0434 0.033 Uiso 1 1 calc R . . H7B H 0.9385 -0.0399 -0.0323 0.033 Uiso 1 1 calc R . . C8 C 0.9766(12) -0.1097(9) -0.1850(17) 0.039(4) Uani 1 1 d . . . H8A H 1.0447 -0.0905 -0.2068 0.059 Uiso 1 1 calc R . . H8B H 0.9232 -0.0966 -0.2608 0.059 Uiso 1 1 calc R . . H8C H 0.9830 -0.1563 -0.1851 0.059 Uiso 1 1 calc R . . C9 C 0.8336(11) -0.1717(6) 0.0920(15) 0.021(3) Uani 1 1 d . . . C10 C 0.9372(12) -0.2012(7) 0.1487(17) 0.028(3) Uani 1 1 d . . . H10A H 0.9247 -0.2461 0.1777 0.034 Uiso 1 1 calc R . . H10B H 0.9874 -0.2015 0.0677 0.034 Uiso 1 1 calc R . . C11 C 1.0818(11) -0.1736(7) 0.3339(15) 0.024(3) Uani 1 1 d . . . H11 H 1.1290 -0.2064 0.3068 0.028 Uiso 1 1 calc R . . C12 C 1.0145(11) -0.0925(7) 0.4406(16) 0.027(3) Uani 1 1 d . . . H12 H 1.0071 -0.0562 0.5024 0.032 Uiso 1 1 calc R . . C13 C 0.9373(13) -0.1155(7) 0.3458(17) 0.032(4) Uani 1 1 d . . . H13 H 0.8671 -0.1003 0.3308 0.038 Uiso 1 1 calc R . . C14 C 0.7342(11) -0.1958(7) 0.1258(16) 0.023(3) Uani 1 1 d . . . C15 C 0.7306(11) -0.2592(6) 0.2145(14) 0.019(3) Uani 1 1 d U . . H15A H 0.7919 -0.2616 0.2861 0.023 Uiso 1 1 calc R . . H15B H 0.6653 -0.2609 0.2707 0.023 Uiso 1 1 calc R . . C16 C 0.7329(12) -0.3155(7) 0.1075(15) 0.024(3) Uani 1 1 d . . . H16A H 0.7307 -0.3556 0.1633 0.037 Uiso 1 1 calc R . . H16B H 0.7978 -0.3138 0.0526 0.037 Uiso 1 1 calc R . . H16C H 0.6716 -0.3132 0.0376 0.037 Uiso 1 1 calc R . . C17 C 0.6410(11) -0.1660(6) 0.0774(17) 0.024(3) Uani 1 1 d . . . C18 C 0.5335(12) -0.1896(7) 0.1224(17) 0.028(3) Uani 1 1 d . . . H18A H 0.4819 -0.1852 0.0373 0.033 Uiso 1 1 calc R . . H18B H 0.5383 -0.2355 0.1486 0.033 Uiso 1 1 calc R . . C19 C 0.4143(10) -0.1693(6) 0.3354(14) 0.017(3) Uani 1 1 d . . . H19 H 0.3808 -0.2099 0.3327 0.021 Uiso 1 1 calc R . . C20 C 0.4518(12) -0.0708(7) 0.3899(16) 0.029(3) Uani 1 1 d . . . H20 H 0.4492 -0.0298 0.4346 0.035 Uiso 1 1 calc R . . C21 C 0.5189(12) -0.0885(7) 0.2850(16) 0.028(3) Uani 1 1 d . . . H21 H 0.5714 -0.0628 0.2426 0.034 Uiso 1 1 calc R . . C22 C 0.6467(10) -0.1100(6) -0.0103(14) 0.017(3) Uani 1 1 d . . . C23 C 0.5452(11) -0.0782(6) -0.0732(16) 0.022(3) Uani 1 1 d . . . H23A H 0.5537 -0.0312 -0.0679 0.027 Uiso 1 1 calc R . . H23B H 0.4861 -0.0900 -0.0104 0.027 Uiso 1 1 calc R . . C24 C 0.5164(11) -0.0972(7) -0.2345(16) 0.024(3) Uani 1 1 d . . . H24A H 0.4517 -0.0751 -0.2685 0.036 Uiso 1 1 calc R . . H24B H 0.5051 -0.1435 -0.2402 0.036 Uiso 1 1 calc R . . H24C H 0.5742 -0.0853 -0.2977 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 Mn1 0.0156(10) 0.0104(10) 0.0171(11) 0.0006(7) -0.0005(7) 0.0008(7) Cl1 0.043(2) 0.0102(16) 0.0247(19) 0.0017(13) 0.0051(15) 0.0000(14) N1 0.014(6) 0.019(6) 0.024(6) -0.007(5) -0.004(5) -0.004(4) C1 0.017(7) 0.004(6) 0.033(8) 0.008(5) 0.000(6) -0.003(5) Cl2 0.0350(19) 0.0137(16) 0.0158(17) 0.0006(12) 0.0044(14) 0.0011(13) N2 0.019(6) 0.004(5) 0.021(6) 0.003(4) 0.000(5) 0.001(4) C2 0.018(7) 0.017(7) 0.037(9) 0.008(6) 0.005(6) 0.002(6) N3 0.013(6) 0.020(6) 0.040(8) 0.000(5) -0.003(5) 0.004(5) C3 0.020(7) 0.009(7) 0.052(10) 0.011(6) -0.001(6) -0.003(5) N4 0.020(6) 0.029(7) 0.018(6) -0.003(5) -0.003(5) 0.007(5) C4 0.028(8) 0.008(6) 0.026(8) -0.006(5) 0.000(6) -0.004(5) N5 0.030(7) 0.008(6) 0.031(7) 0.000(5) 0.009(5) 0.002(5) C5 0.020(7) 0.015(7) 0.023(8) -0.001(5) -0.002(6) 0.002(5) N6 0.022(4) 0.013(4) 0.019(4) -0.004(3) 0.002(3) -0.009(3) C6 0.019(7) 0.014(7) 0.037(9) -0.001(6) 0.004(6) -0.004(5) C7 0.018(7) 0.025(8) 0.040(9) 0.000(6) 0.006(6) -0.004(6) C8 0.021(8) 0.070(13) 0.027(9) -0.007(8) 0.000(7) -0.011(8) C9 0.026(8) 0.016(7) 0.019(7) 0.001(5) -0.002(6) 0.008(6) C10 0.026(8) 0.022(8) 0.036(9) -0.003(6) -0.006(6) 0.004(6) C11 0.020(7) 0.029(8) 0.022(8) -0.001(6) -0.001(6) -0.006(6) C12 0.025(8) 0.030(8) 0.024(8) -0.009(6) -0.003(6) 0.014(6) C13 0.037(9) 0.029(9) 0.030(9) -0.003(7) 0.001(7) 0.013(7) C14 0.022(7) 0.019(7) 0.027(8) 0.002(6) 0.005(6) -0.003(6) C15 0.024(5) 0.019(5) 0.015(4) 0.000(4) 0.006(4) -0.001(4) C16 0.038(9) 0.019(7) 0.017(7) -0.004(5) 0.002(6) -0.004(6) C17 0.023(7) 0.010(7) 0.041(9) -0.002(6) 0.011(6) 0.003(5) C18 0.028(8) 0.029(8) 0.027(8) -0.004(6) 0.009(6) -0.010(6) C19 0.015(6) 0.017(7) 0.020(7) 0.003(5) 0.001(5) -0.003(5) C20 0.039(9) 0.022(8) 0.025(8) -0.003(6) 0.006(7) -0.012(7) C21 0.034(9) 0.025(8) 0.027(8) -0.008(6) 0.007(7) -0.012(6) C22 0.020(7) 0.012(6) 0.018(7) -0.005(5) 0.002(5) -0.001(5) C23 0.022(7) 0.013(7) 0.033(8) 0.004(6) 0.010(6) 0.016(5) C24 0.016(7) 0.027(8) 0.028(8) 0.004(6) -0.005(6) 0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N3 2.183(12) 3_756 ? Mn1 N1 2.226(11) . ? Mn1 N5 2.231(11) 3_656 ? Mn1 Cl1 2.460(4) . ? Mn1 Cl2 2.501(4) . ? N1 C1 1.343(17) . ? N1 C2 1.359(18) . ? C1 N2 1.314(17) . ? N2 C3 1.390(16) . ? N2 C4 1.496(16) . ? C2 C3 1.38(2) . ? N3 C11 1.333(18) . ? N3 C12 1.380(17) . ? N3 Mn1 2.183(12) 3_756 ? N4 C11 1.325(18) . ? N4 C13 1.391(18) . ? N4 C10 1.464(18) . ? C4 C5 1.533(18) . ? N5 C19 1.313(17) . ? N5 C20 1.385(18) . ? N5 Mn1 2.231(11) 3_656 ? C5 C22 1.400(18) . ? C5 C6 1.427(19) . ? N6 C19 1.349(16) . ? N6 C21 1.413(17) . ? N6 C18 1.489(17) . ? C6 C9 1.423(19) . ? C6 C7 1.484(18) . ? C7 C8 1.53(2) . ? C9 C14 1.402(19) . ? C9 C10 1.519(19) . ? C12 C13 1.36(2) . ? C14 C17 1.39(2) . ? C14 C15 1.552(18) . ? C15 C16 1.523(18) . ? C17 C22 1.420(19) . ? C17 C18 1.522(19) . ? C20 C21 1.35(2) . ? C22 C23 1.535(18) . ? C23 C24 1.54(2) . ? 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 N3 Mn1 N1 122.4(4) 3_756 . ? N3 Mn1 N5 108.8(5) 3_756 3_656 ? N1 Mn1 N5 128.8(4) . 3_656 ? N3 Mn1 Cl1 90.3(3) 3_756 . ? N1 Mn1 Cl1 91.2(3) . . ? N5 Mn1 Cl1 89.9(3) 3_656 . ? N3 Mn1 Cl2 91.3(3) 3_756 . ? N1 Mn1 Cl2 87.4(3) . . ? N5 Mn1 Cl2 90.1(3) 3_656 . ? Cl1 Mn1 Cl2 178.31(15) . . ? C1 N1 C2 103.9(11) . . ? C1 N1 Mn1 128.2(9) . . ? C2 N1 Mn1 127.9(9) . . ? N2 C1 N1 113.0(11) . . ? C1 N2 C3 107.4(11) . . ? C1 N2 C4 128.8(10) . . ? C3 N2 C4 123.8(12) . . ? N1 C2 C3 111.2(12) . . ? C11 N3 C12 104.6(12) . . ? C11 N3 Mn1 129.8(9) . 3_756 ? C12 N3 Mn1 125.6(10) . 3_756 ? C2 C3 N2 104.5(13) . . ? C11 N4 C13 108.5(12) . . ? C11 N4 C10 126.7(12) . . ? C13 N4 C10 124.4(12) . . ? N2 C4 C5 109.3(11) . . ? C19 N5 C20 106.8(11) . . ? C19 N5 Mn1 130.1(9) . 3_656 ? C20 N5 Mn1 122.4(9) . 3_656 ? C22 C5 C6 120.8(12) . . ? C22 C5 C4 120.5(12) . . ? C6 C5 C4 118.6(12) . . ? C19 N6 C21 106.1(11) . . ? C19 N6 C18 126.3(11) . . ? C21 N6 C18 125.9(11) . . ? C9 C6 C5 118.3(12) . . ? C9 C6 C7 122.2(13) . . ? C5 C6 C7 119.5(13) . . ? C6 C7 C8 112.6(13) . . ? C14 C9 C6 119.8(12) . . ? C14 C9 C10 123.5(12) . . ? C6 C9 C10 116.6(13) . . ? N4 C10 C9 112.4(12) . . ? N4 C11 N3 111.5(13) . . ? C13 C12 N3 111.1(13) . . ? C12 C13 N4 104.2(13) . . ? C17 C14 C9 122.0(13) . . ? C17 C14 C15 120.1(12) . . ? C9 C14 C15 117.8(12) . . ? C16 C15 C14 109.4(11) . . ? C14 C17 C22 118.9(12) . . ? C14 C17 C18 122.0(13) . . ? C22 C17 C18 119.0(13) . . ? N6 C18 C17 111.5(11) . . ? N5 C19 N6 111.7(11) . . ? C21 C20 N5 109.1(13) . . ? C20 C21 N6 106.3(12) . . ? C5 C22 C17 120.2(12) . . ? C5 C22 C23 119.7(12) . . ? C17 C22 C23 120.1(12) . . ? C22 C23 C24 113.4(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.346 _refine_diff_density_min -1.117 _refine_diff_density_rms 0.220 # Attachment '- TIF7.CIF' data_PNA21.CIF _database_code_depnum_ccdc_archive 'CCDC 781854' #TrackingRef '- TIF7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cd Complex' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Cd Cl2 N6' _chemical_formula_weight 585.84 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 9.1574(12) _cell_length_b 21.172(3) _cell_length_c 12.8437(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2490.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8076 _exptl_absorpt_correction_T_max 0.8966 _exptl_absorpt_process_details 'SADABS Blessing, Acta Cryst. A51 (1995) 33-38' _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 1K' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10792 _diffrn_reflns_av_R_equivalents 0.1492 _diffrn_reflns_av_sigmaI/netI 0.2171 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2931 _reflns_number_gt 1252 _reflns_threshold_expression >2s(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material ? _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^)+(0.0095P)^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_number_reflns 2931 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1525 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 0.764 _refine_ls_restrained_S_all 0.764 _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 Cd1 Cd 0.43135(8) 0.61430(4) 0.2500 0.0356(2) Uani 1 2 d S . . Cl1 Cl 0.4910(3) 0.49409(11) 0.2500 0.0372(6) Uani 1 2 d S . . Cl2 Cl 0.3696(3) 0.73149(12) 0.2500 0.0570(8) Uani 1 2 d S . . N12 N 0.4332(7) 0.3708(3) -0.1034(4) 0.0467(16) Uani 1 1 d . . . N15 N -0.0145(10) 0.5306(4) 0.2500 0.047(2) Uani 1 2 d S . . N19 N 0.1887(9) 0.5882(4) 0.2500 0.040(2) Uani 1 2 d S . . N24 N 0.2707(6) 0.3381(3) 0.0115(4) 0.0388(16) Uani 1 1 d . . . C1 C 0.1324(13) 0.5301(5) 0.2500 0.051(3) Uani 1 2 d S . . H1 H 0.1895 0.4926 0.2500 0.061 Uiso 1 2 calc SR . . C2 C 0.0698(13) 0.6279(5) 0.2500 0.046(3) Uani 1 2 d S . . H2 H 0.0741 0.6727 0.2500 0.055 Uiso 1 2 calc SR . . C3 C -0.0562(14) 0.5926(5) 0.2500 0.058(3) Uani 1 2 d S . . H3 H -0.1535 0.6083 0.2500 0.069 Uiso 1 2 calc SR . . C4 C -0.1150(12) 0.4751(5) 0.2500 0.059(3) Uani 1 2 d S . . H4A H -0.1784 0.4769 0.1876 0.071 Uiso 0.50 1 calc PR . . H4B H -0.1784 0.4769 0.3124 0.071 Uiso 0.50 1 calc PR . . C5 C -0.0315(10) 0.4138(4) 0.2500 0.034(3) Uani 1 2 d S . . C6 C 0.0117(7) 0.3860(4) 0.1544(5) 0.0421(19) Uani 1 1 d . . . C7 C -0.0355(8) 0.4172(4) 0.0533(5) 0.063(3) Uani 1 1 d . . . H7A H -0.0339 0.4636 0.0619 0.076 Uiso 1 1 calc R . . H7B H 0.0345 0.4060 -0.0025 0.076 Uiso 1 1 calc R . . C8 C -0.1878(10) 0.3964(5) 0.0215(5) 0.109(4) Uani 1 1 d . . . H8A H -0.1864 0.3514 0.0035 0.164 Uiso 1 1 calc R . . H8B H -0.2198 0.4210 -0.0390 0.164 Uiso 1 1 calc R . . H8C H -0.2555 0.4033 0.0795 0.164 Uiso 1 1 calc R . . C9 C 0.0928(8) 0.3308(3) 0.1550(5) 0.0355(18) Uani 1 1 d . . . C10 C 0.1440(8) 0.3037(3) 0.0525(5) 0.052(2) Uani 1 1 d . . . H10A H 0.1703 0.2588 0.0623 0.063 Uiso 1 1 calc R . . H10B H 0.0633 0.3058 0.0013 0.063 Uiso 1 1 calc R . . C11 C 0.3365(8) 0.3281(4) -0.0812(5) 0.045(2) Uani 1 1 d . . . H11 H 0.3143 0.2934 -0.1254 0.054 Uiso 1 1 calc R . . C12 C 0.4363(9) 0.4112(3) -0.0185(6) 0.060(2) Uani 1 1 d . . . H12 H 0.4965 0.4475 -0.0116 0.072 Uiso 1 1 calc R . . C13 C 0.3390(8) 0.3901(4) 0.0531(6) 0.060(2) Uani 1 1 d . . . H13 H 0.3213 0.4080 0.1198 0.072 Uiso 1 1 calc R . . C14 C 0.1347(11) 0.3055(5) 0.2500 0.042(3) Uani 1 2 d S . . C15 C 0.2253(12) 0.2426(5) 0.2500 0.059(3) Uani 1 2 d S . . H15A H 0.2887 0.2413 0.1876 0.071 Uiso 0.50 1 calc PR . . H15B H 0.2887 0.2413 0.3124 0.071 Uiso 0.50 1 calc PR . . C16 C 0.1225(12) 0.1846(5) 0.2500 0.061(3) Uani 1 2 d S . . H16A H 0.1808 0.1458 0.2500 0.091 Uiso 1 2 calc SR . . H16B H 0.0607 0.1856 0.1877 0.091 Uiso 0.50 1 calc PR . . H16C H 0.0607 0.1856 0.3123 0.091 Uiso 0.50 1 calc 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 Cd1 0.0349(5) 0.0360(4) 0.0359(4) 0.000 0.000 -0.0020(4) Cl1 0.0347(16) 0.0303(15) 0.0466(15) 0.000 0.000 0.0015(12) Cl2 0.047(2) 0.0344(17) 0.089(2) 0.000 0.000 0.0051(14) N12 0.049(4) 0.045(4) 0.047(4) -0.012(3) 0.004(3) -0.007(4) N15 0.040(7) 0.040(6) 0.060(6) 0.000 0.000 0.007(5) N19 0.029(6) 0.041(6) 0.050(6) 0.000 0.000 0.001(5) N24 0.043(4) 0.046(4) 0.028(4) -0.011(3) 0.001(3) -0.011(3) C1 0.044(8) 0.044(8) 0.064(8) 0.000 0.000 0.003(7) C2 0.052(8) 0.030(7) 0.055(7) 0.000 0.000 0.001(7) C3 0.073(10) 0.036(7) 0.064(8) 0.000 0.000 0.031(7) C4 0.052(9) 0.048(8) 0.077(9) 0.000 0.000 -0.014(7) C5 0.029(7) 0.025(6) 0.049(7) 0.000 0.000 0.000(5) C6 0.037(5) 0.052(5) 0.037(5) 0.006(4) -0.006(3) -0.012(4) C7 0.048(7) 0.085(7) 0.056(5) 0.021(4) -0.019(4) -0.009(5) C8 0.078(8) 0.188(11) 0.061(6) 0.057(7) -0.034(5) -0.035(8) C9 0.043(5) 0.035(4) 0.028(4) 0.002(4) 0.000(4) -0.005(4) C10 0.060(6) 0.062(6) 0.036(5) -0.012(4) 0.008(4) -0.026(5) C11 0.059(6) 0.051(5) 0.025(4) -0.008(4) 0.000(4) -0.015(4) C12 0.045(6) 0.063(6) 0.072(6) -0.010(5) 0.007(5) -0.026(5) C13 0.047(6) 0.076(7) 0.056(5) -0.010(5) 0.015(4) -0.018(5) C14 0.047(8) 0.036(7) 0.043(7) 0.000 0.000 -0.013(6) C15 0.045(9) 0.071(9) 0.062(8) 0.000 0.000 -0.010(7) C16 0.053(9) 0.037(8) 0.093(9) 0.000 0.000 0.008(6) _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 Cd1 N12 2.277(6) 2_665 ? Cd1 N12 2.277(6) 5_665 ? Cd1 N19 2.290(8) . ? Cd1 Cl2 2.545(3) . ? Cd1 Cl1 2.603(2) . ? N12 C11 1.298(8) . ? N12 C12 1.386(7) . ? N12 Cd1 2.277(6) 5_665 ? N15 C1 1.345(11) . ? N15 C3 1.367(11) . ? N15 C4 1.493(12) . ? N19 C1 1.335(12) . ? N19 C2 1.375(12) . ? N24 C11 1.351(7) . ? N24 C13 1.374(8) . ? N24 C10 1.468(8) . ? C2 C3 1.375(14) . ? C4 C5 1.506(12) . ? C5 C6 1.418(8) . ? C5 C6 1.418(8) 6_556 ? C6 C9 1.384(9) . ? C6 C7 1.520(8) . ? C7 C8 1.518(9) . ? C9 C14 1.387(8) . ? C9 C10 1.510(8) . ? C12 C13 1.356(9) . ? C14 C9 1.387(8) 6_556 ? C14 C15 1.570(13) . ? C15 C16 1.548(12) . ? 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 N12 Cd1 N12 111.6(3) 2_665 5_665 ? N12 Cd1 N19 124.21(15) 2_665 . ? N12 Cd1 N19 124.21(15) 5_665 . ? N12 Cd1 Cl2 89.20(15) 2_665 . ? N12 Cd1 Cl2 89.20(15) 5_665 . ? N19 Cd1 Cl2 91.1(2) . . ? N12 Cd1 Cl1 91.21(15) 2_665 . ? N12 Cd1 Cl1 91.21(15) 5_665 . ? N19 Cd1 Cl1 88.2(2) . . ? Cl2 Cd1 Cl1 179.27(9) . . ? C11 N12 C12 105.7(6) . . ? C11 N12 Cd1 130.6(5) . 5_665 ? C12 N12 Cd1 123.6(5) . 5_665 ? C1 N15 C3 106.7(10) . . ? C1 N15 C4 127.6(10) . . ? C3 N15 C4 125.7(10) . . ? C1 N19 C2 104.9(9) . . ? C1 N19 Cd1 126.7(8) . . ? C2 N19 Cd1 128.4(7) . . ? C11 N24 C13 105.4(6) . . ? C11 N24 C10 126.2(6) . . ? C13 N24 C10 128.2(6) . . ? N19 C1 N15 112.2(10) . . ? N19 C2 C3 109.4(9) . . ? N15 C3 C2 106.7(10) . . ? N15 C4 C5 111.4(9) . . ? C6 C5 C6 119.9(9) . 6_556 ? C6 C5 C4 120.0(5) . . ? C6 C5 C4 120.0(5) 6_556 . ? C9 C6 C5 119.7(7) . . ? C9 C6 C7 121.5(6) . . ? C5 C6 C7 118.7(7) . . ? C8 C7 C6 111.4(6) . . ? C6 C9 C14 118.6(7) . . ? C6 C9 C10 118.9(6) . . ? C14 C9 C10 122.3(7) . . ? N24 C10 C9 111.7(5) . . ? N12 C11 N24 112.8(6) . . ? C13 C12 N12 108.5(7) . . ? C12 C13 N24 107.4(7) . . ? C9 C14 C9 123.3(10) . 6_556 ? C9 C14 C15 118.3(5) . . ? C9 C14 C15 118.3(5) 6_556 . ? C16 C15 C14 110.6(9) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.529 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.111