# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1598 data_fig2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'trans(N)-bis(2-aminoisobutyrato)(2,2'-bipyridine)cobalt(III) perchlorate sodium perchlorate' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H25 Cl2 Co N4 Na O12.50' _chemical_formula_weight 650.24 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.776(3) _cell_length_b 11.218(2) _cell_length_c 14.186(3) _cell_angle_alpha 76.904(14) _cell_angle_beta 79.31(3) _cell_angle_gamma 79.08(3) _cell_volume 1320.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 12.45 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.8 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4 Four Circle' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 497 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.88 _diffrn_reflns_number 7521 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.1510 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6367 _reflns_number_gt 3392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6367 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1596 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 1.47713(8) 0.32198(6) 0.28490(5) 0.01613(17) Uani 1 1 d . . . O1 O 1.5638(4) 0.4541(3) 0.3020(2) 0.0225(8) Uani 1 1 d . . . O2 O 1.7048(5) 0.5119(3) 0.3934(3) 0.0358(10) Uani 1 1 d . . . O3 O 1.3009(4) 0.3643(3) 0.3773(2) 0.0190(8) Uani 1 1 d . . . O4 O 1.0930(4) 0.5056(3) 0.3998(2) 0.0248(8) Uani 1 1 d . . . N1 N 1.5812(5) 0.2236(3) 0.3928(3) 0.0199(9) Uani 1 1 d . . . HN1 H 1.5071 0.1969 0.4444 0.05(2) Uiso 1 1 calc R . . HN2 H 1.6435 0.1550 0.3736 0.015(13) Uiso 1 1 calc R . . N2 N 1.3649(5) 0.4390(4) 0.1877(3) 0.0192(9) Uani 1 1 d . . . HN3 H 1.4311 0.4911 0.1489 0.037(17) Uiso 1 1 calc R . . HN4 H 1.3334 0.3965 0.1482 0.017(13) Uiso 1 1 calc R . . C1 C 1.6800(6) 0.2973(5) 0.4253(4) 0.0219(11) Uani 1 1 d . . . C2 C 1.8541(6) 0.2486(5) 0.3958(4) 0.0327(14) Uani 1 1 d . . . H2A H 1.9192 0.2997 0.4136 0.06(2) Uiso 1 1 calc R . . H2B H 1.8759 0.2525 0.3249 0.08(2) Uiso 1 1 calc R . . H2C H 1.8785 0.1626 0.4300 0.09(3) Uiso 1 1 calc R . . C3 C 1.6456(7) 0.2880(5) 0.5363(4) 0.0346(14) Uani 1 1 d . . . H3A H 1.6644 0.2009 0.5691 0.042 Uiso 1 1 calc R . . H3B H 1.5359 0.3229 0.5549 0.041(17) Uiso 1 1 calc R . . H3C H 1.7146 0.3343 0.5559 0.031(15) Uiso 1 1 calc R . . C4 C 1.6469(6) 0.4326(4) 0.3719(4) 0.0219(11) Uani 1 1 d . . . C5 C 1.2026(6) 0.4597(4) 0.3451(3) 0.0185(10) Uani 1 1 d . . . C6 C 1.2248(6) 0.5138(4) 0.2350(3) 0.0180(10) Uani 1 1 d . . . C7 C 1.0785(6) 0.5050(6) 0.1959(4) 0.0314(14) Uani 1 1 d . . . H7A H 1.0911 0.5370 0.1251 0.026(14) Uiso 1 1 calc R . . H7B H 0.9875 0.5541 0.2279 0.06(2) Uiso 1 1 calc R . . H7C H 1.0625 0.4183 0.2094 0.020(14) Uiso 1 1 calc R . . C8 C 1.2533(7) 0.6480(4) 0.2188(4) 0.0324(14) Uani 1 1 d . . . H8A H 1.1649 0.6957 0.2541 0.028(15) Uiso 1 1 calc R . . H8B H 1.2630 0.6846 0.1487 0.019(13) Uiso 1 1 calc R . . H8C H 1.3503 0.6496 0.2431 0.023 Uiso 1 1 calc R . . N3 N 1.4000(5) 0.1801(4) 0.2663(3) 0.0209(10) Uani 1 1 d . . . N4 N 1.6454(5) 0.2767(4) 0.1862(3) 0.0233(10) Uani 1 1 d . . . C9 C 1.2666(7) 0.1414(5) 0.3099(4) 0.0308(13) Uani 1 1 d . . . H9 H 1.2005 0.1853 0.3559 0.037 Uiso 1 1 calc R . . C10 C 1.2195(8) 0.0387(5) 0.2909(5) 0.0400(15) Uani 1 1 d . . . H10 H 1.1215 0.0140 0.3215 0.048 Uiso 1 1 calc R . . C11 C 1.3199(10) -0.0263(5) 0.2259(5) 0.053(2) Uani 1 1 d . . . H11 H 1.2921 -0.0978 0.2122 0.064 Uiso 1 1 calc R . . C12 C 1.4590(9) 0.0126(6) 0.1815(5) 0.0425(17) Uani 1 1 d . . . H12 H 1.525(7) -0.029(5) 0.139(4) 0.045(19) Uiso 1 1 d . . . C13 C 1.4973(7) 0.1178(5) 0.2015(4) 0.0271(13) Uani 1 1 d . . . C14 C 1.6362(7) 0.1740(5) 0.1555(4) 0.0285(13) Uani 1 1 d . . . C15 C 1.7510(8) 0.1305(6) 0.0838(4) 0.0457(18) Uani 1 1 d . . . H15 H 1.7434 0.0582 0.0618 0.055 Uiso 1 1 calc R . . C16 C 1.8755(9) 0.1942(8) 0.0454(5) 0.056(2) Uani 1 1 d . . . H16 H 1.958(8) 0.167(6) -0.002(4) 0.06(2) Uiso 1 1 d . . . C17 C 1.8818(7) 0.3018(7) 0.0753(4) 0.0484(18) Uani 1 1 d . . . H17 H 1.9651 0.3481 0.0479 0.058 Uiso 1 1 calc R . . C18 C 1.7642(6) 0.3405(6) 0.1462(4) 0.0329(14) Uani 1 1 d . . . H18 H 1.7675 0.4145 0.1672 0.040 Uiso 1 1 calc R . . Na Na 0.8529(2) 0.61383(17) 0.44414(14) 0.0242(5) Uani 1 1 d . . . Cl1 Cl 0.7864(2) 0.89629(13) 0.39760(12) 0.0425(4) Uani 1 1 d . . . O5 O 0.8051(6) 0.9955(4) 0.3175(3) 0.0510(12) Uani 1 1 d . . . O6 O 0.9088(12) 0.8352(10) 0.4394(7) 0.045(2) Uani 0.60 1 d P . . O6' O 0.9507(18) 0.8145(14) 0.3928(14) 0.065(6) Uani 0.40 1 d P . . O7 O 0.7255(17) 0.8056(10) 0.3549(9) 0.091(5) Uani 0.60 1 d P . . O7' O 0.6781(18) 0.8278(14) 0.4190(12) 0.062(5) Uani 0.40 1 d P . . O8 O 0.6582(12) 0.9387(8) 0.4661(8) 0.085(4) Uani 0.60 1 d P . . O8' O 0.801(3) 0.9554(14) 0.4803(11) 0.129(9) Uani 0.40 1 d P . . Cl2 Cl 0.65993(18) 0.69628(13) 1.02819(9) 0.0322(3) Uani 1 1 d . . . O9 O 0.7377(5) 0.7205(4) 0.9290(3) 0.0363(10) Uani 1 1 d . . . O10 O 0.5639(7) 0.8056(4) 1.0503(4) 0.0741(17) Uani 1 1 d . . . O11 O 0.7745(6) 0.6489(5) 1.0919(3) 0.0638(14) Uani 1 1 d . . . O12 O 0.5620(6) 0.6027(4) 1.0345(3) 0.0562(13) Uani 1 1 d . . . OW1 O 0.8746(14) 0.8426(10) 1.1510(8) 0.093(4) Uani 0.50 1 d P . . HW1 H 0.9772 0.8024 1.1712 0.111 Uiso 0.50 1 calc PR . . HW2 H 0.7947 0.8644 1.2061 0.111 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0158(4) 0.0165(3) 0.0169(4) -0.0057(3) -0.0023(3) -0.0017(3) O1 0.023(2) 0.0183(18) 0.028(2) -0.0025(15) -0.0100(17) -0.0058(16) O2 0.042(3) 0.027(2) 0.045(2) -0.0105(18) -0.018(2) -0.0086(19) O3 0.021(2) 0.0176(17) 0.0155(17) -0.0040(14) 0.0010(15) -0.0003(15) O4 0.023(2) 0.030(2) 0.0189(18) -0.0100(15) 0.0034(16) 0.0013(17) N1 0.024(2) 0.014(2) 0.023(2) -0.0037(17) -0.005(2) -0.0014(19) N2 0.019(2) 0.023(2) 0.015(2) -0.0023(18) -0.0018(18) -0.0024(19) C1 0.018(3) 0.024(3) 0.023(3) -0.006(2) -0.005(2) 0.000(2) C2 0.024(3) 0.032(3) 0.045(4) -0.011(3) -0.012(3) 0.002(3) C3 0.041(4) 0.036(3) 0.031(3) -0.009(3) -0.011(3) -0.007(3) C4 0.015(3) 0.021(3) 0.029(3) -0.007(2) -0.001(2) -0.002(2) C5 0.020(3) 0.018(2) 0.020(3) -0.007(2) -0.005(2) -0.002(2) C6 0.012(2) 0.019(2) 0.020(3) -0.005(2) 0.001(2) 0.002(2) C7 0.024(3) 0.049(4) 0.020(3) -0.006(3) -0.007(2) 0.001(3) C8 0.039(4) 0.021(3) 0.031(3) -0.004(2) 0.004(3) 0.001(3) N3 0.023(3) 0.019(2) 0.021(2) -0.0033(18) -0.003(2) -0.0028(19) N4 0.018(2) 0.030(2) 0.021(2) -0.0076(19) -0.0022(19) 0.002(2) C9 0.034(3) 0.023(3) 0.036(3) -0.003(2) -0.008(3) -0.006(3) C10 0.041(4) 0.032(3) 0.051(4) 0.000(3) -0.014(3) -0.019(3) C11 0.088(6) 0.023(3) 0.060(5) -0.017(3) -0.028(4) -0.011(4) C12 0.064(5) 0.026(3) 0.040(4) -0.013(3) -0.009(4) -0.005(3) C13 0.034(3) 0.020(3) 0.028(3) -0.009(2) -0.011(3) 0.007(2) C14 0.026(3) 0.027(3) 0.026(3) -0.009(2) -0.002(3) 0.013(3) C15 0.048(4) 0.054(4) 0.027(3) -0.018(3) -0.004(3) 0.021(3) C16 0.038(4) 0.085(6) 0.026(3) -0.010(4) 0.011(3) 0.018(4) C17 0.020(3) 0.087(5) 0.025(3) 0.004(3) 0.004(3) -0.001(3) C18 0.022(3) 0.054(4) 0.021(3) -0.003(3) -0.002(2) -0.008(3) Na 0.0237(12) 0.0186(10) 0.0310(11) -0.0089(9) -0.0052(9) 0.0011(9) Cl1 0.0511(11) 0.0191(7) 0.0494(10) 0.0033(7) -0.0064(8) 0.0006(7) O5 0.078(4) 0.027(2) 0.040(2) 0.0073(19) -0.007(2) -0.007(2) O6 0.031(6) 0.038(6) 0.056(6) -0.001(4) -0.013(5) 0.011(4) O6' 0.023(8) 0.022(7) 0.135(18) -0.013(9) 0.013(9) 0.002(6) O7 0.122(12) 0.026(5) 0.147(12) 0.001(7) -0.088(10) -0.019(6) O7' 0.039(8) 0.042(9) 0.092(12) 0.024(9) -0.003(9) -0.029(7) O8 0.088(8) 0.034(5) 0.087(8) 0.009(5) 0.052(6) 0.015(5) O8' 0.30(3) 0.051(9) 0.054(9) -0.007(7) -0.061(15) -0.046(15) Cl2 0.0372(9) 0.0362(8) 0.0225(7) -0.0104(6) -0.0037(6) 0.0006(7) O9 0.040(3) 0.044(2) 0.024(2) -0.0060(18) 0.0012(19) -0.012(2) O10 0.092(4) 0.062(3) 0.069(3) -0.041(3) -0.013(3) 0.021(3) O11 0.070(4) 0.080(4) 0.044(3) 0.004(3) -0.031(3) -0.015(3) O12 0.059(3) 0.062(3) 0.051(3) -0.010(2) 0.007(2) -0.037(3) OW1 0.080(9) 0.096(9) 0.103(9) -0.049(8) -0.002(7) 0.007(7) _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 O1 1.869(3) . ? Co O3 1.894(3) . ? Co N4 1.916(4) . ? Co N3 1.930(4) . ? Co N1 1.940(4) . ? Co N2 1.947(4) . ? O1 C4 1.291(6) . ? O2 C4 1.223(6) . ? O2 Na 2.190(4) 1_655 ? O3 C5 1.294(5) . ? O3 Na 2.680(4) 2_766 ? O4 C5 1.228(5) . ? O4 Na 2.279(4) . ? O4 Na 2.393(4) 2_766 ? N1 C1 1.497(6) . ? N2 C6 1.491(6) . ? C1 C3 1.530(7) . ? C1 C4 1.534(7) . ? C1 C2 1.536(7) . ? C5 C6 1.533(6) . ? C5 Na 2.889(5) 2_766 ? C6 C7 1.517(7) . ? C6 C8 1.532(7) . ? N3 C9 1.320(7) . ? N3 C13 1.355(6) . ? N4 C14 1.341(6) . ? N4 C18 1.342(7) . ? C9 C10 1.391(7) . ? C10 C11 1.385(9) . ? C11 C12 1.367(9) . ? C12 C13 1.388(7) . ? C13 C14 1.456(8) . ? C14 C15 1.395(7) . ? C15 C16 1.378(10) . ? C16 C17 1.381(10) . ? C17 C18 1.381(8) . ? Na O2 2.190(4) 1_455 ? Na O4 2.393(4) 2_766 ? Na O7 2.420(11) . ? Na O6' 2.468(16) . ? Na O7' 2.581(17) . ? Na O6 2.605(11) . ? Na O3 2.680(4) 2_766 ? Na C5 2.889(5) 2_766 ? Na Cl1 3.051(2) . ? Na Na 3.590(4) 2_766 ? Cl1 O7' 1.284(14) . ? Cl1 O6 1.322(10) . ? Cl1 O5 1.408(4) . ? Cl1 O8 1.427(8) . ? Cl1 O8' 1.509(14) . ? Cl1 O7 1.514(10) . ? Cl1 O6' 1.554(15) . ? O6 O6' 0.756(16) . ? O6 O8' 1.65(2) . ? O7 O7' 0.993(16) . ? O7' O8 1.507(18) . ? O8 O8' 1.36(2) . ? Cl2 O10 1.414(4) . ? Cl2 O11 1.424(5) . ? Cl2 O9 1.436(4) . ? Cl2 O12 1.456(4) . ? 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 Co O3 89.00(15) . . ? O1 Co N4 94.13(17) . . ? O3 Co N4 175.98(18) . . ? O1 Co N3 176.62(17) . . ? O3 Co N3 93.75(16) . . ? N4 Co N3 83.22(18) . . ? O1 Co N1 86.22(16) . . ? O3 Co N1 88.50(16) . . ? N4 Co N1 94.22(18) . . ? N3 Co N1 91.86(17) . . ? O1 Co N2 87.72(16) . . ? O3 Co N2 85.93(15) . . ? N4 Co N2 91.67(17) . . ? N3 Co N2 94.45(17) . . ? N1 Co N2 171.83(17) . . ? C4 O1 Co 117.1(3) . . ? C4 O2 Na 165.5(4) . 1_655 ? C5 O3 Co 115.2(3) . . ? C5 O3 Na 85.8(3) . 2_766 ? Co O3 Na 155.57(17) . 2_766 ? C5 O4 Na 157.4(3) . . ? C5 O4 Na 100.9(3) . 2_766 ? Na O4 Na 100.38(14) . 2_766 ? C1 N1 Co 111.0(3) . . ? C6 N2 Co 111.3(3) . . ? N1 C1 C3 111.1(4) . . ? N1 C1 C4 108.5(4) . . ? C3 C1 C4 110.6(4) . . ? N1 C1 C2 109.2(4) . . ? C3 C1 C2 109.3(4) . . ? C4 C1 C2 108.0(4) . . ? O2 C4 O1 123.7(5) . . ? O2 C4 C1 119.8(5) . . ? O1 C4 C1 116.4(4) . . ? O4 C5 O3 121.9(4) . . ? O4 C5 C6 120.2(4) . . ? O3 C5 C6 117.9(4) . . ? O4 C5 Na 54.4(2) . 2_766 ? O3 C5 Na 67.7(2) . 2_766 ? C6 C5 Na 173.5(3) . 2_766 ? N2 C6 C7 110.4(4) . . ? N2 C6 C8 109.4(4) . . ? C7 C6 C8 111.9(4) . . ? N2 C6 C5 108.2(4) . . ? C7 C6 C5 107.9(4) . . ? C8 C6 C5 108.9(4) . . ? C9 N3 C13 119.8(5) . . ? C9 N3 Co 126.4(4) . . ? C13 N3 Co 113.8(4) . . ? C14 N4 C18 119.9(5) . . ? C14 N4 Co 114.8(4) . . ? C18 N4 Co 125.2(4) . . ? N3 C9 C10 122.4(6) . . ? C11 C10 C9 117.9(6) . . ? C12 C11 C10 119.9(6) . . ? C11 C12 C13 119.4(6) . . ? N3 C13 C12 120.6(6) . . ? N3 C13 C14 114.0(5) . . ? C12 C13 C14 125.4(5) . . ? N4 C14 C15 120.8(6) . . ? N4 C14 C13 114.1(4) . . ? C15 C14 C13 125.0(5) . . ? C16 C15 C14 118.9(6) . . ? C15 C16 C17 119.9(6) . . ? C18 C17 C16 118.5(6) . . ? N4 C18 C17 121.9(6) . . ? O2 Na O4 99.48(15) 1_455 . ? O2 Na O4 105.53(15) 1_455 2_766 ? O4 Na O4 79.62(14) . 2_766 ? O2 Na O7 89.5(3) 1_455 . ? O4 Na O7 127.8(4) . . ? O4 Na O7 146.8(3) 2_766 . ? O2 Na O6' 138.1(5) 1_455 . ? O4 Na O6' 92.8(3) . . ? O4 Na O6' 116.1(5) 2_766 . ? O7 Na O6' 52.6(5) . . ? O2 Na O7' 97.8(4) 1_455 . ? O4 Na O7' 144.9(3) . . ? O4 Na O7' 124.3(4) 2_766 . ? O7 Na O7' 22.6(4) . . ? O6' Na O7' 55.0(5) . . ? O2 Na O6 143.5(3) 1_455 . ? O4 Na O6 104.4(2) . . ? O4 Na O6 105.6(2) 2_766 . ? O7 Na O6 54.0(3) . . ? O6' Na O6 16.9(4) . . ? O7' Na O6 48.2(4) . . ? O2 Na O3 102.22(15) 1_455 2_766 ? O4 Na O3 129.82(14) . 2_766 ? O4 Na O3 51.14(11) 2_766 2_766 ? O7 Na O3 97.2(4) . 2_766 ? O6' Na O3 100.0(4) . 2_766 ? O7' Na O3 74.9(4) . 2_766 ? O6 Na O3 83.1(2) . 2_766 ? O2 Na C5 104.28(16) 1_455 2_766 ? O4 Na C5 104.08(15) . 2_766 ? O4 Na C5 24.67(12) 2_766 2_766 ? O7 Na C5 123.4(4) . 2_766 ? O6' Na C5 111.3(5) . 2_766 ? O7' Na C5 100.9(4) . 2_766 ? O6 Na C5 96.3(2) . 2_766 ? O3 Na C5 26.53(11) 2_766 2_766 ? O2 Na Cl1 118.16(13) 1_455 . ? O4 Na Cl1 122.36(12) . . ? O4 Na Cl1 123.76(11) 2_766 . ? O7 Na Cl1 29.3(3) . . ? O6' Na Cl1 30.4(3) . . ? O7' Na Cl1 24.6(3) . . ? O6 Na Cl1 25.5(2) . . ? O3 Na Cl1 84.89(9) 2_766 . ? C5 Na Cl1 106.47(11) 2_766 . ? O2 Na Na 106.44(13) 1_455 2_766 ? O4 Na Na 40.98(9) . 2_766 ? O4 Na Na 38.65(9) 2_766 2_766 ? O7 Na Na 161.1(3) . 2_766 ? O6' Na Na 108.9(4) . 2_766 ? O7' Na Na 153.5(4) . 2_766 ? O6 Na Na 109.8(2) . 2_766 ? O3 Na Na 89.33(10) 2_766 2_766 ? C5 Na Na 63.17(11) 2_766 2_766 ? Cl1 Na Na 135.26(10) . 2_766 ? O7' Cl1 O6 108.6(9) . . ? O7' Cl1 O5 127.3(8) . . ? O6 Cl1 O5 120.2(5) . . ? O7' Cl1 O8 67.3(8) . . ? O6 Cl1 O8 112.9(6) . . ? O5 Cl1 O8 107.1(4) . . ? O7' Cl1 O8' 113.6(11) . . ? O6 Cl1 O8' 70.8(10) . . ? O5 Cl1 O8' 100.6(6) . . ? O8 Cl1 O8' 55.2(9) . . ? O7' Cl1 O7 40.5(7) . . ? O6 Cl1 O7 107.3(7) . . ? O5 Cl1 O7 102.8(5) . . ? O8 Cl1 O7 105.0(8) . . ? O8' Cl1 O7 153.3(9) . . ? O7' Cl1 O6' 110.2(10) . . ? O6 Cl1 O6' 29.1(8) . . ? O5 Cl1 O6' 103.7(7) . . ? O8 Cl1 O6' 141.4(8) . . ? O8' Cl1 O6' 96.9(12) . . ? O7 Cl1 O6' 89.9(8) . . ? O7' Cl1 Na 56.7(7) . . ? O6 Cl1 Na 58.0(5) . . ? O5 Cl1 Na 139.7(2) . . ? O8 Cl1 Na 109.5(4) . . ? O8' Cl1 Na 113.7(6) . . ? O7 Cl1 Na 51.5(4) . . ? O6' Cl1 Na 53.6(6) . . ? O6' O6 Cl1 93(2) . . ? O6' O6 O8' 142(2) . . ? Cl1 O6 O8' 59.9(7) . . ? O6' O6 Na 71.3(19) . . ? Cl1 O6 Na 96.5(6) . . ? O8' O6 Na 132.5(10) . . ? O6 O6' Cl1 58.2(15) . . ? O6 O6' Na 92(2) . . ? Cl1 O6' Na 96.0(7) . . ? O7' O7 Cl1 57.2(11) . . ? O7' O7 Na 87.8(14) . . ? Cl1 O7 Na 99.1(6) . . ? O7 O7' Cl1 82.3(13) . . ? O7 O7' O8 137.1(16) . . ? Cl1 O7' O8 60.9(8) . . ? O7 O7' Na 69.6(13) . . ? Cl1 O7' Na 98.7(9) . . ? O8 O7' Na 133.1(10) . . ? O8' O8 Cl1 65.4(8) . . ? O8' O8 O7' 109.1(12) . . ? Cl1 O8 O7' 51.8(6) . . ? O8 O8' Cl1 59.3(7) . . ? O8 O8' O6 98.7(10) . . ? Cl1 O8' O6 49.3(6) . . ? O10 Cl2 O11 112.3(3) . . ? O10 Cl2 O9 109.6(3) . . ? O11 Cl2 O9 109.2(3) . . ? O10 Cl2 O12 109.3(3) . . ? O11 Cl2 O12 109.5(3) . . ? O9 Cl2 O12 106.7(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.581 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.110 data_stala _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'trans(N)-bis(alaninato)(2,2'-bipyridine)cobalt(III) perchlorate monohydrate' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Cl Co N4 O9' _chemical_formula_weight 508.76 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 P2(1)/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 10.556(7) _cell_length_b 10.345(7) _cell_length_c 18.62(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.06(8) _cell_angle_gamma 90.00 _cell_volume 2008(3) _cell_formula_units_Z 4 _cell_measurement_temperature 144(2) _cell_measurement_reflns_used 27 _cell_measurement_2theta_min 5.745 _cell_measurement_2theta_max 27.937 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5277 _exptl_absorpt_correction_T_max 0.8179 _exptl_absorpt_process_details 'psi scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 144(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4 four circle' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3872 _diffrn_reflns_av_R_equivalents 0.0902 _diffrn_reflns_av_sigmaI/netI 0.0910 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3531 _reflns_number_gt 2250 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCAnS _computing_cell_refinement XSCAnS _computing_data_reduction XSCAnS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics xp _computing_publication_material xcif _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^)+(0.0496P)^2^+2.2925P] 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 9999 _refine_ls_number_reflns 3531 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.80109(7) 0.84722(7) 0.14931(4) 0.0208(2) Uani 1 1 d . . . N1 N 0.9031(4) 0.7453(4) 0.2246(2) 0.0277(11) Uani 1 1 d . . . H1N H 0.8539 0.6795 0.2388 0.044(19) Uiso 1 1 calc R . . H2N H 0.9712 0.7090 0.2066 0.08(3) Uiso 1 1 calc R . . N2 N 0.7140(4) 0.9688(4) 0.0791(2) 0.0226(10) Uani 1 1 d . . . H3N H 0.6498 0.9273 0.0485 0.041(18) Uiso 1 1 calc R . . H4N H 0.6776 1.0338 0.1027 0.08(3) Uiso 1 1 calc R . . O2 O 0.8024(3) 0.9754(3) 0.22168(19) 0.0252(9) Uani 1 1 d . . . O3 O 0.9547(3) 0.9194(4) 0.1268(2) 0.0285(9) Uani 1 1 d . . . C1 C 0.9515(6) 0.8272(6) 0.2881(3) 0.0412(17) Uani 1 1 d . . . H1B H 0.9221 0.7863 0.3313 0.049 Uiso 1 1 calc R . . C2 C 1.0920(6) 0.8321(7) 0.3036(5) 0.068(3) Uani 1 1 d . . . H2B H 1.1262 0.7442 0.3112 0.102 Uiso 1 1 calc R . . H2C H 1.1188 0.8836 0.3476 0.102 Uiso 1 1 calc R . . H2D H 1.1250 0.8718 0.2625 0.102 Uiso 1 1 calc R . . C3 C 0.8883(5) 0.9603(5) 0.2786(3) 0.0261(13) Uani 1 1 d . . . C4 C 0.9391(6) 1.0149(6) 0.0826(3) 0.0347(15) Uani 1 1 d . . . C5 C 0.8074(7) 1.0237(9) 0.0368(5) 0.073(3) Uani 1 1 d . . . H5A H 0.8113 0.9572 -0.0018 0.088 Uiso 1 1 calc R . . C6 C 0.7727(6) 1.1405(6) -0.0047(3) 0.0412(16) Uani 1 1 d . . . H6A H 0.6895 1.1283 -0.0356 0.062 Uiso 1 1 calc R . . H6B H 0.8381 1.1594 -0.0352 0.062 Uiso 1 1 calc R . . H6C H 0.7672 1.2128 0.0287 0.062 Uiso 1 1 calc R . . O1 O 0.9158(4) 1.0432(4) 0.3251(2) 0.0325(10) Uani 1 1 d . . . O4 O 1.0253(4) 1.0898(4) 0.0739(2) 0.0427(11) Uani 1 1 d . . . N3 N 0.7963(4) 0.7086(4) 0.0806(2) 0.0208(10) Uani 1 1 d . . . N4 N 0.6424(4) 0.7734(4) 0.1664(2) 0.0216(10) Uani 1 1 d . . . C7 C 0.8770(5) 0.6902(5) 0.0334(3) 0.0278(14) Uani 1 1 d . . . H7A H 0.9435 0.7515 0.0316 0.033 Uiso 1 1 calc R . . C8 C 0.8681(5) 0.5866(6) -0.0126(3) 0.0298(14) Uani 1 1 d . . . H8A H 0.9257 0.5778 -0.0467 0.036 Uiso 1 1 calc R . . C9 C 0.7742(6) 0.4950(6) -0.0089(3) 0.0301(14) Uani 1 1 d . . . H9A H 0.7677 0.4216 -0.0399 0.036 Uiso 1 1 calc R . . C10 C 0.6900(6) 0.5104(5) 0.0400(3) 0.0300(14) Uani 1 1 d . . . H10A H 0.6256 0.4478 0.0440 0.036 Uiso 1 1 calc R . . C11 C 0.7023(5) 0.6203(5) 0.0833(3) 0.0223(12) Uani 1 1 d . . . C12 C 0.6109(5) 0.6595(5) 0.1327(3) 0.0238(12) Uani 1 1 d . . . C13 C 0.4995(5) 0.5949(6) 0.1402(3) 0.0328(14) Uani 1 1 d . . . H13A H 0.4809 0.5128 0.1183 0.039 Uiso 1 1 calc R . . C14 C 0.4155(6) 0.6523(7) 0.1804(3) 0.0376(15) Uani 1 1 d . . . H14A H 0.3382 0.6095 0.1863 0.045 Uiso 1 1 calc R . . C15 C 0.4436(5) 0.7709(6) 0.2118(3) 0.0364(16) Uani 1 1 d . . . H15A H 0.3845 0.8131 0.2376 0.044 Uiso 1 1 calc R . . C16 C 0.5611(5) 0.8284(6) 0.2052(3) 0.0291(14) Uani 1 1 d . . . H16A H 0.5834 0.9085 0.2289 0.035 Uiso 1 1 calc R . . Cl Cl 0.52917(13) 0.79628(14) -0.09477(8) 0.0326(4) Uani 1 1 d . . . O5 O 0.5386(5) 0.7946(5) -0.0176(3) 0.0615(15) Uani 1 1 d . . . O6 O 0.4027(4) 0.7568(5) -0.1261(2) 0.0575(14) Uani 1 1 d . . . O7 O 0.5492(5) 0.9247(4) -0.1181(3) 0.0692(17) Uani 1 1 d . . . O8 O 0.6212(4) 0.7125(4) -0.1188(3) 0.0570(14) Uani 1 1 d . . . O1W O 0.7728(6) 0.5570(6) 0.3023(3) 0.0465(13) Uani 1 1 d . . . H1W H 0.820(8) 0.565(8) 0.339(4) 0.07(3) Uiso 1 1 d . . . H2W H 0.716(11) 0.586(12) 0.315(6) 0.15(6) Uiso 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 0.0181(4) 0.0179(4) 0.0263(4) 0.0001(4) 0.0027(3) 0.0003(3) N1 0.021(3) 0.026(3) 0.035(3) 0.000(2) 0.003(2) -0.001(2) N2 0.022(2) 0.020(2) 0.027(3) 0.000(2) 0.006(2) -0.003(2) O2 0.024(2) 0.023(2) 0.028(2) -0.0012(17) 0.0033(17) 0.0006(17) O3 0.019(2) 0.024(2) 0.043(2) -0.001(2) 0.0060(18) -0.0041(17) C1 0.039(4) 0.038(4) 0.040(4) -0.008(3) -0.014(3) 0.003(3) C2 0.038(4) 0.049(5) 0.106(7) -0.029(5) -0.025(4) 0.004(4) C3 0.025(3) 0.026(3) 0.027(3) -0.001(3) 0.006(3) -0.004(3) C4 0.027(3) 0.038(4) 0.040(4) 0.000(3) 0.009(3) -0.011(3) C5 0.045(5) 0.080(6) 0.090(6) 0.056(5) -0.003(4) -0.021(4) C6 0.040(4) 0.034(4) 0.052(4) 0.020(3) 0.014(3) 0.004(3) O1 0.040(2) 0.025(2) 0.033(2) -0.004(2) 0.0066(19) -0.0059(19) O4 0.036(2) 0.045(3) 0.048(3) 0.001(2) 0.011(2) -0.015(2) N3 0.017(2) 0.020(2) 0.024(2) -0.002(2) -0.0007(19) 0.002(2) N4 0.018(2) 0.022(3) 0.024(2) 0.003(2) 0.001(2) 0.000(2) C7 0.030(3) 0.024(3) 0.030(3) 0.001(3) 0.007(3) 0.001(3) C8 0.029(3) 0.035(4) 0.026(3) 0.001(3) 0.008(3) 0.010(3) C9 0.041(4) 0.020(3) 0.025(3) -0.001(3) -0.006(3) 0.008(3) C10 0.035(3) 0.021(3) 0.032(3) 0.002(3) -0.003(3) -0.004(3) C11 0.025(3) 0.015(3) 0.024(3) 0.004(2) -0.002(2) -0.001(2) C12 0.024(3) 0.024(3) 0.021(3) 0.005(3) -0.004(2) -0.005(3) C13 0.032(3) 0.028(3) 0.037(4) 0.005(3) 0.000(3) -0.012(3) C14 0.033(3) 0.044(4) 0.036(3) 0.009(3) 0.003(3) -0.012(3) C15 0.030(3) 0.049(4) 0.033(4) 0.003(3) 0.014(3) 0.002(3) C16 0.030(3) 0.031(4) 0.027(3) -0.001(3) 0.008(3) -0.001(3) Cl 0.0262(8) 0.0280(8) 0.0411(9) 0.0080(7) -0.0026(6) -0.0008(7) O5 0.057(3) 0.076(4) 0.044(3) 0.003(3) -0.016(2) 0.002(3) O6 0.035(3) 0.092(4) 0.045(3) -0.014(3) 0.002(2) -0.024(3) O7 0.063(3) 0.028(3) 0.127(5) 0.024(3) 0.046(3) 0.009(2) O8 0.049(3) 0.040(3) 0.082(4) 0.000(3) 0.009(3) 0.018(2) O1W 0.037(3) 0.065(4) 0.039(3) 0.010(3) 0.010(3) 0.006(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 O2 1.889(4) . ? Co O3 1.891(4) . ? Co N4 1.912(4) . ? Co N3 1.917(5) . ? Co N2 1.939(5) . ? Co N1 1.940(5) . ? N1 C1 1.478(7) . ? N2 C5 1.469(8) . ? O2 C3 1.290(7) . ? O3 C4 1.280(7) . ? C1 C2 1.467(9) . ? C1 C3 1.529(8) . ? C3 O1 1.221(6) . ? C4 O4 1.226(7) . ? C4 C5 1.515(9) . ? C5 C6 1.450(9) . ? N3 C7 1.331(7) . ? N3 C11 1.356(6) . ? N4 C16 1.334(7) . ? N4 C12 1.352(7) . ? C7 C8 1.366(8) . ? C8 C9 1.381(8) . ? C9 C10 1.379(8) . ? C10 C11 1.388(7) . ? C11 C12 1.489(8) . ? C12 C13 1.379(7) . ? C13 C14 1.381(8) . ? C14 C15 1.372(9) . ? C15 C16 1.398(8) . ? Cl O7 1.424(5) . ? Cl O5 1.424(5) . ? Cl O8 1.426(5) . ? Cl O6 1.430(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co O3 88.30(17) . . ? O2 Co N4 94.03(18) . . ? O3 Co N4 176.80(18) . . ? O2 Co N3 176.00(18) . . ? O3 Co N3 94.64(18) . . ? N4 Co N3 83.14(19) . . ? O2 Co N2 88.59(19) . . ? O3 Co N2 85.77(18) . . ? N4 Co N2 92.09(19) . . ? N3 Co N2 94.3(2) . . ? O2 Co N1 85.69(19) . . ? O3 Co N1 88.68(19) . . ? N4 Co N1 93.7(2) . . ? N3 Co N1 91.7(2) . . ? N2 Co N1 172.14(19) . . ? C1 N1 Co 110.5(4) . . ? C5 N2 Co 109.0(4) . . ? C3 O2 Co 115.2(3) . . ? C4 O3 Co 114.8(4) . . ? C2 C1 N1 112.9(6) . . ? C2 C1 C3 113.6(5) . . ? N1 C1 C3 109.5(5) . . ? O1 C3 O2 123.8(5) . . ? O1 C3 C1 119.9(5) . . ? O2 C3 C1 116.2(5) . . ? O4 C4 O3 123.4(6) . . ? O4 C4 C5 121.5(6) . . ? O3 C4 C5 115.0(5) . . ? C6 C5 N2 118.2(6) . . ? C6 C5 C4 118.8(6) . . ? N2 C5 C4 108.0(6) . . ? C7 N3 C11 118.5(5) . . ? C7 N3 Co 126.5(4) . . ? C11 N3 Co 114.9(4) . . ? C16 N4 C12 119.4(5) . . ? C16 N4 Co 125.1(4) . . ? C12 N4 Co 115.4(4) . . ? N3 C7 C8 122.6(5) . . ? C7 C8 C9 119.1(5) . . ? C10 C9 C8 119.8(5) . . ? C9 C10 C11 117.8(5) . . ? N3 C11 C10 122.2(5) . . ? N3 C11 C12 112.9(5) . . ? C10 C11 C12 124.8(5) . . ? N4 C12 C13 121.8(5) . . ? N4 C12 C11 112.8(5) . . ? C13 C12 C11 125.2(5) . . ? C12 C13 C14 118.6(6) . . ? C15 C14 C13 120.1(6) . . ? C14 C15 C16 118.5(6) . . ? N4 C16 C15 121.5(6) . . ? O7 Cl O5 109.2(3) . . ? O7 Cl O8 109.3(3) . . ? O5 Cl O8 111.5(3) . . ? O7 Cl O6 108.4(3) . . ? O5 Cl O6 108.7(3) . . ? O8 Cl O6 109.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.749 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.096