# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1832 data_[Co(DCD)(acac)(NO2)] _publ_requested_category 'FM' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C13 H26 Cl2 Co N4 O4, Cl O4' _chemical_formula_sum 'C13 H26 Cl3 Co N4 O8' _chemical_formula_weight 531.66 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 15.7714(3) _cell_length_b 11.4969(2) _cell_length_c 12.75700(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.67 _cell_angle_gamma 90.00 _cell_volume 2191.35(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6909 _cell_measurement_theta_min 5.983 _cell_measurement_theta_max 12.051 _exptl_crystal_description prism _exptl_crystal_colour Purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7874 _exptl_absorpt_correction_T_max 0.9000 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method multi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13351 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4817 _reflns_number_gt 3681 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+4.8907P] 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 4817 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.19879(4) 0.12907(4) 0.27491(4) 0.03203(17) Uani 1 d . . . Cl1 Cl 0.43829(16) -0.0154(2) 0.6078(3) 0.1495(12) Uani 1 d . . . Cl2 Cl 0.39636(13) -0.28412(16) 0.3404(2) 0.0957(6) Uani 1 d . . . O1 O 0.2319(2) 0.0542(2) 0.1598(2) 0.0400(7) Uani 1 d . . . O2 O 0.3108(2) 0.2023(3) 0.3353(3) 0.0452(7) Uani 1 d . . . O3 O 0.2121(3) 0.2495(5) 0.4661(4) 0.0870(15) Uani 1 d . . . O4 O 0.0808(3) 0.2312(5) 0.3661(4) 0.0990(18) Uani 1 d . . . N1 N 0.1543(3) 0.2565(3) 0.1714(3) 0.0405(8) Uani 1 d . . . H1NA H 0.051(3) 0.089(5) 0.248(4) 0.049 Uiso 1 d . . . N2 N 0.0811(2) 0.0635(3) 0.2100(3) 0.0388(8) Uani 1 d . . . H2NA H 0.170(3) 0.333(5) 0.206(4) 0.047 Uiso 1 d . . . H2NB H 0.186(3) 0.247(4) 0.130(4) 0.047 Uiso 1 d . . . N3 N 0.2291(2) -0.0245(3) 0.3708(3) 0.0416(8) Uani 1 d . . . N4 N 0.1593(3) 0.2112(3) 0.3822(3) 0.0418(8) Uani 1 d . . . C1 C 0.0572(3) 0.2424(4) 0.1126(4) 0.0462(10) Uani 1 d . . . H1A H 0.0406 0.2806 0.0411 0.055 Uiso 1 calc R . . H1B H 0.0224 0.2759 0.1555 0.055 Uiso 1 calc R . . C2 C 0.0405(3) 0.1137(4) 0.0985(4) 0.0490(11) Uani 1 d . . . H2A H -0.0232 0.0975 0.0710 0.059 Uiso 1 calc R . . H2B H 0.0683 0.0818 0.0471 0.059 Uiso 1 calc R . . C3 C 0.0878(3) -0.0643(4) 0.2207(5) 0.0532(12) Uani 1 d . . . H3A H 0.1185 -0.0962 0.1723 0.064 Uiso 1 calc R . . H3B H 0.0287 -0.0990 0.2019 0.064 Uiso 1 calc R . . C4 C 0.1400(3) -0.0870(4) 0.3394(4) 0.0510(12) Uani 1 d . . . H4A H 0.1500 -0.1700 0.3509 0.061 Uiso 1 calc R . . H4B H 0.1061 -0.0604 0.3862 0.061 Uiso 1 calc R . . C5 C 0.2595(4) -0.0101(5) 0.4946(4) 0.0642(15) Uani 1 d . . . H5A H 0.2117 0.0274 0.5144 0.077 Uiso 1 calc R . . H5C H 0.2674 -0.0870 0.5276 0.077 Uiso 1 calc R . . C6 C 0.3432(6) 0.0569(6) 0.5461(6) 0.109(3) Uani 1 d . . . H6A H 0.3325 0.1086 0.6007 0.131 Uiso 1 calc R . . H6C H 0.3532 0.1056 0.4891 0.131 Uiso 1 calc R . . C7 C 0.2951(3) -0.0970(4) 0.3369(4) 0.0467(11) Uani 1 d . . . H7A H 0.3484 -0.0507 0.3464 0.056 Uiso 1 calc R . . H7B H 0.2696 -0.1142 0.2586 0.056 Uiso 1 calc R . . C8 C 0.3231(4) -0.2113(4) 0.3986(5) 0.0600(13) Uani 1 d . . . H8A H 0.2709 -0.2591 0.3916 0.072 Uiso 1 calc R . . H8B H 0.3532 -0.1964 0.4766 0.072 Uiso 1 calc R . . C9 C 0.3127(5) 0.0055(6) 0.0406(5) 0.0739(17) Uani 1 d . . . H9A H 0.2611 -0.0435 0.0116 0.111 Uiso 1 calc R . . H9B H 0.3655 -0.0418 0.0654 0.111 Uiso 1 calc R . . H9C H 0.3173 0.0573 -0.0163 0.111 Uiso 1 calc R . . C10 C 0.3033(3) 0.0748(4) 0.1359(4) 0.0464(11) Uani 1 d . . . C11 C 0.3694(3) 0.1525(5) 0.1921(4) 0.0563(13) Uani 1 d . . . H11A H 0.4162 0.1659 0.1641 0.068 Uiso 1 calc R . . C12 C 0.3704(3) 0.2115(4) 0.2870(4) 0.0509(11) Uani 1 d . . . C13 C 0.4461(4) 0.2910(7) 0.3462(6) 0.083(2) Uani 1 d . . . H13A H 0.4349 0.3241 0.4096 0.125 Uiso 1 calc R . . H13B H 0.4509 0.3520 0.2971 0.125 Uiso 1 calc R . . H13C H 0.5010 0.2475 0.3697 0.125 Uiso 1 calc R . . Cl3 Cl 0.86512(9) 0.08070(11) 0.29494(13) 0.0615(4) Uani 1 d . . . O5 O 0.9412(4) 0.0176(5) 0.3589(6) 0.126(2) Uani 1 d . . . O6 O 0.7895(3) 0.0049(4) 0.2656(4) 0.0817(13) Uani 1 d . . . O7 O 0.8812(4) 0.1233(5) 0.1987(5) 0.1031(17) Uani 1 d . . . O8 O 0.8480(4) 0.1769(4) 0.3545(5) 0.1043(17) Uani 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 0.0390(3) 0.0285(3) 0.0321(3) -0.0034(2) 0.0164(2) -0.0026(2) Cl1 0.0840(15) 0.1109(19) 0.232(3) -0.006(2) 0.0206(18) -0.0057(13) Cl2 0.0874(12) 0.0681(10) 0.1445(17) 0.0125(11) 0.0553(12) 0.0305(9) O1 0.0511(17) 0.0371(15) 0.0375(15) -0.0039(12) 0.0220(14) 0.0015(13) O2 0.0431(16) 0.0468(18) 0.0469(17) -0.0060(14) 0.0158(14) -0.0090(14) O3 0.087(3) 0.112(4) 0.072(3) -0.053(3) 0.040(2) -0.029(3) O4 0.072(3) 0.156(5) 0.073(3) -0.044(3) 0.030(2) 0.024(3) N1 0.054(2) 0.0334(18) 0.0388(19) 0.0014(15) 0.0214(17) 0.0024(16) N2 0.0394(19) 0.0355(19) 0.044(2) -0.0074(15) 0.0163(16) -0.0031(15) N3 0.047(2) 0.0354(18) 0.045(2) 0.0030(15) 0.0184(17) -0.0015(16) N4 0.053(2) 0.0404(19) 0.0352(18) -0.0061(15) 0.0192(17) -0.0016(17) C1 0.050(3) 0.050(3) 0.037(2) 0.0037(19) 0.013(2) 0.012(2) C2 0.046(2) 0.056(3) 0.038(2) -0.013(2) 0.005(2) 0.001(2) C3 0.048(3) 0.033(2) 0.080(4) -0.009(2) 0.023(3) -0.010(2) C4 0.052(3) 0.038(2) 0.071(3) 0.007(2) 0.032(3) -0.004(2) C5 0.094(4) 0.056(3) 0.044(3) 0.009(2) 0.024(3) 0.008(3) C6 0.154(8) 0.064(4) 0.062(4) 0.007(3) -0.031(4) -0.016(5) C7 0.050(3) 0.038(2) 0.057(3) 0.006(2) 0.023(2) 0.0010(19) C8 0.061(3) 0.044(3) 0.075(4) 0.006(2) 0.022(3) 0.008(2) C9 0.089(4) 0.082(4) 0.067(4) -0.005(3) 0.048(3) 0.021(3) C10 0.055(3) 0.046(2) 0.045(2) 0.007(2) 0.027(2) 0.014(2) C11 0.044(3) 0.071(3) 0.062(3) 0.005(3) 0.028(2) -0.001(2) C12 0.038(2) 0.054(3) 0.058(3) 0.007(2) 0.013(2) -0.006(2) C13 0.057(3) 0.097(5) 0.097(5) -0.019(4) 0.027(3) -0.030(3) Cl3 0.0632(8) 0.0472(7) 0.0821(9) 0.0214(6) 0.0344(7) 0.0090(6) O5 0.090(4) 0.093(4) 0.171(6) 0.056(4) 0.008(4) 0.021(3) O6 0.077(3) 0.065(3) 0.110(4) 0.008(2) 0.039(3) -0.005(2) O7 0.122(4) 0.099(4) 0.112(4) 0.035(3) 0.072(4) 0.006(3) O8 0.141(5) 0.064(3) 0.132(4) -0.009(3) 0.078(4) -0.005(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 1.885(3) . ? Co O1 1.913(3) . ? Co N4 1.923(3) . ? Co N2 1.927(4) . ? Co N1 1.946(4) . ? Co N3 2.114(4) . ? Cl1 C6 1.675(9) . ? Cl2 C8 1.771(6) . ? O1 C10 1.280(5) . ? O2 C12 1.282(6) . ? O3 N4 1.209(5) . ? O4 N4 1.211(6) . ? N1 C1 1.483(6) . ? N2 C3 1.477(6) . ? N2 C2 1.477(6) . ? N3 C7 1.501(6) . ? N3 C5 1.505(6) . ? N3 C4 1.514(6) . ? C1 C2 1.504(7) . ? C3 C4 1.497(7) . ? C5 C6 1.487(10) . ? C7 C8 1.523(7) . ? C9 C10 1.501(7) . ? C10 C11 1.386(7) . ? C11 C12 1.384(7) . ? C12 C13 1.501(7) . ? Cl3 O5 1.416(5) . ? Cl3 O8 1.416(5) . ? Cl3 O7 1.419(5) . ? Cl3 O6 1.427(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 O2 Co O1 93.70(13) . . ? O2 Co N4 87.94(15) . . ? O1 Co N4 175.70(15) . . ? O2 Co N2 176.42(15) . . ? O1 Co N2 87.47(14) . . ? N4 Co N2 90.66(16) . . ? O2 Co N1 91.61(16) . . ? O1 Co N1 86.87(14) . . ? N4 Co N1 89.12(16) . . ? N2 Co N1 85.08(16) . . ? O2 Co N3 97.34(14) . . ? O1 Co N3 90.11(13) . . ? N4 Co N3 93.63(15) . . ? N2 Co N3 86.03(15) . . ? N1 Co N3 170.72(16) . . ? C10 O1 Co 125.2(3) . . ? C12 O2 Co 125.1(3) . . ? C1 N1 Co 110.5(3) . . ? C3 N2 C2 118.3(4) . . ? C3 N2 Co 108.6(3) . . ? C2 N2 Co 108.8(3) . . ? C7 N3 C5 110.2(4) . . ? C7 N3 C4 109.3(3) . . ? C5 N3 C4 106.7(4) . . ? C7 N3 Co 110.3(3) . . ? C5 N3 Co 116.9(3) . . ? C4 N3 Co 103.0(3) . . ? O3 N4 O4 117.2(4) . . ? O3 N4 Co 121.4(3) . . ? O4 N4 Co 121.3(3) . . ? N1 C1 C2 106.3(4) . . ? N2 C2 C1 105.3(4) . . ? N2 C3 C4 105.5(4) . . ? C3 C4 N3 110.4(4) . . ? C6 C5 N3 117.4(5) . . ? C5 C6 Cl1 119.0(5) . . ? N3 C7 C8 116.3(4) . . ? C7 C8 Cl2 108.1(4) . . ? O1 C10 C11 124.8(4) . . ? O1 C10 C9 114.7(5) . . ? C11 C10 C9 120.6(5) . . ? C12 C11 C10 124.3(4) . . ? O2 C12 C11 125.1(4) . . ? O2 C12 C13 113.4(5) . . ? C11 C12 C13 121.5(5) . . ? O5 Cl3 O8 111.2(4) . . ? O5 Cl3 O7 108.8(4) . . ? O8 Cl3 O7 108.2(3) . . ? O5 Cl3 O6 108.7(3) . . ? O8 Cl3 O6 109.3(3) . . ? O7 Cl3 O6 110.5(3) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.752 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.087 #===END data_[Co(eta-2-DCD)(acac)(NO2)2] _publ_requested_category 'FM' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C13 H26 Cl2 Co N5 O6' _chemical_formula_sum 'C13 H26 Cl2 Co N5 O6' _chemical_formula_weight 478.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 19.242(14) _cell_length_b 7.475(3) _cell_length_c 14.545(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.42(5) _cell_angle_gamma 90.00 _cell_volume 2034.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.443 _cell_measurement_theta_max 10.398 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.7325 _exptl_absorpt_correction_T_max 0.9345 _exptl_absorpt_process_details 'DIFCAD4 program' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '2\t/\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time '3600 seconds' _diffrn_standards_decay_% 'decline to 1 %' _diffrn_reflns_number 3572 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.1291 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.96 _reflns_number_total 3572 _reflns_number_gt 1780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius' _computing_cell_refinement 'Nonius' _computing_data_reduction 'local program' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-XP' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+5.2907P] 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 3572 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1915 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2353 _refine_ls_wR_factor_gt 0.1912 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.14641(7) 0.13501(16) 0.84168(8) 0.0406(4) Uani 1 d . . . Cl1 Cl 0.4119(2) 0.8848(5) 0.7041(3) 0.1059(13) Uani 1 d . . . Cl2 Cl 0.4615(2) 0.2164(5) 1.0370(3) 0.1000(12) Uani 1 d . . . O1 O 0.2287(4) 0.0035(8) 0.8940(5) 0.0562(18) Uani 1 d . . . O2 O 0.0835(4) 0.0021(8) 0.8972(4) 0.0502(17) Uani 1 d . . . O3 O 0.0596(4) -0.0109(10) 0.6802(5) 0.069(2) Uani 1 d . . . O4 O 0.1572(5) -0.1522(10) 0.7236(6) 0.083(3) Uani 1 d . . . O5 O 0.1253(4) 0.3290(10) 0.9937(5) 0.074(2) Uani 1 d . . . O6 O 0.2303(5) 0.3536(11) 0.9750(5) 0.074(2) Uani 1 d . . . N1 N 0.0675(4) 0.2933(10) 0.7907(5) 0.0459(19) Uani 1 d . . . H1NA H 0.0369 0.2391 0.7426 0.055 Uiso 1 calc R . . H1NB H 0.0439 0.3192 0.8357 0.055 Uiso 1 calc R . . N2 N 0.2023(4) 0.2857(9) 0.7746(5) 0.0409(18) Uani 1 d . . . H2 H 0.2294 0.3576 0.8194 0.049 Uiso 1 calc R . . N3 N 0.3456(5) 0.4174(13) 0.7930(6) 0.067(3) Uani 1 d . . . N4 N 0.1194(5) -0.0281(11) 0.7343(6) 0.046(2) Uani 1 d . . . N5 N 0.1692(5) 0.2935(10) 0.9507(5) 0.0449(19) Uani 1 d . . . C1 C 0.0945(5) 0.4600(12) 0.7569(7) 0.051(3) Uani 1 d . . . H1A H 0.0566 0.5208 0.7123 0.061 Uiso 1 calc R . . H1B H 0.1130 0.5398 0.8094 0.061 Uiso 1 calc R . . C2 C 0.1516(5) 0.4064(12) 0.7108(7) 0.046(2) Uani 1 d . . . H2A H 0.1767 0.5116 0.6967 0.055 Uiso 1 calc R . . H2B H 0.1312 0.3454 0.6519 0.055 Uiso 1 calc R . . C3 C 0.2529(5) 0.1955(13) 0.7271(7) 0.052(3) Uani 1 d . . . H3A H 0.2265 0.1431 0.6683 0.063 Uiso 1 calc R . . H3B H 0.2767 0.0993 0.7671 0.063 Uiso 1 calc R . . C4 C 0.3089(6) 0.3230(15) 0.7062(7) 0.062(3) Uani 1 d . . . H4A H 0.3435 0.2564 0.6809 0.075 Uiso 1 calc R . . H4B H 0.2861 0.4094 0.6590 0.075 Uiso 1 calc R . . C5A C 0.3901(13) 0.555(3) 0.7664(18) 0.097(7) Uani 0.70 d P A 1 H5A1 H 0.4296 0.5816 0.8195 0.117 Uiso 0.70 calc PR A 1 H5A2 H 0.4097 0.5128 0.7147 0.117 Uiso 0.70 calc PR A 1 C6A C 0.3506(12) 0.711(3) 0.7387(16) 0.096(7) Uani 0.70 d P A 1 H6A1 H 0.3315 0.7558 0.7904 0.115 Uiso 0.70 calc PR A 1 H6A2 H 0.3110 0.6862 0.6855 0.115 Uiso 0.70 calc PR A 1 C5B C 0.361(2) 0.630(6) 0.784(3) 0.039(8) Uiso 0.30 d P A 2 H5B1 H 0.3175 0.6924 0.7541 0.047 Uiso 0.30 calc PR A 2 H5B2 H 0.3798 0.6818 0.8457 0.047 Uiso 0.30 calc PR A 2 C6B C 0.4174(16) 0.650(4) 0.722(2) 0.038(7) Uiso 0.30 d P A 2 H6B1 H 0.4033 0.5849 0.6626 0.046 Uiso 0.30 calc PR A 2 H6B2 H 0.4647 0.6128 0.7552 0.046 Uiso 0.30 calc PR A 2 C7 C 0.3946(7) 0.3014(19) 0.8565(8) 0.080(4) Uani 1 d . . . H7A H 0.4408 0.3044 0.8406 0.096 Uiso 1 calc R . . H7B H 0.3770 0.1795 0.8489 0.096 Uiso 1 calc R . . C8 C 0.4028(7) 0.3573(18) 0.9561(7) 0.082(4) Uani 1 d . . . H8A H 0.3562 0.3565 0.9712 0.099 Uiso 1 calc R . . H8B H 0.4208 0.4789 0.9634 0.099 Uiso 1 calc R . . C9 C 0.3020(7) -0.2171(18) 0.9809(8) 0.088(4) Uani 1 d . . . H9A H 0.3053 -0.3157 0.9398 0.132 Uiso 1 calc R . . H9B H 0.3084 -0.2599 1.0446 0.132 Uiso 1 calc R . . H9C H 0.3385 -0.1311 0.9781 0.132 Uiso 1 calc R . . C10 C 0.2291(6) -0.1299(14) 0.9497(6) 0.056(3) Uani 1 d . . . C11 C 0.1728(7) -0.1933(14) 0.9807(7) 0.062(3) Uani 1 d . . . H11 H 0.1818 -0.2852 1.0250 0.075 Uiso 1 calc R . . C12 C 0.1036(6) -0.1341(14) 0.9526(6) 0.051(2) Uani 1 d . . . C13 C 0.0451(6) -0.2266(14) 0.9864(7) 0.069(3) Uani 1 d . . . H13A H 0.0514 -0.2070 1.0530 0.104 Uiso 1 calc R . . H13B H 0.0468 -0.3526 0.9743 0.104 Uiso 1 calc R . . H13C H -0.0003 -0.1796 0.9535 0.104 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0546(8) 0.0315(6) 0.0371(6) 0.0032(6) 0.0137(5) 0.0014(7) Cl1 0.142(3) 0.068(2) 0.100(3) 0.003(2) 0.012(2) -0.034(2) Cl2 0.093(3) 0.103(3) 0.092(2) 0.017(2) -0.004(2) 0.016(2) O1 0.070(5) 0.041(4) 0.056(4) 0.009(3) 0.012(4) 0.015(4) O2 0.061(5) 0.042(4) 0.050(4) 0.008(3) 0.019(3) -0.001(3) O3 0.072(6) 0.072(5) 0.067(5) -0.018(4) 0.021(4) -0.011(4) O4 0.127(8) 0.041(5) 0.084(6) -0.014(4) 0.029(5) 0.006(5) O5 0.093(6) 0.081(6) 0.059(4) -0.027(4) 0.041(5) -0.009(5) O6 0.071(5) 0.082(6) 0.066(5) -0.025(5) 0.011(4) -0.010(5) N1 0.053(5) 0.037(4) 0.050(4) 0.001(4) 0.018(4) -0.001(4) N2 0.047(5) 0.031(4) 0.046(4) -0.008(3) 0.016(4) -0.007(4) N3 0.068(6) 0.070(7) 0.059(6) 0.013(5) 0.010(5) -0.014(5) N4 0.051(6) 0.040(5) 0.046(5) 0.005(4) 0.009(4) 0.001(4) N5 0.057(6) 0.045(5) 0.030(4) 0.009(4) 0.005(4) 0.005(4) C1 0.062(7) 0.038(5) 0.054(6) 0.006(5) 0.015(5) -0.003(5) C2 0.052(6) 0.036(6) 0.050(5) 0.011(4) 0.011(5) 0.002(5) C3 0.058(7) 0.056(6) 0.052(6) -0.002(5) 0.029(5) -0.001(5) C4 0.063(7) 0.078(8) 0.054(6) 0.004(6) 0.029(6) -0.007(6) C5A 0.100(18) 0.068(13) 0.107(17) 0.017(13) -0.010(14) 0.001(14) C6A 0.13(2) 0.101(17) 0.072(13) -0.008(13) 0.047(13) -0.025(15) C7 0.075(9) 0.105(10) 0.059(7) -0.011(7) 0.012(7) 0.000(8) C8 0.087(9) 0.097(9) 0.058(7) 0.014(7) 0.008(6) 0.030(8) C9 0.105(11) 0.087(9) 0.069(8) 0.020(7) 0.012(7) 0.051(8) C10 0.087(8) 0.043(6) 0.036(5) -0.003(5) 0.013(5) 0.024(6) C11 0.088(9) 0.047(6) 0.051(6) 0.017(5) 0.013(6) 0.003(6) C12 0.078(8) 0.048(6) 0.032(4) -0.006(5) 0.019(5) -0.003(6) C13 0.105(10) 0.051(6) 0.056(6) 0.024(5) 0.029(7) -0.016(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(7) . ? Co O2 1.887(6) . ? Co N1 1.932(8) . ? Co N5 1.946(8) . ? Co N4 1.954(8) . ? Co N2 1.965(7) . ? Cl1 C6B 1.77(3) . ? Cl1 C6A 1.90(2) . ? Cl2 C8 1.776(11) . ? O1 C10 1.284(11) . ? O2 C12 1.300(11) . ? O3 N4 1.242(10) . ? O4 N4 1.210(10) . ? O5 N5 1.192(10) . ? O6 N5 1.230(10) . ? N1 C1 1.478(11) . ? N1 H1NA 0.9000 . ? N1 H1NB 0.9000 . ? N2 C3 1.482(11) . ? N2 C2 1.485(11) . ? N2 H2 0.9100 . ? N3 C7 1.446(15) . ? N3 C5A 1.45(2) . ? N3 C4 1.475(13) . ? N3 C5B 1.63(5) . ? C1 C2 1.468(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.520(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5A C6A 1.40(3) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C5B C6B 1.57(4) . ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C7 C8 1.480(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.517(15) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.353(15) . ? C11 C12 1.373(15) . ? C11 H11 0.9300 . ? C12 C13 1.497(13) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 O2 96.7(3) . . ? O1 Co N1 173.9(3) . . ? O2 Co N1 87.8(3) . . ? O1 Co N5 88.8(3) . . ? O2 Co N5 91.0(3) . . ? N1 Co N5 87.0(3) . . ? O1 Co N4 92.3(3) . . ? O2 Co N4 86.3(3) . . ? N1 Co N4 92.1(4) . . ? N5 Co N4 177.2(4) . . ? O1 Co N2 89.7(3) . . ? O2 Co N2 173.5(3) . . ? N1 Co N2 86.0(3) . . ? N5 Co N2 90.6(3) . . ? N4 Co N2 92.0(3) . . ? C6B Cl1 C6A 46.0(11) . . ? C10 O1 Co 123.1(7) . . ? C12 O2 Co 123.3(7) . . ? C1 N1 Co 109.8(6) . . ? C1 N1 H1NA 109.7 . . ? Co N1 H1NA 109.7 . . ? C1 N1 H1NB 109.7 . . ? Co N1 H1NB 109.7 . . ? H1NA N1 H1NB 108.2 . . ? C3 N2 C2 113.1(7) . . ? C3 N2 Co 117.8(6) . . ? C2 N2 Co 107.6(5) . . ? C3 N2 H2 105.8 . . ? C2 N2 H2 105.8 . . ? Co N2 H2 105.8 . . ? C7 N3 C5A 105.0(12) . . ? C7 N3 C4 111.8(9) . . ? C5A N3 C4 107.9(12) . . ? C7 N3 C5B 122.2(17) . . ? C5A N3 C5B 32.0(13) . . ? C4 N3 C5B 117.2(15) . . ? O4 N4 O3 119.6(9) . . ? O4 N4 Co 121.7(7) . . ? O3 N4 Co 118.5(7) . . ? O5 N5 O6 120.9(8) . . ? O5 N5 Co 120.6(7) . . ? O6 N5 Co 118.4(7) . . ? C2 C1 N1 106.3(7) . . ? C2 C1 H1A 110.5 . . ? N1 C1 H1A 110.5 . . ? C2 C1 H1B 110.5 . . ? N1 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? C1 C2 N2 109.5(7) . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? N2 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 112.4(8) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 110.4(8) . . ? N3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C6A C5A N3 111(2) . . ? C6A C5A H5A1 109.5 . . ? N3 C5A H5A1 109.5 . . ? C6A C5A H5A2 109.5 . . ? N3 C5A H5A2 109.5 . . ? H5A1 C5A H5A2 108.1 . . ? C5A C6A Cl1 108.4(17) . . ? C5A C6A H6A1 110.0 . . ? Cl1 C6A H6A1 110.0 . . ? C5A C6A H6A2 110.0 . . ? Cl1 C6A H6A2 110.0 . . ? H6A1 C6A H6A2 108.4 . . ? C6B C5B N3 108(3) . . ? C6B C5B H5B1 110.1 . . ? N3 C5B H5B1 110.1 . . ? C6B C5B H5B2 110.1 . . ? N3 C5B H5B2 110.1 . . ? H5B1 C5B H5B2 108.5 . . ? C5B C6B Cl1 99(2) . . ? C5B C6B H6B1 112.0 . . ? Cl1 C6B H6B1 112.0 . . ? C5B C6B H6B2 112.0 . . ? Cl1 C6B H6B2 112.0 . . ? H6B1 C6B H6B2 109.7 . . ? N3 C7 C8 111.2(10) . . ? N3 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N3 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 Cl2 112.8(9) . . ? C7 C8 H8A 109.0 . . ? Cl2 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? Cl2 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 126.5(10) . . ? O1 C10 C9 113.2(10) . . ? C11 C10 C9 120.4(10) . . ? C10 C11 C12 125.8(9) . . ? C10 C11 H11 117.1 . . ? C12 C11 H11 117.1 . . ? O2 C12 C11 124.5(9) . . ? O2 C12 C13 115.3(10) . . ? C11 C12 C13 120.3(10) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.438 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.112