# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sreebrata Goswami' _publ_contact_author_email ICSG@IACS.RES.IN _publ_section_title ; Tailor Made Synthesis of Amphiphilic Azoaromatics via Regioselective C-N Bond Fusion. Comparative Studies of Surface Properties of the Two Positional Isomers and Cobalt Complexes ; loop_ _publ_author_name 'Sreebrata Goswami' 'Sucheta Joy' 'Mrityunjoy Mahato' 'Prabir Pal' 'Gautam Buddha Talapatra' # Attachment 'Dalton_B919871G.cif' data_HL4 _database_code_depnum_ccdc_archive 'CCDC 748929' #TrackingRef 'Dalton_B919871G.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 N4' _chemical_formula_sum 'C29 H38 N4' _chemical_formula_weight 442.63 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 22.778(3) _cell_length_b 9.7111(12) _cell_length_c 11.8355(14) _cell_angle_alpha 90.00 _cell_angle_beta 104.600(4) _cell_angle_gamma 90.00 _cell_volume 2533.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4204 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 24.5 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9810 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method '\p and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 27148 _diffrn_reflns_av_R_equivalents 0.2098 _diffrn_reflns_av_sigmaI/netI 0.1260 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 24.53 _reflns_number_total 4204 _reflns_number_gt 1774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4204 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1908 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2110 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 0.90 _refine_ls_restrained_S_all 0.898 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.14943(16) 0.7936(3) -0.8166(3) 0.0406(9) Uani 1 1 d . . . N2 N -0.09709(16) 0.7730(3) -0.6257(3) 0.0392(9) Uani 1 1 d . . . N3 N -0.06813(16) 0.6869(3) -0.5522(3) 0.0382(9) Uani 1 1 d . . . N4 N 0.09771(16) 0.9146(3) -0.1694(3) 0.0412(10) Uani 1 1 d . . . H4A H 0.1084 1.0009 -0.1741 0.049 Uiso 1 1 d R . . C1 C -0.13457(19) 0.7071(4) -0.7267(3) 0.0354(11) Uani 1 1 d . . . C2 C -0.15358(19) 0.5708(4) -0.7313(4) 0.0425(12) Uani 1 1 d . . . H2 H -0.1425 0.5141 -0.6661 0.051 Uiso 1 1 calc R . . C3 C -0.1890(2) 0.5224(4) -0.8342(4) 0.0456(12) Uani 1 1 d . . . H3 H -0.2026 0.4318 -0.8397 0.055 Uiso 1 1 calc R . . C4 C -0.2048(2) 0.6084(5) -0.9308(4) 0.0486(13) Uani 1 1 d . . . H4 H -0.2282 0.5768 -1.0021 0.058 Uiso 1 1 calc R . . C5 C -0.1843(2) 0.7425(4) -0.9171(4) 0.0463(12) Uani 1 1 d . . . H5 H -0.1952 0.8011 -0.9811 0.056 Uiso 1 1 calc R . . C6 C -0.03047(19) 0.7472(4) -0.4517(3) 0.0362(11) Uani 1 1 d . . . C7 C 0.00985(19) 0.6605(4) -0.3766(3) 0.0367(11) Uani 1 1 d . . . H7 H 0.0088 0.5664 -0.3914 0.044 Uiso 1 1 calc R . . C8 C 0.05134(19) 0.7123(4) -0.2805(3) 0.0353(10) Uani 1 1 d . . . H8 H 0.0776 0.6528 -0.2303 0.042 Uiso 1 1 calc R . . C9 C 0.05420(19) 0.8534(4) -0.2582(3) 0.0331(10) Uani 1 1 d . . . C10 C 0.01286(19) 0.9399(4) -0.3336(3) 0.0400(11) Uani 1 1 d . . . H10 H 0.0140 1.0342 -0.3196 0.048 Uiso 1 1 calc R . . C11 C -0.0291(2) 0.8875(4) -0.4272(3) 0.0393(11) Uani 1 1 d . . . H11 H -0.0569 0.9461 -0.4749 0.047 Uiso 1 1 calc R . . C12 C 0.1399(2) 0.8457(4) -0.0795(3) 0.0369(11) Uani 1 1 d . . . C13 C 0.1231(2) 0.7395(4) -0.0155(3) 0.0380(11) Uani 1 1 d . . . H13 H 0.0827 0.7127 -0.0310 0.046 Uiso 1 1 calc R . . C14 C 0.1659(2) 0.6733(4) 0.0710(3) 0.0392(11) Uani 1 1 d . . . H14 H 0.1538 0.6011 0.1115 0.047 Uiso 1 1 calc R . . C15 C 0.2267(2) 0.7118(4) 0.0990(3) 0.0374(11) Uani 1 1 d . . . C16 C 0.2419(2) 0.8230(4) 0.0381(3) 0.0398(11) Uani 1 1 d . . . H16 H 0.2817 0.8545 0.0574 0.048 Uiso 1 1 calc R . . C17 C 0.2000(2) 0.8881(4) -0.0501(4) 0.0393(11) Uani 1 1 d . . . H17 H 0.2120 0.9609 -0.0900 0.047 Uiso 1 1 calc R . . C18 C 0.27394(19) 0.6344(4) 0.1882(3) 0.0435(12) Uani 1 1 d . . . H18A H 0.3004 0.5875 0.1482 0.052 Uiso 1 1 calc R . . H18B H 0.2537 0.5644 0.2230 0.052 Uiso 1 1 calc R . . C19 C 0.3128(2) 0.7211(4) 0.2854(4) 0.0435(12) Uani 1 1 d . . . H19A H 0.3352 0.7876 0.2516 0.052 Uiso 1 1 calc R . . H19B H 0.2864 0.7718 0.3234 0.052 Uiso 1 1 calc R . . C20 C 0.3572(2) 0.6379(4) 0.3763(3) 0.0411(11) Uani 1 1 d . . . H20A H 0.3349 0.5682 0.4071 0.049 Uiso 1 1 calc R . . H20B H 0.3848 0.5909 0.3389 0.049 Uiso 1 1 calc R . . C21 C 0.3938(2) 0.7225(4) 0.4765(3) 0.0424(11) Uani 1 1 d . . . H21A H 0.3661 0.7774 0.5083 0.051 Uiso 1 1 calc R . . H21B H 0.4193 0.7855 0.4466 0.051 Uiso 1 1 calc R . . C22 C 0.4335(2) 0.6388(4) 0.5744(3) 0.0440(12) Uani 1 1 d . . . H22A H 0.4081 0.5751 0.6037 0.053 Uiso 1 1 calc R . . H22B H 0.4615 0.5847 0.5428 0.053 Uiso 1 1 calc R . . C23 C 0.4698(2) 0.7233(4) 0.6756(3) 0.0469(12) Uani 1 1 d . . . H23A H 0.4420 0.7791 0.7062 0.056 Uiso 1 1 calc R . . H23B H 0.4961 0.7854 0.6469 0.056 Uiso 1 1 calc R . . C24 C 0.5083(2) 0.6380(4) 0.7746(4) 0.0465(12) Uani 1 1 d . . . H24A H 0.4819 0.5771 0.8042 0.056 Uiso 1 1 calc R . . H24B H 0.5355 0.5808 0.7436 0.056 Uiso 1 1 calc R . . C25 C 0.5456(2) 0.7222(4) 0.8751(4) 0.0463(12) Uani 1 1 d . . . H25A H 0.5186 0.7819 0.9043 0.056 Uiso 1 1 calc R . . H25B H 0.5732 0.7803 0.8462 0.056 Uiso 1 1 calc R . . C26 C 0.5821(2) 0.6357(4) 0.9755(4) 0.0461(12) Uani 1 1 d . . . H26A H 0.6076 0.5729 0.9454 0.055 Uiso 1 1 calc R . . H26B H 0.5542 0.5806 1.0066 0.055 Uiso 1 1 calc R . . C27 C 0.6219(2) 0.7187(4) 1.0745(4) 0.0472(12) Uani 1 1 d . . . H27A H 0.6523 0.7670 1.0452 0.057 Uiso 1 1 calc R . . H27B H 0.5971 0.7874 1.0999 0.057 Uiso 1 1 calc R . . C28 C 0.6535(2) 0.6332(5) 1.1786(4) 0.0513(13) Uani 1 1 d . . . H28A H 0.6773 0.5626 1.1527 0.062 Uiso 1 1 calc R . . H28B H 0.6231 0.5874 1.2096 0.062 Uiso 1 1 calc R . . C29 C 0.6952(2) 0.7160(5) 1.2763(4) 0.0632(15) Uani 1 1 d . . . H29A H 0.7267 0.7583 1.2475 0.095 Uiso 1 1 calc R . . H29B H 0.7130 0.6558 1.3400 0.095 Uiso 1 1 calc R . . H29C H 0.6720 0.7861 1.3027 0.095 Uiso 1 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 N1 0.043(2) 0.035(2) 0.039(2) -0.0037(18) 0.0016(19) 0.0007(18) N2 0.045(2) 0.034(2) 0.036(2) -0.0005(17) 0.0044(18) 0.0000(18) N3 0.037(2) 0.034(2) 0.041(2) -0.0008(18) 0.0041(19) 0.0019(18) N4 0.050(3) 0.0251(19) 0.044(2) 0.0001(17) 0.003(2) 0.0004(18) C1 0.031(3) 0.029(2) 0.043(3) -0.003(2) 0.005(2) -0.001(2) C2 0.046(3) 0.032(3) 0.048(3) 0.002(2) 0.010(2) 0.002(2) C3 0.049(3) 0.031(2) 0.053(3) -0.007(2) 0.007(2) -0.001(2) C4 0.053(3) 0.043(3) 0.043(3) -0.010(2) 0.001(2) 0.000(2) C5 0.054(3) 0.037(3) 0.045(3) -0.001(2) 0.006(2) 0.007(2) C6 0.034(3) 0.036(3) 0.036(2) -0.002(2) 0.005(2) -0.002(2) C7 0.045(3) 0.027(2) 0.037(2) -0.004(2) 0.010(2) -0.004(2) C8 0.040(3) 0.026(2) 0.040(3) 0.0031(19) 0.011(2) 0.000(2) C9 0.039(3) 0.027(2) 0.033(2) 0.0001(19) 0.010(2) -0.002(2) C10 0.047(3) 0.030(2) 0.039(2) -0.005(2) 0.004(2) 0.003(2) C11 0.040(3) 0.037(3) 0.038(3) 0.000(2) 0.007(2) 0.008(2) C12 0.048(3) 0.029(2) 0.032(2) -0.0038(19) 0.006(2) 0.003(2) C13 0.037(3) 0.037(3) 0.035(2) 0.000(2) 0.000(2) 0.003(2) C14 0.045(3) 0.037(3) 0.036(2) -0.001(2) 0.012(2) -0.001(2) C15 0.043(3) 0.036(3) 0.031(2) -0.005(2) 0.005(2) 0.006(2) C16 0.039(3) 0.037(3) 0.040(3) -0.001(2) 0.004(2) 0.001(2) C17 0.041(3) 0.034(2) 0.043(3) -0.002(2) 0.010(2) -0.003(2) C18 0.046(3) 0.040(3) 0.042(3) 0.005(2) 0.006(2) 0.005(2) C19 0.046(3) 0.035(3) 0.048(3) 0.003(2) 0.008(2) 0.005(2) C20 0.048(3) 0.033(2) 0.043(3) 0.000(2) 0.011(2) 0.003(2) C21 0.043(3) 0.036(2) 0.045(3) 0.003(2) 0.006(2) 0.003(2) C22 0.045(3) 0.044(3) 0.043(3) 0.002(2) 0.010(2) 0.002(2) C23 0.048(3) 0.043(3) 0.048(3) -0.001(2) 0.009(2) 0.003(2) C24 0.052(3) 0.038(3) 0.047(3) 0.000(2) 0.006(2) 0.000(2) C25 0.042(3) 0.046(3) 0.052(3) 0.000(2) 0.014(2) -0.003(2) C26 0.048(3) 0.042(3) 0.047(3) 0.003(2) 0.008(2) -0.002(2) C27 0.047(3) 0.044(3) 0.051(3) -0.004(2) 0.011(2) -0.003(2) C28 0.047(3) 0.053(3) 0.050(3) -0.001(2) 0.004(2) -0.001(3) C29 0.053(4) 0.077(4) 0.055(3) -0.008(3) 0.004(3) -0.001(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 N1 C1 1.330(5) . ? N1 C5 1.348(5) . ? N2 N3 1.266(4) . ? N2 C1 1.432(5) . ? N3 C6 1.407(5) . ? N4 C9 1.384(5) . ? N4 C12 1.410(5) . ? N4 H4A 0.8785 . ? C1 C2 1.390(5) . ? C2 C3 1.364(5) . ? C2 H2 0.9300 . ? C3 C4 1.388(6) . ? C3 H3 0.9300 . ? C4 C5 1.378(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.390(5) . ? C6 C11 1.391(5) . ? C7 C8 1.377(5) . ? C7 H7 0.9300 . ? C8 C9 1.394(5) . ? C8 H8 0.9300 . ? C9 C10 1.402(5) . ? C10 C11 1.366(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.387(5) . ? C12 C13 1.389(5) . ? C13 C14 1.381(5) . ? C13 H13 0.9300 . ? C14 C15 1.390(5) . ? C14 H14 0.9300 . ? C15 C16 1.390(5) . ? C15 C18 1.505(5) . ? C16 C17 1.377(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.518(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.511(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.509(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.515(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.514(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.520(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.515(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.520(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.520(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.509(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.527(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 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 C1 N1 C5 116.6(4) . . ? N3 N2 C1 112.1(3) . . ? N2 N3 C6 114.1(3) . . ? C9 N4 C12 126.2(3) . . ? C9 N4 H4A 121.2 . . ? C12 N4 H4A 110.8 . . ? N1 C1 C2 123.8(4) . . ? N1 C1 N2 111.3(3) . . ? C2 C1 N2 124.9(4) . . ? C3 C2 C1 118.1(4) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.5(4) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 123.9(4) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? C7 C6 C11 118.9(4) . . ? C7 C6 N3 116.9(4) . . ? C11 C6 N3 124.1(4) . . ? C8 C7 C6 120.8(4) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.3(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? N4 C9 C8 123.8(4) . . ? N4 C9 C10 117.6(4) . . ? C8 C9 C10 118.5(4) . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C6 120.6(4) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? C17 C12 C13 118.2(4) . . ? C17 C12 N4 119.4(4) . . ? C13 C12 N4 122.4(4) . . ? C14 C13 C12 120.7(4) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 121.7(4) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 116.7(4) . . ? C16 C15 C18 121.6(4) . . ? C14 C15 C18 121.7(4) . . ? C17 C16 C15 122.2(4) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C12 120.4(4) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C15 C18 C19 115.6(4) . . ? C15 C18 H18A 108.4 . . ? C19 C18 H18A 108.4 . . ? C15 C18 H18B 108.4 . . ? C19 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C20 C19 C18 113.6(4) . . ? C20 C19 H19A 108.8 . . ? C18 C19 H19A 108.8 . . ? C20 C19 H19B 108.8 . . ? C18 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C21 C20 C19 114.0(3) . . ? C21 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 114.5(3) . . ? C20 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? C20 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C21 114.6(4) . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22B 108.6 . . ? C21 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C22 C23 C24 114.1(4) . . ? C22 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? C22 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C23 114.3(4) . . ? C25 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 C25 C26 113.8(4) . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C25 C26 C27 114.3(4) . . ? C25 C26 H26A 108.7 . . ? C27 C26 H26A 108.7 . . ? C25 C26 H26B 108.7 . . ? C27 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C26 114.0(4) . . ? C28 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.6 . . ? C27 C28 C29 113.9(4) . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.53 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.215 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.050 #===END data_[Co(L1)(L5)]ClO4 _database_code_depnum_ccdc_archive 'CCDC 748930' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H53 Co N8, Cl O4' _chemical_formula_sum 'C47 H53 Cl Co N8 O4' _chemical_formula_weight 888.35 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.636(2) _cell_length_b 10.519(3) _cell_length_c 24.613(6) _cell_angle_alpha 79.300(6) _cell_angle_beta 85.997(6) _cell_angle_gamma 85.014(6) _cell_volume 2185.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9321 _cell_measurement_theta_min 0.8 _cell_measurement_theta_max 17.8 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8544 _exptl_absorpt_correction_T_max 0.9141 _exptl_absorpt_process_details 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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9321 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 17.78 _reflns_number_total 2895 _reflns_number_gt 2045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.0907P)^2^+3.5271P] 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 2895 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1682 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.01906(15) 0.63771(13) 0.66244(6) 0.0216(6) Uani 1 1 d . . . Cl1 Cl -0.3829(3) 0.2490(3) 0.57596(12) 0.0280(9) Uani 1 1 d . . . N4 N 0.0554(8) 0.5255(8) 0.6107(3) 0.017(2) Uiso 1 1 d . . . O1 O -0.3049(7) 0.2349(6) 0.5232(3) 0.0314(19) Uani 1 1 d . . . N5 N -0.1818(9) 0.7128(7) 0.6141(3) 0.021(2) Uiso 1 1 d . . . N8 N 0.1741(9) 0.6002(8) 0.6997(3) 0.017(2) Uiso 1 1 d . . . C25 C 0.4067(12) 0.7090(11) 0.7112(4) 0.023(3) Uani 1 1 d . . . H25 H 0.4521 0.6371 0.7342 0.028 Uiso 1 1 calc R . . C24 C 0.2614(12) 0.7026(9) 0.6880(4) 0.020(3) Uani 1 1 d . . . O3 O -0.3829(8) 0.3837(6) 0.5824(3) 0.039(2) Uani 1 1 d . . . C33 C 0.2502(11) 0.2919(10) 0.7979(4) 0.031(3) Uani 1 1 d . . . H33 H 0.2155 0.2529 0.8331 0.038 Uiso 1 1 calc R . . O2 O -0.3020(7) 0.1656(6) 0.6197(3) 0.0298(19) Uani 1 1 d . . . O4 O -0.5411(8) 0.2145(6) 0.5767(3) 0.0347(19) Uani 1 1 d . . . C29 C 0.2378(11) 0.4743(9) 0.7233(4) 0.017(3) Uiso 1 1 d . . . C30 C 0.3493(11) 0.4069(11) 0.6928(4) 0.023(3) Uani 1 1 d . . . H30 H 0.3818 0.4451 0.6571 0.028 Uiso 1 1 calc R . . C34 C 0.1869(11) 0.4163(10) 0.7758(4) 0.022(3) Uiso 1 1 d . . . H34 H 0.1118 0.4593 0.7962 0.026 Uiso 1 1 calc R . . C16 C 0.1868(11) 0.4595(10) 0.5309(4) 0.025(3) Uiso 1 1 d . . . H16 H 0.2517 0.4784 0.4991 0.030 Uiso 1 1 calc R . . N1 N -0.1190(9) 0.7070(8) 0.7245(4) 0.021(2) Uani 1 1 d . . . C12 C -0.2018(13) 0.4934(12) 0.7433(5) 0.019(3) Uani 1 1 d . . . C17 C 0.1453(11) 0.5508(9) 0.5645(4) 0.022(3) Uiso 1 1 d . . . H17 H 0.1818 0.6329 0.5542 0.027 Uiso 1 1 calc R . . C15 C 0.1273(11) 0.3387(9) 0.5467(4) 0.025(3) Uani 1 1 d . . . H15 H 0.1518 0.2756 0.5250 0.030 Uiso 1 1 calc R . . C7 C -0.1946(12) 0.6172(13) 0.7596(5) 0.020(3) Uani 1 1 d . . . C19 C -0.2487(12) 0.9036(10) 0.5487(4) 0.029(3) Uani 1 1 d . . . H19 H -0.2275 0.9867 0.5307 0.035 Uiso 1 1 calc R . . C22 C -0.3112(11) 0.6627(10) 0.6040(4) 0.026(3) Uiso 1 1 d . . . H22 H -0.3323 0.5805 0.6230 0.031 Uiso 1 1 calc R . . C8 C -0.2765(14) 0.6345(11) 0.8098(6) 0.029(3) Uani 1 1 d . . . H8 H -0.2736 0.7122 0.8224 0.035 Uiso 1 1 calc R . . N6 N -0.0088(10) 0.8794(8) 0.5947(3) 0.025(2) Uani 1 1 d . . . C18 C -0.1476(13) 0.8322(10) 0.5852(4) 0.027(3) Uiso 1 1 d . . . C21 C -0.4137(11) 0.7273(9) 0.5670(4) 0.024(3) Uani 1 1 d . . . H21 H -0.5025 0.6894 0.5607 0.029 Uiso 1 1 calc R . . C11 C -0.2906(14) 0.3984(11) 0.7740(6) 0.032(3) Uani 1 1 d . . . H11 H -0.2948 0.3199 0.7621 0.039 Uiso 1 1 calc R . . C26 C 0.4769(12) 0.8210(13) 0.6993(4) 0.026(3) Uani 1 1 d . . . H26 H 0.5688 0.8256 0.7162 0.031 Uiso 1 1 calc R . . C10 C -0.3710(13) 0.4192(12) 0.8212(6) 0.040(3) Uani 1 1 d . . . H10 H -0.4329 0.3568 0.8413 0.047 Uiso 1 1 calc R . . C9 C -0.3589(13) 0.5392(15) 0.8396(5) 0.041(3) Uani 1 1 d . . . H9 H -0.4093 0.5520 0.8730 0.050 Uiso 1 1 calc R . . C35 C 0.4357(12) 0.0900(10) 0.7912(5) 0.036(3) Uani 1 1 d . . . H35A H 0.3735 0.0268 0.7808 0.043 Uiso 1 1 calc R . . H35B H 0.5385 0.0802 0.7732 0.043 Uiso 1 1 calc R . . C20 C -0.3838(13) 0.8500(11) 0.5388(4) 0.031(3) Uiso 1 1 d . . . H20 H -0.4530 0.8961 0.5137 0.037 Uiso 1 1 calc R . . C32 C 0.3633(12) 0.2245(11) 0.7689(5) 0.029(3) Uiso 1 1 d . . . C2 C -0.1410(11) 0.9444(10) 0.7136(4) 0.025(3) Uani 1 1 d . . . H2 H -0.2054 0.9490 0.6845 0.030 Uiso 1 1 calc R . . C6 C 0.0147(11) 0.8178(11) 0.7844(4) 0.032(3) Uani 1 1 d . . . H6 H 0.0559 0.7379 0.8026 0.039 Uiso 1 1 calc R . . C1 C -0.0841(12) 0.8247(11) 0.7419(4) 0.022(3) Uiso 1 1 d . . . C31 C 0.4114(12) 0.2835(11) 0.7155(5) 0.031(3) Uani 1 1 d . . . H31 H 0.4856 0.2400 0.6949 0.037 Uiso 1 1 calc R . . C37 C 0.5387(13) -0.0697(10) 0.8722(5) 0.041(3) Uani 1 1 d . . . H37A H 0.4908 -0.1378 0.8592 0.049 Uiso 1 1 calc R . . H37B H 0.6447 -0.0676 0.8564 0.049 Uiso 1 1 calc R . . C5 C 0.0516(12) 0.9327(12) 0.7995(4) 0.042(3) Uani 1 1 d . . . H5 H 0.1159 0.9290 0.8286 0.051 Uiso 1 1 calc R . . C36 C 0.4510(14) 0.0583(10) 0.8519(5) 0.047(4) Uani 1 1 d . . . H36A H 0.3475 0.0580 0.8700 0.057 Uiso 1 1 calc R . . H36B H 0.5033 0.1265 0.8631 0.057 Uiso 1 1 calc R . . C38 C 0.5421(17) -0.1021(11) 0.9342(6) 0.076(5) Uani 1 1 d . . . H38A H 0.4356 -0.1050 0.9495 0.091 Uiso 1 1 calc R . . H38B H 0.5867 -0.0318 0.9468 0.091 Uiso 1 1 calc R . . N3 N -0.0948(9) 0.3830(9) 0.6742(4) 0.020(2) Uani 1 1 d . . . C13 C -0.0020(12) 0.4048(9) 0.6261(5) 0.017(3) Uani 1 1 d . . . C14 C 0.0342(12) 0.3114(10) 0.5934(4) 0.027(3) Uiso 1 1 d . . . H14 H -0.0050 0.2302 0.6035 0.032 Uiso 1 1 calc R . . C4 C -0.0061(13) 1.0513(12) 0.7717(5) 0.040(3) Uiso 1 1 d . . . H4 H 0.0197 1.1273 0.7819 0.048 Uiso 1 1 calc R . . C39 C 0.6312(16) -0.2276(12) 0.9579(6) 0.067(4) Uani 1 1 d . . . H39A H 0.7402 -0.2222 0.9459 0.081 Uiso 1 1 calc R . . H39B H 0.5932 -0.2977 0.9431 0.081 Uiso 1 1 calc R . . C3 C -0.1012(12) 1.0573(11) 0.7292(4) 0.033(3) Uani 1 1 d . . . H3 H -0.1398 1.1376 0.7104 0.040 Uiso 1 1 calc R . . C40 C 0.618(2) -0.2606(14) 1.0216(7) 0.110(6) Uani 1 1 d . . . H40A H 0.5098 -0.2767 1.0323 0.131 Uiso 1 1 calc R . . H40B H 0.6380 -0.1832 1.0352 0.131 Uiso 1 1 calc R . . C28 C 0.2814(13) 0.9294(9) 0.6381(4) 0.025(3) Uani 1 1 d . . . H28 H 0.2407 1.0012 0.6139 0.030 Uiso 1 1 calc R . . C27 C 0.4186(14) 0.9323(11) 0.6626(5) 0.029(3) Uani 1 1 d . . . H27 H 0.4730 1.0067 0.6552 0.035 Uiso 1 1 calc R . . C43 C 0.779(2) -0.6239(18) 1.0784(8) 0.136(8) Uani 1 1 d . . . H43A H 0.7447 -0.6205 1.1166 0.163 Uiso 1 1 calc R . . H43B H 0.7451 -0.7025 1.0693 0.163 Uiso 1 1 calc R . . C42 C 0.6985(19) -0.492(2) 1.0359(7) 0.122(7) Uani 1 1 d . . . H42A H 0.7451 -0.4892 0.9987 0.147 Uiso 1 1 calc R . . H42B H 0.5879 -0.5006 1.0347 0.147 Uiso 1 1 calc R . . C41 C 0.721(2) -0.3770(19) 1.0541(8) 0.124(8) Uani 1 1 d . . . H41A H 0.8301 -0.3593 1.0482 0.149 Uiso 1 1 calc R . . H41B H 0.6938 -0.3864 1.0935 0.149 Uiso 1 1 calc R . . N2 N -0.1139(9) 0.4870(9) 0.6955(4) 0.016(2) Uani 1 1 d . . . N7 N 0.0672(9) 0.7947(8) 0.6298(3) 0.017(2) Uani 1 1 d . . . C23 C 0.2041(12) 0.8142(10) 0.6508(4) 0.019(3) Uiso 1 1 d . . . C44 C 0.939(2) -0.6254(19) 1.0725(7) 0.138(7) Uani 1 1 d . . . H44A H 0.9836 -0.7003 1.0963 0.208 Uiso 1 1 calc R . . H44B H 0.9717 -0.5483 1.0823 0.208 Uiso 1 1 calc R . . H44C H 0.9719 -0.6287 1.0347 0.208 Uiso 1 1 calc R . . C46 C -0.015(3) 0.1015(19) 0.9270(6) 0.152(9) Uani 1 1 d . . . H46A H -0.0254 0.0313 0.9072 0.182 Uiso 1 1 calc R . . H46B H 0.0906 0.1278 0.9206 0.182 Uiso 1 1 calc R . . C48 C -0.054(2) 0.0605(17) 0.9875(9) 0.152(8) Uani 1 1 d . . . H48A H -0.1617 0.0395 0.9931 0.182 Uiso 1 1 calc R . . H48B H -0.0415 0.1315 1.0065 0.182 Uiso 1 1 calc R . . C45 C -0.136(2) 0.219(2) 0.9078(8) 0.189(11) Uani 1 1 d . . . H45A H -0.1173 0.2516 0.8690 0.284 Uiso 1 1 calc R . . H45B H -0.1251 0.2870 0.9283 0.284 Uiso 1 1 calc R . . H45C H -0.2397 0.1913 0.9144 0.284 Uiso 1 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 Co1 0.0185(9) 0.0140(10) 0.0350(10) -0.0108(7) 0.0019(7) -0.0058(7) Cl1 0.024(2) 0.024(2) 0.038(2) -0.0106(17) 0.0020(18) -0.0066(16) O1 0.035(5) 0.031(5) 0.030(5) -0.011(4) 0.012(4) -0.009(4) C25 0.014(8) 0.008(8) 0.049(8) -0.012(6) 0.001(6) 0.002(6) C24 0.016(8) 0.015(7) 0.029(7) -0.008(6) 0.010(6) -0.008(6) O3 0.059(5) 0.010(5) 0.049(5) -0.013(4) 0.012(4) -0.009(4) C33 0.026(7) 0.039(8) 0.032(7) -0.010(6) 0.003(6) -0.013(6) O2 0.024(4) 0.031(5) 0.032(5) 0.006(4) -0.012(4) -0.004(4) O4 0.026(5) 0.030(5) 0.049(5) -0.006(4) -0.010(4) -0.001(4) C30 0.026(7) 0.030(8) 0.018(7) -0.011(6) 0.006(6) -0.012(6) N1 0.016(5) 0.018(6) 0.031(6) -0.012(5) 0.014(5) -0.008(5) C12 0.015(7) 0.017(10) 0.026(9) -0.008(8) 0.002(7) -0.007(7) C15 0.034(7) 0.016(7) 0.029(7) -0.017(6) -0.006(6) 0.001(6) C7 0.007(7) 0.035(11) 0.023(10) -0.017(8) 0.003(7) 0.002(7) C19 0.042(8) 0.017(7) 0.032(7) -0.013(6) 0.005(6) -0.009(6) C8 0.035(8) 0.016(8) 0.040(9) -0.014(7) 0.007(7) -0.016(7) N6 0.028(6) 0.019(6) 0.029(6) -0.008(5) -0.008(5) 0.008(5) C21 0.023(7) 0.023(7) 0.033(7) -0.023(6) 0.000(6) -0.007(6) C11 0.027(8) 0.028(9) 0.044(9) -0.014(8) 0.009(7) -0.010(8) C26 0.018(7) 0.023(8) 0.042(8) -0.019(7) 0.010(6) -0.007(8) C10 0.034(8) 0.042(11) 0.047(10) -0.017(8) 0.024(8) -0.026(7) C9 0.039(8) 0.052(10) 0.037(8) -0.017(9) 0.014(7) -0.014(8) C35 0.041(8) 0.026(8) 0.043(9) -0.016(7) 0.001(6) 0.004(6) C2 0.030(7) 0.021(8) 0.025(7) -0.007(6) 0.006(5) -0.005(6) C6 0.027(7) 0.026(8) 0.046(8) -0.007(7) -0.007(6) -0.004(6) C31 0.028(7) 0.019(8) 0.052(9) -0.022(7) -0.015(6) 0.008(6) C37 0.054(9) 0.011(8) 0.054(10) -0.002(7) -0.015(7) 0.019(7) C5 0.036(8) 0.051(10) 0.048(8) -0.025(8) -0.008(6) -0.017(7) C36 0.059(9) 0.027(9) 0.060(10) -0.020(7) -0.017(7) 0.008(7) C38 0.122(13) 0.029(9) 0.080(12) -0.019(8) -0.057(10) 0.038(9) N3 0.024(6) 0.011(6) 0.028(7) -0.009(6) 0.002(5) -0.001(5) C13 0.023(7) 0.008(7) 0.021(7) -0.006(6) -0.001(6) -0.002(5) C39 0.080(11) 0.056(11) 0.061(11) -0.007(8) -0.015(8) 0.021(9) C3 0.035(8) 0.014(8) 0.051(9) -0.011(6) 0.009(7) -0.004(6) C40 0.148(16) 0.063(11) 0.117(17) -0.018(11) -0.069(13) 0.050(12) C28 0.026(8) 0.005(7) 0.042(8) -0.003(6) 0.012(7) -0.006(6) C27 0.024(9) 0.013(9) 0.051(8) -0.008(7) 0.006(7) -0.011(7) C43 0.076(14) 0.156(18) 0.139(17) 0.060(14) -0.026(13) 0.022(13) C42 0.078(13) 0.19(2) 0.097(14) -0.045(16) 0.004(10) 0.011(14) C41 0.111(16) 0.129(17) 0.161(19) -0.104(17) -0.010(14) -0.008(14) N2 0.012(6) 0.007(7) 0.030(7) -0.003(6) 0.003(5) -0.005(5) N7 0.018(6) 0.010(5) 0.025(6) -0.009(5) 0.001(5) -0.002(5) C44 0.113(17) 0.18(2) 0.096(14) 0.013(13) 0.009(13) 0.043(15) C46 0.25(3) 0.17(2) 0.022(10) 0.009(11) 0.035(13) -0.031(19) C48 0.099(16) 0.138(19) 0.22(3) -0.048(19) 0.017(16) 0.026(12) C45 0.118(17) 0.25(3) 0.15(2) 0.053(18) -0.025(15) 0.073(18) _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 N2 1.871(8) . ? Co1 N7 1.888(8) . ? Co1 N5 1.925(7) . ? Co1 N1 1.930(8) . ? Co1 N4 1.934(7) . ? Co1 N8 1.934(7) . ? Cl1 O2 1.436(6) . ? Cl1 O4 1.442(7) . ? Cl1 O1 1.446(6) . ? Cl1 O3 1.454(7) . ? N4 C17 1.331(10) . ? N4 C13 1.380(11) . ? N5 C22 1.333(11) . ? N5 C18 1.369(11) . ? N8 C24 1.345(11) . ? N8 C29 1.424(11) . ? C25 C26 1.346(13) . ? C25 C24 1.427(13) . ? C25 H25 0.9300 . ? C24 C23 1.423(12) . ? C33 C32 1.391(13) . ? C33 C34 1.400(12) . ? C33 H33 0.9300 . ? C29 C34 1.381(12) . ? C29 C30 1.405(12) . ? C30 C31 1.392(13) . ? C30 H30 0.9300 . ? C34 H34 0.9300 . ? C16 C17 1.388(12) . ? C16 C15 1.390(12) . ? C16 H16 0.9300 . ? N1 C7 1.338(12) . ? N1 C1 1.445(12) . ? C12 N2 1.363(12) . ? C12 C11 1.390(14) . ? C12 C7 1.440(13) . ? C17 H17 0.9300 . ? C15 C14 1.356(12) . ? C15 H15 0.9300 . ? C7 C8 1.414(14) . ? C19 C18 1.371(13) . ? C19 C20 1.394(13) . ? C19 H19 0.9300 . ? C22 C21 1.361(12) . ? C22 H22 0.9300 . ? C8 C9 1.352(13) . ? C8 H8 0.9300 . ? N6 N7 1.290(9) . ? N6 C18 1.387(12) . ? C21 C20 1.383(13) . ? C21 H21 0.9300 . ? C11 C10 1.355(13) . ? C11 H11 0.9300 . ? C26 C27 1.418(13) . ? C26 H26 0.9300 . ? C10 C9 1.432(14) . ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? C35 C36 1.482(13) . ? C35 C32 1.517(14) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C20 H20 0.9300 . ? C32 C31 1.397(13) . ? C2 C1 1.387(13) . ? C2 C3 1.391(13) . ? C2 H2 0.9300 . ? C6 C1 1.383(13) . ? C6 C5 1.396(13) . ? C6 H6 0.9300 . ? C31 H31 0.9300 . ? C37 C38 1.502(15) . ? C37 C36 1.504(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C5 C4 1.377(14) . ? C5 H5 0.9300 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C38 C39 1.509(15) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? N3 N2 1.291(10) . ? N3 C13 1.377(11) . ? C13 C14 1.383(13) . ? C14 H14 0.9300 . ? C4 C3 1.364(13) . ? C4 H4 0.9300 . ? C39 C40 1.540(17) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C3 H3 0.9300 . ? C40 C41 1.58(2) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C28 C27 1.372(13) . ? C28 C23 1.407(13) . ? C28 H28 0.9300 . ? C27 H27 0.9300 . ? C43 C44 1.38(2) . ? C43 C42 1.70(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C42 C41 1.40(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? N7 C23 1.368(12) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C46 C48 1.49(2) . ? C46 C45 1.57(2) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C48 C48 1.56(3) 2_557 ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 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 N2 Co1 N7 177.1(4) . . ? N2 Co1 N5 97.6(3) . . ? N7 Co1 N5 80.6(4) . . ? N2 Co1 N1 83.9(4) . . ? N7 Co1 N1 94.0(4) . . ? N5 Co1 N1 92.9(3) . . ? N2 Co1 N4 80.3(4) . . ? N7 Co1 N4 101.8(3) . . ? N5 Co1 N4 89.8(3) . . ? N1 Co1 N4 164.1(4) . . ? N2 Co1 N8 97.7(3) . . ? N7 Co1 N8 84.3(4) . . ? N5 Co1 N8 164.6(3) . . ? N1 Co1 N8 90.9(3) . . ? N4 Co1 N8 90.6(3) . . ? O2 Cl1 O4 110.1(4) . . ? O2 Cl1 O1 109.3(4) . . ? O4 Cl1 O1 109.1(4) . . ? O2 Cl1 O3 110.2(4) . . ? O4 Cl1 O3 109.5(4) . . ? O1 Cl1 O3 108.6(4) . . ? C17 N4 C13 119.4(9) . . ? C17 N4 Co1 129.5(7) . . ? C13 N4 Co1 111.0(6) . . ? C22 N5 C18 119.2(9) . . ? C22 N5 Co1 129.6(7) . . ? C18 N5 Co1 111.2(7) . . ? C24 N8 C29 121.8(8) . . ? C24 N8 Co1 110.7(6) . . ? C29 N8 Co1 125.5(6) . . ? C26 C25 C24 118.7(9) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? N8 C24 C23 118.1(9) . . ? N8 C24 C25 124.6(9) . . ? C23 C24 C25 117.2(9) . . ? C32 C33 C34 122.3(10) . . ? C32 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C34 C29 C30 119.7(9) . . ? C34 C29 N8 120.2(9) . . ? C30 C29 N8 120.1(9) . . ? C31 C30 C29 120.5(9) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C29 C34 C33 119.0(9) . . ? C29 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C17 C16 C15 117.2(9) . . ? C17 C16 H16 121.4 . . ? C15 C16 H16 121.4 . . ? C7 N1 C1 120.1(8) . . ? C7 N1 Co1 111.6(7) . . ? C1 N1 Co1 125.9(7) . . ? N2 C12 C11 127.5(11) . . ? N2 C12 C7 110.9(11) . . ? C11 C12 C7 121.5(12) . . ? N4 C17 C16 122.6(9) . . ? N4 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C14 C15 C16 121.1(9) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? N1 C7 C8 126.3(11) . . ? N1 C7 C12 117.1(11) . . ? C8 C7 C12 116.5(11) . . ? C18 C19 C20 119.0(10) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? N5 C22 C21 122.5(9) . . ? N5 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? C9 C8 C7 120.7(10) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? N7 N6 C18 109.8(8) . . ? N5 C18 C19 120.9(10) . . ? N5 C18 N6 117.9(10) . . ? C19 C18 N6 121.1(10) . . ? C22 C21 C20 119.1(10) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C10 C11 C12 120.5(10) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C25 C26 C27 123.8(10) . . ? C25 C26 H26 118.1 . . ? C27 C26 H26 118.1 . . ? C11 C10 C9 118.7(10) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C8 C9 C10 121.9(10) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C36 C35 C32 115.9(9) . . ? C36 C35 H35A 108.3 . . ? C32 C35 H35A 108.3 . . ? C36 C35 H35B 108.3 . . ? C32 C35 H35B 108.3 . . ? H35A C35 H35B 107.4 . . ? C21 C20 C19 119.1(10) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C33 C32 C31 118.0(10) . . ? C33 C32 C35 124.1(10) . . ? C31 C32 C35 117.9(10) . . ? C1 C2 C3 119.6(10) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C1 C6 C5 119.0(10) . . ? C1 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C1 C2 120.2(10) . . ? C6 C1 N1 119.6(10) . . ? C2 C1 N1 120.0(9) . . ? C30 C31 C32 120.5(10) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C38 C37 C36 113.1(9) . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C4 C5 C6 120.7(10) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C35 C36 C37 114.8(9) . . ? C35 C36 H36A 108.6 . . ? C37 C36 H36A 108.6 . . ? C35 C36 H36B 108.6 . . ? C37 C36 H36B 108.6 . . ? H36A C36 H36B 107.5 . . ? C37 C38 C39 116.5(10) . . ? C37 C38 H38A 108.2 . . ? C39 C38 H38A 108.2 . . ? C37 C38 H38B 108.2 . . ? C39 C38 H38B 108.2 . . ? H38A C38 H38B 107.3 . . ? N2 N3 C13 109.9(8) . . ? N3 C13 N4 117.4(8) . . ? N3 C13 C14 122.6(9) . . ? N4 C13 C14 120.0(10) . . ? C15 C14 C13 119.7(10) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C3 C4 C5 119.9(11) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C38 C39 C40 113.6(11) . . ? C38 C39 H39A 108.8 . . ? C40 C39 H39A 108.8 . . ? C38 C39 H39B 108.8 . . ? C40 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C4 C3 C2 120.5(10) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C39 C40 C41 120.8(13) . . ? C39 C40 H40A 107.1 . . ? C41 C40 H40A 107.1 . . ? C39 C40 H40B 107.1 . . ? C41 C40 H40B 107.1 . . ? H40A C40 H40B 106.8 . . ? C27 C28 C23 117.9(10) . . ? C27 C28 H28 121.1 . . ? C23 C28 H28 121.1 . . ? C28 C27 C26 119.4(10) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C44 C43 C42 109.7(15) . . ? C44 C43 H43A 109.7 . . ? C42 C43 H43A 109.7 . . ? C44 C43 H43B 109.7 . . ? C42 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? C41 C42 C43 111.3(16) . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C42 C41 C40 110.1(14) . . ? C42 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? C42 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.2 . . ? N3 N2 C12 122.5(9) . . ? N3 N2 Co1 121.3(7) . . ? C12 N2 Co1 116.2(8) . . ? N6 N7 C23 124.6(8) . . ? N6 N7 Co1 120.4(6) . . ? C23 N7 Co1 114.7(7) . . ? N7 C23 C28 125.4(10) . . ? N7 C23 C24 111.7(10) . . ? C28 C23 C24 122.9(10) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C48 C46 C45 104.8(16) . . ? C48 C46 H46A 110.8 . . ? C45 C46 H46A 110.8 . . ? C48 C46 H46B 110.8 . . ? C45 C46 H46B 110.8 . . ? H46A C46 H46B 108.9 . . ? C46 C48 C48 111(2) . 2_557 ? C46 C48 H48A 109.4 . . ? C48 C48 H48A 109.4 2_557 . ? C46 C48 H48B 109.4 . . ? C48 C48 H48B 109.4 2_557 . ? H48A C48 H48B 108.0 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 17.78 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.623 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.111