data_j1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 Cl4 Co2 N10 O3' _chemical_formula_weight 908.34 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8436(9) _cell_length_b 9.7124(11) _cell_length_c 12.4551(13) _cell_angle_alpha 85.689(2) _cell_angle_beta 77.5370(10) _cell_angle_gamma 83.590(2) _cell_volume 919.40(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3178 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 26.43 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 1.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8255 _exptl_absorpt_correction_T_max 0.9636 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX-II CCD' _diffrn_measurement_method 'OMEGA SCANS' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11541 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3999 _reflns_number_gt 3281 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+1.3312P] 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 3999 _refine_ls_number_parameters 271 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.16615(6) 0.14650(5) 0.93228(4) 0.02405(16) Uani 1 1 d . . . Cl1 Cl 0.27765(17) -0.00593(14) 1.45363(8) 0.0535(3) Uani 1 1 d . . . Cl2 Cl 0.05512(17) 0.28794(14) 1.46781(9) 0.0568(3) Uani 1 1 d . . . N1 N 0.2599(4) -0.0063(3) 0.8400(2) 0.0284(6) Uani 1 1 d . . . N2 N 0.2453(4) 0.0255(3) 1.0420(2) 0.0249(6) Uani 1 1 d . . . N3 N 0.0541(4) 0.2506(3) 1.0549(2) 0.0272(6) Uani 1 1 d . . . N4 N 0.0024(4) 0.2584(3) 0.8611(3) 0.0301(7) Uani 1 1 d . . . N5 N 0.3467(4) 0.2504(3) 0.8866(2) 0.0291(6) Uani 1 1 d . . . O1 O 0.3401(3) 0.3691(3) 0.9006(3) 0.0398(7) Uani 1 1 d . . . C1 C 0.2803(5) -0.0448(4) 0.7360(3) 0.0380(9) Uani 1 1 d . . . H1A H 0.2390 0.0101 0.6787 0.046 Uiso 1 1 calc R . . C2 C 0.3717(5) -0.1782(5) 0.7241(3) 0.0424(10) Uani 1 1 d . . . H2A H 0.4026 -0.2281 0.6588 0.051 Uiso 1 1 calc R . . C3 C 0.4075(5) -0.2223(4) 0.8255(3) 0.0369(9) Uani 1 1 d . . . H3A H 0.4672 -0.3087 0.8435 0.044 Uiso 1 1 calc R . . C4 C 0.3393(4) -0.1155(4) 0.8969(3) 0.0276(7) Uani 1 1 d . . . C5 C 0.3237(4) -0.0963(4) 1.0097(3) 0.0265(7) Uani 1 1 d . . . H5A H 0.3661 -0.1653 1.0584 0.032 Uiso 1 1 calc R . . C6 C 0.2059(4) 0.0757(4) 1.1474(3) 0.0255(7) Uani 1 1 d . . . C7 C 0.2601(5) 0.0110(4) 1.2403(3) 0.0315(8) Uani 1 1 d . . . H7A H 0.3301 -0.0755 1.2356 0.038 Uiso 1 1 calc R . . C8 C 0.2095(5) 0.0759(4) 1.3395(3) 0.0361(9) Uani 1 1 d . . . C9 C 0.1096(5) 0.2038(5) 1.3456(3) 0.0383(9) Uani 1 1 d . . . C10 C 0.0547(5) 0.2679(4) 1.2540(3) 0.0339(8) Uani 1 1 d . . . H10A H -0.0142 0.3550 1.2590 0.041 Uiso 1 1 calc R . . C11 C 0.1018(4) 0.2035(4) 1.1550(3) 0.0275(7) Uani 1 1 d . . . C12 C -0.0683(5) 0.3482(4) 1.0382(3) 0.0309(8) Uani 1 1 d . . . H12A H -0.1314 0.4074 1.0937 0.037 Uiso 1 1 calc R . . C13 C -0.0972(5) 0.3569(4) 0.9296(3) 0.0326(8) Uani 1 1 d . . . C14 C -0.2182(5) 0.4333(4) 0.8746(4) 0.0422(10) Uani 1 1 d . . . H14A H -0.3027 0.5069 0.9025 0.051 Uiso 1 1 calc R . . C15 C -0.1900(6) 0.3802(4) 0.7714(4) 0.0460(11) Uani 1 1 d . . . H15A H -0.2520 0.4107 0.7150 0.055 Uiso 1 1 calc R . . C16 C -0.0531(5) 0.2731(4) 0.7655(3) 0.0369(9) Uani 1 1 d . . . H16A H -0.0067 0.2191 0.7034 0.044 Uiso 1 1 calc R . . O2 O 0.5541(16) 0.5346(13) 0.4945(10) 0.100(3) Uani 0.50 1 d P A -1 C17 C 0.5968(12) 0.3800(10) 0.5229(8) 0.041(2) Uani 0.50 1 d P A -1 H17A H 0.6208 0.3272 0.4553 0.049 Uiso 0.50 1 calc PR A -1 H17B H 0.7023 0.3663 0.5555 0.049 Uiso 0.50 1 calc PR A -1 C18 C 0.4455(12) 0.3302(12) 0.6019(8) 0.063(3) Uani 0.50 1 d PD A -1 H18A H 0.3906 0.2609 0.5695 0.075 Uiso 0.50 1 calc PR A -1 H18B H 0.4799 0.2888 0.6701 0.075 Uiso 0.50 1 calc PR A -1 C19 C 0.3344(9) 0.4505(7) 0.6219(5) 0.0246(14) Uani 0.50 1 d PD A -1 H19A H 0.3522 0.4915 0.6886 0.030 Uiso 0.50 1 calc PR A -1 H19B H 0.2110 0.4290 0.6349 0.030 Uiso 0.50 1 calc PR A -1 C20 C 0.3723(15) 0.5550(12) 0.5221(9) 0.053(3) Uani 0.50 1 d PD A -1 H20A H 0.3187 0.5324 0.4613 0.064 Uiso 0.50 1 calc PR A -1 H20B H 0.3308 0.6514 0.5427 0.064 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0254(3) 0.0275(3) 0.0209(2) 0.00210(17) -0.00878(18) -0.00421(18) Cl1 0.0661(7) 0.0774(8) 0.0242(5) 0.0109(5) -0.0195(5) -0.0268(6) Cl2 0.0633(7) 0.0801(8) 0.0302(5) -0.0218(5) 0.0008(5) -0.0283(6) N1 0.0308(16) 0.0324(16) 0.0229(15) -0.0009(12) -0.0058(12) -0.0077(12) N2 0.0247(14) 0.0303(15) 0.0215(14) 0.0000(11) -0.0075(11) -0.0064(11) N3 0.0239(14) 0.0295(15) 0.0303(16) -0.0006(12) -0.0084(12) -0.0071(12) N4 0.0309(16) 0.0311(16) 0.0315(16) 0.0067(12) -0.0132(13) -0.0099(13) N5 0.0245(15) 0.0342(17) 0.0296(16) 0.0037(12) -0.0085(12) -0.0049(12) O1 0.0325(14) 0.0286(14) 0.0562(18) -0.0004(12) -0.0030(13) -0.0078(11) C1 0.040(2) 0.051(2) 0.0245(18) -0.0060(16) -0.0039(16) -0.0134(18) C2 0.038(2) 0.054(3) 0.036(2) -0.0171(19) 0.0017(17) -0.0133(19) C3 0.0262(18) 0.037(2) 0.047(2) -0.0096(17) -0.0005(16) -0.0078(15) C4 0.0236(16) 0.0307(18) 0.0288(18) -0.0001(14) -0.0048(14) -0.0067(14) C5 0.0218(16) 0.0282(17) 0.0309(18) 0.0026(14) -0.0086(14) -0.0049(13) C6 0.0243(16) 0.0327(18) 0.0221(16) 0.0005(13) -0.0071(13) -0.0113(14) C7 0.0320(19) 0.040(2) 0.0271(18) 0.0045(15) -0.0133(15) -0.0142(16) C8 0.038(2) 0.053(2) 0.0219(18) 0.0050(16) -0.0102(15) -0.0212(18) C9 0.038(2) 0.059(3) 0.0216(18) -0.0077(17) -0.0013(15) -0.0256(19) C10 0.0297(19) 0.039(2) 0.034(2) -0.0094(16) -0.0014(15) -0.0137(16) C11 0.0251(17) 0.0341(18) 0.0256(17) -0.0006(14) -0.0062(13) -0.0124(14) C12 0.0228(17) 0.0264(17) 0.046(2) -0.0022(15) -0.0113(15) -0.0064(14) C13 0.0262(18) 0.0270(17) 0.047(2) 0.0069(16) -0.0131(16) -0.0068(14) C14 0.034(2) 0.0303(19) 0.069(3) 0.0112(19) -0.027(2) -0.0089(16) C15 0.042(2) 0.043(2) 0.062(3) 0.021(2) -0.033(2) -0.0156(18) C16 0.038(2) 0.039(2) 0.040(2) 0.0155(17) -0.0216(17) -0.0172(17) O2 0.109(9) 0.097(8) 0.107(8) -0.032(7) -0.035(7) -0.032(6) C17 0.045(5) 0.035(5) 0.036(5) 0.008(4) -0.002(4) -0.002(4) C18 0.053(6) 0.111(9) 0.035(5) 0.006(5) -0.024(4) -0.032(6) C19 0.035(4) 0.031(3) 0.009(3) -0.004(2) 0.003(2) -0.019(3) C20 0.066(7) 0.045(6) 0.056(7) -0.022(5) -0.028(6) 0.007(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 N5 1.798(3) . ? Co1 N3 1.892(3) . ? Co1 N2 1.897(3) . ? Co1 N4 1.911(3) . ? Co1 N1 1.927(3) . ? Cl1 C8 1.732(4) . ? Cl2 C9 1.731(4) . ? N1 C1 1.346(5) . ? N1 C4 1.394(5) . ? N2 C5 1.320(4) . ? N2 C6 1.394(4) . ? N3 C12 1.310(5) . ? N3 C11 1.407(4) . ? N4 C16 1.347(5) . ? N4 C13 1.386(5) . ? N5 O1 1.172(4) . ? C1 C2 1.411(6) . ? C2 C3 1.379(6) . ? C3 C4 1.401(5) . ? C4 C5 1.408(5) . ? C6 C7 1.399(5) . ? C6 C11 1.404(5) . ? C7 C8 1.390(5) . ? C8 C9 1.390(6) . ? C9 C10 1.386(6) . ? C10 C11 1.384(5) . ? C12 C13 1.414(6) . ? C13 C14 1.403(5) . ? C14 C15 1.385(7) . ? C15 C16 1.403(6) . ? O2 C20 1.388(16) . ? O2 C17 1.534(15) . ? C17 C18 1.470(13) . ? C18 C19 1.382(12) . ? C19 C20 1.544(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Co1 N3 96.50(13) . . ? N5 Co1 N2 101.93(13) . . ? N3 Co1 N2 82.74(12) . . ? N5 Co1 N4 96.97(13) . . ? N3 Co1 N4 83.25(13) . . ? N2 Co1 N4 157.59(13) . . ? N5 Co1 N1 96.97(13) . . ? N3 Co1 N1 162.15(13) . . ? N2 Co1 N1 83.06(12) . . ? N4 Co1 N1 106.63(13) . . ? C1 N1 C4 106.5(3) . . ? C1 N1 Co1 141.7(3) . . ? C4 N1 Co1 111.8(2) . . ? C5 N2 C6 128.8(3) . . ? C5 N2 Co1 116.1(2) . . ? C6 N2 Co1 115.1(2) . . ? C12 N3 C11 128.3(3) . . ? C12 N3 Co1 116.3(3) . . ? C11 N3 Co1 115.1(2) . . ? C16 N4 C13 107.3(3) . . ? C16 N4 Co1 141.1(3) . . ? C13 N4 Co1 111.6(2) . . ? O1 N5 Co1 124.4(3) . . ? N1 C1 C2 110.4(4) . . ? C3 C2 C1 106.8(4) . . ? C2 C3 C4 107.0(4) . . ? N1 C4 C3 109.3(3) . . ? N1 C4 C5 114.6(3) . . ? C3 C4 C5 136.0(4) . . ? N2 C5 C4 114.3(3) . . ? N2 C6 C7 126.1(3) . . ? N2 C6 C11 113.5(3) . . ? C7 C6 C11 120.4(3) . . ? C6 C7 C8 118.7(4) . . ? C9 C8 C7 120.4(3) . . ? C9 C8 Cl1 121.5(3) . . ? C7 C8 Cl1 118.0(3) . . ? C8 C9 C10 121.1(3) . . ? C8 C9 Cl2 120.3(3) . . ? C10 C9 Cl2 118.6(3) . . ? C11 C10 C9 119.1(4) . . ? C10 C11 N3 127.1(3) . . ? C10 C11 C6 120.3(3) . . ? N3 C11 C6 112.7(3) . . ? N3 C12 C13 113.5(3) . . ? N4 C13 C12 115.1(3) . . ? N4 C13 C14 109.2(4) . . ? C12 C13 C14 135.2(4) . . ? C15 C14 C13 106.3(4) . . ? C14 C15 C16 107.5(4) . . ? N4 C16 C15 109.7(4) . . ? C20 O2 C17 104.3(9) . . ? C18 C17 O2 108.5(9) . . ? C19 C18 C17 102.3(8) . . ? C18 C19 C20 109.6(7) . . ? O2 C20 C19 100.5(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.108 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.095