# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 859524' #TrackingRef '1.CIF' _database_code_depnum_ccdc_archive 'CCDC ?' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H24 Co K N4 O3' _chemical_formula_weight 502.49 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' K K 0.2009 0.2494 '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 13.449(5) _cell_length_b 21.788(8) _cell_length_c 8.202(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.794(7) _cell_angle_gamma 90.00 _cell_volume 2352.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5438 _cell_measurement_theta_min 3.0944 _cell_measurement_theta_max 27.4719 _exptl_crystal_description cuboid _exptl_crystal_colour red _exptl_crystal_size_max 0.3600 _exptl_crystal_size_mid 0.3600 _exptl_crystal_size_min 0.0400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7214 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Mercury70(2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18130 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5283 _reflns_number_gt 4268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+2.4121P] 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 5283 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.011 _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 C1 C 0.3393(3) 0.68721(18) 1.0097(5) 0.0439(9) Uani 1 1 d . . . C2 C 0.3922(4) 0.7366(2) 1.0966(7) 0.0618(12) Uani 1 1 d . . . H2A H 0.3561 0.7695 1.1277 0.074 Uiso 1 1 calc R . . C3 C 0.4973(4) 0.7372(3) 1.1370(8) 0.0790(16) Uani 1 1 d . . . H3A H 0.5309 0.7700 1.1967 0.095 Uiso 1 1 calc R . . C4 C 0.5526(4) 0.6896(3) 1.0894(8) 0.0791(16) Uani 1 1 d . . . H4A H 0.6232 0.6906 1.1149 0.095 Uiso 1 1 calc R . . C5 C 0.5033(4) 0.6415(3) 1.0053(7) 0.0682(13) Uani 1 1 d . . . H5A H 0.5412 0.6096 0.9735 0.082 Uiso 1 1 calc R . . C6 C 0.3963(3) 0.6381(2) 0.9643(6) 0.0501(10) Uani 1 1 d . . . C7 C -0.0472(3) 0.66326(17) 0.9077(5) 0.0407(8) Uani 1 1 d . . . C8 C -0.1126(3) 0.71276(19) 0.9226(6) 0.0532(11) Uani 1 1 d . . . H8A H -0.0854 0.7500 0.9655 0.064 Uiso 1 1 calc R . . C9 C -0.2170(4) 0.7063(2) 0.8739(7) 0.0676(14) Uani 1 1 d . . . H9A H -0.2590 0.7394 0.8832 0.081 Uiso 1 1 calc R . . C10 C -0.2597(3) 0.6511(2) 0.8116(7) 0.0626(12) Uani 1 1 d . . . H10A H -0.3298 0.6470 0.7817 0.075 Uiso 1 1 calc R . . C11 C -0.1980(3) 0.6027(2) 0.7944(5) 0.0497(10) Uani 1 1 d . . . H11A H -0.2269 0.5657 0.7523 0.060 Uiso 1 1 calc R . . C12 C -0.0907(3) 0.60769(17) 0.8394(5) 0.0379(8) Uani 1 1 d . . . C13 C -0.0316(3) 0.55436(17) 0.8171(4) 0.0379(8) Uani 1 1 d . . . H13A H -0.0666 0.5183 0.7828 0.046 Uiso 1 1 calc R . . C14 C 0.3514(3) 0.58488(19) 0.8762(6) 0.0494(10) Uani 1 1 d . . . H14A H 0.3949 0.5572 0.8402 0.059 Uiso 1 1 calc R . . C15 C 0.2132(3) 0.51753(17) 0.7449(5) 0.0439(9) Uani 1 1 d . . . H15A H 0.1861 0.5306 0.6301 0.053 Uiso 1 1 calc R . . C16 C 0.2857(4) 0.4648(2) 0.7407(7) 0.0588(12) Uani 1 1 d . . . H16A H 0.3148 0.4517 0.8533 0.071 Uiso 1 1 calc R . . H16B H 0.3406 0.4779 0.6884 0.071 Uiso 1 1 calc R . . C17 C 0.2285(4) 0.4117(2) 0.6429(7) 0.0713(14) Uani 1 1 d . . . H17A H 0.2056 0.4241 0.5278 0.086 Uiso 1 1 calc R . . H17B H 0.2745 0.3773 0.6448 0.086 Uiso 1 1 calc R . . C18 C 0.1389(4) 0.3915(2) 0.7112(7) 0.0617(12) Uani 1 1 d . . . H18A H 0.1625 0.3738 0.8209 0.074 Uiso 1 1 calc R . . H18B H 0.1027 0.3598 0.6398 0.074 Uiso 1 1 calc R . . C19 C 0.0659(3) 0.44444(17) 0.7241(6) 0.0512(10) Uani 1 1 d . . . H19A H 0.0340 0.4585 0.6135 0.061 Uiso 1 1 calc R . . H19B H 0.0129 0.4305 0.7798 0.061 Uiso 1 1 calc R . . C20 C 0.1246(3) 0.49678(16) 0.8218(5) 0.0396(8) Uani 1 1 d . . . H20A H 0.1532 0.4813 0.9338 0.048 Uiso 1 1 calc R . . C21 C 0.1175(3) 0.65071(16) 0.6790(5) 0.0432(9) Uani 1 1 d . . . C22 C 0.1904(3) 0.58851(17) 1.1299(5) 0.0426(9) Uani 1 1 d . . . C23 C 0.4004(7) 0.5571(6) 0.4947(12) 0.152(4) Uani 1 1 d . . . N1 N 0.0661(2) 0.55287(13) 0.8412(4) 0.0360(6) Uani 1 1 d . . . N2 N 0.2561(2) 0.57220(14) 0.8429(4) 0.0414(7) Uani 1 1 d . . . N3 N 0.0964(3) 0.66960(17) 0.5473(5) 0.0613(10) Uani 1 1 d . . . N4 N 0.2142(3) 0.5704(2) 1.2636(5) 0.0647(11) Uani 1 1 d . . . O1 O 0.2389(2) 0.69030(12) 0.9721(3) 0.0437(6) Uani 1 1 d . . . O2 O 0.0506(2) 0.67202(12) 0.9635(4) 0.0443(6) Uani 1 1 d . . . Co1 Co 0.15316(4) 0.62072(2) 0.90509(6) 0.03358(17) Uani 1 1 d . . . K1 K 0.14556(9) 0.71615(4) 1.26378(11) 0.0564(3) Uani 1 1 d . . . O3 O 0.4671(10) 0.5963(6) 0.4564(17) 0.256(5) 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 C1 0.043(2) 0.044(2) 0.044(2) 0.0043(16) 0.0073(17) -0.0080(16) C2 0.051(3) 0.063(3) 0.068(3) -0.007(2) 0.004(2) -0.017(2) C3 0.059(3) 0.092(4) 0.080(4) -0.018(3) 0.000(3) -0.027(3) C4 0.043(3) 0.104(4) 0.086(4) -0.007(3) 0.003(3) -0.016(3) C5 0.042(3) 0.081(3) 0.082(4) 0.009(3) 0.014(2) -0.003(2) C6 0.038(2) 0.063(3) 0.050(2) 0.004(2) 0.0091(18) -0.0048(18) C7 0.042(2) 0.0402(19) 0.041(2) 0.0056(15) 0.0113(17) 0.0054(15) C8 0.050(2) 0.042(2) 0.070(3) 0.0029(19) 0.015(2) 0.0090(17) C9 0.052(3) 0.065(3) 0.086(4) 0.006(3) 0.014(3) 0.022(2) C10 0.036(2) 0.076(3) 0.074(3) 0.008(3) 0.008(2) 0.008(2) C11 0.043(2) 0.057(2) 0.047(2) 0.0019(19) 0.0061(19) -0.0016(18) C12 0.0373(19) 0.0417(18) 0.0347(19) 0.0067(14) 0.0076(15) 0.0038(14) C13 0.041(2) 0.0383(18) 0.0340(19) -0.0003(14) 0.0073(15) -0.0054(14) C14 0.044(2) 0.050(2) 0.058(3) 0.0029(19) 0.0195(19) 0.0057(18) C15 0.050(2) 0.0390(19) 0.044(2) -0.0029(16) 0.0128(18) 0.0038(16) C16 0.061(3) 0.049(2) 0.070(3) -0.009(2) 0.024(2) 0.010(2) C17 0.092(4) 0.053(3) 0.071(3) -0.017(2) 0.021(3) 0.019(3) C18 0.075(3) 0.039(2) 0.070(3) -0.015(2) 0.011(3) 0.005(2) C19 0.061(3) 0.0341(19) 0.055(3) -0.0060(17) 0.004(2) 0.0002(17) C20 0.049(2) 0.0324(17) 0.0373(19) -0.0012(14) 0.0089(16) 0.0030(15) C21 0.050(2) 0.0288(17) 0.051(2) 0.0019(16) 0.0122(18) -0.0037(15) C22 0.047(2) 0.0375(19) 0.045(2) -0.0055(16) 0.0128(18) -0.0003(16) C23 0.097(6) 0.232(12) 0.120(7) 0.090(7) 0.007(5) -0.014(7) N1 0.0403(17) 0.0322(14) 0.0358(16) 0.0002(12) 0.0083(13) -0.0001(12) N2 0.0444(18) 0.0369(16) 0.0450(18) -0.0003(13) 0.0141(14) 0.0024(13) N3 0.087(3) 0.052(2) 0.045(2) 0.0116(17) 0.015(2) -0.003(2) N4 0.082(3) 0.070(3) 0.040(2) 0.0063(18) 0.0058(19) 0.001(2) O1 0.0402(15) 0.0364(13) 0.0539(17) -0.0032(12) 0.0078(12) -0.0041(11) O2 0.0386(15) 0.0382(13) 0.0546(17) -0.0091(12) 0.0059(12) 0.0014(11) Co1 0.0354(3) 0.0293(3) 0.0360(3) -0.00025(17) 0.0072(2) 0.00024(18) K1 0.0911(8) 0.0403(5) 0.0385(5) -0.0025(3) 0.0151(5) -0.0083(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.323(5) . ? C1 C6 1.409(6) . ? C1 C2 1.402(6) . ? C2 C3 1.385(7) . ? C2 H2A 0.9300 . ? C3 C4 1.378(9) . ? C3 H3A 0.9300 . ? C4 C5 1.351(8) . ? C4 H4A 0.9300 . ? C5 C6 1.412(6) . ? C5 H5A 0.9300 . ? C6 C14 1.434(6) . ? C7 O2 1.315(5) . ? C7 C12 1.410(5) . ? C7 C8 1.413(5) . ? C8 C9 1.386(7) . ? C8 H8A 0.9300 . ? C9 C10 1.384(7) . ? C9 H9A 0.9300 . ? C10 C11 1.366(6) . ? C10 H10A 0.9300 . ? C11 C12 1.418(6) . ? C11 H11A 0.9300 . ? C12 C13 1.440(5) . ? C13 N1 1.289(5) . ? C13 H13A 0.9300 . ? C14 N2 1.284(5) . ? C14 H14A 0.9300 . ? C15 N2 1.486(5) . ? C15 C16 1.512(5) . ? C15 C20 1.527(5) . ? C15 H15A 0.9800 . ? C16 C17 1.524(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.496(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.533(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.519(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N1 1.479(4) . ? C20 H20A 0.9800 . ? C21 N3 1.136(5) . ? C21 Co1 1.932(4) . ? C21 K1 2.989(4) 4_575 ? C22 N4 1.148(5) . ? C22 Co1 1.941(4) . ? C22 K1 3.094(4) . ? C23 O3 1.322(14) . ? N1 Co1 1.892(3) . ? N2 Co1 1.894(3) . ? N3 K1 2.739(4) 1_554 ? N3 K1 3.050(4) 4_575 ? N4 K1 3.308(5) . ? O1 Co1 1.916(3) . ? O1 K1 2.788(3) 4_575 ? O1 K1 2.974(3) . ? O2 Co1 1.911(3) . ? O2 K1 2.709(3) . ? O2 K1 3.333(3) 4_575 ? Co1 K1 3.6211(14) . ? Co1 K1 3.7334(16) 4_575 ? K1 N3 2.739(4) 1_556 ? K1 O1 2.788(3) 4_576 ? K1 C21 2.989(4) 4_576 ? K1 N3 3.050(4) 4_576 ? K1 O2 3.333(3) 4_576 ? K1 Co1 3.7334(16) 4_576 ? K1 K1 4.3582(17) 4_576 ? 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 C1 C6 124.1(4) . . ? O1 C1 C2 117.8(4) . . ? C6 C1 C2 118.0(4) . . ? C3 C2 C1 121.1(5) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 119.5(5) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C1 C6 C5 118.8(4) . . ? C1 C6 C14 123.5(4) . . ? C5 C6 C14 117.8(4) . . ? O2 C7 C12 124.5(3) . . ? O2 C7 C8 117.1(4) . . ? C12 C7 C8 118.4(4) . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.9(4) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C11 C10 C9 119.6(4) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C12 121.4(4) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C7 C12 C11 119.1(4) . . ? C7 C12 C13 123.2(3) . . ? C11 C12 C13 117.6(4) . . ? N1 C13 C12 124.9(3) . . ? N1 C13 H13A 117.5 . . ? C12 C13 H13A 117.5 . . ? N2 C14 C6 125.5(4) . . ? N2 C14 H14A 117.3 . . ? C6 C14 H14A 117.3 . . ? N2 C15 C16 116.1(4) . . ? N2 C15 C20 105.3(3) . . ? C16 C15 C20 110.3(3) . . ? N2 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? C20 C15 H15A 108.3 . . ? C15 C16 C17 109.3(4) . . ? C15 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? C15 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? C18 C17 C16 112.7(4) . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17B 109.1 . . ? C16 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C17 C18 C19 112.4(4) . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C18 109.3(4) . . ? C20 C19 H19A 109.8 . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19B 109.8 . . ? C18 C19 H19B 109.8 . . ? H19A C19 H19B 108.3 . . ? N1 C20 C19 116.5(3) . . ? N1 C20 C15 106.1(3) . . ? C19 C20 C15 111.7(3) . . ? N1 C20 H20A 107.4 . . ? C19 C20 H20A 107.4 . . ? C15 C20 H20A 107.4 . . ? N3 C21 Co1 178.5(4) . . ? N3 C21 K1 82.2(3) . 4_575 ? Co1 C21 K1 96.33(15) . 4_575 ? N4 C22 Co1 178.4(4) . . ? N4 C22 K1 90.4(3) . . ? Co1 C22 K1 88.91(14) . . ? C13 N1 C20 123.5(3) . . ? C13 N1 Co1 125.2(3) . . ? C20 N1 Co1 111.3(2) . . ? C14 N2 C15 123.2(3) . . ? C14 N2 Co1 125.1(3) . . ? C15 N2 Co1 111.6(2) . . ? C21 N3 K1 152.1(4) . 1_554 ? C21 N3 K1 76.1(3) . 4_575 ? K1 N3 K1 97.51(12) 1_554 4_575 ? C22 N4 K1 69.3(3) . . ? C1 O1 Co1 123.5(2) . . ? C1 O1 K1 119.3(2) . 4_575 ? Co1 O1 K1 103.49(11) . 4_575 ? C1 O1 K1 113.6(2) . . ? Co1 O1 K1 93.00(10) . . ? K1 O1 K1 98.24(9) 4_575 . ? C7 O2 Co1 123.4(2) . . ? C7 O2 K1 128.3(2) . . ? Co1 O2 K1 101.82(11) . . ? C7 O2 K1 113.1(2) . 4_575 ? Co1 O2 K1 86.30(10) . 4_575 ? K1 O2 K1 91.74(8) . 4_575 ? N1 Co1 N2 86.24(13) . . ? N1 Co1 O2 95.10(12) . . ? N2 Co1 O2 177.99(13) . . ? N1 Co1 O1 178.66(12) . . ? N2 Co1 O1 95.08(13) . . ? O2 Co1 O1 83.60(11) . . ? N1 Co1 C21 88.87(14) . . ? N2 Co1 C21 88.95(15) . . ? O2 Co1 C21 89.57(15) . . ? O1 Co1 C21 91.41(14) . . ? N1 Co1 C22 90.30(15) . . ? N2 Co1 C22 89.63(15) . . ? O2 Co1 C22 91.86(14) . . ? O1 Co1 C22 89.45(14) . . ? C21 Co1 C22 178.41(16) . . ? N1 Co1 K1 123.72(9) . . ? N2 Co1 K1 133.10(11) . . ? O2 Co1 K1 47.07(9) . . ? O1 Co1 K1 55.10(8) . . ? C21 Co1 K1 122.89(11) . . ? C22 Co1 K1 58.69(11) . . ? N1 Co1 K1 132.98(10) . 4_575 ? N2 Co1 K1 115.02(10) . 4_575 ? O2 Co1 K1 62.98(9) . 4_575 ? O1 Co1 K1 46.57(9) . 4_575 ? C21 Co1 K1 52.72(11) . 4_575 ? C22 Co1 K1 128.66(11) . 4_575 ? K1 Co1 K1 72.66(3) . 4_575 ? O2 K1 N3 119.32(12) . 1_556 ? O2 K1 O1 152.43(9) . 4_576 ? N3 K1 O1 84.66(11) 1_556 4_576 ? O2 K1 O1 53.09(8) . . ? N3 K1 O1 145.86(11) 1_556 . ? O1 K1 O1 114.85(9) 4_576 . ? O2 K1 C21 96.86(10) . 4_576 ? N3 K1 C21 121.06(12) 1_556 4_576 ? O1 K1 C21 56.81(10) 4_576 4_576 ? O1 K1 C21 92.90(10) . 4_576 ? O2 K1 N3 75.80(10) . 4_576 ? N3 K1 N3 137.31(14) 1_556 4_576 ? O1 K1 N3 77.12(10) 4_576 4_576 ? O1 K1 N3 76.31(9) . 4_576 ? C21 K1 N3 21.66(10) 4_576 4_576 ? O2 K1 C22 56.50(10) . . ? N3 K1 C22 93.83(12) 1_556 . ? O1 K1 C22 141.14(10) 4_576 . ? O1 K1 C22 53.09(9) . . ? C21 K1 C22 144.52(11) 4_576 . ? N3 K1 C22 124.17(11) 4_576 . ? O2 K1 N4 74.84(9) . . ? N3 K1 N4 76.16(11) 1_556 . ? O1 K1 N4 127.70(10) 4_576 . ? O1 K1 N4 69.75(9) . . ? C21 K1 N4 162.51(11) 4_576 . ? N3 K1 N4 144.15(10) 4_576 . ? C22 K1 N4 20.30(10) . . ? O2 K1 O2 123.33(10) . 4_576 ? N3 K1 O2 70.74(10) 1_556 4_576 ? O1 K1 O2 48.25(7) 4_576 4_576 ? O1 K1 O2 143.24(7) . 4_576 ? C21 K1 O2 50.35(9) 4_576 4_576 ? N3 K1 O2 68.30(9) 4_576 4_576 ? C22 K1 O2 162.47(9) . 4_576 ? N4 K1 O2 146.86(9) . 4_576 ? O2 K1 Co1 31.10(6) . . ? N3 K1 Co1 121.94(9) 1_556 . ? O1 K1 Co1 146.49(7) 4_576 . ? O1 K1 Co1 31.90(5) . . ? C21 K1 Co1 113.05(9) 4_576 . ? N3 K1 Co1 91.98(8) 4_576 . ? C22 K1 Co1 32.40(8) . . ? N4 K1 Co1 52.69(7) . . ? O2 K1 Co1 153.69(6) 4_576 . ? O2 K1 Co1 126.74(6) . 4_576 ? N3 K1 Co1 94.87(9) 1_556 4_576 ? O1 K1 Co1 29.94(5) 4_576 4_576 ? O1 K1 Co1 116.16(6) . 4_576 ? C21 K1 Co1 30.95(8) 4_576 4_576 ? N3 K1 Co1 52.61(7) 4_576 4_576 ? C22 K1 Co1 166.15(8) . 4_576 ? N4 K1 Co1 157.57(8) . 4_576 ? O2 K1 Co1 30.72(5) 4_576 4_576 ? Co1 K1 Co1 142.69(3) . 4_576 ? O2 K1 K1 152.26(6) . 4_576 ? N3 K1 K1 43.94(9) 1_556 4_576 ? O1 K1 K1 42.48(6) 4_576 4_576 ? O1 K1 K1 154.45(6) . 4_576 ? C21 K1 K1 82.31(9) 4_576 4_576 ? N3 K1 K1 103.29(8) 4_576 4_576 ? C22 K1 K1 132.50(8) . 4_576 ? N4 K1 K1 112.28(7) . 4_576 ? O2 K1 K1 38.41(5) 4_576 4_576 ? Co1 K1 K1 164.64(4) . 4_576 ? Co1 K1 K1 52.48(2) 4_576 4_576 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.232 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.084 data_1R _database_code_depnum_ccdc_archive 'CCDC 859525' #TrackingRef '1R.CIF' _database_code_depnum_ccdc_archive 'CCDC ?' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H24 Co K N4 O3' _chemical_formula_weight 502.49 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' K K 0.2009 0.2494 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.969(10) _cell_length_b 8.164(5) _cell_length_c 19.974(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.823(13) _cell_angle_gamma 90.00 _cell_volume 2275(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2030 _cell_measurement_theta_min 4.0125 _cell_measurement_theta_max 26.0143 _exptl_crystal_description cuboid _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7307 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17856 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.44 _reflns_number_total 9850 _reflns_number_gt 6560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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 _chemical_absolute_configuration unk _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^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 0.04(3) _refine_ls_number_reflns 9850 _refine_ls_number_parameters 581 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 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 K1 K 0.01124(15) 0.7567(2) 0.53771(8) 0.0661(5) Uani 1 1 d . . . K2 K 0.49079(15) 0.2689(2) 0.96416(8) 0.0667(5) Uani 1 1 d . . . Co1 Co 0.04855(6) 0.39976(8) 0.64554(4) 0.0395(2) Uani 1 1 d . . . Co2 Co 0.44910(6) -0.37499(8) 0.85592(4) 0.0389(2) Uani 1 1 d . . . C1 C 0.1277(4) 0.2921(8) 0.7695(3) 0.0446(15) Uani 1 1 d . . . H1A H 0.1163 0.3928 0.7947 0.053 Uiso 1 1 calc R . . C2 C 0.1993(5) 0.1916(10) 0.8102(3) 0.0516(18) Uani 1 1 d . . . H2A H 0.2580 0.2540 0.8177 0.062 Uiso 1 1 calc R . . H2B H 0.2144 0.0934 0.7855 0.062 Uiso 1 1 calc R . . C3 C 0.1601(5) 0.1432(12) 0.8782(3) 0.063(2) Uani 1 1 d . . . H3B H 0.1548 0.2402 0.9059 0.076 Uiso 1 1 calc R . . H3C H 0.2044 0.0683 0.9013 0.076 Uiso 1 1 calc R . . C4 C 0.0605(5) 0.0607(10) 0.8685(3) 0.0660(19) Uani 1 1 d . . . H4B H 0.0678 -0.0442 0.8465 0.079 Uiso 1 1 calc R . . H4C H 0.0350 0.0405 0.9120 0.079 Uiso 1 1 calc R . . C5 C -0.0104(5) 0.1660(11) 0.8266(3) 0.0571(19) Uani 1 1 d . . . H5A H -0.0704 0.1077 0.8191 0.069 Uiso 1 1 calc R . . H5B H -0.0231 0.2669 0.8502 0.069 Uiso 1 1 calc R . . C6 C 0.0331(4) 0.2043(8) 0.7598(3) 0.0454(13) Uani 1 1 d . . . H6A H 0.0459 0.0993 0.7383 0.055 Uiso 1 1 calc R . . C7 C -0.1154(5) 0.3132(10) 0.7143(3) 0.0453(16) Uani 1 1 d . . . H7A H -0.1433 0.2711 0.7520 0.054 Uiso 1 1 calc R . . C8 C -0.1802(5) 0.3905(10) 0.6609(3) 0.0462(17) Uani 1 1 d . . . C9 C -0.2794(6) 0.3963(13) 0.6741(4) 0.068(2) Uani 1 1 d . . . H9A H -0.2995 0.3565 0.7147 0.082 Uiso 1 1 calc R . . C10 C -0.3450(5) 0.4583(13) 0.6291(4) 0.071(2) Uani 1 1 d . . . H10A H -0.4098 0.4584 0.6377 0.085 Uiso 1 1 calc R . . C11 C -0.3125(5) 0.5240(11) 0.5677(4) 0.062(2) Uani 1 1 d . . . H11A H -0.3560 0.5702 0.5364 0.074 Uiso 1 1 calc R . . C12 C -0.2166(5) 0.5183(11) 0.5554(4) 0.057(2) Uani 1 1 d . . . H12A H -0.1956 0.5577 0.5150 0.069 Uiso 1 1 calc R . . C13 C -0.1498(4) 0.4532(8) 0.6037(3) 0.0408(16) Uani 1 1 d . . . C14 C 0.2143(5) 0.4624(10) 0.5702(3) 0.055(2) Uani 1 1 d . . . C15 C 0.2556(6) 0.5126(12) 0.5085(3) 0.063(2) Uani 1 1 d . . . H15A H 0.2192 0.5705 0.4762 0.076 Uiso 1 1 calc R . . C16 C 0.3478(6) 0.4741(12) 0.4986(4) 0.068(2) Uani 1 1 d . . . H16A H 0.3722 0.5019 0.4576 0.081 Uiso 1 1 calc R . . C17 C 0.4095(5) 0.3947(11) 0.5459(4) 0.065(2) Uani 1 1 d . . . H17A H 0.4732 0.3737 0.5374 0.078 Uiso 1 1 calc R . . C18 C 0.3726(5) 0.3507(9) 0.6037(4) 0.0523(18) Uani 1 1 d . . . H18A H 0.4118 0.2958 0.6353 0.063 Uiso 1 1 calc R . . C19 C 0.2751(4) 0.3843(9) 0.6194(3) 0.0427(16) Uani 1 1 d . . . C20 C 0.2432(4) 0.3348(9) 0.6844(3) 0.0383(14) Uani 1 1 d . . . H20A H 0.284(4) 0.297(6) 0.716(2) 0.039(14) Uiso 1 1 d . . . C21 C 0.0407(5) 0.6077(9) 0.6904(3) 0.0428(15) Uani 1 1 d . . . C22 C 0.0581(5) 0.1870(10) 0.6051(3) 0.0479(18) Uani 1 1 d . . . C23 C -0.175(2) 0.932(2) 0.6521(8) 0.280(15) Uani 1 1 d . . . C24 C 0.3623(4) -0.2050(8) 0.7465(3) 0.0442(14) Uani 1 1 d . . . H24A H 0.3764 -0.0938 0.7626 0.053 Uiso 1 1 calc R . . C25 C 0.2859(5) -0.1902(10) 0.6897(3) 0.0534(18) Uani 1 1 d . . . H25A H 0.2696 -0.2978 0.6720 0.064 Uiso 1 1 calc R . . H25B H 0.2284 -0.1407 0.7060 0.064 Uiso 1 1 calc R . . C26 C 0.3262(6) -0.0836(11) 0.6350(4) 0.068(2) Uani 1 1 d . . . H26A H 0.2797 -0.0783 0.5973 0.081 Uiso 1 1 calc R . . H26B H 0.3355 0.0267 0.6521 0.081 Uiso 1 1 calc R . . C27 C 0.4189(5) -0.1451(10) 0.6109(3) 0.068(2) Uani 1 1 d . . . H27A H 0.4426 -0.0687 0.5784 0.082 Uiso 1 1 calc R . . H27B H 0.4083 -0.2495 0.5886 0.082 Uiso 1 1 calc R . . C28 C 0.4938(5) -0.1660(11) 0.6677(3) 0.059(2) Uani 1 1 d . . . H28A H 0.5107 -0.0598 0.6865 0.071 Uiso 1 1 calc R . . H28B H 0.5511 -0.2144 0.6506 0.071 Uiso 1 1 calc R . . C29 C 0.4555(4) -0.2758(8) 0.7221(3) 0.0441(13) Uani 1 1 d . . . H29A H 0.4403 -0.3824 0.7017 0.053 Uiso 1 1 calc R . . C30 C 0.6133(5) -0.3042(11) 0.7825(4) 0.062(2) Uani 1 1 d . . . H30A H 0.6400 -0.2642 0.7440 0.074 Uiso 1 1 calc R . . C31 C 0.6772(5) -0.3551(11) 0.8336(4) 0.0512(19) Uani 1 1 d . . . C32 C 0.7760(5) -0.3452(14) 0.8245(4) 0.070(2) Uani 1 1 d . . . H32A H 0.7962 -0.2984 0.7852 0.084 Uiso 1 1 calc R . . C33 C 0.8433(5) -0.4005(16) 0.8701(5) 0.094(3) Uani 1 1 d . . . H33A H 0.9081 -0.3974 0.8615 0.113 Uiso 1 1 calc R . . C34 C 0.8133(6) -0.4600(15) 0.9280(4) 0.082(3) Uani 1 1 d . . . H34A H 0.8595 -0.4914 0.9606 0.099 Uiso 1 1 calc R . . C35 C 0.7203(5) -0.4772(13) 0.9422(4) 0.064(2) Uani 1 1 d . . . H35A H 0.7057 -0.5262 0.9825 0.077 Uiso 1 1 calc R . . C36 C 0.6427(6) -0.4226(10) 0.8974(3) 0.055(2) Uani 1 1 d . . . C37 C 0.2898(4) -0.4423(9) 0.9368(3) 0.0395(15) Uani 1 1 d . . . C38 C 0.2548(5) -0.5016(11) 0.9963(3) 0.058(2) Uani 1 1 d . . . H38A H 0.2970 -0.5457 1.0289 0.069 Uiso 1 1 calc R . . C39 C 0.1563(6) -0.4955(13) 1.0074(4) 0.071(2) Uani 1 1 d . . . H39A H 0.1336 -0.5349 1.0473 0.085 Uiso 1 1 calc R . . C40 C 0.0935(5) -0.4309(13) 0.9589(4) 0.077(3) Uani 1 1 d . . . H40A H 0.0286 -0.4228 0.9667 0.093 Uiso 1 1 calc R . . C41 C 0.1267(5) -0.3790(10) 0.8994(3) 0.0530(18) Uani 1 1 d . . . H41A H 0.0833 -0.3423 0.8659 0.064 Uiso 1 1 calc R . . C42 C 0.2255(5) -0.3796(10) 0.8874(3) 0.0461(16) Uani 1 1 d . . . C43 C 0.2521(5) -0.3140(9) 0.8266(3) 0.0474(17) Uani 1 1 d . . . H43A H 0.2033 -0.2726 0.7981 0.057 Uiso 1 1 calc R . . C44 C 0.4553(6) -0.1602(11) 0.8942(3) 0.055(2) Uani 1 1 d . . . C45 C 0.4467(5) -0.5922(11) 0.8147(4) 0.0554(19) Uani 1 1 d . . . C46 C 0.6277(7) 0.1019(12) 0.7729(4) 0.076(2) Uani 1 1 d . . . O1 O -0.0581(3) 0.4536(6) 0.5862(2) 0.0464(12) Uani 1 1 d . . . O2 O 0.1226(3) 0.4933(6) 0.5766(2) 0.0497(12) Uani 1 1 d . . . O3 O 0.5201(4) -0.3061(7) 0.7825(3) 0.0668(15) Uani 1 1 d . . . O4 O 0.3397(4) -0.3051(7) 0.8058(2) 0.0611(14) Uani 1 1 d . . . O5 O 0.6729(9) 0.1262(17) 0.8410(6) 0.224(6) Uani 1 1 d . . . O6 O -0.1482(9) 0.9266(12) 0.7109(8) 0.237(8) Uani 1 1 d . . . N1 N -0.0256(3) 0.3017(8) 0.7115(2) 0.0421(13) Uani 1 1 d . . . N2 N 0.1582(3) 0.3407(7) 0.7022(2) 0.0387(12) Uani 1 1 d . . . N3 N 0.5572(3) -0.4384(7) 0.9114(2) 0.0379(13) Uani 1 1 d . . . N4 N 0.3820(3) -0.4520(7) 0.9312(2) 0.0360(12) Uani 1 1 d . . . N5 N 0.0599(6) 0.0624(10) 0.5811(3) 0.077(2) Uani 1 1 d . . . N6 N 0.0292(5) 0.7278(9) 0.7186(3) 0.0694(18) Uani 1 1 d . . . N7 N 0.4520(7) -0.0325(11) 0.9175(3) 0.090(3) Uani 1 1 d . . . N8 N 0.4472(5) -0.7191(8) 0.7902(3) 0.0648(18) 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 K1 0.0918(14) 0.0494(11) 0.0562(10) 0.0000(8) -0.0059(10) -0.0113(10) K2 0.0939(14) 0.0470(10) 0.0575(10) -0.0020(8) -0.0148(10) -0.0054(10) Co1 0.0380(5) 0.0445(5) 0.0357(5) 0.0007(4) -0.0023(4) -0.0004(4) Co2 0.0350(5) 0.0454(5) 0.0360(5) 0.0026(4) -0.0021(4) -0.0025(4) C1 0.049(4) 0.045(3) 0.040(3) 0.008(3) -0.001(3) -0.002(3) C2 0.045(4) 0.067(4) 0.043(4) 0.009(3) 0.001(3) 0.005(3) C3 0.060(5) 0.083(5) 0.045(4) 0.019(4) -0.014(3) 0.009(4) C4 0.063(4) 0.087(5) 0.048(4) 0.024(4) 0.008(3) 0.000(4) C5 0.050(4) 0.077(5) 0.045(3) 0.018(4) 0.006(3) -0.001(4) C6 0.047(3) 0.048(3) 0.041(3) 0.009(3) 0.003(3) 0.005(3) C7 0.040(4) 0.058(4) 0.036(3) 0.009(3) -0.012(3) 0.009(3) C8 0.038(4) 0.058(4) 0.042(4) 0.003(3) -0.002(3) -0.007(4) C9 0.052(4) 0.085(6) 0.067(5) 0.004(5) 0.004(4) 0.004(5) C10 0.041(4) 0.097(6) 0.074(5) -0.001(5) -0.001(4) 0.007(4) C11 0.057(5) 0.066(4) 0.061(4) 0.004(4) -0.019(4) 0.014(4) C12 0.051(4) 0.069(5) 0.050(4) -0.001(4) -0.011(4) 0.012(4) C13 0.016(3) 0.046(4) 0.061(4) 0.000(3) -0.003(3) -0.004(3) C14 0.056(5) 0.063(5) 0.046(4) -0.006(4) 0.010(4) -0.011(4) C15 0.065(5) 0.086(6) 0.038(4) 0.010(4) 0.009(4) -0.005(5) C16 0.060(5) 0.101(7) 0.044(4) 0.000(4) 0.021(4) -0.013(5) C17 0.040(4) 0.089(6) 0.066(4) -0.017(4) 0.015(3) -0.005(4) C18 0.039(4) 0.057(4) 0.061(4) -0.006(3) 0.008(3) -0.001(3) C19 0.034(3) 0.048(4) 0.046(3) -0.006(3) -0.004(3) 0.001(3) C20 0.035(3) 0.042(3) 0.038(3) 0.001(3) -0.003(3) -0.002(3) C21 0.042(3) 0.045(4) 0.041(3) -0.001(3) -0.005(3) 0.000(3) C22 0.051(4) 0.053(4) 0.039(4) 0.002(3) -0.005(3) -0.012(4) C23 0.57(4) 0.116(12) 0.135(12) -0.002(10) -0.196(18) -0.023(18) C24 0.037(3) 0.043(3) 0.051(3) 0.002(3) -0.008(3) -0.001(3) C25 0.059(4) 0.054(4) 0.045(4) 0.009(3) -0.015(3) 0.001(4) C26 0.079(5) 0.073(5) 0.050(4) 0.014(4) -0.013(4) 0.007(4) C27 0.082(5) 0.082(5) 0.041(3) 0.018(3) -0.002(4) 0.005(4) C28 0.052(4) 0.072(5) 0.055(4) 0.012(4) 0.010(3) -0.003(4) C29 0.039(3) 0.051(3) 0.042(3) 0.009(3) 0.003(2) 0.004(3) C30 0.039(4) 0.072(5) 0.077(5) 0.005(4) 0.024(4) -0.011(4) C31 0.038(4) 0.057(5) 0.058(4) 0.000(4) -0.008(3) 0.000(4) C32 0.035(4) 0.110(7) 0.064(5) 0.011(5) 0.002(3) -0.007(5) C33 0.033(4) 0.150(10) 0.097(7) 0.007(7) -0.013(4) 0.006(6) C34 0.043(4) 0.140(9) 0.061(5) 0.025(5) -0.012(4) 0.003(5) C35 0.045(4) 0.092(6) 0.053(4) 0.002(4) -0.013(4) -0.010(5) C36 0.078(5) 0.053(4) 0.033(3) -0.008(3) -0.012(4) 0.004(4) C37 0.035(3) 0.040(3) 0.043(3) 0.001(3) -0.001(3) 0.000(3) C38 0.046(4) 0.079(5) 0.048(4) -0.004(4) -0.001(3) -0.008(4) C39 0.060(5) 0.106(7) 0.048(4) 0.015(4) 0.010(4) -0.022(5) C40 0.042(4) 0.120(8) 0.070(5) 0.014(5) 0.011(4) 0.015(5) C41 0.035(3) 0.074(5) 0.050(4) -0.005(3) 0.001(3) 0.011(3) C42 0.045(4) 0.053(4) 0.040(3) -0.002(3) 0.002(3) 0.002(4) C43 0.039(4) 0.050(4) 0.053(4) 0.001(3) -0.001(3) 0.005(3) C44 0.064(5) 0.060(5) 0.039(4) -0.002(4) -0.008(3) 0.004(4) C45 0.040(4) 0.062(5) 0.062(4) 0.019(4) -0.013(3) 0.001(4) C46 0.088(6) 0.084(6) 0.054(4) -0.015(4) -0.013(4) 0.004(5) O1 0.038(3) 0.064(3) 0.037(2) 0.007(2) -0.001(2) 0.003(2) O2 0.046(3) 0.057(3) 0.046(3) 0.016(2) 0.002(2) 0.008(2) O3 0.074(4) 0.065(3) 0.061(3) 0.002(3) -0.003(3) -0.008(3) O4 0.070(4) 0.056(3) 0.056(3) 0.005(2) -0.008(3) -0.002(3) O5 0.285(14) 0.185(11) 0.187(10) 0.006(9) -0.129(10) 0.022(10) O6 0.260(13) 0.094(6) 0.381(18) 0.044(10) 0.244(13) 0.027(8) N1 0.030(3) 0.059(3) 0.038(3) 0.009(2) 0.002(2) 0.011(2) N2 0.037(3) 0.048(3) 0.031(2) 0.003(2) 0.002(2) 0.002(3) N3 0.018(2) 0.053(3) 0.043(3) 0.011(3) -0.006(2) -0.007(3) N4 0.025(2) 0.054(3) 0.029(2) 0.011(2) 0.007(2) -0.003(2) N5 0.116(7) 0.053(4) 0.062(4) -0.010(4) -0.006(4) -0.008(4) N6 0.067(4) 0.061(4) 0.079(4) -0.012(4) -0.004(3) 0.002(3) N7 0.160(9) 0.066(5) 0.042(4) -0.005(4) -0.007(5) -0.011(5) N8 0.072(5) 0.044(4) 0.077(4) -0.006(3) -0.011(3) 0.007(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 K1 N5 2.718(8) 1_565 ? K1 O2 2.744(5) . ? K1 O1 2.845(5) . ? K1 N5 2.984(8) 2_556 ? K1 C22 3.020(7) 2_556 ? K1 O1 3.050(5) 2_556 ? K1 C21 3.290(7) . ? K1 Co1 3.646(3) . ? K1 Co1 3.893(3) 2_556 ? K1 K1 4.357(3) 2_546 ? K1 K1 4.357(3) 2_556 ? K2 N7 2.677(9) . ? K2 N3 2.789(6) 1_565 ? K2 N4 2.800(6) 1_565 ? K2 N7 2.944(8) 2_657 ? K2 C44 2.948(7) 2_657 ? K2 N3 3.107(6) 2_657 ? K2 N4 3.227(6) 2_657 ? K2 C45 3.224(7) 1_565 ? K2 Co2 3.653(3) 1_565 ? K2 Co2 3.835(3) 2_657 ? K2 K2 4.329(3) 2_657 ? K2 K2 4.329(3) 2_647 ? Co1 N1 1.894(5) . ? Co1 O1 1.909(4) . ? Co1 O2 1.920(5) . ? Co1 N2 1.921(5) . ? Co1 C21 1.926(7) . ? Co1 C22 1.923(8) . ? Co1 K1 3.893(3) 2_546 ? Co2 O4 1.875(5) . ? Co2 O3 1.896(5) . ? Co2 N3 1.901(5) . ? Co2 C44 1.913(9) . ? Co2 N4 1.917(5) . ? Co2 C45 1.955(10) . ? Co2 K2 3.653(3) 1_545 ? Co2 K2 3.835(3) 2_647 ? C1 N2 1.484(7) . ? C1 C2 1.502(9) . ? C1 C6 1.508(8) . ? C1 H1A 0.9800 . ? C2 C3 1.542(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.549(10) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.529(9) . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.526(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.468(7) . ? C6 H6A 0.9800 . ? C7 N1 1.262(8) . ? C7 C8 1.505(9) . ? C7 H7A 0.9300 . ? C8 C13 1.339(9) . ? C8 C9 1.424(10) . ? C9 C10 1.351(10) . ? C9 H9A 0.9300 . ? C10 C11 1.432(10) . ? C10 H10A 0.9300 . ? C11 C12 1.374(10) . ? C11 H11A 0.9300 . ? C12 C13 1.413(9) . ? C12 H12A 0.9300 . ? C13 O1 1.344(7) . ? C14 O2 1.317(8) . ? C14 C19 1.417(10) . ? C14 C15 1.446(9) . ? C15 C16 1.351(10) . ? C15 H15A 0.9300 . ? C16 C17 1.406(11) . ? C16 H16A 0.9300 . ? C17 C18 1.338(9) . ? C17 H17A 0.9300 . ? C18 C19 1.439(9) . ? C18 H18A 0.9300 . ? C19 C20 1.451(9) . ? C20 N2 1.257(7) . ? C20 H20A 0.89(5) . ? C21 N6 1.146(9) . ? C22 N5 1.125(11) . ? C22 K1 3.020(7) 2_546 ? C23 O6 1.214(19) . ? C24 O4 1.485(7) . ? C24 C29 1.526(8) . ? C24 C25 1.523(8) . ? C24 H24A 0.9800 . ? C25 C26 1.527(10) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.491(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.513(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.527(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O3 1.491(7) . ? C29 H29A 0.9800 . ? C30 O3 1.303(9) . ? C30 C31 1.385(11) . ? C30 H30A 0.9300 . ? C31 C32 1.403(10) . ? C31 C36 1.490(11) . ? C32 C33 1.354(11) . ? C32 H32A 0.9300 . ? C33 C34 1.342(11) . ? C33 H33A 0.9300 . ? C34 C35 1.351(10) . ? C34 H34A 0.9300 . ? C35 C36 1.442(10) . ? C35 H35A 0.9300 . ? C36 N3 1.246(9) . ? C37 N4 1.301(7) . ? C37 C38 1.393(9) . ? C37 C42 1.399(9) . ? C38 C39 1.405(10) . ? C38 H38A 0.9300 . ? C39 C40 1.380(11) . ? C39 H39A 0.9300 . ? C40 C41 1.365(10) . ? C40 H40A 0.9300 . ? C41 C42 1.412(9) . ? C41 H41A 0.9300 . ? C42 C43 1.394(9) . ? C43 O4 1.313(7) . ? C43 H43A 0.9300 . ? C44 N7 1.144(11) . ? C44 K2 2.948(7) 2_647 ? C45 N8 1.146(11) . ? C45 K2 3.224(7) 1_545 ? C46 O5 1.484(12) . ? O1 K1 3.050(5) 2_546 ? N3 K2 2.789(6) 1_545 ? N3 K2 3.107(6) 2_647 ? N4 K2 2.800(6) 1_545 ? N4 K2 3.227(6) 2_647 ? N5 K1 2.718(8) 1_545 ? N5 K1 2.984(8) 2_546 ? N7 K2 2.944(8) 2_647 ? 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 K1 O2 120.0(2) 1_565 . ? N5 K1 O1 140.72(19) 1_565 . ? O2 K1 O1 54.54(14) . . ? N5 K1 N5 144.1(2) 1_565 2_556 ? O2 K1 N5 88.3(2) . 2_556 ? O1 K1 N5 72.74(18) . 2_556 ? N5 K1 C22 122.5(2) 1_565 2_556 ? O2 K1 C22 105.72(19) . 2_556 ? O1 K1 C22 93.4(2) . 2_556 ? N5 K1 C22 21.6(2) 2_556 2_556 ? N5 K1 O1 73.42(19) 1_565 2_556 ? O2 K1 O1 120.11(15) . 2_556 ? O1 K1 O1 145.63(13) . 2_556 ? N5 K1 O1 73.19(18) 2_556 2_556 ? C22 K1 O1 53.45(19) 2_556 2_556 ? N5 K1 C21 91.5(2) 1_565 . ? O2 K1 C21 53.44(16) . . ? O1 K1 C21 52.55(16) . . ? N5 K1 C21 124.2(2) 2_556 . ? C22 K1 C21 145.6(2) 2_556 . ? O1 K1 C21 157.68(16) 2_556 . ? N5 K1 Co1 121.29(17) 1_565 . ? O2 K1 Co1 31.10(10) . . ? O1 K1 Co1 31.21(9) . . ? N5 K1 Co1 94.45(16) 2_556 . ? C22 K1 Co1 115.93(18) 2_556 . ? O1 K1 Co1 150.54(11) 2_556 . ? C21 K1 Co1 31.71(13) . . ? N5 K1 Co1 93.61(16) 1_565 2_556 ? O2 K1 Co1 126.44(11) . 2_556 ? O1 K1 Co1 121.36(11) . 2_556 ? N5 K1 Co1 50.51(16) 2_556 2_556 ? C22 K1 Co1 28.94(17) 2_556 2_556 ? O1 K1 Co1 28.77(8) 2_556 2_556 ? C21 K1 Co1 173.50(14) . 2_556 ? Co1 K1 Co1 144.40(5) . 2_556 ? N5 K1 K1 169.6(2) 1_565 2_546 ? O2 K1 K1 52.70(11) . 2_546 ? O1 K1 K1 44.19(10) . 2_546 ? N5 K1 K1 37.96(16) 2_556 2_546 ? C22 K1 K1 58.86(17) 2_556 2_546 ? O1 K1 K1 103.17(12) 2_556 2_546 ? C21 K1 K1 88.73(14) . 2_546 ? Co1 K1 K1 57.40(5) . 2_546 ? Co1 K1 K1 87.00(6) 2_556 2_546 ? N5 K1 K1 42.47(16) 1_565 2_556 ? O2 K1 K1 149.58(14) . 2_556 ? O1 K1 K1 155.88(13) . 2_556 ? N5 K1 K1 101.97(17) 2_556 2_556 ? C22 K1 K1 80.54(17) 2_556 2_556 ? O1 K1 K1 40.56(10) 2_556 2_556 ? C21 K1 K1 132.09(14) . 2_556 ? Co1 K1 K1 163.50(6) . 2_556 ? Co1 K1 K1 52.08(4) 2_556 2_556 ? K1 K1 K1 139.07(9) 2_546 2_556 ? N7 K2 N3 136.2(2) . 1_565 ? N7 K2 N4 124.6(2) . 1_565 ? N3 K2 N4 53.18(15) 1_565 1_565 ? N7 K2 N7 145.9(2) . 2_657 ? N3 K2 N7 75.5(2) 1_565 2_657 ? N4 K2 N7 82.1(2) 1_565 2_657 ? N7 K2 C44 123.5(2) . 2_657 ? N3 K2 C44 96.9(2) 1_565 2_657 ? N4 K2 C44 100.1(2) 1_565 2_657 ? N7 K2 C44 22.4(2) 2_657 2_657 ? N7 K2 N3 74.30(19) . 2_657 ? N3 K2 N3 149.08(16) 1_565 2_657 ? N4 K2 N3 119.70(15) 1_565 2_657 ? N7 K2 N3 73.7(2) 2_657 2_657 ? C44 K2 N3 52.7(2) 2_657 2_657 ? N7 K2 N4 78.9(2) . 2_657 ? N3 K2 N4 122.72(16) 1_565 2_657 ? N4 K2 N4 151.95(14) 1_565 2_657 ? N7 K2 N4 70.7(2) 2_657 2_657 ? C44 K2 N4 51.8(2) 2_657 2_657 ? N3 K2 N4 46.47(12) 2_657 2_657 ? N7 K2 C45 88.6(2) . 1_565 ? N3 K2 C45 53.19(19) 1_565 1_565 ? N4 K2 C45 54.50(19) 1_565 1_565 ? N7 K2 C45 125.5(2) 2_657 1_565 ? C44 K2 C45 147.9(3) 2_657 1_565 ? N3 K2 C45 153.28(18) 2_657 1_565 ? N4 K2 C45 150.47(17) 2_657 1_565 ? N7 K2 Co2 120.14(17) . 1_565 ? N3 K2 Co2 30.77(10) 1_565 1_565 ? N4 K2 Co2 31.13(9) 1_565 1_565 ? N7 K2 Co2 93.77(17) 2_657 1_565 ? C44 K2 Co2 115.94(19) 2_657 1_565 ? N3 K2 Co2 150.76(11) 2_657 1_565 ? N4 K2 Co2 153.49(12) 2_657 1_565 ? C45 K2 Co2 32.27(17) 1_565 1_565 ? N7 K2 Co2 94.34(16) . 2_657 ? N3 K2 Co2 123.71(12) 1_565 2_657 ? N4 K2 Co2 124.13(11) 1_565 2_657 ? N7 K2 Co2 51.55(17) 2_657 2_657 ? C44 K2 Co2 29.21(18) 2_657 2_657 ? N3 K2 Co2 29.48(9) 2_657 2_657 ? N4 K2 Co2 29.95(8) 2_657 2_657 ? C45 K2 Co2 176.89(17) 1_565 2_657 ? Co2 K2 Co2 145.06(5) 1_565 2_657 ? N7 K2 K2 171.7(2) . 2_657 ? N3 K2 K2 45.70(12) 1_565 2_657 ? N4 K2 K2 48.17(12) 1_565 2_657 ? N7 K2 K2 37.42(16) 2_657 2_657 ? C44 K2 K2 59.30(19) 2_657 2_657 ? N3 K2 K2 105.12(13) 2_657 2_657 ? N4 K2 K2 106.91(12) 2_657 2_657 ? C45 K2 K2 88.86(18) 1_565 2_657 ? Co2 K2 K2 56.66(5) 1_565 2_657 ? Co2 K2 K2 88.41(6) 2_657 2_657 ? N7 K2 K2 41.93(16) . 2_647 ? N3 K2 K2 156.53(14) 1_565 2_647 ? N4 K2 K2 150.23(14) 1_565 2_647 ? N7 K2 K2 104.16(18) 2_657 2_647 ? C44 K2 K2 81.92(19) 2_657 2_647 ? N3 K2 K2 39.96(10) 2_657 2_647 ? N4 K2 K2 40.27(10) 2_657 2_647 ? C45 K2 K2 130.04(18) 1_565 2_647 ? Co2 K2 K2 162.06(7) 1_565 2_647 ? Co2 K2 K2 52.73(4) 2_657 2_647 ? K2 K2 K2 141.08(9) 2_657 2_647 ? N1 Co1 O1 95.3(2) . . ? N1 Co1 O2 178.1(2) . . ? O1 Co1 O2 84.01(19) . . ? N1 Co1 N2 86.0(2) . . ? O1 Co1 N2 177.6(2) . . ? O2 Co1 N2 94.6(2) . . ? N1 Co1 C21 90.2(3) . . ? O1 Co1 C21 91.5(3) . . ? O2 Co1 C21 91.6(3) . . ? N2 Co1 C21 90.5(3) . . ? N1 Co1 C22 87.8(3) . . ? O1 Co1 C22 90.9(3) . . ? O2 Co1 C22 90.4(3) . . ? N2 Co1 C22 87.2(3) . . ? C21 Co1 C22 177.1(3) . . ? N1 Co1 K1 133.00(17) . . ? O1 Co1 K1 50.57(15) . . ? O2 Co1 K1 47.57(15) . . ? N2 Co1 K1 129.46(17) . . ? C21 Co1 K1 63.9(2) . . ? C22 Co1 K1 119.0(2) . . ? N1 Co1 K1 115.34(18) . 2_546 ? O1 Co1 K1 50.27(14) . 2_546 ? O2 Co1 K1 62.86(16) . 2_546 ? N2 Co1 K1 127.37(16) . 2_546 ? C21 Co1 K1 133.4(2) . 2_546 ? C22 Co1 K1 49.4(2) . 2_546 ? K1 Co1 K1 70.53(5) . 2_546 ? O4 Co2 O3 86.6(2) . . ? O4 Co2 N3 176.4(2) . . ? O3 Co2 N3 95.8(2) . . ? O4 Co2 C44 87.4(3) . . ? O3 Co2 C44 91.3(3) . . ? N3 Co2 C44 89.9(3) . . ? O4 Co2 N4 95.8(2) . . ? O3 Co2 N4 177.3(2) . . ? N3 Co2 N4 81.9(2) . . ? C44 Co2 N4 90.1(3) . . ? O4 Co2 C45 93.1(3) . . ? O3 Co2 C45 86.7(3) . . ? N3 Co2 C45 89.7(3) . . ? C44 Co2 C45 177.9(3) . . ? N4 Co2 C45 92.0(3) . . ? O4 Co2 K2 131.34(17) . 1_545 ? O3 Co2 K2 128.29(19) . 1_545 ? N3 Co2 K2 48.63(16) . 1_545 ? C44 Co2 K2 119.3(2) . 1_545 ? N4 Co2 K2 49.04(17) . 1_545 ? C45 Co2 K2 61.7(2) . 1_545 ? O4 Co2 K2 122.87(17) . 2_647 ? O3 Co2 K2 122.38(18) . 2_647 ? N3 Co2 K2 53.55(17) . 2_647 ? C44 Co2 K2 48.8(2) . 2_647 ? N4 Co2 K2 57.20(17) . 2_647 ? C45 Co2 K2 132.1(2) . 2_647 ? K2 Co2 K2 70.61(5) 1_545 2_647 ? N2 C1 C2 115.0(5) . . ? N2 C1 C6 107.4(5) . . ? C2 C1 C6 111.5(5) . . ? N2 C1 H1A 107.5 . . ? C2 C1 H1A 107.5 . . ? C6 C1 H1A 107.5 . . ? C1 C2 C3 111.1(6) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 110.9(6) . . ? C2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? C4 C3 H3C 109.5 . . ? H3B C3 H3C 108.1 . . ? C5 C4 C3 112.2(6) . . ? C5 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4C 109.2 . . ? C3 C4 H4C 109.2 . . ? H4B C4 H4C 107.9 . . ? C6 C5 C4 108.6(5) . . ? C6 C5 H5A 110.0 . . ? C4 C5 H5A 110.0 . . ? C6 C5 H5B 110.0 . . ? C4 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N1 C6 C1 106.5(5) . . ? N1 C6 C5 116.9(5) . . ? C1 C6 C5 111.6(5) . . ? N1 C6 H6A 107.1 . . ? C1 C6 H6A 107.1 . . ? C5 C6 H6A 107.1 . . ? N1 C7 C8 124.4(6) . . ? N1 C7 H7A 117.8 . . ? C8 C7 H7A 117.8 . . ? C13 C8 C9 119.9(7) . . ? C13 C8 C7 124.1(6) . . ? C9 C8 C7 116.0(6) . . ? C10 C9 C8 121.5(8) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C9 C10 C11 118.5(7) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C12 C11 C10 119.6(7) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 120.5(7) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C8 C13 O1 124.7(6) . . ? C8 C13 C12 120.0(6) . . ? O1 C13 C12 115.3(6) . . ? O2 C14 C19 124.8(6) . . ? O2 C14 C15 117.3(7) . . ? C19 C14 C15 117.9(7) . . ? C16 C15 C14 118.9(8) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C15 C16 C17 124.5(7) . . ? C15 C16 H16A 117.8 . . ? C17 C16 H16A 117.8 . . ? C18 C17 C16 117.0(7) . . ? C18 C17 H17A 121.5 . . ? C16 C17 H17A 121.5 . . ? C17 C18 C19 123.1(7) . . ? C17 C18 H18A 118.4 . . ? C19 C18 H18A 118.4 . . ? C14 C19 C18 118.5(6) . . ? C14 C19 C20 123.1(6) . . ? C18 C19 C20 118.5(6) . . ? N2 C20 C19 125.3(6) . . ? N2 C20 H20A 113(3) . . ? C19 C20 H20A 121(3) . . ? N6 C21 Co1 174.6(7) . . ? N6 C21 K1 97.2(5) . . ? Co1 C21 K1 84.4(2) . . ? N5 C22 Co1 177.3(9) . . ? N5 C22 K1 77.4(5) . 2_546 ? Co1 C22 K1 101.6(3) . 2_546 ? O4 C24 C29 105.3(5) . . ? O4 C24 C25 117.9(5) . . ? C29 C24 C25 111.7(5) . . ? O4 C24 H24A 107.1 . . ? C29 C24 H24A 107.1 . . ? C25 C24 H24A 107.1 . . ? C26 C25 C24 108.0(6) . . ? C26 C25 H25A 110.1 . . ? C24 C25 H25A 110.1 . . ? C26 C25 H25B 110.1 . . ? C24 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? C27 C26 C25 113.3(7) . . ? C27 C26 H26A 108.9 . . ? C25 C26 H26A 108.9 . . ? C27 C26 H26B 108.9 . . ? C25 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C26 C27 C28 112.1(6) . . ? C26 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? C26 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 110.3(6) . . ? C27 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? O3 C29 C24 107.3(4) . . ? O3 C29 C28 117.0(5) . . ? C24 C29 C28 109.8(5) . . ? O3 C29 H29A 107.4 . . ? C24 C29 H29A 107.4 . . ? C28 C29 H29A 107.4 . . ? O3 C30 C31 127.2(7) . . ? O3 C30 H30A 116.4 . . ? C31 C30 H30A 116.4 . . ? C30 C31 C32 119.3(7) . . ? C30 C31 C36 121.1(7) . . ? C32 C31 C36 119.6(7) . . ? C33 C32 C31 123.3(8) . . ? C33 C32 H32A 118.3 . . ? C31 C32 H32A 118.3 . . ? C34 C33 C32 117.7(7) . . ? C34 C33 H33A 121.2 . . ? C32 C33 H33A 121.2 . . ? C33 C34 C35 124.3(8) . . ? C33 C34 H34A 117.9 . . ? C35 C34 H34A 117.9 . . ? C34 C35 C36 122.6(8) . . ? C34 C35 H35A 118.7 . . ? C36 C35 H35A 118.7 . . ? N3 C36 C35 121.8(7) . . ? N3 C36 C31 125.8(7) . . ? C35 C36 C31 112.4(7) . . ? N4 C37 C38 116.3(6) . . ? N4 C37 C42 124.4(6) . . ? C38 C37 C42 119.3(6) . . ? C37 C38 C39 120.6(7) . . ? C37 C38 H38A 119.7 . . ? C39 C38 H38A 119.7 . . ? C40 C39 C38 119.8(7) . . ? C40 C39 H39A 120.1 . . ? C38 C39 H39A 120.1 . . ? C41 C40 C39 119.9(7) . . ? C41 C40 H40A 120.1 . . ? C39 C40 H40A 120.1 . . ? C40 C41 C42 121.6(7) . . ? C40 C41 H41A 119.2 . . ? C42 C41 H41A 119.2 . . ? C37 C42 C43 124.5(6) . . ? C37 C42 C41 118.7(6) . . ? C43 C42 C41 116.8(6) . . ? O4 C43 C42 126.1(6) . . ? O4 C43 H43A 116.9 . . ? C42 C43 H43A 116.9 . . ? N7 C44 Co2 175.0(9) . . ? N7 C44 K2 78.6(5) . 2_647 ? Co2 C44 K2 102.0(3) . 2_647 ? N8 C45 Co2 178.7(8) . . ? N8 C45 K2 94.2(5) . 1_545 ? Co2 C45 K2 86.0(3) . 1_545 ? C13 O1 Co1 124.3(4) . . ? C13 O1 K1 115.8(4) . . ? Co1 O1 K1 98.22(19) . . ? C13 O1 K1 117.1(4) . 2_546 ? Co1 O1 K1 100.96(18) . 2_546 ? K1 O1 K1 95.25(12) . 2_546 ? C14 O2 Co1 123.7(5) . . ? C14 O2 K1 131.5(5) . . ? Co1 O2 K1 101.33(19) . . ? C30 O3 C29 124.4(6) . . ? C30 O3 Co2 124.4(5) . . ? C29 O3 Co2 110.8(4) . . ? C43 O4 C24 121.4(5) . . ? C43 O4 Co2 124.2(4) . . ? C24 O4 Co2 113.2(4) . . ? C7 N1 C6 122.3(5) . . ? C7 N1 Co1 125.4(5) . . ? C6 N1 Co1 112.3(4) . . ? C20 N2 C1 124.3(5) . . ? C20 N2 Co1 125.4(4) . . ? C1 N2 Co1 110.2(4) . . ? C36 N3 Co2 125.6(5) . . ? C36 N3 K2 120.9(5) . 1_545 ? Co2 N3 K2 100.6(2) . 1_545 ? C36 N3 K2 111.8(4) . 2_647 ? Co2 N3 K2 97.0(2) . 2_647 ? K2 N3 K2 94.34(15) 1_545 2_647 ? C37 N4 Co2 124.9(4) . . ? C37 N4 K2 123.9(4) . 1_545 ? Co2 N4 K2 99.8(2) . 1_545 ? C37 N4 K2 115.2(4) . 2_647 ? Co2 N4 K2 92.9(2) . 2_647 ? K2 N4 K2 91.56(14) 1_545 2_647 ? C22 N5 K1 162.9(8) . 1_545 ? C22 N5 K1 81.0(6) . 2_546 ? K1 N5 K1 99.6(2) 1_545 2_546 ? C44 N7 K2 165.5(9) . . ? C44 N7 K2 79.0(6) . 2_647 ? K2 N7 K2 100.6(2) . 2_647 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.693 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.068 data_1s _database_code_depnum_ccdc_archive 'CCDC 859526' #TrackingRef '1s.CIF' _database_code_depnum_ccdc_archive 'CCDC ?' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H22 Co K N4 O3' _chemical_formula_weight 488.47 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' K K 0.2009 0.2494 '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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.873(15) _cell_length_b 8.124(9) _cell_length_c 19.53(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.96(2) _cell_angle_gamma 90.00 _cell_volume 2200(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2180 _cell_measurement_theta_min 2.5069 _cell_measurement_theta_max 27.3910 _exptl_crystal_description cuboid _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.000 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6915 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17034 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8661 _reflns_number_gt 5498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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 _chemical_absolute_configuration unk _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1175P)^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 -0.04(2) _refine_ls_number_reflns 8661 _refine_ls_number_parameters 563 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2199 _refine_ls_wR_factor_gt 0.1849 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.018 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co2 Co 0.54435(7) 1.37000(11) 0.14857(5) 0.0537(3) Uani 1 1 d . . . Co1 Co 0.95937(7) 0.60542(10) 0.35138(5) 0.0530(3) Uani 1 1 d . . . K2 K 0.49466(19) 0.7279(3) 0.04097(11) 0.0882(7) Uani 1 1 d . . . K1 K 1.00303(18) 0.2431(3) 0.45765(11) 0.0817(7) Uani 1 1 d . . . O3 O 0.4782(4) 1.2906(10) 0.2251(3) 0.0790(19) Uani 1 1 d . . . O4 O 0.6586(4) 1.3022(9) 0.1970(3) 0.0725(17) Uani 1 1 d . . . O2 O 0.8889(4) 0.5067(9) 0.4235(3) 0.0668(16) Uani 1 1 d . . . O1 O 1.0695(4) 0.5510(9) 0.4092(3) 0.0680(18) Uani 1 1 d . . . N4 N 0.6086(4) 1.4526(9) 0.0710(3) 0.0488(15) Uani 1 1 d . . . N3 N 0.4315(4) 1.4327(10) 0.0965(3) 0.061(2) Uani 1 1 d . . . N7 N 0.5447(9) 1.0260(15) 0.0830(4) 0.109(4) Uani 1 1 d . . . N1 N 1.0317(4) 0.7091(11) 0.2836(3) 0.0607(17) Uani 1 1 d . . . N2 N 0.8480(4) 0.6601(9) 0.2971(3) 0.0541(16) Uani 1 1 d . . . N8 N 0.5486(6) 1.7083(13) 0.2173(5) 0.086(2) Uani 1 1 d . . . N5 N 0.9393(7) 0.9416(14) 0.4230(4) 0.090(3) Uani 1 1 d . . . N6 N 0.9752(7) 0.2695(13) 0.2767(4) 0.085(2) Uani 1 1 d . . . C40 C 0.8986(8) 1.4363(19) 0.0325(5) 0.110(5) Uani 1 1 d . . . H40A H 0.9638 1.4335 0.0227 0.132 Uiso 1 1 calc R . . C33 C 0.1454(7) 1.377(2) 0.1453(6) 0.122(5) Uani 1 1 d . . . H33A H 0.0810 1.3638 0.1558 0.147 Uiso 1 1 calc R . . C34 C 0.1722(7) 1.450(2) 0.0845(6) 0.126(6) Uani 1 1 d . . . H34A H 0.1246 1.4855 0.0531 0.151 Uiso 1 1 calc R . . C38 C 0.7357(7) 1.5028(15) -0.0022(4) 0.073(3) Uani 1 1 d . . . H38A H 0.6926 1.5411 -0.0361 0.088 Uiso 1 1 calc R . . C35 C 0.2678(7) 1.4722(18) 0.0699(5) 0.089(4) Uani 1 1 d . . . H35A H 0.2835 1.5279 0.0302 0.107 Uiso 1 1 calc R . . C41 C 0.8682(7) 1.3786(19) 0.0926(5) 0.089(4) Uani 1 1 d . . . H41A H 0.9131 1.3341 0.1239 0.107 Uiso 1 1 calc R . . C45 C 0.5480(6) 1.5882(14) 0.1926(4) 0.061(2) Uani 1 1 d . . . C39 C 0.8313(8) 1.500(2) -0.0149(5) 0.103(4) Uani 1 1 d . . . H39A H 0.8523 1.5421 -0.0561 0.124 Uiso 1 1 calc R . . C37 C 0.6997(7) 1.4488(13) 0.0611(4) 0.064(2) Uani 1 1 d . . . C32 C 0.2201(6) 1.325(2) 0.1897(6) 0.104(4) Uani 1 1 d . . . H32A H 0.2036 1.2795 0.2315 0.124 Uiso 1 1 calc R . . C30 C 0.3837(6) 1.2847(14) 0.2283(5) 0.071(3) Uani 1 1 d . . . H30A H 0.3583 1.2435 0.2682 0.085 Uiso 1 1 calc R . . C43 C 0.7464(5) 1.3157(13) 0.1743(4) 0.061(2) Uani 1 1 d . . . H43A H 0.7968 1.2779 0.2027 0.073 Uiso 1 1 calc R . . C36 C 0.3450(7) 1.4092(15) 0.1156(5) 0.077(3) Uani 1 1 d . . . C42 C 0.7709(5) 1.3837(13) 0.1095(4) 0.058(2) Uani 1 1 d . . . C44 C 0.5396(7) 1.1534(15) 0.1087(5) 0.077(3) Uani 1 1 d . . . C31 C 0.3180(6) 1.3360(17) 0.1759(5) 0.076(3) Uani 1 1 d . . . C16 C 0.6658(8) 0.5177(17) 0.5105(6) 0.091(3) Uani 1 1 d . . . H16A H 0.6439 0.4901 0.5534 0.109 Uiso 1 1 calc R . . C10 C 1.3555(7) 0.565(2) 0.3583(6) 0.106(4) Uani 1 1 d . . . H10A H 1.4206 0.5650 0.3485 0.127 Uiso 1 1 calc R . . C11 C 1.3262(7) 0.4953(17) 0.4160(6) 0.091(3) Uani 1 1 d . . . H11A H 1.3729 0.4489 0.4453 0.110 Uiso 1 1 calc R . . C1 C 0.8755(5) 0.7110(11) 0.2275(4) 0.063(2) Uani 1 1 d . . . H1A H 0.8887 0.6111 0.2013 0.076 Uiso 1 1 calc R . . C6 C 0.9686(5) 0.8052(12) 0.2367(3) 0.0637(18) Uani 1 1 d . . . H6A H 0.9535 0.9081 0.2602 0.076 Uiso 1 1 calc R . . C15 C 0.7595(7) 0.4855(16) 0.4954(4) 0.079(3) Uani 1 1 d . . . H15A H 0.7989 0.4287 0.5267 0.095 Uiso 1 1 calc R . . C12 C 1.2287(7) 0.4874(15) 0.4358(5) 0.078(3) Uani 1 1 d . . . H12A H 1.2113 0.4385 0.4766 0.094 Uiso 1 1 calc R . . C17 C 0.6013(7) 0.5923(16) 0.4620(5) 0.090(3) Uani 1 1 d . . . H17A H 0.5374 0.6123 0.4724 0.108 Uiso 1 1 calc R . . C5 C 1.0087(6) 0.8517(16) 0.1673(4) 0.077(3) Uani 1 1 d . . . H5A H 1.0688 0.9115 0.1740 0.092 Uiso 1 1 calc R . . H5B H 1.0213 0.7532 0.1411 0.092 Uiso 1 1 calc R . . C7 C 1.1228(6) 0.7101(13) 0.2811(4) 0.065(2) Uani 1 1 d . . . H7A H 1.1487 0.7678 0.2449 0.078 Uiso 1 1 calc R . . C9 C 1.2907(6) 0.6338(18) 0.3144(5) 0.086(3) Uani 1 1 d . . . H9A H 1.3117 0.6834 0.2747 0.103 Uiso 1 1 calc R . . C2 C 0.7978(7) 0.8104(15) 0.1871(5) 0.078(3) Uani 1 1 d . . . H2A H 0.7800 0.9068 0.2131 0.094 Uiso 1 1 calc R . . H2B H 0.7406 0.7435 0.1793 0.094 Uiso 1 1 calc R . . C14 C 0.7965(6) 0.5375(11) 0.4330(4) 0.055(2) Uani 1 1 d . . . C22 C 0.9471(6) 0.8169(14) 0.3950(4) 0.061(2) Uani 1 1 d . . . C13 C 1.1603(5) 0.5579(13) 0.3902(4) 0.064(2) Uani 1 1 d . . . C21 C 0.9690(6) 0.3997(11) 0.3041(4) 0.059(2) Uani 1 1 d . . . C20 C 0.7620(5) 0.6575(11) 0.3181(4) 0.0521(19) Uani 1 1 d . . . C18 C 0.6344(6) 0.6326(16) 0.4016(5) 0.075(3) Uani 1 1 d . . . H18A H 0.5920 0.6773 0.3687 0.090 Uiso 1 1 calc R . . C19 C 0.7331(5) 0.6098(13) 0.3850(4) 0.0559(18) Uani 1 1 d . . . C8 C 1.1904(6) 0.6322(16) 0.3278(5) 0.071(3) Uani 1 1 d . . . C27 C 0.5860(7) 1.1263(15) 0.3953(4) 0.094(3) Uani 1 1 d . . . H27A H 0.5663 1.0461 0.4288 0.112 Uiso 1 1 calc R . . H27B H 0.5926 1.2316 0.4184 0.112 Uiso 1 1 calc R . . C28 C 0.5071(7) 1.1404(17) 0.3400(4) 0.088(3) Uani 1 1 d . . . H28A H 0.4481 1.1817 0.3590 0.105 Uiso 1 1 calc R . . H28B H 0.4941 1.0341 0.3191 0.105 Uiso 1 1 calc R . . C24 C 0.6391(5) 1.1993(11) 0.2569(4) 0.0613(19) Uani 1 1 d . . . H24A H 0.6256 1.0877 0.2400 0.074 Uiso 1 1 calc R . . C29 C 0.5465(5) 1.2649(11) 0.2857(3) 0.0623(18) Uani 1 1 d . . . H29A H 0.5595 1.3710 0.3080 0.075 Uiso 1 1 calc R . . C26 C 0.6831(8) 1.0766(14) 0.3698(5) 0.086(3) Uani 1 1 d . . . H26A H 0.7305 1.0817 0.4074 0.103 Uiso 1 1 calc R . . H26B H 0.6799 0.9636 0.3538 0.103 Uiso 1 1 calc R . . C4 C 0.9334(7) 0.9607(15) 0.1283(5) 0.090(3) Uani 1 1 d . . . H4B H 0.9575 0.9920 0.0842 0.108 Uiso 1 1 calc R . . H4C H 0.9219 1.0602 0.1543 0.108 Uiso 1 1 calc R . . C3 C 0.8382(7) 0.8632(17) 0.1182(4) 0.086(3) Uani 1 1 d . . . H3B H 0.7911 0.9311 0.0937 0.103 Uiso 1 1 calc R . . H3C H 0.8497 0.7663 0.0907 0.103 Uiso 1 1 calc R . . C25 C 0.7154(6) 1.1853(12) 0.3125(4) 0.060(2) Uani 1 1 d . . . H25A H 0.7735 1.1401 0.2936 0.072 Uiso 1 1 calc R . . H25B H 0.7305 1.2939 0.3304 0.072 Uiso 1 1 calc R . . H20A H 0.712(4) 0.707(7) 0.285(3) 0.041(15) Uiso 1 1 d . . . O2W O 0.3565(11) 0.876(2) 0.1701(9) 0.260(9) Uani 1 1 d . . . O1W O 1.1502(15) 0.113(3) 0.3483(9) 0.293(10) 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 Co2 0.0450(5) 0.0648(8) 0.0508(6) 0.0041(5) -0.0066(4) -0.0038(5) Co1 0.0450(5) 0.0670(8) 0.0466(6) 0.0004(5) -0.0044(4) -0.0013(5) K2 0.1189(19) 0.0662(16) 0.0770(14) -0.0019(12) -0.0314(13) 0.0004(13) K1 0.0985(17) 0.0676(16) 0.0778(14) -0.0063(12) -0.0151(11) -0.0010(12) O3 0.059(4) 0.099(5) 0.079(4) 0.002(4) 0.001(3) -0.003(3) O4 0.067(4) 0.076(5) 0.073(4) 0.010(3) -0.004(3) -0.002(3) O2 0.061(4) 0.073(4) 0.067(4) 0.013(3) 0.002(3) 0.011(3) O1 0.050(3) 0.091(5) 0.063(3) 0.010(3) -0.006(2) -0.002(3) N4 0.034(3) 0.068(4) 0.044(3) 0.014(3) -0.006(2) -0.006(3) N3 0.031(3) 0.090(6) 0.061(4) 0.020(3) -0.010(3) -0.011(3) N7 0.185(11) 0.070(7) 0.071(5) -0.003(5) -0.031(6) -0.012(7) N1 0.048(3) 0.077(4) 0.056(3) 0.011(3) -0.004(3) 0.003(3) N2 0.051(3) 0.060(4) 0.051(3) -0.008(3) -0.010(2) -0.001(3) N8 0.080(5) 0.076(6) 0.100(6) -0.013(5) -0.015(4) 0.007(4) N5 0.112(7) 0.085(7) 0.073(5) -0.013(5) -0.001(5) -0.022(5) N6 0.086(6) 0.084(6) 0.084(5) -0.007(5) 0.010(4) 0.007(4) C40 0.074(7) 0.175(14) 0.082(7) 0.026(7) 0.018(5) -0.007(7) C33 0.047(5) 0.207(17) 0.111(9) -0.031(11) -0.016(5) -0.009(8) C34 0.045(5) 0.242(19) 0.090(8) -0.020(10) -0.019(5) 0.020(8) C38 0.086(6) 0.089(7) 0.045(4) 0.008(4) 0.005(4) -0.012(5) C35 0.056(5) 0.133(11) 0.077(6) 0.007(7) -0.017(4) -0.007(6) C41 0.063(5) 0.130(10) 0.074(6) 0.009(6) 0.014(5) 0.019(6) C45 0.053(4) 0.067(6) 0.062(5) 0.013(4) -0.007(3) 0.002(4) C39 0.093(8) 0.155(12) 0.063(6) 0.009(6) 0.016(5) -0.019(8) C37 0.074(6) 0.065(6) 0.053(5) 0.010(4) -0.005(4) 0.001(4) C32 0.031(4) 0.175(13) 0.104(7) -0.030(8) 0.001(4) 0.004(6) C30 0.043(4) 0.099(7) 0.070(5) -0.002(5) 0.010(3) -0.006(4) C43 0.042(4) 0.074(6) 0.066(5) -0.002(4) -0.008(3) 0.004(4) C36 0.062(5) 0.089(8) 0.078(6) -0.018(6) -0.020(4) 0.007(5) C42 0.046(4) 0.067(6) 0.061(4) -0.003(4) 0.001(3) 0.008(4) C44 0.093(7) 0.081(8) 0.057(5) 0.020(5) -0.028(4) -0.013(5) C31 0.045(4) 0.112(9) 0.070(6) -0.015(6) 0.003(4) -0.004(5) C16 0.082(7) 0.110(9) 0.084(7) -0.004(6) 0.030(6) -0.009(6) C10 0.046(5) 0.169(13) 0.103(8) -0.005(9) 0.008(5) 0.021(6) C11 0.065(6) 0.109(8) 0.098(7) -0.028(6) -0.037(5) 0.013(5) C1 0.050(4) 0.077(5) 0.063(4) 0.002(4) -0.002(3) 0.002(4) C6 0.052(4) 0.091(6) 0.048(4) 0.011(4) 0.001(3) -0.007(4) C15 0.070(6) 0.107(9) 0.060(5) 0.001(5) 0.014(4) -0.006(6) C12 0.070(6) 0.087(7) 0.077(6) -0.019(5) -0.025(4) 0.015(5) C17 0.068(6) 0.111(8) 0.093(7) 0.003(6) 0.036(5) -0.006(5) C5 0.076(5) 0.102(7) 0.053(4) 0.023(5) 0.013(4) 0.013(5) C7 0.058(5) 0.075(6) 0.063(5) 0.000(4) 0.001(4) 0.000(4) C9 0.051(5) 0.127(10) 0.081(6) -0.010(6) 0.008(4) 0.003(6) C2 0.074(6) 0.087(7) 0.073(6) 0.015(5) -0.003(4) 0.010(5) C14 0.054(4) 0.057(5) 0.054(4) -0.005(4) 0.009(3) -0.012(4) C22 0.054(4) 0.085(7) 0.043(4) -0.009(4) 0.001(3) -0.017(4) C13 0.038(4) 0.089(7) 0.063(5) -0.004(5) -0.009(3) -0.006(4) C21 0.057(4) 0.053(5) 0.066(5) -0.001(4) -0.006(3) 0.000(3) C20 0.040(4) 0.057(5) 0.059(4) -0.003(3) 0.001(3) -0.002(3) C18 0.053(4) 0.098(7) 0.073(5) -0.016(5) -0.004(4) 0.003(5) C19 0.053(4) 0.060(5) 0.055(4) -0.001(4) 0.003(3) -0.002(4) C8 0.045(4) 0.098(8) 0.070(5) -0.009(5) -0.002(3) 0.004(5) C27 0.100(7) 0.119(8) 0.063(5) 0.040(5) 0.028(5) 0.020(6) C28 0.073(6) 0.120(9) 0.071(5) 0.020(6) 0.020(4) 0.023(6) C24 0.059(4) 0.066(5) 0.058(4) 0.014(4) -0.005(3) 0.004(3) C29 0.053(4) 0.084(5) 0.049(4) 0.009(3) -0.008(3) 0.006(3) C26 0.112(8) 0.069(6) 0.075(6) 0.018(5) -0.013(5) 0.021(5) C4 0.085(6) 0.117(8) 0.068(5) 0.031(5) 0.011(4) 0.021(6) C3 0.092(7) 0.113(9) 0.052(4) 0.016(5) -0.007(4) 0.000(6) C25 0.067(5) 0.065(5) 0.048(4) -0.006(3) -0.013(3) 0.012(4) O2W 0.241(17) 0.190(17) 0.35(2) 0.121(17) -0.007(15) -0.006(13) O1W 0.34(2) 0.26(2) 0.275(19) -0.027(17) -0.011(17) 0.07(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 Co2 O3 1.893(6) . ? Co2 O4 1.900(6) . ? Co2 N3 1.907(6) . ? Co2 C44 1.924(13) . ? Co2 N4 1.905(6) . ? Co2 C45 1.970(11) . ? Co2 K2 3.640(4) 1_565 ? Co2 K2 3.898(5) 2_655 ? Co1 C21 1.917(9) . ? Co1 N1 1.887(7) . ? Co1 O2 1.918(6) . ? Co1 N2 1.897(6) . ? Co1 O1 1.921(6) . ? Co1 C22 1.928(11) . ? Co1 K1 3.641(4) . ? Co1 K1 3.912(5) 2_756 ? K2 N7 2.643(12) . ? K2 N4 2.790(8) 1_545 ? K2 N3 2.786(8) 1_545 ? K2 N7 2.960(10) 2_645 ? K2 C44 3.008(9) 2_645 ? K2 N4 3.156(7) 2_645 ? K2 C45 3.234(9) 1_545 ? K2 N3 3.348(8) 2_645 ? K2 O2W 3.437(19) . ? K2 Co2 3.640(4) 1_545 ? K2 Co2 3.898(5) 2_645 ? K2 K2 4.370(4) 2_645 ? K1 N5 2.683(11) 1_545 ? K1 O2 2.733(7) . ? K1 O1 2.840(8) . ? K1 N5 2.924(11) 2_746 ? K1 C22 2.999(9) 2_746 ? K1 O1W 3.185(18) . ? K1 O1 3.223(7) 2_746 ? K1 C21 3.277(9) . ? K1 O2 3.330(7) 2_746 ? K1 Co1 3.912(5) 2_746 ? K1 K1 4.388(4) 2_756 ? O3 C30 1.316(10) . ? O3 C29 1.505(9) . ? O4 C43 1.315(9) . ? O4 C24 1.471(9) . ? O2 C14 1.325(9) . ? O2 K1 3.330(7) 2_756 ? O1 C13 1.326(9) . ? O1 K1 3.223(7) 2_756 ? N4 C37 1.285(10) . ? N4 K2 2.790(8) 1_565 ? N4 K2 3.156(7) 2_655 ? N3 C36 1.284(12) . ? N3 K2 2.786(8) 1_565 ? N3 K2 3.348(8) 2_655 ? N7 C44 1.153(15) . ? N7 K2 2.960(10) 2_655 ? N1 C7 1.266(10) . ? N1 C6 1.470(10) . ? N2 C20 1.276(9) . ? N2 C1 1.482(9) . ? N8 C45 1.089(13) . ? N5 C22 1.158(14) . ? N5 K1 2.683(11) 1_565 ? N5 K1 2.924(11) 2_756 ? N6 C21 1.190(12) . ? C40 C39 1.393(16) . ? C40 C41 1.346(13) . ? C40 H40A 0.9300 . ? C33 C32 1.396(16) . ? C33 C34 1.391(18) . ? C33 H33A 0.9300 . ? C34 C35 1.377(13) . ? C34 H34A 0.9300 . ? C38 C39 1.357(13) . ? C38 C37 1.420(11) . ? C38 H38A 0.9300 . ? C35 C36 1.464(13) . ? C35 H35A 0.9300 . ? C41 C42 1.401(11) . ? C41 H41A 0.9300 . ? C45 K2 3.234(9) 1_565 ? C39 H39A 0.9300 . ? C37 C42 1.445(11) . ? C32 C31 1.397(11) . ? C32 H32A 0.9300 . ? C30 C31 1.409(13) . ? C30 H30A 0.9300 . ? C43 C42 1.432(11) . ? C43 H43A 0.9300 . ? C36 C31 1.383(15) . ? C44 K2 3.008(9) 2_655 ? C16 C15 1.368(13) . ? C16 C17 1.416(15) . ? C16 H16A 0.9300 . ? C10 C11 1.337(15) . ? C10 C9 1.343(15) . ? C10 H10A 0.9300 . ? C11 C12 1.421(13) . ? C11 H11A 0.9300 . ? C1 C6 1.507(11) . ? C1 C2 1.543(11) . ? C1 H1A 0.9800 . ? C6 C5 1.530(9) . ? C6 H6A 0.9800 . ? C15 C14 1.403(11) . ? C15 H15A 0.9300 . ? C12 C13 1.401(12) . ? C12 H12A 0.9300 . ? C17 C18 1.322(13) . ? C17 H17A 0.9300 . ? C5 C4 1.550(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C8 1.434(13) . ? C7 H7A 0.9300 . ? C9 C8 1.425(11) . ? C9 H9A 0.9300 . ? C2 C3 1.536(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C14 C19 1.393(11) . ? C22 K1 2.999(9) 2_756 ? C13 C8 1.434(13) . ? C20 C19 1.434(11) . ? C20 H20A 1.01(6) . ? C18 C19 1.430(11) . ? C18 H18A 0.9300 . ? C27 C28 1.515(13) . ? C27 C26 1.507(13) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.576(12) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C24 C25 1.494(10) . ? C24 C29 1.517(10) . ? C24 H24A 0.9800 . ? C29 H29A 0.9800 . ? C26 C25 1.506(12) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C4 C3 1.546(15) . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? 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 O3 Co2 O4 85.8(3) . . ? O3 Co2 N3 95.8(3) . . ? O4 Co2 N3 177.4(3) . . ? O3 Co2 C44 89.8(4) . . ? O4 Co2 C44 87.3(4) . . ? N3 Co2 C44 90.7(4) . . ? O3 Co2 N4 178.8(3) . . ? O4 Co2 N4 95.3(3) . . ? N3 Co2 N4 83.1(3) . . ? C44 Co2 N4 90.7(4) . . ? O3 Co2 C45 88.2(4) . . ? O4 Co2 C45 92.0(3) . . ? N3 Co2 C45 90.1(3) . . ? C44 Co2 C45 177.9(4) . . ? N4 Co2 C45 91.4(3) . . ? O3 Co2 K2 129.8(2) . 1_565 ? O4 Co2 K2 131.1(2) . 1_565 ? N3 Co2 K2 48.9(2) . 1_565 ? C44 Co2 K2 119.6(3) . 1_565 ? N4 Co2 K2 49.0(2) . 1_565 ? C45 Co2 K2 62.3(3) . 1_565 ? O3 Co2 K2 126.4(2) . 2_655 ? O4 Co2 K2 118.3(2) . 2_655 ? N3 Co2 K2 59.2(2) . 2_655 ? C44 Co2 K2 49.0(3) . 2_655 ? N4 Co2 K2 53.3(2) . 2_655 ? C45 Co2 K2 133.0(2) . 2_655 ? K2 Co2 K2 70.77(7) 1_565 2_655 ? C21 Co1 N1 90.2(4) . . ? C21 Co1 O2 92.0(3) . . ? N1 Co1 O2 177.2(3) . . ? C21 Co1 N2 90.2(3) . . ? N1 Co1 N2 86.9(3) . . ? O2 Co1 N2 94.7(3) . . ? C21 Co1 O1 90.9(3) . . ? N1 Co1 O1 94.8(3) . . ? O2 Co1 O1 83.5(3) . . ? N2 Co1 O1 178.0(2) . . ? C21 Co1 C22 177.3(4) . . ? N1 Co1 C22 88.2(4) . . ? O2 Co1 C22 89.6(3) . . ? N2 Co1 C22 87.5(3) . . ? O1 Co1 C22 91.5(3) . . ? C21 Co1 K1 63.7(3) . . ? N1 Co1 K1 132.7(2) . . ? O2 Co1 K1 47.33(19) . . ? N2 Co1 K1 128.7(2) . . ? O1 Co1 K1 50.6(2) . . ? C22 Co1 K1 119.0(3) . . ? C21 Co1 K1 134.4(3) . 2_756 ? N1 Co1 K1 119.0(2) . 2_756 ? O2 Co1 K1 58.3(2) . 2_756 ? N2 Co1 K1 123.09(19) . 2_756 ? O1 Co1 K1 55.06(19) . 2_756 ? C22 Co1 K1 48.3(3) . 2_756 ? K1 Co1 K1 70.93(7) . 2_756 ? N7 K2 N4 121.9(3) . 1_545 ? N7 K2 N3 138.7(3) . 1_545 ? N4 K2 N3 53.93(19) 1_545 1_545 ? N7 K2 N7 143.2(3) . 2_645 ? N4 K2 N7 79.4(3) 1_545 2_645 ? N3 K2 N7 77.9(3) 1_545 2_645 ? N7 K2 C44 121.2(3) . 2_645 ? N4 K2 C44 96.5(3) 1_545 2_645 ? N3 K2 C44 99.4(3) 1_545 2_645 ? N7 K2 C44 22.3(3) 2_645 2_645 ? N7 K2 N4 78.1(3) . 2_645 ? N4 K2 N4 148.26(15) 1_545 2_645 ? N3 K2 N4 128.8(2) 1_545 2_645 ? N7 K2 N4 71.7(3) 2_645 2_645 ? C44 K2 N4 52.4(3) 2_645 2_645 ? N7 K2 C45 89.3(3) . 1_545 ? N4 K2 C45 54.2(2) 1_545 1_545 ? N3 K2 C45 53.6(2) 1_545 1_545 ? N7 K2 C45 125.8(3) 2_645 1_545 ? C44 K2 C45 147.5(3) 2_645 1_545 ? N4 K2 C45 157.3(2) 2_645 1_545 ? N7 K2 N3 73.1(3) . 2_645 ? N4 K2 N3 112.37(19) 1_545 2_645 ? N3 K2 N3 148.1(2) 1_545 2_645 ? N7 K2 N3 70.9(3) 2_645 2_645 ? C44 K2 N3 50.4(3) 2_645 2_645 ? N4 K2 N3 45.63(15) 2_645 2_645 ? C45 K2 N3 147.4(2) 1_545 2_645 ? N7 K2 O2W 66.3(4) . . ? N4 K2 O2W 116.9(3) 1_545 . ? N3 K2 O2W 80.0(3) 1_545 . ? N7 K2 O2W 134.6(4) 2_645 . ? C44 K2 O2W 135.3(3) 2_645 . ? N4 K2 O2W 93.1(3) 2_645 . ? C45 K2 O2W 64.3(3) 1_545 . ? N3 K2 O2W 127.4(3) 2_645 . ? N7 K2 Co2 120.7(2) . 1_545 ? N4 K2 Co2 31.04(12) 1_545 1_545 ? N3 K2 Co2 31.06(13) 1_545 1_545 ? N7 K2 Co2 93.2(2) 2_645 1_545 ? C44 K2 Co2 114.9(3) 2_645 1_545 ? N4 K2 Co2 159.24(15) 2_645 1_545 ? C45 K2 Co2 32.6(2) 1_545 1_545 ? N3 K2 Co2 143.40(15) 2_645 1_545 ? O2W K2 Co2 87.5(3) . 1_545 ? N7 K2 Co2 92.9(2) . 2_645 ? N4 K2 Co2 119.79(15) 1_545 2_645 ? N3 K2 Co2 126.11(16) 1_545 2_645 ? N7 K2 Co2 51.0(2) 2_645 2_645 ? C44 K2 Co2 28.9(2) 2_645 2_645 ? N4 K2 Co2 28.97(11) 2_645 2_645 ? C45 K2 Co2 173.60(18) 1_545 2_645 ? N3 K2 Co2 29.28(11) 2_645 2_645 ? O2W K2 Co2 122.0(3) . 2_645 ? Co2 K2 Co2 143.36(8) 1_545 2_645 ? N7 K2 K2 162.5(3) . 2_645 ? N4 K2 K2 46.05(14) 1_545 2_645 ? N3 K2 K2 50.01(17) 1_545 2_645 ? N7 K2 K2 36.2(2) 2_645 2_645 ? C44 K2 K2 57.5(2) 2_645 2_645 ? N4 K2 K2 107.71(16) 2_645 2_645 ? C45 K2 K2 90.0(2) 1_545 2_645 ? N3 K2 K2 98.81(17) 2_645 2_645 ? O2W K2 K2 128.4(3) . 2_645 ? Co2 K2 K2 57.37(8) 1_545 2_645 ? Co2 K2 K2 86.15(9) 2_645 2_645 ? N5 K1 O2 118.1(3) 1_545 . ? N5 K1 O1 145.9(2) 1_545 . ? O2 K1 O1 54.58(19) . . ? N5 K1 N5 141.6(3) 1_545 2_746 ? O2 K1 N5 84.4(3) . 2_746 ? O1 K1 N5 72.3(2) . 2_746 ? N5 K1 C22 119.2(3) 1_545 2_746 ? O2 K1 C22 101.0(2) . 2_746 ? O1 K1 C22 94.4(3) . 2_746 ? N5 K1 C22 22.5(3) 2_746 2_746 ? N5 K1 O1W 75.0(5) 1_545 . ? O2 K1 O1W 118.4(4) . . ? O1 K1 O1W 81.1(5) . . ? N5 K1 O1W 123.6(5) 2_746 . ? C22 K1 O1W 125.3(4) 2_746 . ? N5 K1 O1 69.7(2) 1_545 2_746 ? O2 K1 O1 112.45(19) . 2_746 ? O1 K1 O1 144.0(2) . 2_746 ? N5 K1 O1 73.0(2) 2_746 2_746 ? C22 K1 O1 52.4(2) 2_746 2_746 ? O1W K1 O1 127.3(5) . 2_746 ? N5 K1 C21 95.0(3) 1_545 . ? O2 K1 C21 53.7(2) . . ? O1 K1 C21 52.5(2) . . ? N5 K1 C21 122.9(3) 2_746 . ? C22 K1 C21 145.3(3) 2_746 . ? O1W K1 C21 65.8(4) . . ? O1 K1 C21 152.5(2) 2_746 . ? N5 K1 O2 77.7(3) 1_545 2_746 ? O2 K1 O2 149.95(15) . 2_746 ? O1 K1 O2 126.62(18) . 2_746 ? N5 K1 O2 70.0(2) 2_746 2_746 ? C22 K1 O2 50.4(2) 2_746 2_746 ? O1W K1 O2 89.6(4) . 2_746 ? O1 K1 O2 45.89(15) 2_746 2_746 ? C21 K1 O2 155.4(2) . 2_746 ? N5 K1 Co1 123.2(2) 1_545 . ? O2 K1 Co1 31.07(13) . . ? O1 K1 Co1 31.51(12) . . ? N5 K1 Co1 92.6(2) 2_746 . ? C22 K1 Co1 114.5(2) 2_746 . ? O1W K1 Co1 89.0(4) . . ? O1 K1 Co1 143.22(14) 2_746 . ? C21 K1 Co1 31.62(16) . . ? O2 K1 Co1 157.82(14) 2_746 . ? N5 K1 Co1 90.7(2) 1_545 2_746 ? O2 K1 Co1 120.94(14) . 2_746 ? O1 K1 Co1 122.35(14) . 2_746 ? N5 K1 Co1 51.2(2) 2_746 2_746 ? C22 K1 Co1 28.7(2) 2_746 2_746 ? O1W K1 Co1 118.5(4) . 2_746 ? O1 K1 Co1 29.25(11) 2_746 2_746 ? C21 K1 Co1 173.71(18) . 2_746 ? O2 K1 Co1 29.33(10) 2_746 2_746 ? Co1 K1 Co1 142.09(7) . 2_746 ? N5 K1 K1 158.4(3) 1_545 2_756 ? O2 K1 K1 49.31(15) . 2_756 ? O1 K1 K1 47.20(14) . 2_756 ? N5 K1 K1 36.6(2) 2_746 2_756 ? C22 K1 K1 57.3(2) 2_746 2_756 ? O1W K1 K1 125.5(5) . 2_756 ? O1 K1 K1 97.67(16) 2_746 2_756 ? C21 K1 K1 88.95(18) . 2_756 ? O2 K1 K1 106.56(15) 2_746 2_756 ? Co1 K1 K1 57.42(8) . 2_756 ? Co1 K1 K1 84.77(9) 2_746 2_756 ? C30 O3 C29 124.0(7) . . ? C30 O3 Co2 124.1(6) . . ? C29 O3 Co2 111.1(4) . . ? C43 O4 C24 121.0(7) . . ? C43 O4 Co2 125.0(5) . . ? C24 O4 Co2 112.8(5) . . ? C14 O2 Co1 122.9(5) . . ? C14 O2 K1 132.0(5) . . ? Co1 O2 K1 101.6(2) . . ? C14 O2 K1 102.0(5) . 2_756 ? Co1 O2 K1 92.4(3) . 2_756 ? K1 O2 K1 92.20(18) . 2_756 ? C13 O1 Co1 124.7(5) . . ? C13 O1 K1 116.9(6) . . ? Co1 O1 K1 97.9(3) . . ? C13 O1 K1 122.1(5) . 2_756 ? Co1 O1 K1 95.7(2) . 2_756 ? K1 O1 K1 92.52(17) . 2_756 ? C37 N4 Co2 126.9(5) . . ? C37 N4 K2 122.7(6) . 1_565 ? Co2 N4 K2 99.9(3) . 1_565 ? C37 N4 K2 107.9(5) . 2_655 ? Co2 N4 K2 97.7(3) . 2_655 ? K2 N4 K2 94.43(17) 1_565 2_655 ? C36 N3 Co2 124.3(7) . . ? C36 N3 K2 123.4(7) . 1_565 ? Co2 N3 K2 100.0(3) . 1_565 ? C36 N3 K2 118.3(6) . 2_655 ? Co2 N3 K2 91.6(3) . 2_655 ? K2 N3 K2 90.40(18) 1_565 2_655 ? C44 N7 K2 159.7(11) . . ? C44 N7 K2 81.2(7) . 2_655 ? K2 N7 K2 102.4(3) . 2_655 ? C7 N1 C6 123.1(7) . . ? C7 N1 Co1 125.9(6) . . ? C6 N1 Co1 110.8(5) . . ? C20 N2 C1 124.9(6) . . ? C20 N2 Co1 124.7(5) . . ? C1 N2 Co1 110.4(4) . . ? C22 N5 K1 152.0(8) . 1_565 ? C22 N5 K1 82.4(8) . 2_756 ? K1 N5 K1 102.9(3) 1_565 2_756 ? C39 C40 C41 119.1(11) . . ? C39 C40 H40A 120.4 . . ? C41 C40 H40A 120.4 . . ? C32 C33 C34 116.6(10) . . ? C32 C33 H33A 121.7 . . ? C34 C33 H33A 121.7 . . ? C35 C34 C33 121.3(11) . . ? C35 C34 H34A 119.4 . . ? C33 C34 H34A 119.4 . . ? C39 C38 C37 122.0(10) . . ? C39 C38 H38A 119.0 . . ? C37 C38 H38A 119.0 . . ? C34 C35 C36 121.2(11) . . ? C34 C35 H35A 119.4 . . ? C36 C35 H35A 119.4 . . ? C40 C41 C42 121.9(10) . . ? C40 C41 H41A 119.1 . . ? C42 C41 H41A 119.1 . . ? N8 C45 Co2 178.9(9) . . ? N8 C45 K2 95.1(7) . 1_565 ? Co2 C45 K2 85.1(3) . 1_565 ? C40 C39 C38 121.5(10) . . ? C40 C39 H39A 119.3 . . ? C38 C39 H39A 119.3 . . ? N4 C37 C38 120.1(8) . . ? N4 C37 C42 124.4(7) . . ? C38 C37 C42 115.4(9) . . ? C33 C32 C31 124.5(12) . . ? C33 C32 H32A 117.7 . . ? C31 C32 H32A 117.7 . . ? O3 C30 C31 125.2(8) . . ? O3 C30 H30A 117.4 . . ? C31 C30 H30A 117.4 . . ? O4 C43 C42 125.5(7) . . ? O4 C43 H43A 117.2 . . ? C42 C43 H43A 117.2 . . ? N3 C36 C31 126.5(9) . . ? N3 C36 C35 116.3(10) . . ? C31 C36 C35 117.2(9) . . ? C41 C42 C37 120.0(8) . . ? C41 C42 C43 117.2(8) . . ? C37 C42 C43 122.8(7) . . ? N7 C44 Co2 174.1(12) . . ? N7 C44 K2 76.5(7) . 2_655 ? Co2 C44 K2 102.2(4) . 2_655 ? C30 C31 C36 123.9(8) . . ? C30 C31 C32 116.8(10) . . ? C36 C31 C32 119.1(10) . . ? C15 C16 C17 121.4(10) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C11 C10 C9 119.9(10) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 124.6(10) . . ? C10 C11 H11A 117.7 . . ? C12 C11 H11A 117.7 . . ? N2 C1 C6 106.2(6) . . ? N2 C1 C2 114.7(6) . . ? C6 C1 C2 112.1(8) . . ? N2 C1 H1A 107.9 . . ? C6 C1 H1A 107.9 . . ? C2 C1 H1A 107.9 . . ? N1 C6 C1 107.1(7) . . ? N1 C6 C5 117.2(7) . . ? C1 C6 C5 110.9(7) . . ? N1 C6 H6A 107.1 . . ? C1 C6 H6A 107.1 . . ? C5 C6 H6A 107.1 . . ? C16 C15 C14 120.5(11) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C11 C12 C13 116.0(10) . . ? C11 C12 H12A 122.0 . . ? C13 C12 H12A 122.0 . . ? C18 C17 C16 118.1(9) . . ? C18 C17 H17A 120.9 . . ? C16 C17 H17A 120.9 . . ? C4 C5 C6 108.5(7) . . ? C4 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? C4 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N1 C7 C8 127.2(8) . . ? N1 C7 H7A 116.4 . . ? C8 C7 H7A 116.4 . . ? C10 C9 C8 121.0(11) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C1 C2 C3 109.0(8) . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O2 C14 C19 125.2(7) . . ? O2 C14 C15 116.7(9) . . ? C19 C14 C15 118.0(8) . . ? N5 C22 Co1 178.0(8) . . ? N5 C22 K1 75.1(7) . 2_756 ? Co1 C22 K1 103.0(4) . 2_756 ? O1 C13 C12 115.7(9) . . ? O1 C13 C8 124.2(8) . . ? C12 C13 C8 120.1(8) . . ? N6 C21 Co1 177.9(8) . . ? N6 C21 K1 93.2(7) . . ? Co1 C21 K1 84.7(3) . . ? N2 C20 C19 126.3(7) . . ? N2 C20 H20A 114(3) . . ? C19 C20 H20A 119(3) . . ? C17 C18 C19 122.3(10) . . ? C17 C18 H18A 118.8 . . ? C19 C18 H18A 118.8 . . ? C14 C19 C18 119.3(8) . . ? C14 C19 C20 122.6(7) . . ? C18 C19 C20 118.1(8) . . ? C9 C8 C13 118.4(9) . . ? C9 C8 C7 120.0(9) . . ? C13 C8 C7 121.6(7) . . ? C28 C27 C26 114.7(8) . . ? C28 C27 H27A 108.6 . . ? C26 C27 H27A 108.6 . . ? C28 C27 H27B 108.6 . . ? C26 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C27 C28 C29 105.7(8) . . ? C27 C28 H28A 110.6 . . ? C29 C28 H28A 110.6 . . ? C27 C28 H28B 110.6 . . ? C29 C28 H28B 110.6 . . ? H28A C28 H28B 108.7 . . ? O4 C24 C25 118.4(7) . . ? O4 C24 C29 106.1(6) . . ? C25 C24 C29 110.2(6) . . ? O4 C24 H24A 107.2 . . ? C25 C24 H24A 107.2 . . ? C29 C24 H24A 107.2 . . ? C24 C29 O3 106.0(5) . . ? C24 C29 C28 109.9(7) . . ? O3 C29 C28 113.3(7) . . ? C24 C29 H29A 109.2 . . ? O3 C29 H29A 109.2 . . ? C28 C29 H29A 109.2 . . ? C25 C26 C27 112.3(8) . . ? C25 C26 H26A 109.1 . . ? C27 C26 H26A 109.1 . . ? C25 C26 H26B 109.1 . . ? C27 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? C5 C4 C3 109.2(9) . . ? C5 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? C5 C4 H4C 109.8 . . ? C3 C4 H4C 109.8 . . ? H4B C4 H4C 108.3 . . ? C2 C3 C4 111.5(8) . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3C 109.3 . . ? C4 C3 H3C 109.3 . . ? H3B C3 H3C 108.0 . . ? C26 C25 C24 111.3(8) . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.834 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.083