Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Louise Broge' _publ_contact_author_address ; Natural Sciences, Faculty of Life Science University of Copenhagen Thorvaldsensvej 40 Frederiksberg DK-1871 DENMARK ; _publ_contact_author_email LUB@LIFE.KU.DK _publ_section_title ; Bowl Adamanzanes - Bicyclic Tetraamines: Syntheses and Crystal Structures of Complexes with Cobalt(III) and Chelately Coordinated Oxo-anions. ; loop_ _publ_author_name 'Louise Broge' 'Kristian Jensen' 'Nicolai Jensen' 'Ulla Pretzmann' 'Inger Sotofte' 'Johan Springborg' # Attachment 'Fig2.cif' data_js11ak _database_code_depnum_ccdc_archive 'CCDC 642044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(C11H24N4)(H2O)Br](ClO4)2,H2O' _chemical_formula_sum 'C11 H28 Br Cl2 Co N4 O10' _chemical_formula_weight 586.11 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 9.2909(7) _cell_length_b 12.4894(9) _cell_length_c 18.1813(13) _cell_angle_alpha 90.00 _cell_angle_beta 102.579(2) _cell_angle_gamma 90.00 _cell_volume 2059.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14427 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 28.00 _exptl_crystal_description ? _exptl_crystal_colour purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 3.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7591 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS,ver2.03 (Sheldrick,2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD Platform' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14427 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4963 _reflns_number_gt 4331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS,1998)' _computing_cell_refinement 'SAINT (Bruker AXS,1998)' _computing_data_reduction 'SAINT (Bruker AXS,1998)' _computing_structure_solution 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_structure_refinement 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_molecular_graphics 'SHELXTL,ver.6.12 (Sheldrick,2001)' _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^)+(0.0574P)^2^+4.0542P] 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 4963 _refine_ls_number_parameters 356 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.028 _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 Co Co 0.22754(4) 0.29652(3) 0.04163(2) 0.01997(11) Uani 1 1 d . . . Br Br 0.21507(4) 0.46458(2) -0.029977(19) 0.02916(11) Uani 1 1 d . . . O1 O 0.1070(3) 0.2448(2) -0.05492(14) 0.0306(5) Uani 1 1 d D . . H111 H 0.019(2) 0.274(3) -0.066(2) 0.037 Uiso 1 1 d D . . H112 H 0.159(4) 0.260(3) -0.0891(18) 0.037 Uiso 1 1 d D . . N1 N 0.0590(3) 0.3363(3) 0.08304(18) 0.0339(6) Uani 1 1 d . . . H1 H -0.0056 0.3756 0.0467 0.041 Uiso 1 1 calc R . . C1 C 0.1094(4) 0.4072(3) 0.1511(2) 0.0408(9) Uani 1 1 d . . . H11 H 0.1079 0.3664 0.1976 0.049 Uiso 1 1 calc R . . H12 H 0.0415 0.4689 0.1486 0.049 Uiso 1 1 calc R . . C2 C 0.2653(4) 0.4472(3) 0.1530(2) 0.0393(8) Uani 1 1 d . . . H21 H 0.2623 0.5067 0.1168 0.047 Uiso 1 1 calc R . . H22 H 0.3106 0.4740 0.2041 0.047 Uiso 1 1 calc R . . N2 N 0.3547(3) 0.3560(2) 0.13270(15) 0.0264(5) Uani 1 1 d . A . C3 C 0.4872(4) 0.3940(3) 0.10543(19) 0.0306(7) Uani 1 1 d . . . H31 H 0.5676 0.4127 0.1489 0.037 Uiso 1 1 calc R . . H32 H 0.4617 0.4588 0.0738 0.037 Uiso 1 1 calc R . . C4 C 0.5370(3) 0.3057(3) 0.0599(2) 0.0293(7) Uani 1 1 d . . . H41 H 0.5991 0.3361 0.0272 0.035 Uiso 1 1 calc R . . H42 H 0.5970 0.2532 0.0943 0.035 Uiso 1 1 calc R . . N3 N 0.4050(3) 0.2502(2) 0.01194(15) 0.0233(5) Uani 1 1 d . . . H3 H 0.3982 0.2717 -0.0377 0.028 Uiso 1 1 calc R . . C5 C 0.4134(4) 0.1295(3) 0.0138(2) 0.0328(7) Uani 1 1 d . . . H51 H 0.4952 0.1065 0.0553 0.039 Uiso 1 1 calc R . . H52 H 0.4338 0.1028 -0.0342 0.039 Uiso 1 1 calc R . . C6 C 0.2690(4) 0.0825(3) 0.0254(3) 0.0409(9) Uani 1 1 d . . . H61 H 0.1974 0.0783 -0.0236 0.049 Uiso 1 1 calc R . . H62 H 0.2862 0.0090 0.0459 0.049 Uiso 1 1 calc R . . N4 N 0.2065(3) 0.1506(2) 0.07896(19) 0.0350(7) Uani 1 1 d . A . C7 C 0.0420(4) 0.1389(3) 0.0679(3) 0.0490(11) Uani 1 1 d . . . H71 H 0.0185 0.0738 0.0940 0.059 Uiso 1 1 calc R . . H72 H -0.0031 0.1317 0.0136 0.059 Uiso 1 1 calc R . . C8 C -0.0198(5) 0.2367(4) 0.0995(3) 0.0532(12) Uani 1 1 d . . . H81 H -0.1264 0.2431 0.0768 0.064 Uiso 1 1 calc R . . H82 H -0.0080 0.2286 0.1547 0.064 Uiso 1 1 calc R . . C9 C 0.4055(5) 0.2882(3) 0.2023(2) 0.0429(9) Uani 1 1 d D . . H91A H 0.5043 0.3143 0.2280 0.051 Uiso 0.652(15) 1 calc PR A 1 H92A H 0.3382 0.3026 0.2364 0.051 Uiso 0.652(15) 1 calc PR A 1 H91B H 0.5091 0.2675 0.2041 0.051 Uiso 0.348(15) 1 calc PR A 2 H92B H 0.4061 0.3344 0.2466 0.051 Uiso 0.348(15) 1 calc PR A 2 C10 C 0.4154(7) 0.1749(5) 0.1951(3) 0.0338(18) Uani 0.652(15) 1 d PD A 1 H10A H 0.4522 0.1441 0.2459 0.041 Uiso 0.652(15) 1 calc PR A 1 H11A H 0.4891 0.1588 0.1648 0.041 Uiso 0.652(15) 1 calc PR A 1 C11 C 0.2747(6) 0.1205(4) 0.1599(3) 0.0628(14) Uani 1 1 d D . . H12A H 0.2018 0.1359 0.1909 0.075 Uiso 0.652(15) 1 calc PR A 1 H13A H 0.2923 0.0423 0.1620 0.075 Uiso 0.652(15) 1 calc PR A 1 H12B H 0.2001 0.0771 0.1779 0.075 Uiso 0.348(15) 1 calc PR A 2 H13B H 0.3579 0.0718 0.1580 0.075 Uiso 0.348(15) 1 calc PR A 2 C10' C 0.324(2) 0.1895(8) 0.2121(6) 0.062(6) Uani 0.348(15) 1 d PD A 2 H10B H 0.3878 0.1491 0.2534 0.075 Uiso 0.348(15) 1 calc PR A 2 H11B H 0.2372 0.2129 0.2315 0.075 Uiso 0.348(15) 1 calc PR A 2 O10 O 0.2721(4) 0.2560(3) -0.15354(19) 0.0519(8) Uani 1 1 d D . . H101 H 0.294(6) 0.203(3) -0.180(3) 0.062 Uiso 1 1 d D . . H102 H 0.293(6) 0.314(3) -0.176(3) 0.062 Uiso 1 1 d D . . Cl1 Cl 0.28483(9) 0.76678(8) 0.11824(5) 0.0370(2) Uani 1 1 d . . . O2 O 0.1736(11) 0.6917(8) 0.0863(4) 0.0354(18) Uani 0.50 1 d P . . O2' O 0.1698(10) 0.6892(8) 0.1200(5) 0.045(2) Uani 0.50 1 d P . . O3 O 0.2000(6) 0.8596(4) 0.1429(4) 0.0326(12) Uani 0.50 1 d P . . O3' O 0.317(2) 0.8329(10) 0.1712(6) 0.158(7) Uani 0.50 1 d P . . O4 O 0.3809(6) 0.7308(5) 0.1852(3) 0.0461(14) Uani 0.50 1 d P . . O4' O 0.4169(7) 0.6852(8) 0.1175(5) 0.078(3) Uani 0.50 1 d P . . O5 O 0.3566(7) 0.8073(6) 0.0666(4) 0.0508(17) Uani 0.50 1 d P . . O5' O 0.2688(10) 0.8125(6) 0.0435(4) 0.0590(18) Uani 0.50 1 d P . . Cl2 Cl 0.22064(15) -0.02543(8) -0.19865(6) 0.0579(3) Uani 1 1 d . . . O6 O 0.0990(8) 0.0360(6) -0.1793(5) 0.073(3) Uani 0.50 1 d P . . O6' O 0.0792(14) -0.0404(17) -0.2262(10) 0.202(11) Uani 0.50 1 d P . . O7 O 0.2549(9) -0.1203(11) -0.1604(9) 0.110(5) Uani 0.50 1 d P . . O7' O 0.263(3) -0.1277(13) -0.2273(10) 0.270(16) Uani 0.50 1 d P . . O8 O 0.3572(10) 0.0372(7) -0.1689(8) 0.106(4) Uani 0.50 1 d P . . O8' O 0.2696(9) -0.0408(9) -0.1220(4) 0.073(3) Uani 0.50 1 d P . . O9 O 0.202(2) -0.0460(11) -0.2723(6) 0.224(12) Uani 0.50 1 d P . . O9' O 0.2796(7) 0.0529(6) -0.2317(4) 0.0531(16) Uani 0.50 1 d P . . 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 Co 0.01878(19) 0.0171(2) 0.0244(2) 0.00177(14) 0.00563(15) -0.00185(14) Br 0.03350(18) 0.02170(17) 0.03384(19) 0.00686(12) 0.01073(13) 0.00171(12) O1 0.0229(11) 0.0323(12) 0.0347(13) -0.0044(10) 0.0018(9) -0.0042(9) N1 0.0271(13) 0.0391(16) 0.0388(16) 0.0082(13) 0.0145(12) 0.0048(12) C1 0.045(2) 0.047(2) 0.0342(19) 0.0015(16) 0.0183(16) 0.0177(17) C2 0.050(2) 0.0363(19) 0.0328(19) -0.0111(15) 0.0129(16) 0.0103(16) N2 0.0301(13) 0.0248(13) 0.0241(13) -0.0009(10) 0.0056(10) -0.0003(11) C3 0.0279(15) 0.0298(16) 0.0325(17) -0.0056(13) 0.0027(13) -0.0106(13) C4 0.0185(14) 0.0341(17) 0.0349(17) -0.0028(13) 0.0049(12) -0.0072(12) N3 0.0220(12) 0.0211(12) 0.0265(13) -0.0018(10) 0.0049(10) -0.0016(10) C5 0.0296(16) 0.0224(15) 0.045(2) -0.0054(14) 0.0052(14) 0.0048(13) C6 0.0378(19) 0.0171(16) 0.065(3) -0.0016(15) 0.0050(18) -0.0039(13) N4 0.0328(15) 0.0234(14) 0.0484(18) 0.0102(12) 0.0077(13) -0.0065(11) C7 0.0333(19) 0.041(2) 0.076(3) 0.014(2) 0.0192(19) -0.0161(17) C8 0.035(2) 0.061(3) 0.072(3) 0.018(2) 0.029(2) -0.0057(19) C9 0.044(2) 0.052(2) 0.0294(18) 0.0132(16) -0.0001(15) -0.0006(18) C10 0.044(3) 0.040(3) 0.019(3) 0.008(2) 0.010(2) 0.014(2) C11 0.065(3) 0.051(3) 0.067(3) 0.039(2) 0.002(2) -0.012(2) C10' 0.142(18) 0.028(6) 0.023(6) 0.004(4) 0.033(7) 0.031(8) O10 0.0611(19) 0.0503(19) 0.0524(19) -0.0042(14) 0.0300(15) -0.0025(16) Cl1 0.0317(4) 0.0435(5) 0.0350(4) 0.0052(4) 0.0054(3) -0.0138(4) O2 0.035(3) 0.023(3) 0.046(4) -0.007(4) 0.003(4) -0.003(2) O2' 0.024(3) 0.026(3) 0.085(7) 0.007(5) 0.015(5) -0.002(2) O3 0.035(3) 0.021(2) 0.049(3) -0.015(2) 0.025(2) -0.007(2) O3' 0.32(2) 0.116(10) 0.058(6) -0.061(6) 0.092(9) -0.155(12) O4 0.043(3) 0.044(3) 0.042(3) 0.008(3) -0.010(2) -0.003(3) O4' 0.034(3) 0.112(6) 0.088(6) 0.048(5) 0.014(3) 0.011(4) O5 0.038(3) 0.079(5) 0.043(4) 0.014(3) 0.027(3) 0.007(3) O5' 0.080(5) 0.058(4) 0.043(4) 0.008(3) 0.021(4) 0.024(4) Cl2 0.0832(8) 0.0396(5) 0.0357(5) 0.0044(4) -0.0202(5) -0.0034(5) O6 0.040(4) 0.070(5) 0.100(6) 0.056(5) -0.006(4) -0.008(3) O6' 0.104(9) 0.268(19) 0.174(13) 0.184(14) -0.101(9) -0.133(11) O7 0.049(5) 0.129(9) 0.156(11) 0.115(9) 0.031(6) 0.030(5) O7' 0.48(4) 0.132(12) 0.126(13) -0.063(10) -0.093(17) 0.169(18) O8 0.066(5) 0.079(6) 0.180(12) -0.070(7) 0.041(7) -0.007(4) O8' 0.062(5) 0.105(7) 0.039(4) 0.005(4) -0.016(3) -0.011(5) O9 0.40(3) 0.131(10) 0.065(6) -0.067(7) -0.116(11) 0.189(14) O9' 0.036(3) 0.086(5) 0.040(3) -0.009(3) 0.013(3) -0.010(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 Co N3 1.932(3) . ? Co N1 1.944(3) . ? Co N2 1.959(3) . ? Co N4 1.970(3) . ? Co O1 1.974(2) . ? Co Br 2.4594(5) . ? O1 H111 0.882(16) . ? O1 H112 0.889(16) . ? N1 C8 1.507(5) . ? N1 C1 1.510(5) . ? N1 H1 0.9300 . ? C1 C2 1.525(6) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? C2 N2 1.503(4) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? N2 C3 1.500(4) . ? N2 C9 1.510(4) . ? C3 C4 1.511(5) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 N3 1.510(4) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? N3 C5 1.509(4) . ? N3 H3 0.9300 . ? C5 C6 1.521(5) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 N4 1.501(5) . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N4 C7 1.504(5) . ? N4 C11 1.517(5) . ? C7 C8 1.515(7) . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 C10 1.426(7) . ? C9 C10' 1.479(13) . ? C9 H91A 0.9900 . ? C9 H92A 0.9900 . ? C9 H91B 0.9900 . ? C9 H92B 0.9900 . ? C10 C11 1.489(7) . ? C10 H10A 0.9900 . ? C10 H11A 0.9900 . ? C11 C10' 1.289(11) . ? C11 H12A 0.9900 . ? C11 H13A 0.9900 . ? C11 H12B 0.9900 . ? C11 H13B 0.9900 . ? C10' H10B 0.9900 . ? C10' H11B 0.9900 . ? O10 H101 0.863(16) . ? O10 H102 0.872(16) . ? Cl1 O3' 1.254(8) . ? Cl1 O5 1.362(6) . ? Cl1 O4 1.417(5) . ? Cl1 O2 1.422(10) . ? Cl1 O2' 1.448(9) . ? Cl1 O5' 1.451(7) . ? Cl1 O3 1.523(5) . ? Cl1 O4' 1.598(8) . ? O2 O2' 0.622(9) . ? O3 O3' 1.15(2) . ? O3' O4 1.405(18) . ? O4 O4' 1.460(11) . ? O4' O5 1.809(11) . ? O5 O5' 0.834(8) . ? Cl2 O6' 1.314(9) . ? Cl2 O9' 1.327(7) . ? Cl2 O9 1.337(11) . ? Cl2 O7 1.375(8) . ? Cl2 O8' 1.381(7) . ? Cl2 O7' 1.464(13) . ? Cl2 O6 1.471(9) . ? Cl2 O8 1.488(9) . ? O6 O6' 1.27(2) . ? O6' O9 1.56(2) . ? O7 O8' 1.204(16) . ? O7 O7' 1.24(2) . ? O7' O9 1.351(18) . ? O8 O9' 1.227(13) . ? O8 O8' 1.624(15) . ? O9 O9' 1.535(17) . ? 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 Co N1 173.32(12) . . ? N3 Co N2 87.43(11) . . ? N1 Co N2 87.95(13) . . ? N3 Co N4 88.50(12) . . ? N1 Co N4 87.40(13) . . ? N2 Co N4 98.42(12) . . ? N3 Co O1 90.41(11) . . ? N1 Co O1 94.54(12) . . ? N2 Co O1 175.35(11) . . ? N4 Co O1 85.64(12) . . ? N3 Co Br 92.99(8) . . ? N1 Co Br 92.16(9) . . ? N2 Co Br 94.25(8) . . ? N4 Co Br 167.30(10) . . ? O1 Co Br 81.74(7) . . ? Co O1 H111 113(3) . . ? Co O1 H112 105(3) . . ? H111 O1 H112 111(4) . . ? C8 N1 C1 113.5(3) . . ? C8 N1 Co 109.5(2) . . ? C1 N1 Co 109.6(2) . . ? C8 N1 H1 108.1 . . ? C1 N1 H1 108.1 . . ? Co N1 H1 108.1 . . ? N1 C1 C2 109.5(3) . . ? N1 C1 H11 109.8 . . ? C2 C1 H11 109.8 . . ? N1 C1 H12 109.8 . . ? C2 C1 H12 109.8 . . ? H11 C1 H12 108.2 . . ? N2 C2 C1 108.6(3) . . ? N2 C2 H21 110.0 . . ? C1 C2 H21 110.0 . . ? N2 C2 H22 110.0 . . ? C1 C2 H22 110.0 . . ? H21 C2 H22 108.3 . . ? C3 N2 C2 112.2(3) . . ? C3 N2 C9 109.0(3) . . ? C2 N2 C9 107.9(3) . . ? C3 N2 Co 103.18(19) . . ? C2 N2 Co 103.4(2) . . ? C9 N2 Co 121.1(2) . . ? N2 C3 C4 108.7(3) . . ? N2 C3 H31 110.0 . . ? C4 C3 H31 110.0 . . ? N2 C3 H32 110.0 . . ? C4 C3 H32 110.0 . . ? H31 C3 H32 108.3 . . ? N3 C4 C3 110.1(2) . . ? N3 C4 H41 109.6 . . ? C3 C4 H41 109.6 . . ? N3 C4 H42 109.6 . . ? C3 C4 H42 109.6 . . ? H41 C4 H42 108.1 . . ? C5 N3 C4 114.4(2) . . ? C5 N3 Co 109.6(2) . . ? C4 N3 Co 109.67(19) . . ? C5 N3 H3 107.6 . . ? C4 N3 H3 107.6 . . ? Co N3 H3 107.6 . . ? N3 C5 C6 110.2(3) . . ? N3 C5 H51 109.6 . . ? C6 C5 H51 109.6 . . ? N3 C5 H52 109.6 . . ? C6 C5 H52 109.6 . . ? H51 C5 H52 108.1 . . ? N4 C6 C5 110.4(3) . . ? N4 C6 H61 109.6 . . ? C5 C6 H61 109.6 . . ? N4 C6 H62 109.6 . . ? C5 C6 H62 109.6 . . ? H61 C6 H62 108.1 . . ? C6 N4 C7 112.6(3) . . ? C6 N4 C11 110.5(3) . . ? C7 N4 C11 107.6(3) . . ? C6 N4 Co 102.7(2) . . ? C7 N4 Co 102.6(2) . . ? C11 N4 Co 120.8(3) . . ? N4 C7 C8 109.2(3) . . ? N4 C7 H71 109.8 . . ? C8 C7 H71 109.8 . . ? N4 C7 H72 109.8 . . ? C8 C7 H72 109.8 . . ? H71 C7 H72 108.3 . . ? N1 C8 C7 110.5(3) . . ? N1 C8 H81 109.6 . . ? C7 C8 H81 109.6 . . ? N1 C8 H82 109.6 . . ? C7 C8 H82 109.6 . . ? H81 C8 H82 108.1 . . ? C10 C9 C10' 39.5(6) . . ? C10 C9 N2 119.7(4) . . ? C10' C9 N2 119.6(6) . . ? C10 C9 H91A 107.4 . . ? C10' C9 H91A 131.7 . . ? N2 C9 H91A 107.4 . . ? C10 C9 H92A 107.4 . . ? C10' C9 H92A 70.3 . . ? N2 C9 H92A 107.4 . . ? H91A C9 H92A 106.9 . . ? C10 C9 H91B 70.3 . . ? C10' C9 H91B 107.4 . . ? N2 C9 H91B 107.4 . . ? H91A C9 H91B 43.6 . . ? H92A C9 H91B 140.2 . . ? C10 C9 H92B 131.6 . . ? C10' C9 H92B 107.4 . . ? N2 C9 H92B 107.4 . . ? H91A C9 H92B 65.4 . . ? H92A C9 H92B 43.6 . . ? H91B C9 H92B 107.0 . . ? C9 C10 C11 115.1(5) . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? C9 C10 H11A 108.5 . . ? C11 C10 H11A 108.5 . . ? H10A C10 H11A 107.5 . . ? C10' C11 C10 40.7(8) . . ? C10' C11 N4 123.6(6) . . ? C10 C11 N4 116.5(4) . . ? C10' C11 H12A 68.1 . . ? C10 C11 H12A 108.2 . . ? N4 C11 H12A 108.2 . . ? C10' C11 H13A 127.1 . . ? C10 C11 H13A 108.2 . . ? N4 C11 H13A 108.2 . . ? H12A C11 H13A 107.3 . . ? C10' C11 H12B 106.4 . . ? C10 C11 H12B 136.0 . . ? N4 C11 H12B 106.4 . . ? H12A C11 H12B 45.8 . . ? H13A C11 H12B 64.5 . . ? C10' C11 H13B 106.4 . . ? C10 C11 H13B 71.1 . . ? N4 C11 H13B 106.4 . . ? H12A C11 H13B 140.8 . . ? H13A C11 H13B 43.2 . . ? H12B C11 H13B 106.5 . . ? C11 C10' C9 125.2(9) . . ? C11 C10' H10B 106.0 . . ? C9 C10' H10B 106.0 . . ? C11 C10' H11B 106.0 . . ? C9 C10' H11B 106.0 . . ? H10B C10' H11B 106.3 . . ? H101 O10 H102 106(5) . . ? O3' Cl1 O5 102.2(6) . . ? O3' Cl1 O4 63.1(9) . . ? O5 Cl1 O4 113.5(4) . . ? O3' Cl1 O2 141.3(7) . . ? O5 Cl1 O2 112.6(5) . . ? O4 Cl1 O2 114.1(4) . . ? O3' Cl1 O2' 118.7(6) . . ? O5 Cl1 O2' 137.5(5) . . ? O4 Cl1 O2' 95.7(5) . . ? O2 Cl1 O2' 25.0(4) . . ? O3' Cl1 O5' 114.7(7) . . ? O5 Cl1 O5' 34.3(4) . . ? O4 Cl1 O5' 147.8(5) . . ? O2 Cl1 O5' 87.7(5) . . ? O2' Cl1 O5' 111.0(5) . . ? O3' Cl1 O3 47.7(9) . . ? O5 Cl1 O3 106.4(4) . . ? O4 Cl1 O3 104.9(4) . . ? O2 Cl1 O3 104.2(5) . . ? O2' Cl1 O3 94.1(4) . . ? O5' Cl1 O3 91.3(4) . . ? O3' Cl1 O4' 111.6(11) . . ? O5 Cl1 O4' 74.9(4) . . ? O4 Cl1 O4' 57.5(4) . . ? O2 Cl1 O4' 93.8(5) . . ? O2' Cl1 O4' 98.3(5) . . ? O5' Cl1 O4' 99.5(4) . . ? O3 Cl1 O4' 159.3(4) . . ? O2' O2 Cl1 79.8(16) . . ? O2 O2' Cl1 75.2(16) . . ? O3' O3 Cl1 53.8(5) . . ? O3 O3' Cl1 78.5(8) . . ? O3 O3' O4 131.7(8) . . ? Cl1 O3' O4 64.1(7) . . ? O3' O4 Cl1 52.8(5) . . ? O3' O4 O4' 111.4(6) . . ? Cl1 O4 O4' 67.4(4) . . ? O4 O4' Cl1 55.0(4) . . ? O4 O4' O5 90.0(6) . . ? Cl1 O4' O5 46.6(3) . . ? O5' O5 Cl1 78.7(7) . . ? O5' O5 O4' 118.9(10) . . ? Cl1 O5 O4' 58.5(4) . . ? O5 O5' Cl1 67.0(6) . . ? O6' Cl2 O9' 114.2(5) . . ? O6' Cl2 O9 72.0(11) . . ? O9' Cl2 O9 70.3(10) . . ? O6' Cl2 O7 99.9(7) . . ? O9' Cl2 O7 142.3(5) . . ? O9 Cl2 O7 107.8(9) . . ? O6' Cl2 O8' 116.6(8) . . ? O9' Cl2 O8' 118.8(5) . . ? O9 Cl2 O8' 157.7(6) . . ? O7 Cl2 O8' 51.8(7) . . ? O6' Cl2 O7' 93.5(16) . . ? O9' Cl2 O7' 108.3(13) . . ? O9 Cl2 O7' 57.4(8) . . ? O7 Cl2 O7' 51.6(9) . . ? O8' Cl2 O7' 100.5(7) . . ? O6' Cl2 O6 53.7(12) . . ? O9' Cl2 O6 97.9(4) . . ? O9 Cl2 O6 113.7(7) . . ? O7 Cl2 O6 115.7(6) . . ? O8' Cl2 O6 86.2(6) . . ? O7' Cl2 O6 144.9(13) . . ? O6' Cl2 O8 156.4(11) . . ? O9' Cl2 O8 51.3(6) . . ? O9 Cl2 O8 112.2(13) . . ? O7 Cl2 O8 100.6(7) . . ? O8' Cl2 O8 68.8(7) . . ? O7' Cl2 O8 108.4(12) . . ? O6 Cl2 O8 106.1(5) . . ? O6' O6 Cl2 56.8(8) . . ? O6 O6' Cl2 69.5(7) . . ? O6 O6' O9 112.3(9) . . ? Cl2 O6' O9 54.7(7) . . ? O8' O7 O7' 127.4(14) . . ? O8' O7 Cl2 64.4(7) . . ? O7' O7 Cl2 67.9(7) . . ? O7 O7' O9 115.7(13) . . ? O7 O7' Cl2 60.5(8) . . ? O9 O7' Cl2 56.5(6) . . ? O9' O8 Cl2 57.6(5) . . ? O9' O8 O8' 108.9(7) . . ? Cl2 O8 O8' 52.5(4) . . ? O7 O8' Cl2 63.9(5) . . ? O7 O8' O8 101.4(8) . . ? Cl2 O8' O8 58.7(5) . . ? Cl2 O9 O7' 66.0(8) . . ? Cl2 O9 O9' 54.5(5) . . ? O7' O9 O9' 103.2(10) . . ? Cl2 O9 O6' 53.3(7) . . ? O7' O9 O6' 88.0(19) . . ? O9' O9 O6' 91.6(8) . . ? O8 O9' Cl2 71.1(6) . . ? O8 O9' O9 115.9(8) . . ? Cl2 O9' O9 55.1(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 Co N1 C1 C2 14.4(4) . . . . ? N1 C1 C2 N2 -42.0(4) . . . . ? C1 C2 N2 Co 48.3(3) . . . . ? C2 N2 Co N1 -32.9(2) . . . . ? N2 Co N1 C1 10.8(2) . . . . ? Co N2 C3 C4 -48.4(3) . . . . ? N2 C3 C4 N3 39.5(4) . . . . ? C3 C4 N3 Co -10.5(3) . . . . ? C4 N3 Co N2 -14.2(2) . . . . ? N3 Co N2 C3 34.8(2) . . . . ? Co N3 C5 C6 9.5(4) . . . . ? N3 C5 C6 N4 -37.6(4) . . . . ? C5 C6 N4 Co 45.7(3) . . . . ? C6 N4 Co N3 -32.9(2) . . . . ? N4 Co N3 C5 13.7(2) . . . . ? Co N4 C7 C8 -48.3(4) . . . . ? N4 C7 C8 N1 38.5(5) . . . . ? C7 C8 N1 Co -8.7(4) . . . . ? C8 N1 Co N4 -15.7(3) . . . . ? N1 Co N4 C7 35.5(3) . . . . ? Co N2 C9 C10 25.8(5) . . . . ? N2 C9 C10 C11 -59.4(7) . . . . ? C9 C10 C11 N4 62.9(7) . . . . ? C10 C11 N4 Co -32.8(6) . . . . ? C11 N4 Co N2 3.4(3) . . . . ? N4 Co N2 C9 0.8(3) . . . . ? Co N2 C9 C10 25.8(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O10 0.93 2.19 2.994(4) 144.9 . N1 H1 Br 0.93 2.76 3.540(3) 142.3 3_565 O1 H112 O10 0.889(16) 1.736(19) 2.605(4) 165(4) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.182 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.109 # Attachment 'Fig3.cif' data_315ak _database_code_depnum_ccdc_archive 'CCDC 642045' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(C11H24N4)(H2O)(OH)](ClO4)2,1.75H2O' _chemical_formula_sum 'C11 H30.50 Cl2 Co N4 O11.75' _chemical_formula_weight 536.72 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 18.2694(9) _cell_length_b 12.2362(6) _cell_length_c 19.6977(9) _cell_angle_alpha 90.00 _cell_angle_beta 114.9090(10) _cell_angle_gamma 90.00 _cell_volume 3993.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 27972 _cell_measurement_theta_min 1.23 _cell_measurement_theta_max 28.04 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2236 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8550 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS,ver2.03 (Sheldrick,2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD Platform' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27972 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.04 _reflns_number_total 9614 _reflns_number_gt 7300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS,1998)' _computing_cell_refinement 'SAINT (Bruker AXS,1998)' _computing_data_reduction 'SAINT (Bruker AXS,1998)' _computing_structure_solution 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_structure_refinement 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_molecular_graphics 'SHELXTL,ver.6.12 (Sheldrick,2001)' _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^)+(0.0927P)^2^+10.8502P] 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 9614 _refine_ls_number_parameters 591 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1809 _refine_ls_wR_factor_gt 0.1665 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.03392(3) 0.15962(4) 0.07756(3) 0.01210(13) Uani 1 1 d . . . O1 O 0.08659(18) 0.1136(2) 0.01524(17) 0.0226(6) Uani 1 1 d D . . H1O1 H 0.089(3) 0.042(2) 0.032(3) 0.027 Uiso 1 1 d D . . H2O1 H 0.076(3) 0.151(3) -0.0269(17) 0.027 Uiso 1 1 d D . . O2 O -0.05830(17) 0.0868(2) 0.00192(16) 0.0224(6) Uani 1 1 d . . . H2 H -0.0846 0.1315 -0.0320 0.027 Uiso 1 1 calc R . . N1 N 0.0016(2) 0.3002(3) 0.0287(2) 0.0233(7) Uani 1 1 d . . . H1 H -0.0181 0.2884 -0.0226 0.028 Uiso 1 1 calc R . . C1 C -0.0655(3) 0.3472(3) 0.0437(3) 0.0283(10) Uani 1 1 d . . . H11 H -0.1098 0.3708 -0.0040 0.034 Uiso 1 1 calc R . . H12 H -0.0460 0.4119 0.0765 0.034 Uiso 1 1 calc R . . C2 C -0.0977(3) 0.2600(4) 0.0821(3) 0.0284(9) Uani 1 1 d . . . H21 H -0.1247 0.2968 0.1101 0.034 Uiso 1 1 calc R . . H22 H -0.1377 0.2126 0.0436 0.034 Uiso 1 1 calc R . . N2 N -0.0299(2) 0.1927(3) 0.1340(2) 0.0236(7) Uani 1 1 d . . . C3 C -0.0593(3) 0.0826(3) 0.1450(3) 0.0280(10) Uani 1 1 d . . . H31 H -0.1007 0.0547 0.0970 0.034 Uiso 1 1 calc R . . H32 H -0.0834 0.0874 0.1815 0.034 Uiso 1 1 calc R . . C4 C 0.0159(3) 0.0047(3) 0.1752(2) 0.0280(10) Uani 1 1 d . . . H41 H 0.0476 0.0168 0.2295 0.034 Uiso 1 1 calc R . . H42 H -0.0023 -0.0724 0.1675 0.034 Uiso 1 1 calc R . . N3 N 0.0670(2) 0.0270(3) 0.13465(19) 0.0216(7) Uani 1 1 d . . . H3 H 0.0608 -0.0305 0.1018 0.026 Uiso 1 1 calc R . . C5 C 0.1541(3) 0.0349(3) 0.1872(2) 0.0283(10) Uani 1 1 d . . . H51 H 0.1820 -0.0339 0.1859 0.034 Uiso 1 1 calc R . . H52 H 0.1594 0.0459 0.2389 0.034 Uiso 1 1 calc R . . C6 C 0.1943(3) 0.1335(4) 0.1642(2) 0.0266(9) Uani 1 1 d . . . H61 H 0.2459 0.1539 0.2063 0.032 Uiso 1 1 calc R . . H62 H 0.2054 0.1133 0.1208 0.032 Uiso 1 1 calc R . . N4 N 0.1364(2) 0.2261(3) 0.1446(2) 0.0229(7) Uani 1 1 d . . . C7 C 0.1515(3) 0.3063(4) 0.0942(3) 0.0279(9) Uani 1 1 d . . . H71 H 0.1673 0.2667 0.0585 0.033 Uiso 1 1 calc R . . H72 H 0.1961 0.3560 0.1243 0.033 Uiso 1 1 calc R . . C8 C 0.0739(3) 0.3726(3) 0.0510(2) 0.0215(8) Uani 1 1 d . . . H81 H 0.0701 0.4329 0.0829 0.026 Uiso 1 1 calc R . . H82 H 0.0758 0.4051 0.0057 0.026 Uiso 1 1 calc R . . C9 C 0.0089(3) 0.2467(4) 0.2092(3) 0.0308(10) Uani 1 1 d . . . H91 H 0.0337 0.1894 0.2476 0.037 Uiso 1 1 calc R . . H92 H -0.0338 0.2825 0.2198 0.037 Uiso 1 1 calc R . . C10 C 0.0735(3) 0.3319(3) 0.2173(2) 0.0265(9) Uani 1 1 d . . . H101 H 0.0512 0.3849 0.1755 0.032 Uiso 1 1 calc R . . H102 H 0.0881 0.3725 0.2647 0.032 Uiso 1 1 calc R . . C11 C 0.1466(3) 0.2808(4) 0.2170(3) 0.0293(10) Uani 1 1 d . . . H111 H 0.1666 0.2256 0.2575 0.035 Uiso 1 1 calc R . . H112 H 0.1888 0.3377 0.2292 0.035 Uiso 1 1 calc R . . Co2 Co 0.46243(3) 0.84501(4) 0.41623(3) 0.01341(13) Uani 1 1 d . . . O1A O 0.41268(19) 0.9597(2) 0.44890(17) 0.0239(6) Uani 1 1 d D . . H1A1 H 0.413(3) 0.898(3) 0.476(2) 0.029 Uiso 1 1 d D . . H2A1 H 0.3595(13) 0.956(4) 0.437(3) 0.029 Uiso 1 1 d D . . O2A O 0.5404(2) 0.8490(2) 0.52018(17) 0.0347(8) Uani 1 1 d . . . H2A H 0.5612 0.9116 0.5304 0.042 Uiso 1 1 calc R . . N1A N 0.5244(2) 0.9504(3) 0.3889(2) 0.0228(7) Uani 1 1 d . . . H1A H 0.5439 1.0029 0.4265 0.027 Uiso 1 1 calc R . . C1A C 0.4709(3) 1.0062(3) 0.3174(2) 0.0232(8) Uani 1 1 d . . . H11A H 0.4867 0.9841 0.2771 0.028 Uiso 1 1 calc R . . H12A H 0.4776 1.0863 0.3238 0.028 Uiso 1 1 calc R . . C2A C 0.3822(2) 0.9755(3) 0.2954(2) 0.0202(8) Uani 1 1 d . . . H21A H 0.3595 1.0211 0.3234 0.024 Uiso 1 1 calc R . . H22A H 0.3499 0.9878 0.2412 0.024 Uiso 1 1 calc R . . N2A N 0.3794(2) 0.8574(3) 0.31393(19) 0.0191(7) Uani 1 1 d . . . C3A C 0.3022(2) 0.8298(3) 0.3194(3) 0.0265(9) Uani 1 1 d . . . H31A H 0.2599 0.8126 0.2691 0.032 Uiso 1 1 calc R . . H32A H 0.2838 0.8935 0.3392 0.032 Uiso 1 1 calc R . . C4A C 0.3147(3) 0.7315(4) 0.3714(3) 0.0338(11) Uani 1 1 d . . . H41A H 0.2747 0.7340 0.3931 0.041 Uiso 1 1 calc R . . H42A H 0.3061 0.6631 0.3422 0.041 Uiso 1 1 calc R . . N3A N 0.3982(2) 0.7319(3) 0.4332(2) 0.0270(8) Uani 1 1 d . . . H3A H 0.3936 0.7492 0.4772 0.032 Uiso 1 1 calc R . . C5A C 0.4419(3) 0.6243(3) 0.4456(3) 0.0279(10) Uani 1 1 d . . . H51A H 0.4132 0.5752 0.4025 0.033 Uiso 1 1 calc R . . H52A H 0.4430 0.5888 0.4912 0.033 Uiso 1 1 calc R . . C6A C 0.5285(3) 0.6430(3) 0.4544(2) 0.0245(9) Uani 1 1 d . . . H61A H 0.5630 0.6664 0.5063 0.029 Uiso 1 1 calc R . . H62A H 0.5507 0.5740 0.4447 0.029 Uiso 1 1 calc R . . N4A N 0.5286(2) 0.7290(3) 0.40041(19) 0.0195(7) Uani 1 1 d . . . C7A C 0.6092(2) 0.7830(3) 0.4244(3) 0.0274(9) Uani 1 1 d . . . H71A H 0.6453 0.7373 0.4103 0.033 Uiso 1 1 calc R . . H72A H 0.6346 0.7932 0.4794 0.033 Uiso 1 1 calc R . . C8A C 0.5950(3) 0.8938(4) 0.3847(3) 0.0324(11) Uani 1 1 d . . . H81A H 0.6438 0.9398 0.4086 0.039 Uiso 1 1 calc R . . H82A H 0.5847 0.8830 0.3317 0.039 Uiso 1 1 calc R . . C9A C 0.3864(3) 0.7913(4) 0.2523(2) 0.0296(10) Uani 1 1 d . . . H91A H 0.3323 0.7861 0.2102 0.036 Uiso 1 1 calc R . . H92A H 0.4217 0.8314 0.2340 0.036 Uiso 1 1 calc R . . C10A C 0.4192(3) 0.6779(4) 0.2735(3) 0.0307(10) Uani 1 1 d . . . H11B H 0.3891 0.6402 0.2983 0.037 Uiso 1 1 calc R . . H12B H 0.4108 0.6366 0.2276 0.037 Uiso 1 1 calc R . . C11A C 0.5065(3) 0.6782(3) 0.3246(2) 0.0249(9) Uani 1 1 d . . . H21B H 0.5357 0.7178 0.2997 0.030 Uiso 1 1 calc R . . H22B H 0.5260 0.6017 0.3320 0.030 Uiso 1 1 calc R . . Cl1 Cl 0.12569(6) -0.34235(9) 0.17426(6) 0.0277(2) Uani 1 1 d . . . O3 O 0.0484(2) -0.3962(3) 0.1402(2) 0.0402(9) Uani 1 1 d . . . O4 O 0.1204(3) -0.2436(4) 0.1329(2) 0.0647(13) Uani 1 1 d . . . O5 O 0.1429(3) -0.3140(5) 0.2478(2) 0.087(2) Uani 1 1 d . . . O6 O 0.1847(3) -0.4079(5) 0.1669(4) 0.100(2) Uani 1 1 d . . . Cl2 Cl 0.79413(6) 0.95609(8) 0.58233(6) 0.0212(2) Uani 1 1 d . . . O7 O 0.7618(2) 1.0648(3) 0.5610(2) 0.0390(8) Uani 1 1 d . . . O8 O 0.87764(19) 0.9630(3) 0.63267(19) 0.0382(8) Uani 1 1 d . . . O9 O 0.7850(2) 0.8971(3) 0.51687(19) 0.0387(8) Uani 1 1 d . . . O10 O 0.7502(2) 0.9034(3) 0.6188(2) 0.0378(8) Uani 1 1 d . . . Cl3 Cl 0.29204(6) 0.94325(9) 0.05744(6) 0.0250(2) Uani 1 1 d . . . O11 O 0.23983(19) 0.8948(3) 0.0870(2) 0.0403(9) Uani 1 1 d . . . O12 O 0.2727(5) 1.0609(4) 0.0432(4) 0.0506(18) Uani 0.712(10) 1 d P . . O12' O 0.3092(12) 1.0444(12) 0.0888(11) 0.0506(18) Uani 0.288(10) 1 d P . . O13 O 0.3739(3) 0.9345(6) 0.1089(4) 0.057(2) Uani 0.784(11) 1 d P . . O13' O 0.3678(11) 0.874(2) 0.0759(13) 0.057(2) Uani 0.216(11) 1 d P . . O14 O 0.2783(4) 0.8896(7) -0.0096(4) 0.0376(15) Uani 0.624(10) 1 d P . . O14' O 0.2613(8) 0.9420(11) -0.0229(7) 0.0376(15) Uani 0.376(10) 1 d P . . Cl4 Cl 0.38891(10) 0.34466(10) 0.31239(8) 0.0480(4) Uani 1 1 d . . . O15 O 0.3673(4) 0.2668(5) 0.2583(4) 0.062(2) Uani 0.848(13) 1 d P . . O15' O 0.376(2) 0.238(3) 0.302(2) 0.062(2) Uani 0.152(13) 1 d P . . O16 O 0.3516(4) 0.3674(9) 0.3574(3) 0.058(2) Uani 0.794(17) 1 d P . . O16' O 0.3488(16) 0.304(3) 0.3555(15) 0.058(2) Uani 0.206(17) 1 d P . . O17 O 0.4470(4) 0.4166(6) 0.3114(6) 0.069(2) Uani 0.750(15) 1 d P . . O17' O 0.4557(15) 0.395(2) 0.3543(18) 0.069(2) Uani 0.250(15) 1 d P . . O18 O 0.4677(5) 0.2697(7) 0.3732(5) 0.0572(17) Uani 0.50 1 d P . . O18' O 0.3253(5) 0.4224(7) 0.2479(5) 0.0572(17) Uani 0.50 1 d P . . O20 O 0.0754(2) 0.2750(3) 0.39629(19) 0.0338(8) Uani 1 1 d D . . H201 H 0.1240(19) 0.308(4) 0.414(3) 0.041 Uiso 1 1 d D . . H202 H 0.058(3) 0.209(2) 0.379(3) 0.041 Uiso 1 1 d D . . O30 O 0.2122(3) 0.3564(4) 0.3961(3) 0.0602(12) Uani 1 1 d D . . H301 H 0.237(4) 0.404(5) 0.434(3) 0.072 Uiso 1 1 d D . . H302 H 0.257(3) 0.344(6) 0.388(4) 0.072 Uiso 1 1 d D . . O40 O 0.5682(4) 0.2222(6) 0.4118(4) 0.0378(9) Uani 0.50 1 d P . . O40' O 0.6246(4) 0.1666(6) 0.4318(4) 0.0378(9) Uani 0.50 1 d P . . O50 O 0.7043(4) 0.1286(6) 0.4115(4) 0.0378(9) Uani 0.50 1 d P . . 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 0.0177(3) 0.0082(2) 0.0103(2) -0.00134(17) 0.0058(2) -0.00147(17) O1 0.0269(15) 0.0205(14) 0.0233(15) 0.0004(12) 0.0135(13) 0.0004(12) O2 0.0221(14) 0.0189(14) 0.0206(15) -0.0005(11) 0.0034(12) 0.0010(11) N1 0.0283(18) 0.0185(16) 0.0209(18) 0.0013(14) 0.0083(15) 0.0011(14) C1 0.037(2) 0.019(2) 0.026(2) 0.0014(17) 0.010(2) 0.0102(17) C2 0.021(2) 0.035(2) 0.033(2) -0.0046(19) 0.0141(19) 0.0010(17) N2 0.0267(18) 0.0213(17) 0.0273(19) -0.0045(15) 0.0157(16) -0.0043(14) C3 0.038(2) 0.023(2) 0.036(3) -0.0124(18) 0.028(2) -0.0143(18) C4 0.049(3) 0.018(2) 0.020(2) 0.0000(16) 0.019(2) -0.0108(18) N3 0.0283(18) 0.0173(16) 0.0166(17) 0.0000(13) 0.0069(14) -0.0004(13) C5 0.028(2) 0.020(2) 0.022(2) 0.0013(17) -0.0043(18) 0.0068(17) C6 0.021(2) 0.032(2) 0.021(2) -0.0007(18) 0.0039(17) 0.0085(17) N4 0.0251(17) 0.0196(17) 0.0248(19) -0.0018(14) 0.0111(15) -0.0032(13) C7 0.034(2) 0.022(2) 0.032(2) -0.0013(18) 0.019(2) -0.0110(18) C8 0.035(2) 0.0100(17) 0.023(2) 0.0006(15) 0.0157(18) -0.0052(15) C9 0.046(3) 0.029(2) 0.026(2) -0.0085(19) 0.024(2) -0.008(2) C10 0.047(3) 0.0139(19) 0.019(2) -0.0058(16) 0.015(2) -0.0079(17) C11 0.029(2) 0.029(2) 0.026(2) -0.0103(18) 0.0074(19) -0.0071(18) Co2 0.0194(3) 0.0088(2) 0.0118(3) 0.00011(18) 0.0064(2) 0.00202(18) O1A 0.0305(16) 0.0185(14) 0.0244(16) 0.0005(12) 0.0131(13) 0.0074(12) O2A 0.047(2) 0.0222(16) 0.0198(16) -0.0062(12) -0.0012(14) 0.0145(14) N1A 0.0228(17) 0.0158(16) 0.0261(19) 0.0012(14) 0.0067(15) 0.0022(13) C1A 0.032(2) 0.0164(19) 0.024(2) 0.0062(16) 0.0143(18) 0.0012(16) C2A 0.024(2) 0.0149(18) 0.0181(19) 0.0048(15) 0.0048(16) 0.0064(15) N2A 0.0203(16) 0.0155(15) 0.0195(17) 0.0006(13) 0.0065(14) 0.0036(12) C3A 0.0176(19) 0.023(2) 0.036(3) -0.0006(18) 0.0081(18) 0.0005(15) C4A 0.029(2) 0.025(2) 0.055(3) 0.001(2) 0.024(2) -0.0041(18) N3A 0.038(2) 0.0192(17) 0.032(2) 0.0058(15) 0.0233(18) 0.0068(15) C5A 0.046(3) 0.0106(18) 0.034(2) 0.0081(17) 0.024(2) 0.0051(17) C6A 0.039(2) 0.0143(18) 0.019(2) 0.0033(15) 0.0110(19) 0.0083(16) N4A 0.0229(17) 0.0143(15) 0.0193(17) 0.0010(13) 0.0071(14) 0.0057(13) C7A 0.018(2) 0.023(2) 0.035(3) -0.0008(18) 0.0061(18) 0.0052(16) C8A 0.022(2) 0.025(2) 0.056(3) 0.001(2) 0.021(2) 0.0016(17) C9A 0.039(3) 0.024(2) 0.018(2) -0.0026(17) 0.0055(19) 0.0097(19) C10A 0.043(3) 0.023(2) 0.024(2) -0.0066(18) 0.011(2) 0.0018(19) C11A 0.034(2) 0.023(2) 0.020(2) -0.0042(16) 0.0136(19) 0.0059(17) Cl1 0.0260(5) 0.0293(5) 0.0238(5) -0.0026(4) 0.0065(4) -0.0095(4) O3 0.0283(17) 0.0213(16) 0.058(2) -0.0094(16) 0.0051(16) -0.0064(13) O4 0.084(3) 0.048(2) 0.050(3) 0.010(2) 0.015(2) -0.025(2) O5 0.077(3) 0.155(5) 0.030(2) -0.022(3) 0.023(2) -0.072(4) O6 0.054(3) 0.073(4) 0.172(7) -0.024(4) 0.047(4) 0.008(3) Cl2 0.0189(4) 0.0229(5) 0.0239(5) -0.0032(4) 0.0111(4) -0.0014(3) O7 0.0403(19) 0.0256(17) 0.057(2) 0.0056(16) 0.0260(18) 0.0062(14) O8 0.0245(16) 0.050(2) 0.0319(19) 0.0031(16) 0.0044(14) -0.0071(15) O9 0.0394(19) 0.050(2) 0.0283(18) -0.0106(16) 0.0161(16) 0.0044(16) O10 0.0405(19) 0.0350(19) 0.052(2) 0.0000(16) 0.0328(18) -0.0057(15) Cl3 0.0188(5) 0.0330(5) 0.0226(5) 0.0013(4) 0.0082(4) -0.0042(4) O11 0.0215(16) 0.052(2) 0.047(2) 0.0212(18) 0.0145(15) -0.0027(15) O12 0.077(5) 0.025(2) 0.067(5) 0.007(3) 0.048(4) 0.007(3) O12' 0.077(5) 0.025(2) 0.067(5) 0.007(3) 0.048(4) 0.007(3) O13 0.023(2) 0.094(5) 0.039(4) 0.016(3) 0.000(2) -0.016(3) O13' 0.023(2) 0.094(5) 0.039(4) 0.016(3) 0.000(2) -0.016(3) O14 0.041(3) 0.040(4) 0.032(3) -0.014(3) 0.016(3) -0.002(3) O14' 0.041(3) 0.040(4) 0.032(3) -0.014(3) 0.016(3) -0.002(3) Cl4 0.0786(10) 0.0366(7) 0.0473(8) -0.0238(6) 0.0445(8) -0.0333(7) O15 0.074(3) 0.068(4) 0.059(4) -0.043(3) 0.041(3) -0.039(3) O15' 0.074(3) 0.068(4) 0.059(4) -0.043(3) 0.041(3) -0.039(3) O16 0.056(3) 0.077(6) 0.043(3) -0.016(4) 0.025(2) 0.004(4) O16' 0.056(3) 0.077(6) 0.043(3) -0.016(4) 0.025(2) 0.004(4) O17 0.073(4) 0.068(4) 0.088(7) -0.039(5) 0.056(5) -0.051(3) O17' 0.073(4) 0.068(4) 0.088(7) -0.039(5) 0.056(5) -0.051(3) O18 0.038(3) 0.061(4) 0.057(4) 0.033(3) 0.005(3) 0.006(3) O18' 0.038(3) 0.061(4) 0.057(4) 0.033(3) 0.005(3) 0.006(3) O20 0.049(2) 0.0234(16) 0.0247(17) -0.0042(13) 0.0114(16) -0.0018(15) O30 0.061(3) 0.067(3) 0.062(3) -0.025(2) 0.035(3) -0.016(2) O40 0.041(2) 0.041(2) 0.030(2) 0.0007(18) 0.0137(19) -0.0037(17) O40' 0.041(2) 0.041(2) 0.030(2) 0.0007(18) 0.0137(19) -0.0037(17) O50 0.041(2) 0.041(2) 0.030(2) 0.0007(18) 0.0137(19) -0.0037(17) _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 N3 1.921(3) . ? Co1 O2 1.933(3) . ? Co1 O1 1.935(3) . ? Co1 N1 1.938(3) . ? Co1 N4 1.956(3) . ? Co1 N2 1.963(3) . ? O1 H1O1 0.931(19) . ? O1 H2O1 0.893(19) . ? O2 H2 0.8400 . ? N1 C1 1.491(5) . ? N1 C8 1.496(5) . ? N1 H1 0.9300 . ? C1 C2 1.559(6) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? C2 N2 1.480(6) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? N2 C9 1.499(6) . ? N2 C3 1.499(5) . ? C3 C4 1.569(7) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 N3 1.488(5) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? N3 C5 1.492(5) . ? N3 H3 0.9300 . ? C5 C6 1.574(6) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 N4 1.486(5) . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N4 C7 1.503(5) . ? N4 C11 1.514(5) . ? C7 C8 1.542(6) . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 C10 1.532(6) . ? C9 H91 0.9900 . ? C9 H92 0.9900 . ? C10 C11 1.477(6) . ? C10 H101 0.9900 . ? C10 H102 0.9900 . ? C11 H111 0.9900 . ? C11 H112 0.9900 . ? Co2 O1A 1.924(3) . ? Co2 N3A 1.933(4) . ? Co2 N1A 1.935(3) . ? Co2 O2A 1.941(3) . ? Co2 N2A 1.952(3) . ? Co2 N4A 1.972(3) . ? Co2 H1A1 1.87(5) . ? O1A H1A1 0.916(19) . ? O1A H2A1 0.900(19) . ? O2A H2A 0.8400 . ? N1A C8A 1.496(5) . ? N1A C1A 1.498(5) . ? N1A H1A 0.9300 . ? C1A C2A 1.539(6) . ? C1A H11A 0.9900 . ? C1A H12A 0.9900 . ? C2A N2A 1.496(5) . ? C2A H21A 0.9900 . ? C2A H22A 0.9900 . ? N2A C3A 1.499(5) . ? N2A C9A 1.508(5) . ? C3A C4A 1.533(6) . ? C3A H31A 0.9900 . ? C3A H32A 0.9900 . ? C4A N3A 1.498(6) . ? C4A H41A 0.9900 . ? C4A H42A 0.9900 . ? N3A C5A 1.506(5) . ? N3A H3A 0.9300 . ? C5A C6A 1.533(6) . ? C5A H51A 0.9900 . ? C5A H52A 0.9900 . ? C6A N4A 1.498(5) . ? C6A H61A 0.9900 . ? C6A H62A 0.9900 . ? N4A C7A 1.497(5) . ? N4A C11A 1.507(5) . ? C7A C8A 1.532(6) . ? C7A H71A 0.9900 . ? C7A H72A 0.9900 . ? C8A H81A 0.9900 . ? C8A H82A 0.9900 . ? C9A C10A 1.499(6) . ? C9A H91A 0.9900 . ? C9A H92A 0.9900 . ? C10A C11A 1.485(6) . ? C10A H11B 0.9900 . ? C10A H12B 0.9900 . ? C11A H21B 0.9900 . ? C11A H22B 0.9900 . ? Cl1 O5 1.391(5) . ? Cl1 O6 1.400(5) . ? Cl1 O4 1.437(4) . ? Cl1 O3 1.442(3) . ? Cl2 O9 1.425(3) . ? Cl2 O8 1.430(3) . ? Cl2 O10 1.436(3) . ? Cl2 O7 1.444(3) . ? Cl3 O12' 1.359(15) . ? Cl3 O14 1.401(6) . ? Cl3 O13 1.413(5) . ? Cl3 O11 1.438(3) . ? Cl3 O14' 1.439(12) . ? Cl3 O12 1.480(6) . ? Cl3 O13' 1.53(2) . ? O12 O12' 0.888(18) . ? O12' O13 1.722(18) . ? O13 O13' 0.96(3) . ? O13' O14 1.80(2) . ? O14 O14' 0.714(11) . ? Cl4 O17' 1.30(2) . ? Cl4 O15' 1.32(3) . ? Cl4 O16 1.355(6) . ? Cl4 O15 1.358(5) . ? Cl4 O17 1.385(6) . ? Cl4 O16' 1.42(3) . ? Cl4 O18' 1.621(7) . ? Cl4 O18 1.702(7) . ? O15 O15' 0.88(4) . ? O15' O16' 1.57(4) . ? O15' O18 1.71(4) . ? O16 O16' 0.78(3) . ? O17 O17' 0.84(3) . ? O17' O18 1.57(3) . ? O18 O40 1.764(11) . ? O20 H201 0.90(2) . ? O20 H202 0.89(2) . ? O30 H301 0.90(2) . ? O30 H302 0.91(2) . ? O40 O40' 1.156(10) . ? O40' O50 1.728(10) . ? 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 Co1 O2 91.09(13) . . ? N3 Co1 O1 90.45(14) . . ? O2 Co1 O1 83.21(12) . . ? N3 Co1 N1 174.51(15) . . ? O2 Co1 N1 92.41(13) . . ? O1 Co1 N1 94.17(14) . . ? N3 Co1 N4 88.88(15) . . ? O2 Co1 N4 170.86(13) . . ? O1 Co1 N4 87.65(14) . . ? N1 Co1 N4 88.34(15) . . ? N3 Co1 N2 87.58(15) . . ? O2 Co1 N2 89.93(13) . . ? O1 Co1 N2 172.82(13) . . ? N1 Co1 N2 88.19(15) . . ? N4 Co1 N2 99.20(15) . . ? Co1 O1 H1O1 91(3) . . ? Co1 O1 H2O1 118(3) . . ? H1O1 O1 H2O1 140(4) . . ? Co1 O2 H2 109.5 . . ? C1 N1 C8 114.4(3) . . ? C1 N1 Co1 110.4(3) . . ? C8 N1 Co1 109.5(3) . . ? C1 N1 H1 107.4 . . ? C8 N1 H1 107.4 . . ? Co1 N1 H1 107.4 . . ? N1 C1 C2 109.9(3) . . ? N1 C1 H11 109.7 . . ? C2 C1 H11 109.7 . . ? N1 C1 H12 109.7 . . ? C2 C1 H12 109.7 . . ? H11 C1 H12 108.2 . . ? N2 C2 C1 109.9(3) . . ? N2 C2 H21 109.7 . . ? C1 C2 H21 109.7 . . ? N2 C2 H22 109.7 . . ? C1 C2 H22 109.7 . . ? H21 C2 H22 108.2 . . ? C2 N2 C9 110.3(3) . . ? C2 N2 C3 110.7(3) . . ? C9 N2 C3 107.6(3) . . ? C2 N2 Co1 104.3(3) . . ? C9 N2 Co1 120.2(3) . . ? C3 N2 Co1 103.4(2) . . ? N2 C3 C4 106.9(3) . . ? N2 C3 H31 110.3 . . ? C4 C3 H31 110.3 . . ? N2 C3 H32 110.3 . . ? C4 C3 H32 110.3 . . ? H31 C3 H32 108.6 . . ? N3 C4 C3 109.4(3) . . ? N3 C4 H41 109.8 . . ? C3 C4 H41 109.8 . . ? N3 C4 H42 109.8 . . ? C3 C4 H42 109.8 . . ? H41 C4 H42 108.2 . . ? C4 N3 C5 111.5(3) . . ? C4 N3 Co1 110.8(3) . . ? C5 N3 Co1 109.4(3) . . ? C4 N3 H3 108.3 . . ? C5 N3 H3 108.3 . . ? Co1 N3 H3 108.3 . . ? N3 C5 C6 109.9(3) . . ? N3 C5 H51 109.7 . . ? C6 C5 H51 109.7 . . ? N3 C5 H52 109.7 . . ? C6 C5 H52 109.7 . . ? H51 C5 H52 108.2 . . ? N4 C6 C5 106.9(3) . . ? N4 C6 H61 110.3 . . ? C5 C6 H61 110.3 . . ? N4 C6 H62 110.3 . . ? C5 C6 H62 110.3 . . ? H61 C6 H62 108.6 . . ? C6 N4 C7 111.1(3) . . ? C6 N4 C11 107.5(3) . . ? C7 N4 C11 110.5(3) . . ? C6 N4 Co1 103.5(3) . . ? C7 N4 Co1 102.4(3) . . ? C11 N4 Co1 121.5(3) . . ? N4 C7 C8 109.1(3) . . ? N4 C7 H71 109.9 . . ? C8 C7 H71 109.9 . . ? N4 C7 H72 109.9 . . ? C8 C7 H72 109.9 . . ? H71 C7 H72 108.3 . . ? N1 C8 C7 110.1(3) . . ? N1 C8 H81 109.6 . . ? C7 C8 H81 109.6 . . ? N1 C8 H82 109.6 . . ? C7 C8 H82 109.6 . . ? H81 C8 H82 108.2 . . ? N2 C9 C10 115.2(3) . . ? N2 C9 H91 108.5 . . ? C10 C9 H91 108.5 . . ? N2 C9 H92 108.5 . . ? C10 C9 H92 108.5 . . ? H91 C9 H92 107.5 . . ? C11 C10 C9 111.7(4) . . ? C11 C10 H101 109.3 . . ? C9 C10 H101 109.3 . . ? C11 C10 H102 109.3 . . ? C9 C10 H102 109.3 . . ? H101 C10 H102 108.0 . . ? C10 C11 N4 116.0(4) . . ? C10 C11 H111 108.3 . . ? N4 C11 H111 108.3 . . ? C10 C11 H112 108.3 . . ? N4 C11 H112 108.3 . . ? H111 C11 H112 107.4 . . ? O1A Co2 N3A 93.32(14) . . ? O1A Co2 N1A 91.23(14) . . ? N3A Co2 N1A 173.68(16) . . ? O1A Co2 O2A 82.48(13) . . ? N3A Co2 O2A 93.77(16) . . ? N1A Co2 O2A 91.18(16) . . ? O1A Co2 N2A 91.02(13) . . ? N3A Co2 N2A 88.25(15) . . ? N1A Co2 N2A 87.28(14) . . ? O2A Co2 N2A 173.28(13) . . ? O1A Co2 N4A 170.05(14) . . ? N3A Co2 N4A 88.21(14) . . ? N1A Co2 N4A 88.07(14) . . ? O2A Co2 N4A 87.62(13) . . ? N2A Co2 N4A 98.86(14) . . ? O1A Co2 H1A1 27.9(6) . . ? N3A Co2 H1A1 69.8(10) . . ? N1A Co2 H1A1 115.7(10) . . ? O2A Co2 H1A1 70.3(14) . . ? N2A Co2 H1A1 104.5(14) . . ? N4A Co2 H1A1 147.0(8) . . ? Co2 O1A H1A1 73(3) . . ? Co2 O1A H2A1 120(3) . . ? H1A1 O1A H2A1 82(4) . . ? Co2 O2A H2A 109.5 . . ? C8A N1A C1A 113.2(4) . . ? C8A N1A Co2 109.0(2) . . ? C1A N1A Co2 109.8(2) . . ? C8A N1A H1A 108.2 . . ? C1A N1A H1A 108.2 . . ? Co2 N1A H1A 108.2 . . ? N1A C1A C2A 110.2(3) . . ? N1A C1A H11A 109.6 . . ? C2A C1A H11A 109.6 . . ? N1A C1A H12A 109.6 . . ? C2A C1A H12A 109.6 . . ? H11A C1A H12A 108.1 . . ? N2A C2A C1A 107.9(3) . . ? N2A C2A H21A 110.1 . . ? C1A C2A H21A 110.1 . . ? N2A C2A H22A 110.1 . . ? C1A C2A H22A 110.1 . . ? H21A C2A H22A 108.4 . . ? C2A N2A C3A 111.3(3) . . ? C2A N2A C9A 107.4(3) . . ? C3A N2A C9A 109.9(3) . . ? C2A N2A Co2 103.6(2) . . ? C3A N2A Co2 104.7(3) . . ? C9A N2A Co2 119.8(3) . . ? N2A C3A C4A 110.1(3) . . ? N2A C3A H31A 109.6 . . ? C4A C3A H31A 109.6 . . ? N2A C3A H32A 109.6 . . ? C4A C3A H32A 109.6 . . ? H31A C3A H32A 108.2 . . ? N3A C4A C3A 110.8(3) . . ? N3A C4A H41A 109.5 . . ? C3A C4A H41A 109.5 . . ? N3A C4A H42A 109.5 . . ? C3A C4A H42A 109.5 . . ? H41A C4A H42A 108.1 . . ? C4A N3A C5A 114.7(4) . . ? C4A N3A Co2 110.3(3) . . ? C5A N3A Co2 109.6(3) . . ? C4A N3A H3A 107.3 . . ? C5A N3A H3A 107.3 . . ? Co2 N3A H3A 107.3 . . ? N3A C5A C6A 109.8(3) . . ? N3A C5A H51A 109.7 . . ? C6A C5A H51A 109.7 . . ? N3A C5A H52A 109.7 . . ? C6A C5A H52A 109.7 . . ? H51A C5A H52A 108.2 . . ? N4A C6A C5A 109.5(3) . . ? N4A C6A H61A 109.8 . . ? C5A C6A H61A 109.8 . . ? N4A C6A H62A 109.8 . . ? C5A C6A H62A 109.8 . . ? H61A C6A H62A 108.2 . . ? C7A N4A C6A 112.4(3) . . ? C7A N4A C11A 108.1(3) . . ? C6A N4A C11A 109.5(3) . . ? C7A N4A Co2 102.7(2) . . ? C6A N4A Co2 102.1(2) . . ? C11A N4A Co2 121.9(2) . . ? N4A C7A C8A 107.3(3) . . ? N4A C7A H71A 110.3 . . ? C8A C7A H71A 110.3 . . ? N4A C7A H72A 110.3 . . ? C8A C7A H72A 110.3 . . ? H71A C7A H72A 108.5 . . ? N1A C8A C7A 110.2(4) . . ? N1A C8A H81A 109.6 . . ? C7A C8A H81A 109.6 . . ? N1A C8A H82A 109.6 . . ? C7A C8A H82A 109.6 . . ? H81A C8A H82A 108.1 . . ? C10A C9A N2A 115.6(4) . . ? C10A C9A H91A 108.4 . . ? N2A C9A H91A 108.4 . . ? C10A C9A H92A 108.4 . . ? N2A C9A H92A 108.4 . . ? H91A C9A H92A 107.5 . . ? C11A C10A C9A 112.1(4) . . ? C11A C10A H11B 109.2 . . ? C9A C10A H11B 109.2 . . ? C11A C10A H12B 109.2 . . ? C9A C10A H12B 109.2 . . ? H11B C10A H12B 107.9 . . ? C10A C11A N4A 115.7(3) . . ? C10A C11A H21B 108.3 . . ? N4A C11A H21B 108.3 . . ? C10A C11A H22B 108.3 . . ? N4A C11A H22B 108.3 . . ? H21B C11A H22B 107.4 . . ? O5 Cl1 O6 113.9(4) . . ? O5 Cl1 O4 108.2(3) . . ? O6 Cl1 O4 107.0(4) . . ? O5 Cl1 O3 110.2(3) . . ? O6 Cl1 O3 109.7(3) . . ? O4 Cl1 O3 107.6(2) . . ? O9 Cl2 O8 110.0(2) . . ? O9 Cl2 O10 110.4(2) . . ? O8 Cl2 O10 109.7(2) . . ? O9 Cl2 O7 109.0(2) . . ? O8 Cl2 O7 109.5(2) . . ? O10 Cl2 O7 108.3(2) . . ? O12' Cl3 O14 140.4(8) . . ? O12' Cl3 O13 76.8(9) . . ? O14 Cl3 O13 110.8(5) . . ? O12' Cl3 O11 104.9(7) . . ? O14 Cl3 O11 107.7(3) . . ? O13 Cl3 O11 111.1(3) . . ? O12' Cl3 O14' 114.6(10) . . ? O14 Cl3 O14' 29.1(4) . . ? O13 Cl3 O14' 126.4(6) . . ? O11 Cl3 O14' 115.0(5) . . ? O12' Cl3 O12 36.1(7) . . ? O14 Cl3 O12 110.1(5) . . ? O13 Cl3 O12 107.8(4) . . ? O11 Cl3 O12 109.4(3) . . ? O14' Cl3 O12 81.3(6) . . ? O12' Cl3 O13' 112.5(13) . . ? O14 Cl3 O13' 75.5(11) . . ? O13 Cl3 O13' 37.8(9) . . ? O11 Cl3 O13' 111.4(8) . . ? O14' Cl3 O13' 98.7(11) . . ? O12 Cl3 O13' 134.6(9) . . ? O12' O12 Cl3 64.5(11) . . ? O12 O12' Cl3 79.4(14) . . ? O12 O12' O13 124.1(15) . . ? Cl3 O12' O13 53.0(6) . . ? O13' O13 Cl3 77.7(13) . . ? O13' O13 O12' 125.0(15) . . ? Cl3 O13 O12' 50.2(7) . . ? O13 O13' Cl3 64.5(16) . . ? O13 O13' O14 111(2) . . ? Cl3 O13' O14 49.0(6) . . ? O14' O14 Cl3 78.5(13) . . ? O14' O14 O13' 121.5(17) . . ? Cl3 O14 O13' 55.5(10) . . ? O14 O14' Cl3 72.5(13) . . ? O17' Cl4 O15' 128(2) . . ? O17' Cl4 O16 94.8(12) . . ? O15' Cl4 O16 101.6(16) . . ? O17' Cl4 O15 135.4(11) . . ? O15' Cl4 O15 38.3(17) . . ? O16 Cl4 O15 126.6(5) . . ? O17' Cl4 O17 36.1(12) . . ? O15' Cl4 O17 135.0(15) . . ? O16 Cl4 O17 118.6(5) . . ? O15 Cl4 O17 114.0(4) . . ? O17' Cl4 O16' 111.4(18) . . ? O15' Cl4 O16' 69(2) . . ? O16 Cl4 O16' 32.4(12) . . ? O15 Cl4 O16' 99.8(14) . . ? O17 Cl4 O16' 145.0(14) . . ? O17' Cl4 O18' 113.1(14) . . ? O15' Cl4 O18' 116.0(19) . . ? O16 Cl4 O18' 90.0(5) . . ? O15 Cl4 O18' 85.5(5) . . ? O17 Cl4 O18' 85.3(5) . . ? O16' Cl4 O18' 107.1(13) . . ? O17' Cl4 O18 61.2(14) . . ? O15' Cl4 O18 67.5(18) . . ? O16 Cl4 O18 99.2(5) . . ? O15 Cl4 O18 93.1(5) . . ? O17 Cl4 O18 85.7(5) . . ? O16' Cl4 O18 83.5(13) . . ? O18' Cl4 O18 169.4(4) . . ? O15' O15 Cl4 69(2) . . ? O15 O15' Cl4 73(3) . . ? O15 O15' O16' 118(4) . . ? Cl4 O15' O16' 58.4(18) . . ? O15 O15' O18 116(3) . . ? Cl4 O15' O18 66.9(13) . . ? O16' O15' O18 79.3(18) . . ? O16' O16 Cl4 79(2) . . ? O16 O16' Cl4 69(2) . . ? O16 O16' O15' 121(3) . . ? Cl4 O16' O15' 52.2(16) . . ? O17' O17 Cl4 66.5(15) . . ? O17 O17' Cl4 77(2) . . ? O17 O17' O18 120(2) . . ? Cl4 O17' O18 72.1(11) . . ? O17' O18 Cl4 46.7(10) . . ? O17' O18 O15' 91.9(17) . . ? Cl4 O18 O15' 45.6(13) . . ? O17' O18 O40 116.2(10) . . ? Cl4 O18 O40 154.2(6) . . ? O15' O18 O40 139.4(13) . . ? H201 O20 H202 134(5) . . ? H301 O30 H302 94(6) . . ? O40' O40 O18 163.1(7) . . ? O40 O40' O50 142.8(7) . . ? 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 Co1 N1 C1 C2 -9.5(4) . . . . ? N1 C1 C2 N2 36.3(5) . . . . ? C1 C2 N2 Co1 -44.2(4) . . . . ? C2 N2 Co1 N1 32.1(3) . . . . ? N2 Co1 N1 C1 -12.6(3) . . . . ? Co1 N2 C3 C4 48.9(4) . . . . ? N2 C3 C4 N3 -40.7(4) . . . . ? C3 C4 N3 Co1 11.8(4) . . . . ? C4 N3 Co1 N2 13.4(3) . . . . ? N3 Co1 N2 C3 -35.6(3) . . . . ? Co1 N3 C5 C6 -14.5(4) . . . . ? N3 C5 C6 N4 42.4(5) . . . . ? C5 C6 N4 Co1 -48.1(3) . . . . ? C6 N4 Co1 N3 34.0(3) . . . . ? N4 Co1 N3 C5 -10.7(3) . . . . ? Co1 N4 C7 C8 47.8(4) . . . . ? N4 C7 C8 N1 -38.8(5) . . . . ? C7 C8 N1 Co1 9.4(4) . . . . ? C8 N1 Co1 N4 14.9(3) . . . . ? N1 Co1 N4 C7 -35.1(3) . . . . ? Co1 N2 C9 C10 36.2(5) . . . . ? N2 C9 C10 C11 -69.4(5) . . . . ? C9 C10 C11 N4 65.6(5) . . . . ? C10 C11 N4 Co1 -30.5(5) . . . . ? C11 N4 Co1 N2 0.8(3) . . . . ? N4 Co1 N2 C9 -4.2(3) . . . . ? Co1 N2 C9 C10 36.2(5) . . . . ? Co2 N1A C1A C2A 8.9(4) . . . . ? N1A C1A C2A N2A -38.4(4) . . . . ? C1A C2A N2A Co2 48.5(3) . . . . ? C2A N2A Co2 N1A -36.2(2) . . . . ? N2A Co2 N1A C1A 15.6(3) . . . . ? Co2 N2A C3A C4A -42.5(4) . . . . ? N2A C3A C4A N3A 33.6(5) . . . . ? C3A C4A N3A Co2 -7.5(5) . . . . ? C4A N3A Co2 N2A -13.8(3) . . . . ? N3A Co2 N2A C3A 31.5(2) . . . . ? Co2 N3A C5A C6A 9.9(4) . . . . ? N3A C5A C6A N4A -39.5(5) . . . . ? C5A C6A N4A Co2 48.1(3) . . . . ? C6A N4A Co2 N3A -34.8(3) . . . . ? N4A Co2 N3A C5A 14.5(3) . . . . ? Co2 N4A C7A C8A -49.5(4) . . . . ? N4A C7A C8A N1A 44.6(5) . . . . ? C7A C8A N1A Co2 -16.4(5) . . . . ? C8A N1A Co2 N4A -10.0(3) . . . . ? N1A Co2 N4A C7A 33.7(3) . . . . ? Co2 N2A C9A C10A 37.7(5) . . . . ? N2A C9A C10A C11A -70.6(5) . . . . ? C9A C10A C11A N4A 64.4(5) . . . . ? C10A C11A N4A Co2 -28.0(5) . . . . ? C11A N4A Co2 N2A -0.4(3) . . . . ? N4A Co2 N2A C9A -4.3(3) . . . . ? Co2 N2A C9A C10A 37.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O1 O2 0.931(19) 1.71(3) 2.500(4) 141(4) 3 O1 H2O1 O20 0.893(19) 1.76(2) 2.643(4) 169(5) 4_565 O2A H2A O1A 0.84 1.65 2.479(4) 170.2 3_676 O20 H201 O30 0.90(2) 1.88(3) 2.692(6) 148(5) . N1 H1 O4 0.93 2.26 3.100(6) 150.3 3 N3 H3 O2 0.93 2.14 2.973(4) 148.9 3 N1A H1A O1A 0.93 2.29 3.105(5) 146.7 3_676 N3A H3A O40 0.93 2.03 2.905(8) 157.0 3_666 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.754 _refine_diff_density_min -1.340 _refine_diff_density_rms 0.153 # Attachment 'Fig4.cif' data_lb0805k _database_code_depnum_ccdc_archive 'CCDC 642046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(C11H24N4)(SO4)](CF3SO3)' _chemical_formula_sum 'C12 H24 Co F3 N4 O7 S2' _chemical_formula_weight 516.40 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 8.2636(4) _cell_length_b 16.6364(7) _cell_length_c 13.8078(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.6080(10) _cell_angle_gamma 90.00 _cell_volume 1892.11(15) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 22308 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.00 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8726 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS,ver2.03 (Sheldrick,2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD Platform' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22308 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4550 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS,1998)' _computing_cell_refinement 'SAINT (Bruker AXS,1998)' _computing_data_reduction 'SAINT (Bruker AXS,1998)' _computing_structure_solution 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_structure_refinement 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_molecular_graphics 'SHELXTL,ver.6.12 (Sheldrick,2001)' _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^)+(0.0380P)^2^+2.4593P] 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 4550 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.67247(3) 0.175142(15) 0.636817(18) 0.00936(8) Uani 1 1 d . . . N1 N 0.6512(2) 0.28614(10) 0.67753(12) 0.0146(3) Uani 1 1 d . . . H1 H 0.5525 0.3054 0.6498 0.018 Uiso 1 1 calc R . . C1 C 0.6465(3) 0.28947(12) 0.78620(15) 0.0170(4) Uani 1 1 d . . . H11 H 0.5624 0.3279 0.8040 0.020 Uiso 1 1 calc R . . H12 H 0.7529 0.3072 0.8170 0.020 Uiso 1 1 calc R . . C2 C 0.6073(3) 0.20567(12) 0.82044(14) 0.0147(4) Uani 1 1 d . . . H21 H 0.6269 0.2022 0.8920 0.018 Uiso 1 1 calc R . . H22 H 0.4918 0.1930 0.8024 0.018 Uiso 1 1 calc R . . N2 N 0.7149(2) 0.14715(10) 0.77272(12) 0.0125(3) Uani 1 1 d . . . C3 C 0.6493(3) 0.06306(12) 0.77529(14) 0.0146(4) Uani 1 1 d . . . H31 H 0.5294 0.0638 0.7644 0.017 Uiso 1 1 calc R . . H32 H 0.6792 0.0384 0.8395 0.017 Uiso 1 1 calc R . . C4 C 0.7216(3) 0.01483(12) 0.69578(14) 0.0165(4) Uani 1 1 d . . . H41 H 0.8366 0.0021 0.7152 0.020 Uiso 1 1 calc R . . H42 H 0.6616 -0.0363 0.6850 0.020 Uiso 1 1 calc R . . N3 N 0.7095(2) 0.06396(10) 0.60416(12) 0.0120(3) Uani 1 1 d . . . H3 H 0.6195 0.0460 0.5653 0.014 Uiso 1 1 calc R . . C5 C 0.8548(3) 0.05835(13) 0.54568(15) 0.0178(4) Uani 1 1 d . . . H51 H 0.8282 0.0251 0.4871 0.021 Uiso 1 1 calc R . . H52 H 0.9460 0.0325 0.5849 0.021 Uiso 1 1 calc R . . C6 C 0.9040(2) 0.14237(13) 0.51581(15) 0.0170(4) Uani 1 1 d . . . H61 H 1.0175 0.1420 0.4978 0.020 Uiso 1 1 calc R . . H62 H 0.8330 0.1605 0.4588 0.020 Uiso 1 1 calc R . . N4 N 0.8880(2) 0.19886(10) 0.60020(12) 0.0143(3) Uani 1 1 d . . . C7 C 0.8732(3) 0.28470(13) 0.56637(16) 0.0201(4) Uani 1 1 d . . . H71 H 0.8131 0.2866 0.5014 0.024 Uiso 1 1 calc R . . H72 H 0.9827 0.3074 0.5606 0.024 Uiso 1 1 calc R . . C8 C 0.7838(3) 0.33505(13) 0.63804(17) 0.0204(4) Uani 1 1 d . . . H81 H 0.8613 0.3530 0.6921 0.024 Uiso 1 1 calc R . . H82 H 0.7366 0.3833 0.6047 0.024 Uiso 1 1 calc R . . C9 C 0.8854(3) 0.14862(13) 0.82053(15) 0.0172(4) Uani 1 1 d . . . H91 H 0.9306 0.0936 0.8182 0.021 Uiso 1 1 calc R . . H92 H 0.8798 0.1628 0.8898 0.021 Uiso 1 1 calc R . . C10 C 1.0034(3) 0.20609(14) 0.77702(16) 0.0195(4) Uani 1 1 d . . . H101 H 0.9603 0.2615 0.7800 0.023 Uiso 1 1 calc R . . H102 H 1.1085 0.2045 0.8169 0.023 Uiso 1 1 calc R . . C11 C 1.0325(3) 0.18659(14) 0.67270(16) 0.0197(4) Uani 1 1 d . . . H111 H 1.1229 0.2204 0.6532 0.024 Uiso 1 1 calc R . . H112 H 1.0675 0.1298 0.6694 0.024 Uiso 1 1 calc R . . S1 S 0.40774(6) 0.16757(3) 0.52912(3) 0.01325(11) Uani 1 1 d . . . O1 O 0.43924(16) 0.15649(9) 0.63855(10) 0.0129(3) Uani 1 1 d . . . O2 O 0.57375(17) 0.19988(9) 0.50704(10) 0.0146(3) Uani 1 1 d . . . O3 O 0.3775(2) 0.09062(10) 0.48245(12) 0.0260(4) Uani 1 1 d . . . O4 O 0.28269(19) 0.22621(11) 0.50567(12) 0.0251(4) Uani 1 1 d . . . S2 S 0.76232(7) 0.07804(4) 0.21774(5) 0.02458(14) Uani 1 1 d . . . O5 O 0.5987(2) 0.07262(11) 0.24114(16) 0.0360(4) Uani 1 1 d . . . O6 O 0.8791(2) 0.03359(13) 0.27943(17) 0.0464(6) Uani 1 1 d . . . O7 O 0.8119(3) 0.15806(13) 0.1942(2) 0.0536(7) Uani 1 1 d . . . C12 C 0.7614(5) 0.0252(2) 0.1031(2) 0.0598(11) Uani 1 1 d . . . F1 F 0.9070(4) 0.0288(2) 0.0686(2) 0.1239(14) Uani 1 1 d . . . F2 F 0.7252(3) -0.05273(14) 0.11203(18) 0.0778(8) Uani 1 1 d . . . F3 F 0.6547(4) 0.05722(17) 0.03673(16) 0.1053(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.00894(13) 0.00972(13) 0.00934(13) -0.00089(9) 0.00016(9) -0.00067(9) N1 0.0179(9) 0.0115(8) 0.0145(8) -0.0005(6) 0.0012(6) 0.0003(6) C1 0.0223(10) 0.0153(9) 0.0134(9) -0.0040(7) 0.0013(8) 0.0014(8) C2 0.0161(9) 0.0162(9) 0.0121(9) -0.0040(7) 0.0028(7) 0.0002(8) N2 0.0121(8) 0.0134(8) 0.0116(7) -0.0003(6) -0.0001(6) 0.0000(6) C3 0.0181(10) 0.0129(9) 0.0125(9) 0.0020(7) 0.0003(7) -0.0012(7) C4 0.0219(10) 0.0121(9) 0.0155(9) 0.0007(7) 0.0010(8) 0.0022(8) N3 0.0109(8) 0.0123(8) 0.0128(8) -0.0017(6) 0.0003(6) -0.0004(6) C5 0.0154(10) 0.0196(10) 0.0190(10) -0.0049(8) 0.0049(8) 0.0028(8) C6 0.0132(9) 0.0239(11) 0.0146(9) -0.0051(8) 0.0049(7) -0.0013(8) N4 0.0116(8) 0.0169(8) 0.0148(8) -0.0031(7) 0.0024(6) -0.0028(6) C7 0.0231(11) 0.0177(10) 0.0200(10) 0.0013(8) 0.0046(8) -0.0085(8) C8 0.0242(11) 0.0126(9) 0.0243(11) -0.0003(8) 0.0028(9) -0.0061(8) C9 0.0139(9) 0.0207(10) 0.0160(9) -0.0002(8) -0.0046(8) 0.0010(8) C10 0.0117(9) 0.0264(11) 0.0199(10) -0.0034(9) -0.0028(8) -0.0014(8) C11 0.0101(9) 0.0279(11) 0.0207(10) -0.0041(9) -0.0004(8) -0.0017(8) S1 0.0114(2) 0.0168(2) 0.0111(2) -0.00027(17) -0.00170(17) -0.00049(17) O1 0.0094(6) 0.0182(7) 0.0110(6) 0.0012(5) -0.0001(5) -0.0007(5) O2 0.0133(7) 0.0204(7) 0.0099(6) 0.0022(5) 0.0001(5) -0.0023(6) O3 0.0321(9) 0.0259(9) 0.0197(8) -0.0078(7) 0.0004(7) -0.0117(7) O4 0.0179(8) 0.0358(9) 0.0213(8) 0.0087(7) 0.0003(6) 0.0101(7) S2 0.0122(2) 0.0229(3) 0.0380(3) 0.0107(2) -0.0016(2) -0.0001(2) O5 0.0190(9) 0.0291(9) 0.0610(13) -0.0034(9) 0.0096(8) -0.0018(7) O6 0.0329(11) 0.0432(12) 0.0602(14) 0.0185(10) -0.0139(10) 0.0094(9) O7 0.0275(11) 0.0342(11) 0.098(2) 0.0289(12) 0.0000(11) -0.0069(9) C12 0.082(3) 0.061(2) 0.0381(17) 0.0089(16) 0.0156(17) 0.042(2) F1 0.145(3) 0.137(3) 0.104(2) 0.050(2) 0.101(2) 0.081(2) F2 0.111(2) 0.0514(13) 0.0690(15) -0.0245(11) -0.0064(14) 0.0377(13) F3 0.172(3) 0.101(2) 0.0365(12) -0.0121(12) -0.0311(15) 0.079(2) _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 Co N4 1.9308(17) . ? Co N3 1.9339(16) . ? Co N2 1.9379(16) . ? Co N1 1.9424(17) . ? Co O2 1.9522(14) . ? Co O1 1.9541(14) . ? Co S1 2.5476(5) . ? N1 C8 1.502(3) . ? N1 C1 1.505(3) . ? N1 H1 0.9300 . ? C1 C2 1.516(3) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? C2 N2 1.505(3) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? N2 C3 1.502(2) . ? N2 C9 1.507(3) . ? C3 C4 1.520(3) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 N3 1.503(3) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? N3 C5 1.503(3) . ? N3 H3 0.9300 . ? C5 C6 1.522(3) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 N4 1.511(3) . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N4 C7 1.505(3) . ? N4 C11 1.509(3) . ? C7 C8 1.531(3) . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 C10 1.523(3) . ? C9 H91 0.9900 . ? C9 H92 0.9900 . ? C10 C11 1.514(3) . ? C10 H101 0.9900 . ? C10 H102 0.9900 . ? C11 H111 0.9900 . ? C11 H112 0.9900 . ? S1 O4 1.4390(16) . ? S1 O3 1.4458(16) . ? S1 O1 1.5237(14) . ? S1 O2 1.5268(15) . ? S2 O5 1.4183(18) . ? S2 O7 1.438(2) . ? S2 O6 1.4391(19) . ? S2 C12 1.809(4) . ? C12 F3 1.331(4) . ? C12 F1 1.331(5) . ? C12 F2 1.339(5) . ? 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 N4 Co N3 88.16(7) . . ? N4 Co N2 101.75(7) . . ? N3 Co N2 88.64(7) . . ? N4 Co N1 89.33(7) . . ? N3 Co N1 175.15(7) . . ? N2 Co N1 87.81(7) . . ? N4 Co O2 92.45(7) . . ? N3 Co O2 92.86(7) . . ? N2 Co O2 165.76(7) . . ? N1 Co O2 91.40(7) . . ? N4 Co O1 165.25(7) . . ? N3 Co O1 91.47(7) . . ? N2 Co O1 92.98(6) . . ? N1 Co O1 92.02(7) . . ? O2 Co O1 72.83(6) . . ? N4 Co S1 128.62(5) . . ? N3 Co S1 87.77(5) . . ? N2 Co S1 129.31(5) . . ? N1 Co S1 97.04(5) . . ? O2 Co S1 36.75(4) . . ? O1 Co S1 36.66(4) . . ? C8 N1 C1 114.84(16) . . ? C8 N1 Co 108.93(13) . . ? C1 N1 Co 109.49(12) . . ? C8 N1 H1 107.8 . . ? C1 N1 H1 107.8 . . ? Co N1 H1 107.8 . . ? N1 C1 C2 107.48(16) . . ? N1 C1 H11 110.2 . . ? C2 C1 H11 110.2 . . ? N1 C1 H12 110.2 . . ? C2 C1 H12 110.2 . . ? H11 C1 H12 108.5 . . ? N2 C2 C1 108.04(16) . . ? N2 C2 H21 110.1 . . ? C1 C2 H21 110.1 . . ? N2 C2 H22 110.1 . . ? C1 C2 H22 110.1 . . ? H21 C2 H22 108.4 . . ? C3 N2 C2 111.41(15) . . ? C3 N2 C9 109.34(15) . . ? C2 N2 C9 111.22(15) . . ? C3 N2 Co 102.07(11) . . ? C2 N2 Co 101.61(12) . . ? C9 N2 Co 120.68(13) . . ? N2 C3 C4 108.13(16) . . ? N2 C3 H31 110.1 . . ? C4 C3 H31 110.1 . . ? N2 C3 H32 110.1 . . ? C4 C3 H32 110.1 . . ? H31 C3 H32 108.4 . . ? N3 C4 C3 108.50(16) . . ? N3 C4 H41 110.0 . . ? C3 C4 H41 110.0 . . ? N3 C4 H42 110.0 . . ? C3 C4 H42 110.0 . . ? H41 C4 H42 108.4 . . ? C4 N3 C5 114.61(16) . . ? C4 N3 Co 108.97(12) . . ? C5 N3 Co 109.44(12) . . ? C4 N3 H3 107.9 . . ? C5 N3 H3 107.9 . . ? Co N3 H3 107.9 . . ? N3 C5 C6 109.31(16) . . ? N3 C5 H51 109.8 . . ? C6 C5 H51 109.8 . . ? N3 C5 H52 109.8 . . ? C6 C5 H52 109.8 . . ? H51 C5 H52 108.3 . . ? N4 C6 C5 108.69(16) . . ? N4 C6 H61 110.0 . . ? C5 C6 H61 110.0 . . ? N4 C6 H62 110.0 . . ? C5 C6 H62 110.0 . . ? H61 C6 H62 108.3 . . ? C7 N4 C11 112.01(16) . . ? C7 N4 C6 111.15(16) . . ? C11 N4 C6 108.30(16) . . ? C7 N4 Co 102.79(13) . . ? C11 N4 Co 119.73(13) . . ? C6 N4 Co 102.38(12) . . ? N4 C7 C8 110.50(17) . . ? N4 C7 H71 109.6 . . ? C8 C7 H71 109.6 . . ? N4 C7 H72 109.6 . . ? C8 C7 H72 109.6 . . ? H71 C7 H72 108.1 . . ? N1 C8 C7 110.01(16) . . ? N1 C8 H81 109.7 . . ? C7 C8 H81 109.7 . . ? N1 C8 H82 109.7 . . ? C7 C8 H82 109.7 . . ? H81 C8 H82 108.2 . . ? N2 C9 C10 116.30(17) . . ? N2 C9 H91 108.2 . . ? C10 C9 H91 108.2 . . ? N2 C9 H92 108.2 . . ? C10 C9 H92 108.2 . . ? H91 C9 H92 107.4 . . ? C11 C10 C9 113.33(18) . . ? C11 C10 H101 108.9 . . ? C9 C10 H101 108.9 . . ? C11 C10 H102 108.9 . . ? C9 C10 H102 108.9 . . ? H101 C10 H102 107.7 . . ? N4 C11 C10 115.13(17) . . ? N4 C11 H111 108.5 . . ? C10 C11 H111 108.5 . . ? N4 C11 H112 108.5 . . ? C10 C11 H112 108.5 . . ? H111 C11 H112 107.5 . . ? O4 S1 O3 113.88(11) . . ? O4 S1 O1 111.56(9) . . ? O3 S1 O1 110.15(9) . . ? O4 S1 O2 110.91(9) . . ? O3 S1 O2 110.40(9) . . ? O1 S1 O2 98.97(8) . . ? O4 S1 Co 131.70(8) . . ? O3 S1 Co 114.42(8) . . ? O1 S1 Co 49.97(5) . . ? O2 S1 Co 49.91(5) . . ? S1 O1 Co 93.37(7) . . ? S1 O2 Co 93.35(7) . . ? O5 S2 O7 113.85(12) . . ? O5 S2 O6 116.02(13) . . ? O7 S2 O6 114.84(13) . . ? O5 S2 C12 103.37(17) . . ? O7 S2 C12 103.47(18) . . ? O6 S2 C12 102.94(15) . . ? F3 C12 F1 107.7(3) . . ? F3 C12 F2 108.1(4) . . ? F1 C12 F2 106.9(3) . . ? F3 C12 S2 111.4(2) . . ? F1 C12 S2 110.5(3) . . ? F2 C12 S2 112.0(2) . . ? 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 Co N1 C1 C2 -17.40(19) . . . . ? N1 C1 C2 N2 47.2(2) . . . . ? C1 C2 N2 Co -53.13(16) . . . . ? C2 N2 Co N1 34.77(12) . . . . ? N2 Co N1 C1 -10.37(13) . . . . ? Co N2 C3 C4 50.87(16) . . . . ? N2 C3 C4 N3 -46.0(2) . . . . ? C3 C4 N3 Co 17.57(19) . . . . ? C4 N3 Co N2 9.38(13) . . . . ? N3 Co N2 C3 -33.38(12) . . . . ? Co N3 C5 C6 -10.61(19) . . . . ? N3 C5 C6 N4 40.3(2) . . . . ? C5 C6 N4 Co -49.64(17) . . . . ? C6 N4 Co N3 35.68(13) . . . . ? N4 Co N3 C5 -14.85(13) . . . . ? Co N4 C7 C8 45.70(18) . . . . ? N4 C7 C8 N1 -37.0(2) . . . . ? C7 C8 N1 Co 9.1(2) . . . . ? C8 N1 Co N4 14.16(14) . . . . ? N1 Co N4 C7 -33.09(12) . . . . ? Co N2 C9 C10 27.0(2) . . . . ? N2 C9 C10 C11 -62.4(2) . . . . ? C9 C10 C11 N4 67.4(2) . . . . ? C10 C11 N4 Co -36.0(2) . . . . ? C11 N4 Co N2 4.19(16) . . . . ? N4 Co N2 C9 0.16(16) . . . . ? Co N2 C9 C10 27.0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O7 0.93 2.21 2.980(3) 139.4 4_566 N3 H3 O3 0.93 2.37 2.902(2) 116.3 3_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.679 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.080 data_js22ak _database_code_depnum_ccdc_archive 'CCDC 642047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(C11H24N4)(HCOO)](ZnCl4)' _chemical_formula_sum 'C11 H25 Cl4 Co N4 O2 Zn' _chemical_formula_weight 512.46 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 17.2058(7) _cell_length_b 11.4473(5) _cell_length_c 9.5525(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1881.46(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12829 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.99 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 2.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7777 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS,ver2.03 (Sheldrick,2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD Platform' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12829 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.99 _reflns_number_total 2379 _reflns_number_gt 2257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS,1998)' _computing_cell_refinement 'SAINT (Bruker AXS,1998)' _computing_data_reduction 'SAINT (Bruker AXS,1998)' _computing_structure_solution 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_structure_refinement 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_molecular_graphics 'SHELXTL,ver.6.12 (Sheldrick,2001)' _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^)+(0.0244P)^2^+0.8925P] 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 2379 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0490 _refine_ls_wR_factor_gt 0.0483 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Co Co 0.445433(14) 0.2500 0.14088(2) 0.01028(7) Uani 1 2 d S . . N1 N 0.33739(9) 0.2500 0.08103(17) 0.0158(3) Uani 1 2 d S . . H1 H 0.3364 0.2500 -0.0163 0.019 Uiso 1 2 calc SR . . C1 C 0.29924(8) 0.13956(14) 0.13147(15) 0.0210(3) Uani 1 1 d . . . H11 H 0.2671 0.1055 0.0559 0.025 Uiso 1 1 calc R . . H12 H 0.2651 0.1568 0.2123 0.025 Uiso 1 1 calc R . . C2 C 0.36230(8) 0.05381(12) 0.17442(15) 0.0189(3) Uani 1 1 d . . . H21 H 0.3395 -0.0105 0.2304 0.023 Uiso 1 1 calc R . . H22 H 0.3871 0.0197 0.0903 0.023 Uiso 1 1 calc R . . N2 N 0.42163(6) 0.11878(10) 0.25989(11) 0.0132(2) Uani 1 1 d . . . C3 C 0.49788(8) 0.05422(12) 0.26332(14) 0.0162(3) Uani 1 1 d . . . H31 H 0.5076 0.0171 0.1713 0.019 Uiso 1 1 calc R . . H32 H 0.4959 -0.0080 0.3352 0.019 Uiso 1 1 calc R . . C4 C 0.56333(8) 0.13911(12) 0.29722(15) 0.0160(3) Uani 1 1 d . . . H41 H 0.5643 0.1556 0.3989 0.019 Uiso 1 1 calc R . . H42 H 0.6140 0.1047 0.2704 0.019 Uiso 1 1 calc R . . C5 C 0.39018(8) 0.13954(12) 0.40477(14) 0.0170(3) Uani 1 1 d . . . H51 H 0.4043 0.0719 0.4641 0.020 Uiso 1 1 calc R . . H52 H 0.3328 0.1423 0.3992 0.020 Uiso 1 1 calc R . . C6 C 0.41820(11) 0.2500 0.4768(2) 0.0173(4) Uani 1 2 d S . . H61 H 0.4757 0.2500 0.4787 0.021 Uiso 1 2 calc SR . . H62 H 0.3996 0.2500 0.5748 0.021 Uiso 1 2 calc SR . . N3 N 0.54958(9) 0.2500 0.21685(16) 0.0123(3) Uani 1 2 d S . . H3 H 0.5838 0.2500 0.1415 0.015 Uiso 1 2 calc SR . . O1 O 0.47965(5) 0.15565(9) -0.02025(10) 0.0172(2) Uani 1 1 d . . . C7 C 0.49329(12) 0.2500 -0.0848(2) 0.0192(4) Uani 1 2 d S . . H7 H 0.5134(14) 0.2500 -0.181(3) 0.021(6) Uiso 1 2 d S . . Zn Zn 0.236081(12) 0.2500 0.71949(2) 0.01241(7) Uani 1 2 d S . . Cl1 Cl 0.313321(19) 0.09483(3) 0.76666(4) 0.02020(8) Uani 1 1 d . . . Cl2 Cl 0.13134(3) 0.2500 0.86511(5) 0.02247(11) Uani 1 2 d S . . Cl3 Cl 0.19407(3) 0.2500 0.49373(5) 0.02513(12) Uani 1 2 d S . . 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 Co 0.00958(12) 0.01177(12) 0.00948(12) 0.000 0.00058(8) 0.000 N1 0.0119(7) 0.0223(8) 0.0131(7) 0.000 -0.0005(6) 0.000 C1 0.0138(6) 0.0287(8) 0.0205(7) 0.0020(6) -0.0021(5) -0.0067(6) C2 0.0185(7) 0.0179(7) 0.0202(7) -0.0009(5) -0.0011(5) -0.0080(5) N2 0.0129(5) 0.0133(5) 0.0133(5) -0.0002(4) 0.0005(4) -0.0016(4) C3 0.0172(6) 0.0114(6) 0.0201(6) 0.0012(5) 0.0001(5) 0.0026(5) C4 0.0150(6) 0.0149(6) 0.0180(6) 0.0008(5) -0.0023(5) 0.0036(5) C5 0.0168(6) 0.0207(7) 0.0135(6) 0.0035(5) 0.0041(5) -0.0017(5) C6 0.0169(9) 0.0234(10) 0.0117(8) 0.000 0.0020(7) 0.000 N3 0.0107(7) 0.0145(8) 0.0117(7) 0.000 0.0013(6) 0.000 O1 0.0173(5) 0.0203(5) 0.0142(4) -0.0040(4) 0.0018(4) -0.0006(4) C7 0.0158(9) 0.0290(11) 0.0128(9) 0.000 0.0026(7) 0.000 Zn 0.01100(11) 0.01423(11) 0.01201(11) 0.000 -0.00076(7) 0.000 Cl1 0.01883(17) 0.01545(16) 0.02634(18) -0.00036(13) -0.00328(13) 0.00386(12) Cl2 0.0169(2) 0.0349(3) 0.0156(2) 0.000 0.00461(17) 0.000 Cl3 0.0132(2) 0.0495(3) 0.0127(2) 0.000 -0.00223(17) 0.000 _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 Co N2 1.9278(11) 7_565 ? Co N2 1.9278(11) . ? Co N3 1.9333(16) . ? Co N1 1.9449(16) . ? Co O1 1.9704(10) . ? Co O1 1.9704(10) 7_565 ? Co C7 2.308(2) . ? N1 C1 1.5038(16) . ? N1 C1 1.5038(16) 7_565 ? N1 H1 0.9300 . ? C1 C2 1.520(2) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? C2 N2 1.5038(17) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? N2 C5 1.5048(17) . ? N2 C3 1.5062(17) . ? C3 C4 1.5223(19) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 N3 1.5022(16) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? C5 C6 1.5180(17) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 C5 1.5180(17) 7_565 ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N3 C4 1.5022(16) 7_565 ? N3 H3 0.9300 . ? O1 C7 1.2657(14) . ? C7 O1 1.2657(14) 7_565 ? C7 H7 0.98(3) . ? Zn Cl1 2.2638(4) 7_565 ? Zn Cl1 2.2638(4) . ? Zn Cl3 2.2745(5) . ? Zn Cl2 2.2766(5) . ? 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 N2 Co N2 102.37(7) 7_565 . ? N2 Co N3 88.60(4) 7_565 . ? N2 Co N3 88.60(4) . . ? N2 Co N1 88.30(4) 7_565 . ? N2 Co N1 88.30(4) . . ? N3 Co N1 175.05(7) . . ? N2 Co O1 162.03(4) 7_565 . ? N2 Co O1 95.57(4) . . ? N3 Co O1 90.93(5) . . ? N1 Co O1 93.21(5) . . ? N2 Co O1 95.57(4) 7_565 7_565 ? N2 Co O1 162.03(4) . 7_565 ? N3 Co O1 90.93(5) . 7_565 ? N1 Co O1 93.21(5) . 7_565 ? O1 Co O1 66.48(6) . 7_565 ? N2 Co C7 128.80(3) 7_565 . ? N2 Co C7 128.80(3) . . ? N3 Co C7 91.15(7) . . ? N1 Co C7 93.80(7) . . ? O1 Co C7 33.24(3) . . ? O1 Co C7 33.24(3) 7_565 . ? C1 N1 C1 114.43(15) . 7_565 ? C1 N1 Co 108.84(8) . . ? C1 N1 Co 108.84(8) 7_565 . ? C1 N1 H1 108.2 . . ? C1 N1 H1 108.2 7_565 . ? Co N1 H1 108.2 . . ? N1 C1 C2 108.54(11) . . ? N1 C1 H11 110.0 . . ? C2 C1 H11 110.0 . . ? N1 C1 H12 110.0 . . ? C2 C1 H12 110.0 . . ? H11 C1 H12 108.4 . . ? N2 C2 C1 108.16(11) . . ? N2 C2 H21 110.1 . . ? C1 C2 H21 110.1 . . ? N2 C2 H22 110.1 . . ? C1 C2 H22 110.1 . . ? H21 C2 H22 108.4 . . ? C2 N2 C5 109.47(10) . . ? C2 N2 C3 111.13(11) . . ? C5 N2 C3 111.75(10) . . ? C2 N2 Co 102.09(8) . . ? C5 N2 Co 119.71(9) . . ? C3 N2 Co 102.13(8) . . ? N2 C3 C4 109.62(11) . . ? N2 C3 H31 109.7 . . ? C4 C3 H31 109.7 . . ? N2 C3 H32 109.7 . . ? C4 C3 H32 109.7 . . ? H31 C3 H32 108.2 . . ? N3 C4 C3 108.31(11) . . ? N3 C4 H41 110.0 . . ? C3 C4 H41 110.0 . . ? N3 C4 H42 110.0 . . ? C3 C4 H42 110.0 . . ? H41 C4 H42 108.4 . . ? N2 C5 C6 115.73(12) . . ? N2 C5 H51 108.3 . . ? C6 C5 H51 108.3 . . ? N2 C5 H52 108.3 . . ? C6 C5 H52 108.3 . . ? H51 C5 H52 107.4 . . ? C5 C6 C5 112.82(16) . 7_565 ? C5 C6 H61 109.0 . . ? C5 C6 H61 109.0 7_565 . ? C5 C6 H62 109.0 . . ? C5 C6 H62 109.0 7_565 . ? H61 C6 H62 107.8 . . ? C4 N3 C4 115.34(14) 7_565 . ? C4 N3 Co 109.74(8) 7_565 . ? C4 N3 Co 109.74(8) . . ? C4 N3 H3 107.2 7_565 . ? C4 N3 H3 107.2 . . ? Co N3 H3 107.2 . . ? C7 O1 Co 88.18(9) . . ? O1 C7 O1 117.15(17) . 7_565 ? O1 C7 Co 58.58(9) . . ? O1 C7 Co 58.58(9) 7_565 . ? O1 C7 H7 121.42(9) . . ? O1 C7 H7 121.42(9) 7_565 . ? Co C7 H7 179.7(15) . . ? Cl1 Zn Cl1 103.38(2) 7_565 . ? Cl1 Zn Cl3 112.044(13) 7_565 . ? Cl1 Zn Cl3 112.044(13) . . ? Cl1 Zn Cl2 110.065(13) 7_565 . ? Cl1 Zn Cl2 110.065(13) . . ? Cl3 Zn Cl2 109.13(2) . . ? 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 Co N1 C1 C2 -15.53(14) . . . . ? N1 C1 C2 N2 44.98(15) . . . . ? C1 C2 N2 Co -51.67(11) . . . . ? C2 N2 Co N1 34.85(9) . . . . ? N2 Co N1 C1 -11.45(10) . . . . ? Co N2 C3 C4 49.37(11) . . . . ? N2 C3 C4 N3 -41.62(14) . . . . ? C3 C4 N3 Co 12.71(13) . . . . ? C4 N3 Co N2 12.66(9) . . . . ? N3 Co N2 C3 -33.98(8) . . . . ? Co N2 C5 C6 -31.86(16) . . . . ? N2 C5 C6 C5 65.88(19) . . . 7_565 ? C5 C6 C5 N2 -65.88(19) . . 7_565 7_565 ? C6 C5 N2 Co 31.86(16) . 7_565 7_565 . ? C5 N2 Co N2 -1.74(12) 7_565 7_565 . . ? N2 Co N2 C5 1.74(12) 7_565 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl1 0.93 2.76 3.5135(14) 138.9 1_554 N3 H3 Cl3 0.93 2.30 3.1978(16) 163.5 6_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.417 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.092 # Attachment 'Fig6.cif' data_js1a _database_code_depnum_ccdc_archive 'CCDC 642048' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(C11H24N4)(NO3)](NO3)(ClO4)' _chemical_formula_sum 'C11 H24 Cl Co N6 O10' _chemical_formula_weight 494.74 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 monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.0240(6) _cell_length_b 13.3493(9) _cell_length_c 15.3487(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.272(2) _cell_angle_gamma 90.00 _cell_volume 1841.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6504 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 28.01 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8120 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS,ver2.03 (Sheldrick,2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'noemal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD Platform' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6504 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.01 _reflns_number_total 3458 _reflns_number_gt 3310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS,1998)' _computing_cell_refinement 'SAINT (Bruker AXS,1998)' _computing_data_reduction 'SAINT (Bruker AXS,1998)' _computing_structure_solution 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_structure_refinement 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_molecular_graphics 'SHELXTL,ver.6.12 (Sheldrick,2001)' _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^)+(0.0189P)^2^+0.2581P] 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 0.044(15) _refine_ls_number_reflns 3458 _refine_ls_number_parameters 262 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Co Co 0.02951(3) 0.14837(3) 0.26476(3) 0.01336(11) Uani 1 1 d . . . N1 N 0.0113(3) 0.2198(2) 0.3735(2) 0.0191(6) Uani 1 1 d . . . H1 H 0.0110 0.1721 0.4178 0.023 Uiso 1 1 calc R . . C1 C 0.1465(4) 0.2843(3) 0.3937(3) 0.0253(8) Uani 1 1 d . . . H11 H 0.1856 0.2758 0.4557 0.030 Uiso 1 1 calc R . . H12 H 0.1204 0.3557 0.3838 0.030 Uiso 1 1 calc R . . C2 C 0.2629(4) 0.2531(3) 0.3343(3) 0.0239(8) Uani 1 1 d . . . H21 H 0.3384 0.3067 0.3326 0.029 Uiso 1 1 calc R . . H22 H 0.3137 0.1917 0.3577 0.029 Uiso 1 1 calc R . . N2 N 0.1928(3) 0.2335(2) 0.2435(2) 0.0179(6) Uani 1 1 d . . . C3 C 0.2888(4) 0.1668(3) 0.1951(3) 0.0242(8) Uani 1 1 d . . . H31 H 0.3313 0.1129 0.2341 0.029 Uiso 1 1 calc R . . H32 H 0.3717 0.2055 0.1738 0.029 Uiso 1 1 calc R . . C4 C 0.1926(4) 0.1221(3) 0.1185(3) 0.0250(8) Uani 1 1 d . . . H41 H 0.1759 0.1722 0.0710 0.030 Uiso 1 1 calc R . . H42 H 0.2429 0.0632 0.0953 0.030 Uiso 1 1 calc R . . N3 N 0.0466(3) 0.0912(2) 0.1498(2) 0.0177(6) Uani 1 1 d . . . H3 H 0.0476 0.0219 0.1557 0.021 Uiso 1 1 calc R . . C5 C -0.0883(4) 0.1188(3) 0.0908(3) 0.0226(8) Uani 1 1 d . . . H51 H -0.1222 0.0608 0.0541 0.027 Uiso 1 1 calc R . . H52 H -0.0649 0.1746 0.0519 0.027 Uiso 1 1 calc R . . C6 C -0.2078(4) 0.1500(3) 0.1472(3) 0.0211(8) Uani 1 1 d . . . H61 H -0.2907 0.1825 0.1110 0.025 Uiso 1 1 calc R . . H62 H -0.2474 0.0906 0.1760 0.025 Uiso 1 1 calc R . . N4 N -0.1406(3) 0.2220(2) 0.21483(19) 0.0155(6) Uani 1 1 d . . . C7 C -0.2330(4) 0.2315(3) 0.2917(2) 0.0222(8) Uani 1 1 d . . . H71 H -0.2722 0.1650 0.3067 0.027 Uiso 1 1 calc R . . H72 H -0.3184 0.2768 0.2765 0.027 Uiso 1 1 calc R . . C8 C -0.1355(4) 0.2734(3) 0.3691(3) 0.0248(8) Uani 1 1 d . . . H81 H -0.1205 0.3462 0.3614 0.030 Uiso 1 1 calc R . . H82 H -0.1833 0.2627 0.4238 0.030 Uiso 1 1 calc R . . C9 C 0.1624(4) 0.3291(3) 0.1929(3) 0.0218(8) Uani 1 1 d . . . H91 H 0.1626 0.3138 0.1298 0.026 Uiso 1 1 calc R . . H92 H 0.2453 0.3762 0.2086 0.026 Uiso 1 1 calc R . . C10 C 0.0171(4) 0.3816(3) 0.2071(3) 0.0217(7) Uani 1 1 d . . . H101 H 0.0151 0.4476 0.1776 0.026 Uiso 1 1 calc R . . H102 H 0.0131 0.3935 0.2705 0.026 Uiso 1 1 calc R . . C11 C -0.1199(4) 0.3222(3) 0.1725(3) 0.0198(7) Uani 1 1 d . . . H111 H -0.2091 0.3635 0.1796 0.024 Uiso 1 1 calc R . . H112 H -0.1153 0.3113 0.1090 0.024 Uiso 1 1 calc R . . O1 O 0.1550(2) 0.0439(2) 0.32448(17) 0.0201(5) Uani 1 1 d . . . O2 O -0.0817(2) 0.03212(18) 0.30488(17) 0.0177(5) Uani 1 1 d . . . N5 N 0.0403(3) -0.0088(2) 0.3373(2) 0.0184(6) Uani 1 1 d . . . O3 O 0.0471(3) -0.0870(2) 0.3764(2) 0.0260(6) Uani 1 1 d . . . Cl Cl 0.07119(10) -0.43006(7) 0.45986(6) 0.0249(2) Uani 1 1 d . . . O4 O 0.0210(7) -0.5041(4) 0.5156(3) 0.0740(12) Uani 1 1 d . . . O5 O 0.0363(3) -0.4553(2) 0.36970(19) 0.0338(7) Uani 1 1 d . . . O6 O 0.0191(5) -0.3327(3) 0.4768(2) 0.0540(11) Uani 1 1 d . . . O7 O 0.2314(4) -0.4256(3) 0.4762(3) 0.0620(11) Uani 1 1 d . . . N6 N 0.0203(2) 0.14581(19) 0.58416(18) 0.0095(5) Uani 1 1 d . . . O8 O 0.0658(3) 0.08703(19) 0.52853(18) 0.0247(6) Uani 1 1 d . . . O9 O -0.0138(3) 0.2341(2) 0.56212(18) 0.0274(6) Uani 1 1 d . . . O10 O 0.0147(3) 0.1182(2) 0.66151(18) 0.0220(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.01389(17) 0.0138(2) 0.0122(2) 0.0006(2) 0.00017(14) -0.00153(19) N1 0.0230(14) 0.0209(16) 0.0135(15) -0.0001(12) 0.0019(11) -0.0011(11) C1 0.0373(19) 0.0197(19) 0.017(2) -0.0026(15) -0.0055(16) -0.0081(15) C2 0.0250(17) 0.0215(19) 0.023(2) 0.0021(16) -0.0104(15) -0.0077(14) N2 0.0176(13) 0.0182(15) 0.0178(16) 0.0029(12) 0.0005(11) -0.0043(11) C3 0.0180(14) 0.026(2) 0.029(2) 0.0071(16) 0.0073(14) -0.0008(14) C4 0.0299(18) 0.023(2) 0.024(2) -0.0010(16) 0.0124(16) 0.0005(15) N3 0.0213(13) 0.0182(15) 0.0139(15) -0.0009(12) 0.0038(11) 0.0007(11) C5 0.0311(17) 0.0194(18) 0.0159(19) -0.0025(14) -0.0054(14) 0.0031(15) C6 0.0187(15) 0.0231(19) 0.020(2) 0.0020(14) -0.0058(13) -0.0021(13) N4 0.0149(12) 0.0178(15) 0.0134(15) 0.0001(11) -0.0013(10) -0.0011(11) C7 0.0185(15) 0.029(2) 0.020(2) 0.0049(15) 0.0051(13) 0.0031(14) C8 0.0321(18) 0.024(2) 0.019(2) 0.0012(15) 0.0077(15) 0.0080(15) C9 0.0267(16) 0.0172(18) 0.021(2) 0.0116(15) -0.0025(14) -0.0063(14) C10 0.0320(18) 0.0153(16) 0.0169(19) 0.0025(13) -0.0016(15) -0.0015(14) C11 0.0227(15) 0.0167(17) 0.0195(19) 0.0032(15) -0.0003(13) 0.0014(14) O1 0.0173(11) 0.0209(13) 0.0220(14) 0.0067(10) 0.0007(9) -0.0035(9) O2 0.0172(10) 0.0153(12) 0.0202(14) 0.0016(9) -0.0001(9) -0.0009(9) N5 0.0193(12) 0.0169(15) 0.0191(16) -0.0033(13) 0.0023(11) -0.0025(11) O3 0.0340(14) 0.0137(13) 0.0297(16) 0.0053(12) 0.0005(12) -0.0023(11) Cl 0.0380(4) 0.0206(4) 0.0154(5) -0.0018(3) -0.0006(3) 0.0015(4) O4 0.127(4) 0.059(2) 0.040(2) 0.0003(17) 0.030(2) -0.025(2) O5 0.0496(17) 0.0331(17) 0.0180(16) -0.0098(12) -0.0011(13) 0.0002(14) O6 0.092(3) 0.0393(19) 0.028(2) -0.0096(15) -0.0136(19) 0.0342(19) O7 0.0451(19) 0.076(3) 0.061(3) -0.004(2) -0.0138(18) 0.0111(18) N6 0.0091(10) 0.0114(13) 0.0082(14) 0.0015(10) 0.0025(9) -0.0006(9) O8 0.0379(14) 0.0221(14) 0.0149(14) -0.0010(11) 0.0076(11) 0.0043(11) O9 0.0429(14) 0.0208(14) 0.0189(15) 0.0041(11) 0.0049(12) 0.0052(12) O10 0.0281(12) 0.0245(14) 0.0137(14) 0.0024(10) 0.0045(10) -0.0023(10) _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 Co N2 1.912(3) . ? Co N4 1.922(3) . ? Co N3 1.941(3) . ? Co N1 1.943(3) . ? Co O1 1.969(2) . ? Co O2 1.977(2) . ? Co N5 2.373(3) . ? N1 C8 1.501(4) . ? N1 C1 1.503(5) . ? N1 H1 0.9300 . ? C1 C2 1.511(6) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? C2 N2 1.499(5) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? N2 C3 1.489(5) . ? N2 C9 1.506(4) . ? C3 C4 1.519(6) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 N3 1.501(5) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? N3 C5 1.495(4) . ? N3 H3 0.9300 . ? C5 C6 1.502(5) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 N4 1.501(5) . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N4 C11 1.506(5) . ? N4 C7 1.511(4) . ? C7 C8 1.519(5) . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 C10 1.520(5) . ? C9 H91 0.9900 . ? C9 H92 0.9900 . ? C10 C11 1.523(5) . ? C10 H101 0.9900 . ? C10 H102 0.9900 . ? C11 H111 0.9900 . ? C11 H112 0.9900 . ? O1 N5 1.282(4) . ? O2 N5 1.287(4) . ? N5 O3 1.203(4) . ? Cl O4 1.409(5) . ? Cl O6 1.414(3) . ? Cl O5 1.431(3) . ? Cl O7 1.446(4) . ? N6 O10 1.249(4) . ? N6 O8 1.256(4) . ? N6 O9 1.257(3) . ? 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 N2 Co N4 103.16(12) . . ? N2 Co N3 87.24(13) . . ? N4 Co N3 88.03(12) . . ? N2 Co N1 88.98(13) . . ? N4 Co N1 87.96(13) . . ? N3 Co N1 173.73(13) . . ? N2 Co O1 94.66(11) . . ? N4 Co O1 162.17(11) . . ? N3 Co O1 93.12(12) . . ? N1 Co O1 92.17(12) . . ? N2 Co O2 160.18(11) . . ? N4 Co O2 96.65(11) . . ? N3 Co O2 93.42(12) . . ? N1 Co O2 91.83(12) . . ? O1 Co O2 65.52(9) . . ? N2 Co N5 127.34(11) . . ? N4 Co N5 129.49(11) . . ? N3 Co N5 94.36(12) . . ? N1 Co N5 91.91(12) . . ? O1 Co N5 32.68(9) . . ? O2 Co N5 32.85(9) . . ? C8 N1 C1 115.6(3) . . ? C8 N1 Co 109.8(2) . . ? C1 N1 Co 109.1(2) . . ? C8 N1 H1 107.3 . . ? C1 N1 H1 107.3 . . ? Co N1 H1 107.3 . . ? N1 C1 C2 108.3(3) . . ? N1 C1 H11 110.0 . . ? C2 C1 H11 110.0 . . ? N1 C1 H12 110.0 . . ? C2 C1 H12 110.0 . . ? H11 C1 H12 108.4 . . ? N2 C2 C1 110.6(3) . . ? N2 C2 H21 109.5 . . ? C1 C2 H21 109.5 . . ? N2 C2 H22 109.5 . . ? C1 C2 H22 109.5 . . ? H21 C2 H22 108.1 . . ? C3 N2 C2 110.7(3) . . ? C3 N2 C9 109.6(3) . . ? C2 N2 C9 111.9(3) . . ? C3 N2 Co 102.8(2) . . ? C2 N2 Co 102.2(2) . . ? C9 N2 Co 119.0(2) . . ? N2 C3 C4 107.7(3) . . ? N2 C3 H31 110.2 . . ? C4 C3 H31 110.2 . . ? N2 C3 H32 110.2 . . ? C4 C3 H32 110.2 . . ? H31 C3 H32 108.5 . . ? N3 C4 C3 108.4(3) . . ? N3 C4 H41 110.0 . . ? C3 C4 H41 110.0 . . ? N3 C4 H42 110.0 . . ? C3 C4 H42 110.0 . . ? H41 C4 H42 108.4 . . ? C5 N3 C4 115.4(3) . . ? C5 N3 Co 109.0(2) . . ? C4 N3 Co 109.2(2) . . ? C5 N3 H3 107.7 . . ? C4 N3 H3 107.7 . . ? Co N3 H3 107.7 . . ? N3 C5 C6 107.9(3) . . ? N3 C5 H51 110.1 . . ? C6 C5 H51 110.1 . . ? N3 C5 H52 110.1 . . ? C6 C5 H52 110.1 . . ? H51 C5 H52 108.4 . . ? N4 C6 C5 108.1(3) . . ? N4 C6 H61 110.1 . . ? C5 C6 H61 110.1 . . ? N4 C6 H62 110.1 . . ? C5 C6 H62 110.1 . . ? H61 C6 H62 108.4 . . ? C6 N4 C11 109.2(3) . . ? C6 N4 C7 112.1(3) . . ? C11 N4 C7 111.2(3) . . ? C6 N4 Co 101.9(2) . . ? C11 N4 Co 120.0(2) . . ? C7 N4 Co 102.1(2) . . ? N4 C7 C8 108.6(3) . . ? N4 C7 H71 110.0 . . ? C8 C7 H71 110.0 . . ? N4 C7 H72 110.0 . . ? C8 C7 H72 110.0 . . ? H71 C7 H72 108.3 . . ? N1 C8 C7 107.8(3) . . ? N1 C8 H81 110.1 . . ? C7 C8 H81 110.1 . . ? N1 C8 H82 110.1 . . ? C7 C8 H82 110.1 . . ? H81 C8 H82 108.5 . . ? N2 C9 C10 115.8(3) . . ? N2 C9 H91 108.3 . . ? C10 C9 H91 108.3 . . ? N2 C9 H92 108.3 . . ? C10 C9 H92 108.3 . . ? H91 C9 H92 107.4 . . ? C9 C10 C11 113.1(3) . . ? C9 C10 H101 109.0 . . ? C11 C10 H101 109.0 . . ? C9 C10 H102 109.0 . . ? C11 C10 H102 109.0 . . ? H101 C10 H102 107.8 . . ? N4 C11 C10 116.2(3) . . ? N4 C11 H111 108.2 . . ? C10 C11 H111 108.2 . . ? N4 C11 H112 108.2 . . ? C10 C11 H112 108.2 . . ? H111 C11 H112 107.4 . . ? N5 O1 Co 91.28(18) . . ? N5 O2 Co 90.74(17) . . ? O3 N5 O1 123.2(3) . . ? O3 N5 O2 124.3(3) . . ? O1 N5 O2 112.4(3) . . ? O3 N5 Co 178.1(3) . . ? O1 N5 Co 56.04(16) . . ? O2 N5 Co 56.41(15) . . ? O4 Cl O6 113.7(3) . . ? O4 Cl O5 111.6(3) . . ? O6 Cl O5 110.28(19) . . ? O4 Cl O7 107.2(3) . . ? O6 Cl O7 105.9(3) . . ? O5 Cl O7 107.8(2) . . ? O10 N6 O8 120.4(3) . . ? O10 N6 O9 120.1(3) . . ? O8 N6 O9 119.4(3) . . ? 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 Co N1 C1 C2 -12.8(4) . . . . ? N1 C1 C2 N2 41.4(4) . . . . ? C1 C2 N2 Co -48.9(3) . . . . ? C2 N2 Co N1 33.1(2) . . . . ? N2 Co N1 C1 -12.1(2) . . . . ? Co N2 C3 C4 52.6(3) . . . . ? N2 C3 C4 N3 -43.1(4) . . . . ? C3 C4 N3 Co 12.5(4) . . . . ? C4 N3 Co N2 14.2(2) . . . . ? N3 Co N2 C3 -37.1(2) . . . . ? Co N3 C5 C6 -18.5(3) . . . . ? N3 C5 C6 N4 47.5(4) . . . . ? C5 C6 N4 Co -52.6(3) . . . . ? C6 N4 Co N3 33.9(2) . . . . ? N4 Co N3 C5 -9.4(2) . . . . ? Co N4 C7 C8 51.6(3) . . . . ? N4 C7 C8 N1 -43.9(4) . . . . ? C7 C8 N1 Co 14.4(4) . . . . ? C8 N1 Co N4 12.3(2) . . . . ? N1 Co N4 C7 -34.9(2) . . . . ? Co N2 C9 C10 34.5(4) . . . . ? N2 C9 C10 C11 -66.6(4) . . . . ? C9 C10 C11 N4 62.7(4) . . . . ? C10 C11 N4 Co -28.0(4) . . . . ? C11 N4 Co N2 0.0(3) . . . . ? N4 Co N2 C9 -3.1(3) . . . . ? Co N2 C9 C10 34.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O8 0.93 2.07 2.971(4) 163.7 . N3 H3 O10 0.93 1.90 2.818(4) 170.3 2_554 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.670 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.084 # Attachment '7.cif' data_js301ak _database_code_depnum_ccdc_archive 'CCDC 642049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(C11H24N4)(CO3)]ClO4,0.5NaClO4,0.67H2O' _chemical_formula_sum 'C12 H25.33 Cl1.50 Co N4 Na0.50 O9.67' _chemical_formula_weight 503.96 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.4032(6) _cell_length_b 11.9183(6) _cell_length_c 27.5618(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3745.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 25980 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 27.99 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2085 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8365 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS,ver2.03 (Sheldrick,2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD Platform' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25980 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0849 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.99 _reflns_number_total 8924 _reflns_number_gt 7232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS,1998)' _computing_cell_refinement 'SAINT (Bruker AXS,1998)' _computing_data_reduction 'SAINT (Bruker AXS,1998)' _computing_structure_solution 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_structure_refinement 'SHELXTL,ver.6.12 (Sheldrick,2001)' _computing_molecular_graphics 'SHELXTL,ver.6.12 (Sheldrick,2001)' _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^)+(0.0392P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(13) _refine_ls_number_reflns 8924 _refine_ls_number_parameters 541 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.017 _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 0.11683(5) 0.26195(4) 0.167153(18) 0.01164(12) Uani 1 1 d . . . O1 O 0.0065(2) 0.2479(2) 0.21914(9) 0.0147(6) Uani 1 1 d . . . O2 O 0.1564(3) 0.3592(2) 0.22117(9) 0.0141(6) Uani 1 1 d . . . O3 O 0.0390(3) 0.3459(2) 0.28733(9) 0.0156(6) Uani 1 1 d . . . C12 C 0.0654(4) 0.3203(3) 0.24558(14) 0.0127(8) Uani 1 1 d . . . N1 N 0.0227(3) 0.3748(2) 0.13494(12) 0.0140(7) Uani 1 1 d . . . H1 H -0.0121 0.4192 0.1586 0.017 Uiso 1 1 calc R . . C1 C 0.1009(4) 0.4484(3) 0.10469(15) 0.0197(10) Uani 1 1 d . . . H11 H 0.0794 0.5281 0.1094 0.024 Uiso 1 1 calc R . . H12 H 0.0912 0.4298 0.0699 0.024 Uiso 1 1 calc R . . C2 C 0.2280(4) 0.4295(3) 0.11995(14) 0.0182(10) Uani 1 1 d . . . H21 H 0.2817 0.4595 0.0949 0.022 Uiso 1 1 calc R . . H22 H 0.2439 0.4690 0.1509 0.022 Uiso 1 1 calc R . . N2 N 0.2477(3) 0.3054(3) 0.12616(11) 0.0142(7) Uani 1 1 d . . . C3 C 0.3506(4) 0.2815(3) 0.15788(14) 0.0183(9) Uani 1 1 d . . . H31 H 0.3539 0.3369 0.1846 0.022 Uiso 1 1 calc R . . H32 H 0.4239 0.2876 0.1388 0.022 Uiso 1 1 calc R . . C4 C 0.3392(4) 0.1637(3) 0.17861(15) 0.0192(10) Uani 1 1 d . . . H41 H 0.3620 0.1078 0.1538 0.023 Uiso 1 1 calc R . . H42 H 0.3921 0.1550 0.2068 0.023 Uiso 1 1 calc R . . N3 N 0.2148(3) 0.1443(2) 0.19394(11) 0.0141(7) Uani 1 1 d . . . H3 H 0.2118 0.1502 0.2276 0.017 Uiso 1 1 calc R . . C5 C 0.1654(4) 0.0311(3) 0.18013(15) 0.0182(10) Uani 1 1 d . . . H51 H 0.1613 -0.0181 0.2090 0.022 Uiso 1 1 calc R . . H52 H 0.2164 -0.0052 0.1557 0.022 Uiso 1 1 calc R . . C6 C 0.0436(4) 0.0493(3) 0.15943(15) 0.0172(10) Uani 1 1 d . . . H61 H 0.0196 -0.0178 0.1407 0.021 Uiso 1 1 calc R . . H62 H -0.0130 0.0595 0.1863 0.021 Uiso 1 1 calc R . . N4 N 0.0410(3) 0.1504(3) 0.12706(12) 0.0152(8) Uani 1 1 d . . . C7 C -0.0817(4) 0.1960(3) 0.12236(14) 0.0180(9) Uani 1 1 d . . . H71 H -0.1232 0.1904 0.1538 0.022 Uiso 1 1 calc R . . H72 H -0.1261 0.1525 0.0979 0.022 Uiso 1 1 calc R . . C8 C -0.0728(4) 0.3184(3) 0.10675(15) 0.0202(10) Uani 1 1 d . . . H81 H -0.0554 0.3227 0.0716 0.024 Uiso 1 1 calc R . . H82 H -0.1483 0.3570 0.1127 0.024 Uiso 1 1 calc R . . C9 C 0.2618(4) 0.2549(3) 0.07638(13) 0.0184(9) Uani 1 1 d . . . H91 H 0.3460 0.2569 0.0676 0.022 Uiso 1 1 calc R . . H92 H 0.2194 0.3027 0.0528 0.022 Uiso 1 1 calc R . . C10 C 0.2179(4) 0.1343(3) 0.07094(15) 0.0201(10) Uani 1 1 d . . . H101 H 0.2394 0.1061 0.0384 0.024 Uiso 1 1 calc R . . H102 H 0.2573 0.0864 0.0953 0.024 Uiso 1 1 calc R . . C11 C 0.0869(4) 0.1251(3) 0.07739(14) 0.0185(10) Uani 1 1 d . . . H111 H 0.0488 0.1768 0.0541 0.022 Uiso 1 1 calc R . . H112 H 0.0629 0.0479 0.0686 0.022 Uiso 1 1 calc R . . Co2 Co 0.29206(5) 0.19450(4) 0.368231(19) 0.01277(13) Uani 1 1 d . . . O1A O 0.1585(2) 0.0977(2) 0.37061(10) 0.0147(6) Uani 1 1 d . . . O2A O 0.2338(2) 0.1588(2) 0.30413(9) 0.0131(6) Uani 1 1 d . . . O3A O 0.0635(3) 0.0609(2) 0.30096(10) 0.0169(7) Uani 1 1 d . . . C12A C 0.1467(4) 0.1017(3) 0.32391(14) 0.0140(9) Uani 1 1 d . . . N1A N 0.3997(3) 0.0692(3) 0.36796(12) 0.0168(8) Uani 1 1 d . . . H1A H 0.3659 0.0124 0.3495 0.020 Uiso 1 1 calc R . . C1A C 0.4133(4) 0.0256(4) 0.41886(15) 0.0263(11) Uani 1 1 d . . . H11A H 0.4924 0.0441 0.4313 0.032 Uiso 1 1 calc R . . H12A H 0.4042 -0.0570 0.4191 0.032 Uiso 1 1 calc R . . C2A C 0.3204(4) 0.0791(4) 0.45107(16) 0.0266(11) Uani 1 1 d . . . H21A H 0.2442 0.0409 0.4462 0.032 Uiso 1 1 calc R . . H22A H 0.3429 0.0709 0.4856 0.032 Uiso 1 1 calc R . . N2A N 0.3090(3) 0.2001(3) 0.43867(12) 0.0228(9) Uani 1 1 d . . . C3A C 0.1926(4) 0.2462(4) 0.45364(14) 0.0260(10) Uani 1 1 d . . . H31A H 0.1934 0.2640 0.4887 0.031 Uiso 1 1 calc R . . H32A H 0.1305 0.1897 0.4477 0.031 Uiso 1 1 calc R . . C4A C 0.1670(4) 0.3514(4) 0.42465(15) 0.0261(11) Uani 1 1 d . . . H41A H 0.0831 0.3715 0.4277 0.031 Uiso 1 1 calc R . . H42A H 0.2146 0.4147 0.4371 0.031 Uiso 1 1 calc R . . N3A N 0.1969(3) 0.3291(2) 0.37250(11) 0.0149(7) Uani 1 1 d . . . H3A H 0.1272 0.3157 0.3560 0.018 Uiso 1 1 calc R . . C5A C 0.2590(4) 0.4250(3) 0.34731(16) 0.0210(10) Uani 1 1 d . . . H51A H 0.2034 0.4658 0.3261 0.025 Uiso 1 1 calc R . . H52A H 0.2904 0.4782 0.3716 0.025 Uiso 1 1 calc R . . C6A C 0.3577(4) 0.3773(3) 0.31744(15) 0.0184(10) Uani 1 1 d . . . H61A H 0.3262 0.3431 0.2874 0.022 Uiso 1 1 calc R . . H62A H 0.4129 0.4377 0.3082 0.022 Uiso 1 1 calc R . . N4A N 0.4202(3) 0.2900(3) 0.34705(11) 0.0149(8) Uani 1 1 d . . . C7A C 0.4912(4) 0.2119(3) 0.31660(14) 0.0183(10) Uani 1 1 d . . . H71A H 0.5677 0.2469 0.3088 0.022 Uiso 1 1 calc R . . H72A H 0.4496 0.1967 0.2858 0.022 Uiso 1 1 calc R . . C8A C 0.5110(4) 0.1035(3) 0.34335(15) 0.0176(9) Uani 1 1 d . . . H81A H 0.5358 0.0444 0.3203 0.021 Uiso 1 1 calc R . . H82A H 0.5738 0.1135 0.3677 0.021 Uiso 1 1 calc R . . C9A C 0.4057(4) 0.2692(5) 0.46051(16) 0.0387(14) Uani 1 1 d . . . H91A H 0.3698 0.3393 0.4728 0.046 Uiso 1 1 calc R . . H92A H 0.4354 0.2277 0.4891 0.046 Uiso 1 1 calc R . . C10A C 0.5032(6) 0.2997(6) 0.43250(19) 0.069(2) Uani 1 1 d . . . H11B H 0.5520 0.2314 0.4293 0.083 Uiso 1 1 calc R . . H12B H 0.5490 0.3533 0.4524 0.083 Uiso 1 1 calc R . . C11A C 0.4953(4) 0.3486(4) 0.38405(15) 0.0238(11) Uani 1 1 d . . . H21B H 0.5758 0.3538 0.3708 0.029 Uiso 1 1 calc R . . H22B H 0.4656 0.4263 0.3875 0.029 Uiso 1 1 calc R . . Cl1 Cl -0.34338(10) 0.31937(8) 0.21354(4) 0.0208(2) Uani 1 1 d . . . O7 O -0.2564(3) 0.3208(2) 0.25114(12) 0.0344(9) Uani 1 1 d . . . O8 O -0.3807(3) 0.2052(2) 0.20627(11) 0.0339(8) Uani 1 1 d . . . O9 O -0.4403(3) 0.3872(3) 0.22757(12) 0.0365(9) Uani 1 1 d . . . O10 O -0.2967(4) 0.3635(3) 0.16936(12) 0.0500(11) Uani 1 1 d . . . Cl2 Cl -0.17984(9) 0.25819(8) 0.40237(3) 0.0166(2) Uani 1 1 d . . . O11 O -0.0588(3) 0.2342(3) 0.39436(16) 0.0564(12) Uani 1 1 d . . . O12 O -0.1934(4) 0.3640(2) 0.42586(11) 0.0393(10) Uani 1 1 d . . . O13 O -0.2320(3) 0.1714(2) 0.43121(11) 0.0328(9) Uani 1 1 d . . . O14 O -0.2354(3) 0.2622(3) 0.35616(10) 0.0345(8) Uani 1 1 d . . . Cl3 Cl 0.08962(13) 0.34880(11) -0.04528(4) 0.0366(3) Uani 1 1 d . . . O15 O 0.0533(4) 0.3699(3) -0.09349(11) 0.0442(10) Uani 1 1 d . . . O16 O 0.1824(4) 0.4171(4) -0.03180(15) 0.0714(15) Uani 1 1 d . . . O17 O 0.0752(9) 0.2429(8) -0.0310(3) 0.0575(18) Uani 0.50 1 d P . . O17' O -0.0049(8) 0.4072(8) -0.0153(3) 0.0575(18) Uani 0.50 1 d P . . O18 O 0.0068(9) 0.3188(10) -0.0126(3) 0.070(2) Uani 0.50 1 d P . . O18' O 0.1667(9) 0.2396(8) -0.0464(3) 0.070(2) Uani 0.50 1 d P . . Na Na -0.10353(15) 0.19828(13) 0.29045(5) 0.0187(4) Uani 1 1 d . . . O20 O -0.2405(3) 0.0697(2) 0.26973(12) 0.0281(8) Uani 1 1 d D . . H201 H -0.223(4) -0.0007(18) 0.2616(15) 0.034 Uiso 1 1 d D . . H202 H -0.290(3) 0.098(4) 0.2476(13) 0.034 Uiso 1 1 d D . . O30 O 0.4001(10) 0.4448(10) 0.0060(4) 0.040(3) Uani 0.33 1 d PD . . H301 H 0.327(5) 0.447(14) -0.007(5) 0.049 Uiso 0.33 1 d PD . . H302 H 0.448(11) 0.386(9) 0.012(6) 0.049 Uiso 0.33 1 d PD . . 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 0.0127(3) 0.0082(2) 0.0140(3) -0.0008(2) 0.0016(2) -0.0008(2) O1 0.0175(17) 0.0134(13) 0.0133(13) -0.0011(12) 0.0026(12) 0.0013(13) O2 0.0139(17) 0.0128(12) 0.0157(14) -0.0031(11) 0.0026(12) -0.0014(12) O3 0.0170(18) 0.0163(13) 0.0134(14) -0.0038(11) 0.0040(13) 0.0023(12) C12 0.009(2) 0.0102(17) 0.019(2) 0.0024(16) 0.0010(17) 0.0025(16) N1 0.013(2) 0.0124(15) 0.0162(17) 0.0030(14) 0.0031(16) 0.0037(14) C1 0.023(3) 0.0144(18) 0.021(2) 0.0060(16) 0.001(2) 0.0014(19) C2 0.021(3) 0.0135(18) 0.020(2) 0.0029(15) 0.0055(19) -0.0076(18) N2 0.0130(19) 0.0140(14) 0.0157(16) -0.0009(14) 0.0011(14) -0.0005(15) C3 0.010(2) 0.023(2) 0.022(2) -0.0022(17) 0.0039(18) 0.0017(17) C4 0.014(2) 0.021(2) 0.023(2) -0.0011(17) 0.0012(19) 0.0055(18) N3 0.016(2) 0.0116(14) 0.0144(16) -0.0027(13) -0.0031(16) -0.0010(15) C5 0.024(3) 0.0108(17) 0.020(2) 0.0000(16) 0.003(2) -0.0027(18) C6 0.023(3) 0.0109(17) 0.018(2) 0.0014(16) 0.0011(19) -0.0045(18) N4 0.019(2) 0.0107(14) 0.0159(17) -0.0005(14) 0.0010(16) -0.0018(14) C7 0.019(3) 0.0152(18) 0.019(2) 0.0002(17) -0.0019(18) -0.0009(18) C8 0.016(3) 0.021(2) 0.023(2) 0.0049(18) -0.0024(19) -0.002(2) C9 0.020(3) 0.021(2) 0.0151(19) -0.0013(17) 0.0066(18) 0.000(2) C10 0.027(3) 0.0171(19) 0.017(2) -0.0024(16) 0.002(2) 0.000(2) C11 0.023(3) 0.0170(19) 0.015(2) -0.0016(16) 0.0010(19) -0.0013(18) Co2 0.0100(3) 0.0160(2) 0.0123(3) -0.0012(2) -0.0004(2) -0.0007(2) O1A 0.0095(16) 0.0197(13) 0.0149(14) 0.0002(12) 0.0003(13) -0.0035(12) O2A 0.0091(16) 0.0156(13) 0.0144(13) 0.0001(11) -0.0003(12) -0.0023(12) O3A 0.0126(18) 0.0192(14) 0.0187(15) -0.0012(12) -0.0023(13) -0.0052(13) C12A 0.012(2) 0.0137(17) 0.016(2) 0.0006(15) -0.0002(18) 0.0022(16) N1A 0.014(2) 0.0192(16) 0.0170(17) 0.0044(14) -0.0016(17) -0.0013(15) C1A 0.022(3) 0.035(2) 0.023(2) 0.011(2) -0.006(2) -0.004(2) C2A 0.021(3) 0.039(3) 0.019(2) 0.010(2) -0.003(2) -0.002(2) N2A 0.016(2) 0.035(2) 0.0170(18) -0.0001(16) 0.0018(16) -0.0073(18) C3A 0.022(3) 0.041(3) 0.015(2) -0.002(2) 0.0076(19) -0.007(2) C4A 0.015(3) 0.034(2) 0.030(2) -0.012(2) 0.004(2) -0.001(2) N3A 0.0090(19) 0.0159(16) 0.0197(17) -0.0070(14) -0.0015(16) -0.0030(14) C5A 0.018(3) 0.0150(19) 0.030(2) -0.0014(17) -0.006(2) -0.0010(18) C6A 0.013(3) 0.0189(19) 0.023(2) 0.0040(17) 0.0005(19) -0.0051(18) N4A 0.0081(19) 0.0181(17) 0.0185(17) -0.0004(13) -0.0014(15) -0.0035(14) C7A 0.014(2) 0.020(2) 0.020(2) -0.0039(17) 0.0062(19) 0.0005(18) C8A 0.009(2) 0.0196(19) 0.024(2) -0.0051(17) -0.0005(19) -0.0010(18) C9A 0.028(3) 0.067(4) 0.022(2) -0.005(2) -0.009(2) -0.016(3) C10A 0.070(5) 0.110(6) 0.027(3) -0.003(3) -0.015(3) -0.060(5) C11A 0.023(3) 0.027(2) 0.022(2) -0.0046(19) -0.005(2) -0.005(2) Cl1 0.0202(6) 0.0213(5) 0.0210(5) 0.0064(4) -0.0001(5) 0.0018(5) O7 0.028(2) 0.0214(16) 0.054(2) 0.0016(15) -0.0257(18) 0.0003(15) O8 0.040(2) 0.0248(16) 0.0368(19) 0.0027(14) -0.0180(18) -0.0013(17) O9 0.034(2) 0.0344(18) 0.041(2) 0.0071(16) 0.0088(18) 0.0164(17) O10 0.066(3) 0.046(2) 0.038(2) 0.0223(18) 0.032(2) 0.020(2) Cl2 0.0163(6) 0.0139(4) 0.0198(5) -0.0020(4) -0.0023(4) 0.0006(4) O11 0.013(2) 0.037(2) 0.119(4) 0.008(2) -0.010(2) -0.0023(17) O12 0.079(3) 0.0145(14) 0.0245(16) -0.0059(13) 0.0068(19) -0.0028(18) O13 0.051(3) 0.0173(15) 0.0301(17) -0.0012(13) 0.0095(17) -0.0046(16) O14 0.034(2) 0.053(2) 0.0160(15) 0.0007(15) -0.0097(15) -0.0057(19) Cl3 0.0499(10) 0.0397(7) 0.0200(6) 0.0045(5) -0.0054(6) -0.0249(7) O15 0.067(3) 0.046(2) 0.0198(17) 0.0070(16) -0.0088(19) -0.017(2) O16 0.082(4) 0.068(3) 0.064(3) 0.022(2) -0.039(3) -0.048(3) O17 0.060(5) 0.064(4) 0.048(4) 0.012(3) -0.017(3) -0.024(4) O17' 0.060(5) 0.064(4) 0.048(4) 0.012(3) -0.017(3) -0.024(4) O18 0.082(5) 0.080(5) 0.046(3) 0.017(4) 0.013(4) 0.012(5) O18' 0.082(5) 0.080(5) 0.046(3) 0.017(4) 0.013(4) 0.012(5) Na 0.0169(10) 0.0202(7) 0.0192(8) 0.0000(7) 0.0028(7) -0.0039(8) O20 0.032(2) 0.0123(14) 0.040(2) -0.0025(13) -0.0115(17) 0.0044(14) O30 0.027(7) 0.050(7) 0.045(7) 0.010(6) -0.001(6) 0.002(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 Co1 O1 1.914(3) . ? Co1 N4 1.933(3) . ? Co1 N1 1.936(3) . ? Co1 N3 1.939(3) . ? Co1 O2 1.940(3) . ? Co1 N2 1.942(3) . ? Co1 C12 2.345(4) . ? O1 C12 1.315(4) . ? O1 Na 2.406(3) . ? O2 C12 1.320(4) . ? O3 C12 1.228(4) . ? O3 Na 2.397(3) . ? C12 Na 2.712(4) . ? N1 C8 1.497(5) . ? N1 C1 1.503(5) . ? N1 H1 0.9300 . ? C1 C2 1.526(6) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? C2 N2 1.506(5) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? N2 C3 1.490(5) . ? N2 C9 1.507(5) . ? C3 C4 1.522(5) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 N3 1.498(5) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? N3 C5 1.510(5) . ? N3 H3 0.9300 . ? C5 C6 1.518(6) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 N4 1.499(5) . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N4 C11 1.496(5) . ? N4 C7 1.507(5) . ? C7 C8 1.524(5) . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 C10 1.529(5) . ? C9 H91 0.9900 . ? C9 H92 0.9900 . ? C10 C11 1.508(6) . ? C10 H101 0.9900 . ? C10 H102 0.9900 . ? C11 H111 0.9900 . ? C11 H112 0.9900 . ? Co2 O1A 1.912(3) . ? Co2 N1A 1.933(3) . ? Co2 O2A 1.935(3) . ? Co2 N3A 1.941(3) . ? Co2 N4A 1.942(3) . ? Co2 N2A 1.952(3) . ? Co2 C12A 2.337(4) . ? O1A C12A 1.295(5) . ? O2A C12A 1.322(5) . ? O3A C12A 1.240(5) . ? O3A Na 2.528(3) . ? N1A C8A 1.496(5) . ? N1A C1A 1.504(5) . ? N1A H1A 0.9300 . ? C1A C2A 1.522(6) . ? C1A H11A 0.9900 . ? C1A H12A 0.9900 . ? C2A N2A 1.488(5) . ? C2A H21A 0.9900 . ? C2A H22A 0.9900 . ? N2A C3A 1.495(6) . ? N2A C9A 1.501(6) . ? C3A C4A 1.515(6) . ? C3A H31A 0.9900 . ? C3A H32A 0.9900 . ? C4A N3A 1.501(5) . ? C4A H41A 0.9900 . ? C4A H42A 0.9900 . ? N3A C5A 1.513(5) . ? N3A H3A 0.9300 . ? C5A C6A 1.505(6) . ? C5A H51A 0.9900 . ? C5A H52A 0.9900 . ? C6A N4A 1.502(5) . ? C6A H61A 0.9900 . ? C6A H62A 0.9900 . ? N4A C7A 1.493(5) . ? N4A C11A 1.503(5) . ? C7A C8A 1.504(5) . ? C7A H71A 0.9900 . ? C7A H72A 0.9900 . ? C8A H81A 0.9900 . ? C8A H82A 0.9900 . ? C9A C10A 1.402(7) . ? C9A H91A 0.9900 . ? C9A H92A 0.9900 . ? C10A C11A 1.460(7) . ? C10A H11B 0.9900 . ? C10A H12B 0.9900 . ? C11A H21B 0.9900 . ? C11A H22B 0.9900 . ? Cl1 O9 1.423(3) . ? Cl1 O10 1.429(3) . ? Cl1 O7 1.434(3) . ? Cl1 O8 1.440(3) . ? O7 Na 2.519(3) . ? Cl2 O14 1.423(3) . ? Cl2 O12 1.426(3) . ? Cl2 O11 1.427(4) . ? Cl2 O13 1.434(3) . ? Cl2 Na 3.2836(18) . ? O11 Na 2.940(5) . ? O14 Na 2.474(4) . ? Cl3 O17 1.332(9) . ? Cl3 O18 1.354(9) . ? Cl3 O16 1.386(4) . ? Cl3 O15 1.414(3) . ? Cl3 O17' 1.526(10) . ? Cl3 O18' 1.571(10) . ? O17 O18' 1.127(11) . ? O17 O18 1.298(13) . ? O17' O18 1.064(12) . ? Na O20 2.261(4) . ? O20 H201 0.890(15) . ? O20 H202 0.893(16) . ? O30 H301 0.904(17) . ? O30 H302 0.903(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N4 94.21(13) . . ? O1 Co1 N1 92.27(13) . . ? N4 Co1 N1 88.15(14) . . ? O1 Co1 N3 91.74(13) . . ? N4 Co1 N3 88.73(14) . . ? N1 Co1 N3 175.09(14) . . ? O1 Co1 O2 68.33(11) . . ? N4 Co1 O2 162.49(13) . . ? N1 Co1 O2 93.78(13) . . ? N3 Co1 O2 90.34(12) . . ? O1 Co1 N2 164.56(12) . . ? N4 Co1 N2 101.23(14) . . ? N1 Co1 N2 88.51(14) . . ? N3 Co1 N2 88.37(14) . . ? O2 Co1 N2 96.23(12) . . ? O1 Co1 C12 34.09(12) . . ? N4 Co1 C12 128.25(14) . . ? N1 Co1 C12 94.48(14) . . ? N3 Co1 C12 90.43(13) . . ? O2 Co1 C12 34.26(12) . . ? N2 Co1 C12 130.47(13) . . ? C12 O1 Co1 91.2(2) . . ? C12 O1 Na 88.6(2) . . ? Co1 O1 Na 167.40(15) . . ? C12 O2 Co1 89.9(2) . . ? C12 O3 Na 91.0(2) . . ? O3 C12 O1 123.8(4) . . ? O3 C12 O2 125.7(4) . . ? O1 C12 O2 110.5(3) . . ? O3 C12 Co1 177.1(3) . . ? O1 C12 Co1 54.69(18) . . ? O2 C12 Co1 55.80(18) . . ? O3 C12 Na 62.1(2) . . ? O1 C12 Na 62.45(19) . . ? O2 C12 Na 168.1(3) . . ? Co1 C12 Na 116.02(15) . . ? C8 N1 C1 113.9(3) . . ? C8 N1 Co1 109.3(2) . . ? C1 N1 Co1 109.3(2) . . ? C8 N1 H1 108.1 . . ? C1 N1 H1 108.1 . . ? Co1 N1 H1 108.1 . . ? N1 C1 C2 108.9(3) . . ? N1 C1 H11 109.9 . . ? C2 C1 H11 109.9 . . ? N1 C1 H12 109.9 . . ? C2 C1 H12 109.9 . . ? H11 C1 H12 108.3 . . ? N2 C2 C1 108.5(3) . . ? N2 C2 H21 110.0 . . ? C1 C2 H21 110.0 . . ? N2 C2 H22 110.0 . . ? C1 C2 H22 110.0 . . ? H21 C2 H22 108.4 . . ? C3 N2 C2 111.8(3) . . ? C3 N2 C9 111.9(3) . . ? C2 N2 C9 107.7(3) . . ? C3 N2 Co1 102.3(2) . . ? C2 N2 Co1 102.3(2) . . ? C9 N2 Co1 120.3(2) . . ? N2 C3 C4 109.2(3) . . ? N2 C3 H31 109.8 . . ? C4 C3 H31 109.8 . . ? N2 C3 H32 109.8 . . ? C4 C3 H32 109.8 . . ? H31 C3 H32 108.3 . . ? N3 C4 C3 109.2(3) . . ? N3 C4 H41 109.8 . . ? C3 C4 H41 109.8 . . ? N3 C4 H42 109.8 . . ? C3 C4 H42 109.8 . . ? H41 C4 H42 108.3 . . ? C4 N3 C5 114.8(3) . . ? C4 N3 Co1 109.1(2) . . ? C5 N3 Co1 109.6(2) . . ? C4 N3 H3 107.7 . . ? C5 N3 H3 107.7 . . ? Co1 N3 H3 107.7 . . ? N3 C5 C6 108.0(3) . . ? N3 C5 H51 110.1 . . ? C6 C5 H51 110.1 . . ? N3 C5 H52 110.1 . . ? C6 C5 H52 110.1 . . ? H51 C5 H52 108.4 . . ? N4 C6 C5 110.9(3) . . ? N4 C6 H61 109.5 . . ? C5 C6 H61 109.5 . . ? N4 C6 H62 109.5 . . ? C5 C6 H62 109.5 . . ? H61 C6 H62 108.1 . . ? C11 N4 C6 112.1(3) . . ? C11 N4 C7 108.6(3) . . ? C6 N4 C7 111.1(3) . . ? C11 N4 Co1 120.3(3) . . ? C6 N4 Co1 101.8(2) . . ? C7 N4 Co1 102.5(2) . . ? N4 C7 C8 107.9(3) . . ? N4 C7 H71 110.1 . . ? C8 C7 H71 110.1 . . ? N4 C7 H72 110.1 . . ? C8 C7 H72 110.1 . . ? H71 C7 H72 108.4 . . ? N1 C8 C7 109.3(3) . . ? N1 C8 H81 109.8 . . ? C7 C8 H81 109.8 . . ? N1 C8 H82 109.8 . . ? C7 C8 H82 109.8 . . ? H81 C8 H82 108.3 . . ? N2 C9 C10 115.4(3) . . ? N2 C9 H91 108.4 . . ? C10 C9 H91 108.4 . . ? N2 C9 H92 108.4 . . ? C10 C9 H92 108.4 . . ? H91 C9 H92 107.5 . . ? C11 C10 C9 112.4(4) . . ? C11 C10 H101 109.1 . . ? C9 C10 H101 109.1 . . ? C11 C10 H102 109.1 . . ? C9 C10 H102 109.1 . . ? H101 C10 H102 107.9 . . ? N4 C11 C10 116.1(3) . . ? N4 C11 H111 108.3 . . ? C10 C11 H111 108.3 . . ? N4 C11 H112 108.3 . . ? C10 C11 H112 108.3 . . ? H111 C11 H112 107.4 . . ? O1A Co2 N1A 92.25(13) . . ? O1A Co2 O2A 68.00(11) . . ? N1A Co2 O2A 92.55(13) . . ? O1A Co2 N3A 92.97(13) . . ? N1A Co2 N3A 173.74(15) . . ? O2A Co2 N3A 92.60(13) . . ? O1A Co2 N4A 164.46(13) . . ? N1A Co2 N4A 88.52(14) . . ? O2A Co2 N4A 96.46(12) . . ? N3A Co2 N4A 87.37(14) . . ? O1A Co2 N2A 93.74(14) . . ? N1A Co2 N2A 88.12(15) . . ? O2A Co2 N2A 161.74(14) . . ? N3A Co2 N2A 88.10(15) . . ? N4A Co2 N2A 101.79(14) . . ? O1A Co2 C12A 33.64(12) . . ? N1A Co2 C12A 94.74(14) . . ? O2A Co2 C12A 34.45(12) . . ? N3A Co2 C12A 91.52(13) . . ? N4A Co2 C12A 130.83(13) . . ? N2A Co2 C12A 127.31(15) . . ? C12A O1A Co2 91.5(2) . . ? C12A O2A Co2 89.7(2) . . ? C12A O3A Na 112.4(2) . . ? O3A C12A O1A 124.9(4) . . ? O3A C12A O2A 124.5(4) . . ? O1A C12A O2A 110.5(3) . . ? O3A C12A Co2 174.3(3) . . ? O1A C12A Co2 54.86(19) . . ? O2A C12A Co2 55.87(18) . . ? C8A N1A C1A 115.5(3) . . ? C8A N1A Co2 109.2(2) . . ? C1A N1A Co2 109.2(3) . . ? C8A N1A H1A 107.6 . . ? C1A N1A H1A 107.6 . . ? Co2 N1A H1A 107.6 . . ? N1A C1A C2A 109.1(4) . . ? N1A C1A H11A 109.9 . . ? C2A C1A H11A 109.9 . . ? N1A C1A H12A 109.9 . . ? C2A C1A H12A 109.9 . . ? H11A C1A H12A 108.3 . . ? N2A C2A C1A 109.4(4) . . ? N2A C2A H21A 109.8 . . ? C1A C2A H21A 109.8 . . ? N2A C2A H22A 109.8 . . ? C1A C2A H22A 109.8 . . ? H21A C2A H22A 108.2 . . ? C2A N2A C3A 111.7(3) . . ? C2A N2A C9A 112.1(4) . . ? C3A N2A C9A 109.9(4) . . ? C2A N2A Co2 101.8(3) . . ? C3A N2A Co2 101.5(3) . . ? C9A N2A Co2 119.3(3) . . ? N2A C3A C4A 109.2(3) . . ? N2A C3A H31A 109.8 . . ? C4A C3A H31A 109.8 . . ? N2A C3A H32A 109.8 . . ? C4A C3A H32A 109.8 . . ? H31A C3A H32A 108.3 . . ? N3A C4A C3A 108.4(3) . . ? N3A C4A H41A 110.0 . . ? C3A C4A H41A 110.0 . . ? N3A C4A H42A 110.0 . . ? C3A C4A H42A 110.0 . . ? H41A C4A H42A 108.4 . . ? C4A N3A C5A 114.4(3) . . ? C4A N3A Co2 109.3(3) . . ? C5A N3A Co2 109.5(2) . . ? C4A N3A H3A 107.8 . . ? C5A N3A H3A 107.8 . . ? Co2 N3A H3A 107.8 . . ? C6A C5A N3A 108.4(3) . . ? C6A C5A H51A 110.0 . . ? N3A C5A H51A 110.0 . . ? C6A C5A H52A 110.0 . . ? N3A C5A H52A 110.0 . . ? H51A C5A H52A 108.4 . . ? N4A C6A C5A 108.6(3) . . ? N4A C6A H61A 110.0 . . ? C5A C6A H61A 110.0 . . ? N4A C6A H62A 110.0 . . ? C5A C6A H62A 110.0 . . ? H61A C6A H62A 108.4 . . ? C7A N4A C6A 112.6(3) . . ? C7A N4A C11A 111.3(3) . . ? C6A N4A C11A 108.5(3) . . ? C7A N4A Co2 102.2(2) . . ? C6A N4A Co2 102.2(2) . . ? C11A N4A Co2 119.8(2) . . ? N4A C7A C8A 110.0(3) . . ? N4A C7A H71A 109.7 . . ? C8A C7A H71A 109.7 . . ? N4A C7A H72A 109.7 . . ? C8A C7A H72A 109.7 . . ? H71A C7A H72A 108.2 . . ? N1A C8A C7A 109.3(3) . . ? N1A C8A H81A 109.8 . . ? C7A C8A H81A 109.8 . . ? N1A C8A H82A 109.8 . . ? C7A C8A H82A 109.8 . . ? H81A C8A H82A 108.3 . . ? C10A C9A N2A 120.3(4) . . ? C10A C9A H91A 107.3 . . ? N2A C9A H91A 107.3 . . ? C10A C9A H92A 107.3 . . ? N2A C9A H92A 107.3 . . ? H91A C9A H92A 106.9 . . ? C9A C10A C11A 123.9(6) . . ? C9A C10A H11B 106.3 . . ? C11A C10A H11B 106.3 . . ? C9A C10A H12B 106.4 . . ? C11A C10A H12B 106.3 . . ? H11B C10A H12B 106.4 . . ? C10A C11A N4A 118.1(4) . . ? C10A C11A H21B 107.8 . . ? N4A C11A H21B 107.8 . . ? C10A C11A H22B 107.8 . . ? N4A C11A H22B 107.8 . . ? H21B C11A H22B 107.1 . . ? O9 Cl1 O10 108.2(2) . . ? O9 Cl1 O7 109.5(2) . . ? O10 Cl1 O7 110.7(2) . . ? O9 Cl1 O8 110.2(2) . . ? O10 Cl1 O8 109.8(2) . . ? O7 Cl1 O8 108.44(18) . . ? Cl1 O7 Na 141.47(19) . . ? O14 Cl2 O12 109.2(2) . . ? O14 Cl2 O11 107.4(2) . . ? O12 Cl2 O11 110.6(2) . . ? O14 Cl2 O13 109.6(2) . . ? O12 Cl2 O13 109.96(18) . . ? O11 Cl2 O13 110.1(2) . . ? O14 Cl2 Na 44.30(14) . . ? O12 Cl2 Na 130.36(14) . . ? O11 Cl2 Na 63.56(18) . . ? O13 Cl2 Na 118.28(13) . . ? Cl2 O11 Na 90.68(19) . . ? Cl2 O14 Na 112.00(19) . . ? O17 Cl3 O18 57.8(6) . . ? O17 Cl3 O16 124.9(4) . . ? O18 Cl3 O16 120.6(5) . . ? O17 Cl3 O15 114.2(4) . . ? O18 Cl3 O15 117.9(4) . . ? O16 Cl3 O15 111.8(2) . . ? O17 Cl3 O17' 100.7(6) . . ? O18 Cl3 O17' 42.9(5) . . ? O16 Cl3 O17' 97.3(4) . . ? O15 Cl3 O17' 102.7(4) . . ? O17 Cl3 O18' 44.8(5) . . ? O18 Cl3 O18' 100.6(6) . . ? O16 Cl3 O18' 93.7(4) . . ? O15 Cl3 O18' 107.1(4) . . ? O17' Cl3 O18' 141.6(5) . . ? O18' O17 O18 136.7(12) . . ? O18' O17 Cl3 78.9(8) . . ? O18 O17 Cl3 61.9(6) . . ? O18 O17' Cl3 59.9(8) . . ? O17' O18 O17 137.5(12) . . ? O17' O18 Cl3 77.2(9) . . ? O17 O18 Cl3 60.3(6) . . ? O17 O18' Cl3 56.3(7) . . ? O20 Na O3 163.08(12) . . ? O20 Na O1 108.68(12) . . ? O3 Na O1 55.71(9) . . ? O20 Na O14 88.49(13) . . ? O3 Na O14 102.27(11) . . ? O1 Na O14 147.09(12) . . ? O20 Na O7 78.82(11) . . ? O3 Na O7 91.62(11) . . ? O1 Na O7 82.36(11) . . ? O14 Na O7 73.49(12) . . ? O20 Na O3A 96.34(11) . . ? O3 Na O3A 88.20(10) . . ? O1 Na O3A 81.94(10) . . ? O14 Na O3A 124.98(11) . . ? O7 Na O3A 161.09(12) . . ? O20 Na C12 137.63(14) . . ? O3 Na C12 26.91(10) . . ? O1 Na C12 28.99(10) . . ? O14 Na C12 126.90(13) . . ? O7 Na C12 89.12(12) . . ? O3A Na C12 82.20(11) . . ? O20 Na O11 117.69(12) . . ? O3 Na O11 79.06(10) . . ? O1 Na O11 132.03(12) . . ? O14 Na O11 49.28(10) . . ? O7 Na O11 117.04(12) . . ? O3A Na O11 81.49(10) . . ? C12 Na O11 104.04(12) . . ? O20 Na Cl2 101.63(10) . . ? O3 Na Cl2 93.09(8) . . ? O1 Na Cl2 148.48(9) . . ? O14 Na Cl2 23.70(7) . . ? O7 Na Cl2 95.43(9) . . ? O3A Na Cl2 103.47(8) . . ? C12 Na Cl2 120.00(10) . . ? O11 Na Cl2 25.76(7) . . ? Na O20 H201 123(3) . . ? Na O20 H202 111(3) . . ? H201 O20 H202 109(4) . . ? H301 O30 H302 130(10) . . ? 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 Co1 N1 C1 C2 -14.9(4) . . . . ? N1 C1 C2 N2 43.5(4) . . . . ? C1 C2 N2 Co1 -49.8(3) . . . . ? C2 N2 Co1 N1 33.8(2) . . . . ? N2 Co1 N1 C1 -11.2(3) . . . . ? Co1 N2 C3 C4 49.4(3) . . . . ? N2 C3 C4 N3 -42.3(4) . . . . ? C3 C4 N3 Co1 13.2(4) . . . . ? C4 N3 Co1 N2 12.2(3) . . . . ? N3 Co1 N2 C3 -34.1(2) . . . . ? Co1 N3 C5 C6 -11.8(4) . . . . ? N3 C5 C6 N4 41.0(4) . . . . ? C5 C6 N4 Co1 -49.1(3) . . . . ? C6 N4 Co1 N3 33.7(3) . . . . ? N4 Co1 N3 C5 -13.0(3) . . . . ? Co1 N4 C7 C8 50.3(3) . . . . ? N4 C7 C8 N1 -42.7(4) . . . . ? C7 C8 N1 Co1 13.4(4) . . . . ? C8 N1 Co1 N4 12.8(3) . . . . ? N1 Co1 N4 C7 -35.1(2) . . . . ? Co1 N2 C9 C10 -31.8(5) . . . . ? N2 C9 C10 C11 65.4(5) . . . . ? C9 C10 C11 N4 -66.4(4) . . . . ? C10 C11 N4 Co1 33.3(4) . . . . ? C11 N4 Co1 N2 -2.7(3) . . . . ? N4 Co1 N2 C9 2.3(3) . . . . ? Co1 N2 C9 C10 -31.8(5) . . . . ? Co2 N1A C1A C2A 11.2(4) . . . . ? N1A C1A C2A N2A -41.5(5) . . . . ? C1A C2A N2A Co2 50.0(4) . . . . ? C2A N2A Co2 N1A -35.5(3) . . . . ? N2A Co2 N1A C1A 14.1(3) . . . . ? Co2 N2A C3A C4A -51.1(4) . . . . ? N2A C3A C4A N3A 44.9(5) . . . . ? C3A C4A N3A Co2 -15.2(4) . . . . ? C4A N3A Co2 N2A -11.2(3) . . . . ? N3A Co2 N2A C3A 34.2(3) . . . . ? Co2 N3A C5A C6A 13.6(4) . . . . ? N3A C5A C6A N4A -43.6(4) . . . . ? C5A C6A N4A Co2 51.8(3) . . . . ? C6A N4A Co2 N3A -35.4(2) . . . . ? N4A Co2 N3A C5A 12.9(3) . . . . ? Co2 N4A C7A C8A -48.4(4) . . . . ? N4A C7A C8A N1A 42.2(4) . . . . ? C7A C8A N1A Co2 -13.9(4) . . . . ? C8A N1A Co2 N4A -11.1(3) . . . . ? N1A Co2 N4A C7A 32.6(2) . . . . ? Co2 N2A C9A C10A -20.1(7) . . . . ? N2A C9A C10A C11A 48.5(10) . . . . ? C9A C10A C11A N4A -50.9(9) . . . . ? C10A C11A N4A Co2 24.7(6) . . . . ? C11A N4A Co2 N2A -3.1(3) . . . . ? N4A Co2 N2A C9A 0.3(4) . . . . ? Co2 N2A C9A C10A -20.1(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O3A 0.93 2.11 3.002(4) 161.3 3 N3 H3 O2A 0.93 2.13 3.050(4) 171.0 . N1A H1A O10 0.93 2.01 2.906(5) 161.1 3_545 N3A H3A O3 0.93 2.17 2.966(4) 142.5 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.786 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.101