Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_section_title ; Solvent-directed layered Co(II) coordination polymers with unusual solid-state properties: from a nanoporous framework to the dense polythreading 3-D aggregation ; _publ_contact_author ; Miao Du College of Chemistry and Life Science, Tianjin Normal University, Tianjin 300074, P. R. China ; _publ_contact_author_email dumiao@public.tpt.tj.cn _publ_contact_author_name 'Miao Du' loop_ _publ_author_name 'Miao Du' 'Liang-Fu Tang' 'Xiu-Guang Wang' 'Zhi-Hui Zhang' ; Xiao-Jun Zhao ; data_1 _database_code_depnum_ccdc_archive 'CCDC 296384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H57 Co N15 O5' _chemical_formula_weight 983.02 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.457(11) _cell_length_b 25.429(14) _cell_length_c 14.537(8) _cell_angle_alpha 90.00 _cell_angle_beta 122.662(6) _cell_angle_gamma 90.00 _cell_volume 6366(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2380 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 21.39 _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.026 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.793176 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'Apex II 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 16556 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5568 _reflns_number_gt 2971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.1200P)^2^] 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 5568 _refine_ls_number_parameters 346 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.037 _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 0.5000 0.247572(15) 0.2500 0.04380(12) Uani 1 2 d S . . N1 N 0.53025(9) 0.48306(7) -0.15177(13) 0.0592(6) Uani 1 1 d . . . N2 N 0.60900(10) 0.48132(8) -0.07873(15) 0.0699(7) Uani 1 1 d . . . N3 N 0.51539(9) 0.30848(7) 0.15757(12) 0.0492(5) Uani 1 1 d . . . N4 N 0.48349(9) 0.18740(7) 0.34082(12) 0.0493(5) Uani 1 1 d . . . N5 N 0.46864(9) 0.01348(7) 0.65084(12) 0.0487(5) Uani 1 1 d . . . N6 N 0.39093(9) 0.01196(7) 0.57536(12) 0.0520(5) Uani 1 1 d . . . C1 C 0.5000 0.51421(13) -0.2500 0.0640(10) Uani 1 2 d S . . H1A H 0.4589 0.5367 -0.2580 0.077 Uiso 0.50 1 calc PR . . H1B H 0.5411 0.5367 -0.2420 0.077 Uiso 0.50 1 calc PR . . C2 C 0.70157(14) 0.43719(13) 0.0929(2) 0.0961(11) Uani 1 1 d . . . H2A H 0.7372 0.4597 0.0878 0.144 Uiso 1 1 calc R . . H2B H 0.7138 0.4011 0.0893 0.144 Uiso 1 1 calc R . . H2C H 0.7057 0.4434 0.1610 0.144 Uiso 1 1 calc R . . C3 C 0.62000(12) 0.44877(10) -0.00020(18) 0.0663(8) Uani 1 1 d . . . C4 C 0.54744(11) 0.42717(9) -0.02500(16) 0.0569(7) Uani 1 1 d . . . C5 C 0.49187(12) 0.45049(10) -0.12066(17) 0.0603(7) Uani 1 1 d . . . C6 C 0.40641(13) 0.44745(13) -0.1852(2) 0.0896(10) Uani 1 1 d . . . H6A H 0.3885 0.4406 -0.1374 0.134 Uiso 1 1 calc R . . H6B H 0.3898 0.4196 -0.2378 0.134 Uiso 1 1 calc R . . H6C H 0.3852 0.4802 -0.2225 0.134 Uiso 1 1 calc R . . C7 C 0.53602(11) 0.38733(9) 0.03732(16) 0.0546(7) Uani 1 1 d . . . C8 C 0.57921(12) 0.38636(10) 0.15250(16) 0.0621(7) Uani 1 1 d . . . H8 H 0.6155 0.4125 0.1921 0.074 Uiso 1 1 calc R . . C9 C 0.56740(13) 0.34670(10) 0.20569(18) 0.0643(8) Uani 1 1 d . . . H9 H 0.5983 0.3465 0.2816 0.077 Uiso 1 1 calc R . . C10 C 0.47422(13) 0.30879(10) 0.04806(18) 0.0687(8) Uani 1 1 d . . . H10 H 0.4379 0.2823 0.0112 0.082 Uiso 1 1 calc R . . C11 C 0.48312(13) 0.34689(10) -0.01324(19) 0.0691(8) Uani 1 1 d . . . H11 H 0.4531 0.3451 -0.0891 0.083 Uiso 1 1 calc R . . C12 C 0.29931(13) 0.05182(12) 0.3989(2) 0.0791(9) Uani 1 1 d . . . H12A H 0.2698 0.0204 0.3877 0.119 Uiso 1 1 calc R . . H12B H 0.3024 0.0581 0.3361 0.119 Uiso 1 1 calc R . . H12C H 0.2743 0.0811 0.4092 0.119 Uiso 1 1 calc R . . C13 C 0.5000 -0.01811(12) 0.7500 0.0524(10) Uani 1 2 d S . . H13A H 0.4592 -0.0406 0.7428 0.063 Uiso 0.50 1 calc PR . . H13B H 0.5408 -0.0406 0.7572 0.063 Uiso 0.50 1 calc PR . . C14 C 0.59305(12) 0.05353(12) 0.69152(19) 0.0736(9) Uani 1 1 d . . . H14A H 0.6110 0.0456 0.7661 0.110 Uiso 1 1 calc R . . H14B H 0.6057 0.0893 0.6863 0.110 Uiso 1 1 calc R . . H14C H 0.6177 0.0304 0.6670 0.110 Uiso 1 1 calc R . . C15 C 0.50649(11) 0.04615(8) 0.62125(15) 0.0499(6) Uani 1 1 d . . . C16 C 0.45099(11) 0.06823(8) 0.52250(15) 0.0496(6) Uani 1 1 d . . . C17 C 0.37904(11) 0.04541(9) 0.49743(16) 0.0540(7) Uani 1 1 d . . . C18 C 0.46195(11) 0.10819(9) 0.45940(15) 0.0493(6) Uani 1 1 d . . . C19 C 0.52472(11) 0.10829(9) 0.44684(16) 0.0533(7) Uani 1 1 d . . . H19 H 0.5616 0.0817 0.4787 0.064 Uiso 1 1 calc R . . C20 C 0.53304(12) 0.14698(9) 0.38822(16) 0.0544(7) Uani 1 1 d . . . H20 H 0.5754 0.1451 0.3808 0.065 Uiso 1 1 calc R . . C21 C 0.42210(12) 0.18816(10) 0.35185(17) 0.0612(7) Uani 1 1 d . . . H21 H 0.3868 0.2157 0.3200 0.073 Uiso 1 1 calc R . . C22 C 0.40908(12) 0.15010(9) 0.40817(18) 0.0612(7) Uani 1 1 d . . . H22 H 0.3653 0.1521 0.4123 0.073 Uiso 1 1 calc R . . O1 O 0.19824(13) 0.93372(10) 0.41401(17) 0.1210(9) Uani 1 1 d . . . H1 H 0.1740 0.9593 0.4146 0.181 Uiso 1 1 calc R . . O2 O 0.32583(15) 0.92949(12) 0.6419(2) 0.1606(12) Uani 1 1 d . . . H2 H 0.3283 0.9434 0.5930 0.241 Uiso 1 1 calc R . . C24 C 0.2627(2) 0.90282(17) 0.6000(3) 0.1327(16) Uani 1 1 d . . . H24A H 0.2362 0.9170 0.6331 0.159 Uiso 1 1 calc R . . H24B H 0.2792 0.8677 0.6299 0.159 Uiso 1 1 calc R . . C25 C 0.2049(3) 0.89500(18) 0.4916(4) 0.175(2) Uani 1 1 d . . . H25A H 0.1556 0.8934 0.4863 0.210 Uiso 1 1 calc R . . H25B H 0.2132 0.8609 0.4696 0.210 Uiso 1 1 calc R . . O3 O 0.2101(5) 0.2141(4) 0.2320(11) 0.477(8) Uani 0.50 1 d P . . N7 N 0.37928(14) 0.24882(15) 0.1234(3) 0.0528(12) Uani 0.50 1 d PD . . C23 C 0.31347(18) 0.24975(19) 0.0847(4) 0.0593(17) Uani 0.50 1 d PD . . N8 N 0.24027(18) 0.2480(3) 0.0499(3) 0.145(3) Uani 0.50 1 d PD . . N7A N 0.1252(2) 0.25312(17) -0.1351(3) 0.0498(13) Uani 0.50 1 d PD . . C23A C 0.1804(2) 0.2525(2) -0.0492(3) 0.0607(18) Uani 0.50 1 d PD . . 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 0.03037(15) 0.0564(2) 0.03776(16) 0.000 0.01391(13) 0.000 N1 0.0566(9) 0.0617(11) 0.0557(8) -0.0035(8) 0.0280(7) -0.0068(9) N2 0.0611(9) 0.0803(14) 0.0635(9) 0.0002(9) 0.0305(8) -0.0116(10) N3 0.0404(7) 0.0600(11) 0.0437(8) -0.0045(7) 0.0205(6) -0.0043(8) N4 0.0389(7) 0.0599(11) 0.0434(8) 0.0032(7) 0.0186(6) 0.0060(8) N5 0.0472(8) 0.0517(10) 0.0409(7) 0.0030(7) 0.0196(6) 0.0007(8) N6 0.0397(8) 0.0623(11) 0.0406(8) 0.0036(8) 0.0127(6) -0.0049(8) C1 0.0830(17) 0.057(2) 0.0603(15) 0.000 0.0444(13) 0.000 C2 0.0579(13) 0.129(2) 0.0770(15) 0.0179(16) 0.0204(12) -0.0192(16) C3 0.0555(11) 0.0768(16) 0.0646(12) 0.0075(11) 0.0310(9) -0.0060(12) C4 0.0535(10) 0.0646(14) 0.0518(10) 0.0017(10) 0.0278(8) -0.0022(10) C5 0.0547(10) 0.0710(15) 0.0540(10) -0.0016(10) 0.0286(8) -0.0075(11) C6 0.0602(13) 0.114(2) 0.0865(15) 0.0300(15) 0.0340(11) 0.0047(14) C7 0.0460(9) 0.0636(14) 0.0529(10) 0.0017(10) 0.0258(8) -0.0001(10) C8 0.0600(11) 0.0700(15) 0.0562(11) -0.0076(10) 0.0314(9) -0.0151(11) C9 0.0587(11) 0.0737(16) 0.0511(11) -0.0027(11) 0.0234(9) -0.0065(12) C10 0.0627(12) 0.0796(17) 0.0541(11) -0.0007(11) 0.0252(10) -0.0166(12) C11 0.0680(12) 0.0817(17) 0.0466(10) -0.0031(11) 0.0239(9) -0.0141(13) C12 0.0466(11) 0.106(2) 0.0675(13) 0.0256(13) 0.0194(10) -0.0024(13) C13 0.0503(15) 0.0535(18) 0.0395(13) 0.000 0.0151(11) 0.000 C14 0.0444(11) 0.0981(19) 0.0634(12) 0.0093(13) 0.0192(10) -0.0075(12) C15 0.0485(10) 0.0525(13) 0.0446(9) -0.0022(9) 0.0224(8) 0.0016(10) C16 0.0471(9) 0.0540(13) 0.0446(9) 0.0013(9) 0.0227(8) 0.0031(9) C17 0.0435(9) 0.0680(15) 0.0447(10) 0.0031(10) 0.0200(8) -0.0041(10) C18 0.0461(9) 0.0540(12) 0.0434(9) 0.0008(9) 0.0213(8) 0.0014(10) C19 0.0474(10) 0.0534(13) 0.0529(10) 0.0058(9) 0.0229(8) 0.0117(10) C20 0.0467(9) 0.0670(15) 0.0511(10) 0.0050(10) 0.0274(8) 0.0083(10) C21 0.0507(10) 0.0744(15) 0.0636(11) 0.0180(10) 0.0341(8) 0.0149(11) C22 0.0503(9) 0.0727(15) 0.0667(11) 0.0157(11) 0.0356(8) 0.0136(11) O1 0.1225(15) 0.1194(17) 0.0929(12) -0.0104(12) 0.0397(11) 0.0144(14) O2 0.1227(16) 0.182(2) 0.1038(15) 0.0245(15) 0.0133(13) -0.0769(16) C24 0.100(2) 0.163(3) 0.089(2) 0.001(2) 0.0211(18) -0.056(2) C25 0.167(4) 0.112(3) 0.154(4) -0.002(3) 0.026(3) -0.032(3) O3 0.105(5) 0.458(10) 0.569(13) -0.382(9) -0.014(7) 0.025(6) N7 0.0347(13) 0.061(2) 0.0734(18) 0.0083(16) 0.0360(12) 0.0000(16) C23 0.0248(18) 0.069(3) 0.053(2) -0.007(2) 0.0003(19) 0.009(2) N8 0.044(2) 0.292(9) 0.076(3) 0.014(4) 0.018(2) -0.002(4) N7A 0.052(2) 0.056(3) 0.0382(16) 0.0049(17) 0.0218(14) 0.0032(19) C23A 0.027(2) 0.076(4) 0.056(3) -0.011(2) 0.007(2) -0.002(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 Co1 N7 2.140(3) . ? Co1 N7 2.140(3) 2_655 ? Co1 N4 2.163(2) . ? Co1 N4 2.163(2) 2_655 ? Co1 N7A 2.176(4) 7 ? Co1 N7A 2.176(4) 8_556 ? Co1 N3 2.182(2) 2_655 ? Co1 N3 2.182(2) . ? N1 N2 1.371(2) . ? N1 C5 1.375(3) . ? N1 C1 1.448(3) . ? N2 C3 1.327(3) . ? N3 C9 1.327(3) . ? N3 C10 1.340(3) . ? N4 C20 1.343(3) . ? N4 C21 1.349(3) . ? N5 C15 1.354(3) . ? N5 N6 1.360(2) . ? N5 C13 1.462(2) . ? N6 C17 1.330(3) . ? C1 N1 1.448(3) 2_654 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.505(3) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.434(3) . ? C4 C5 1.368(3) . ? C4 C7 1.460(3) . ? C5 C6 1.474(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C11 1.382(3) . ? C7 C8 1.410(3) . ? C8 C9 1.370(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.393(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.489(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N5 1.462(2) 2_656 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.504(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.380(3) . ? C16 C17 1.434(3) . ? C16 C18 1.465(3) . ? C18 C19 1.391(3) . ? C18 C22 1.411(3) . ? C19 C20 1.371(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.383(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? O1 C25 1.447(6) . ? O1 H1 0.8200 . ? O2 C24 1.284(4) . ? O2 H2 0.8200 . ? C24 C25 1.381(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? N7 N7A 0.238(8) 7 ? N7 C23A 1.111(4) 7 ? N7 C23 1.145(4) . ? C23 C23A 0.597(8) 7 ? C23 N7A 1.060(5) 7 ? C23 N8 1.297(5) . ? C23 N8 1.649(6) 7 ? N8 C23A 1.298(5) . ? N8 C23A 1.628(7) 7 ? N8 C23 1.649(6) 7 ? N8 N8 1.701(11) 7 ? N7A N7 0.238(8) 7 ? N7A C23 1.060(5) 7 ? N7A C23A 1.146(4) . ? N7A Co1 2.176(4) 7 ? C23A C23 0.597(8) 7 ? C23A N7 1.111(4) 7 ? C23A N8 1.628(7) 7 ? 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 N7 Co1 N7 178.3(2) . 2_655 ? N7 Co1 N4 92.71(12) . . ? N7 Co1 N4 88.49(12) 2_655 . ? N7 Co1 N4 88.49(12) . 2_655 ? N7 Co1 N4 92.71(12) 2_655 2_655 ? N4 Co1 N4 89.97(11) . 2_655 ? N7 Co1 N7A 6.2(2) . 7 ? N7 Co1 N7A 173.9(2) 2_655 7 ? N4 Co1 N7A 87.47(13) . 7 ? N4 Co1 N7A 91.87(13) 2_655 7 ? N7 Co1 N7A 173.9(2) . 8_556 ? N7 Co1 N7A 6.2(2) 2_655 8_556 ? N4 Co1 N7A 91.87(13) . 8_556 ? N4 Co1 N7A 87.47(13) 2_655 8_556 ? N7A Co1 N7A 179.1(2) 7 8_556 ? N7 Co1 N3 92.05(12) . 2_655 ? N7 Co1 N3 86.74(12) 2_655 2_655 ? N4 Co1 N3 90.25(8) . 2_655 ? N4 Co1 N3 179.41(6) 2_655 2_655 ? N7A Co1 N3 88.69(13) 7 2_655 ? N7A Co1 N3 91.97(13) 8_556 2_655 ? N7 Co1 N3 86.74(12) . . ? N7 Co1 N3 92.05(12) 2_655 . ? N4 Co1 N3 179.41(6) . . ? N4 Co1 N3 90.25(8) 2_655 . ? N7A Co1 N3 91.97(13) 7 . ? N7A Co1 N3 88.69(13) 8_556 . ? N3 Co1 N3 89.54(10) 2_655 . ? N2 N1 C5 111.53(17) . . ? N2 N1 C1 118.68(17) . . ? C5 N1 C1 129.65(15) . . ? C3 N2 N1 105.61(19) . . ? C9 N3 C10 115.6(2) . . ? C9 N3 Co1 122.42(15) . . ? C10 N3 Co1 121.91(15) . . ? C20 N4 C21 116.3(2) . . ? C20 N4 Co1 122.08(16) . . ? C21 N4 Co1 121.62(14) . . ? C15 N5 N6 112.39(16) . . ? C15 N5 C13 128.94(14) . . ? N6 N5 C13 118.67(16) . . ? C17 N6 N5 105.42(17) . . ? N1 C1 N1 113.7(3) 2_654 . ? N1 C1 H1A 108.8 2_654 . ? N1 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 2_654 . ? N1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 110.52(18) . . ? N2 C3 C2 119.1(2) . . ? C4 C3 C2 130.2(2) . . ? C5 C4 C3 105.6(2) . . ? C5 C4 C7 127.5(2) . . ? C3 C4 C7 126.90(17) . . ? C4 C5 N1 106.66(19) . . ? C4 C5 C6 132.4(2) . . ? N1 C5 C6 120.9(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C11 C7 C8 115.3(2) . . ? C11 C7 C4 121.88(19) . . ? C8 C7 C4 122.79(19) . . ? C9 C8 C7 119.7(2) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? N3 C9 C8 125.2(2) . . ? N3 C9 H9 117.4 . . ? C8 C9 H9 117.4 . . ? N3 C10 C11 123.3(2) . . ? N3 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C7 C11 C10 120.8(2) . . ? C7 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C17 C12 H12A 109.5 . . ? C17 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C17 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 N5 113.3(2) 2_656 . ? N5 C13 H13A 108.9 2_656 . ? N5 C13 H13A 108.9 . . ? N5 C13 H13B 108.9 2_656 . ? N5 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 C16 106.82(18) . . ? N5 C15 C14 121.74(18) . . ? C16 C15 C14 131.4(2) . . ? C15 C16 C17 104.77(19) . . ? C15 C16 C18 127.97(19) . . ? C17 C16 C18 127.19(16) . . ? N6 C17 C16 110.58(16) . . ? N6 C17 C12 119.4(2) . . ? C16 C17 C12 129.9(2) . . ? C19 C18 C22 115.4(2) . . ? C19 C18 C16 123.20(19) . . ? C22 C18 C16 121.4(2) . . ? C20 C19 C18 121.1(2) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? N4 C20 C19 123.7(2) . . ? N4 C20 H20 118.1 . . ? C19 C20 H20 118.1 . . ? N4 C21 C22 123.3(2) . . ? N4 C21 H21 118.3 . . ? C22 C21 H21 118.3 . . ? C21 C22 C18 120.2(2) . . ? C21 C22 H22 119.9 . . ? C18 C22 H22 119.9 . . ? C25 O1 H1 109.5 . . ? C24 O2 H2 109.5 . . ? O2 C24 C25 129.8(4) . . ? O2 C24 H24A 104.8 . . ? C25 C24 H24A 104.8 . . ? O2 C24 H24B 104.8 . . ? C25 C24 H24B 104.8 . . ? H24A C24 H24B 105.8 . . ? C24 C25 O1 117.0(4) . . ? C24 C25 H25A 108.1 . . ? O1 C25 H25A 108.1 . . ? C24 C25 H25B 108.1 . . ? O1 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? N7A N7 C23A 92.4(11) 7 7 ? N7A N7 C23 63.3(11) 7 . ? N7A N7 Co1 95.4(11) 7 . ? C23A N7 Co1 171.0(5) 7 . ? C23 N7 Co1 158.1(4) . . ? C23A C23 N7A 82.4(6) 7 7 ? C23A C23 N7 71.5(6) 7 . ? C23A C23 N8 113.4(6) 7 . ? N7A C23 N8 162.5(6) 7 . ? N7 C23 N8 173.9(6) . . ? C23A C23 N8 45.0(5) 7 7 ? N7A C23 N8 127.2(6) 7 7 ? N7 C23 N8 116.0(5) . 7 ? N8 C23 N8 69.4(4) . 7 ? C23 N8 C23A 129.0(5) . . ? C23A N8 C23A 109.9(4) . 7 ? C23 N8 C23 110.6(4) . 7 ? C23A N8 C23 91.2(4) 7 7 ? C23 N8 N8 65.1(3) . 7 ? C23A N8 N8 64.1(4) . 7 ? C23A N8 N8 45.8(2) 7 7 ? C23 N8 N8 45.5(2) 7 7 ? N7 N7A C23 105.2(11) 7 7 ? N7 N7A C23A 75.7(10) 7 . ? N7 N7A Co1 78.3(11) 7 7 ? C23 N7A Co1 173.6(5) 7 7 ? C23A N7A Co1 153.6(5) . 7 ? C23 C23A N7 77.9(5) 7 7 ? C23 C23A N7A 66.5(5) 7 . ? C23 C23A N8 116.0(7) 7 . ? N7 C23A N8 163.7(7) 7 . ? N7A C23A N8 174.6(7) . . ? C23 C23A N8 47.0(5) 7 7 ? N7 C23A N8 124.7(5) 7 7 ? N7A C23A N8 113.1(5) . 7 ? N8 C23A N8 70.1(4) . 7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 N2 C3 -1.6(3) . . . . ? C1 N1 N2 C3 -177.6(2) . . . . ? N7 Co1 N3 C9 145.8(2) . . . . ? N7 Co1 N3 C9 -33.0(2) 2_655 . . . ? N4 Co1 N3 C9 -125.69(19) 2_655 . . . ? N7A Co1 N3 C9 142.4(2) 7 . . . ? N7A Co1 N3 C9 -38.2(2) 8_556 . . . ? N3 Co1 N3 C9 53.76(17) 2_655 . . . ? N7 Co1 N3 C10 -36.1(2) . . . . ? N7 Co1 N3 C10 145.1(2) 2_655 . . . ? N4 Co1 N3 C10 52.39(19) 2_655 . . . ? N7A Co1 N3 C10 -39.5(2) 7 . . . ? N7A Co1 N3 C10 139.9(2) 8_556 . . . ? N3 Co1 N3 C10 -128.2(2) 2_655 . . . ? N7 Co1 N4 C20 137.93(19) . . . . ? N7 Co1 N4 C20 -43.27(19) 2_655 . . . ? N4 Co1 N4 C20 49.44(14) 2_655 . . . ? N7A Co1 N4 C20 141.32(19) 7 . . . ? N7A Co1 N4 C20 -38.03(19) 8_556 . . . ? N3 Co1 N4 C20 -130.01(15) 2_655 . . . ? N7 Co1 N4 C21 -41.29(19) . . . . ? N7 Co1 N4 C21 137.51(19) 2_655 . . . ? N4 Co1 N4 C21 -129.78(16) 2_655 . . . ? N7A Co1 N4 C21 -37.90(19) 7 . . . ? N7A Co1 N4 C21 142.75(19) 8_556 . . . ? N3 Co1 N4 C21 50.77(15) 2_655 . . . ? C13 N5 N6 C17 177.76(19) . . . . ? N2 N1 C1 N1 108.3(2) . . . 2_654 ? C5 N1 C1 N1 -66.9(2) . . . 2_654 ? N1 N2 C3 C4 2.6(3) . . . . ? N1 N2 C3 C2 178.7(2) . . . . ? N2 C3 C4 C5 -2.6(3) . . . . ? C2 C3 C4 C5 -178.2(3) . . . . ? N2 C3 C4 C7 175.5(2) . . . . ? C3 C4 C5 N1 1.5(3) . . . . ? C7 C4 C5 N1 -176.6(2) . . . . ? C3 C4 C5 C6 -176.0(3) . . . . ? C7 C4 C5 C6 5.8(5) . . . . ? C1 N1 C5 C4 175.4(2) . . . . ? N2 N1 C5 C6 177.9(2) . . . . ? C1 N1 C5 C6 -6.7(4) . . . . ? C5 C4 C7 C11 39.3(4) . . . . ? C3 C4 C7 C11 -138.5(3) . . . . ? C5 C4 C7 C8 -142.5(3) . . . . ? C3 C4 C7 C8 39.7(4) . . . . ? C11 C7 C8 C9 0.7(4) . . . . ? C4 C7 C8 C9 -177.6(2) . . . . ? C10 N3 C9 C8 2.7(4) . . . . ? Co1 N3 C9 C8 -179.1(2) . . . . ? C7 C8 C9 N3 -2.4(4) . . . . ? C9 N3 C10 C11 -1.3(4) . . . . ? Co1 N3 C10 C11 -179.5(2) . . . . ? C8 C7 C11 C10 0.5(4) . . . . ? C4 C7 C11 C10 178.9(2) . . . . ? N3 C10 C11 C7 -0.2(4) . . . . ? C15 N5 C13 N5 65.64(19) . . . 2_656 ? N6 N5 C13 N5 -113.48(19) . . . 2_656 ? N6 N5 C15 C16 1.3(2) . . . . ? C13 N5 C15 C16 -177.8(2) . . . . ? N6 N5 C15 C14 -179.2(2) . . . . ? C13 N5 C15 C14 1.7(4) . . . . ? N5 C15 C16 C17 -0.6(2) . . . . ? N5 C15 C16 C18 176.5(2) . . . . ? C14 C15 C16 C18 -2.9(4) . . . . ? N5 N6 C17 C16 1.1(2) . . . . ? N5 N6 C17 C12 177.7(2) . . . . ? C15 C16 C17 N6 -0.3(3) . . . . ? C18 C16 C17 N6 -177.5(2) . . . . ? C15 C16 C17 C12 -176.5(3) . . . . ? C18 C16 C17 C12 6.3(4) . . . . ? C15 C16 C18 C19 40.8(3) . . . . ? C17 C16 C18 C19 -142.6(2) . . . . ? C15 C16 C18 C22 -138.2(2) . . . . ? C17 C16 C18 C22 38.4(3) . . . . ? C16 C18 C19 C20 -179.07(19) . . . . ? C21 N4 C20 C19 -1.1(3) . . . . ? Co1 N4 C20 C19 179.65(15) . . . . ? C18 C19 C20 N4 1.1(3) . . . . ? Co1 N4 C21 C22 179.22(16) . . . . ? N4 C21 C22 C18 1.1(3) . . . . ? C19 C18 C22 C21 -1.0(3) . . . . ? C16 C18 C22 C21 178.04(19) . . . . ? O2 C24 C25 O1 -22.7(8) . . . . ? N4 Co1 N7 N7A 32.9(17) . . . 7 ? N4 Co1 N7 N7A 122.8(17) 2_655 . . 7 ? N3 Co1 N7 N7A -57.4(17) 2_655 . . 7 ? N3 Co1 N7 N7A -146.9(17) . . . 7 ? N4 Co1 N7 C23 46.1(10) . . . . ? N4 Co1 N7 C23 136.0(10) 2_655 . . . ? N7A Co1 N7 C23 13.2(13) 7 . . . ? N3 Co1 N7 C23 -44.2(10) 2_655 . . . ? N3 Co1 N7 C23 -133.7(10) . . . . ? Co1 N7 C23 C23A -175.2(10) . . . 7 ? Co1 N7 C23 N7A -14.8(15) . . . 7 ? N7A N7 C23 N8 -167.6(18) 7 . . 7 ? C23A N7 C23 N8 -7.2(7) 7 . . 7 ? Co1 N7 C23 N8 177.7(8) . . . 7 ? C23A C23 N8 C23A -15.3(16) 7 . . . ? N7A C23 N8 C23A -168.4(17) 7 . . . ? N8 C23 N8 C23A -5.4(6) 7 . . . ? N8 C23 N8 C23A 9.9(10) 7 . . 7 ? C23A C23 N8 C23 -9.9(10) 7 . . 7 ? C23A C23 N8 N8 -9.9(10) 7 . . 7 ? N7 N7A C23A C23 161.4(19) 7 . . 7 ? Co1 N7A C23A C23 171.0(9) 7 . . 7 ? C23 N7A C23A N7 -161.4(19) 7 . . 7 ? Co1 N7A C23A N7 9.7(13) 7 . . 7 ? N7 N7A C23A N8 167.6(17) 7 . . 7 ? C23 N7A C23A N8 6.3(7) 7 . . 7 ? Co1 N7A C23A N8 177.3(7) 7 . . 7 ? C23 N8 C23A C23 15.6(16) . . . 7 ? C23A N8 C23A C23 10.2(11) 7 . . 7 ? N8 N8 C23A C23 10.2(11) 7 . . 7 ? C23 N8 C23A N7 162.1(19) . . . 7 ? C23 N8 C23A N8 5.4(6) . . . 7 ? C23 N8 C23A N8 -10.2(11) 7 . . 7 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.483 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.113 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 296385' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H44 Co N18' _chemical_formula_weight 907.92 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 22.923(3) _cell_length_b 24.682(4) _cell_length_c 8.3340(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4715.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2674 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 22.12 _exptl_crystal_description Prism _exptl_crystal_colour Pale-pink _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.877164 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'APEX II 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 23766 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4162 _reflns_number_gt 1898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0626P)^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 SHELXL _refine_ls_extinction_coef 0.0020(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4162 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1659 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.0000 0.26055(3) -0.2500 0.0445(3) Uani 1 2 d S . . N1 N 0.04719(16) 0.32010(14) -0.1119(5) 0.0471(11) Uani 1 1 d . . . N2 N 0.20091(16) 0.48352(15) 0.3146(4) 0.0421(10) Uani 1 1 d . . . N3 N 0.16698(16) 0.52331(13) 0.2502(5) 0.0434(9) Uani 1 1 d . . . N4 N 0.04676(16) 0.19801(14) -0.1195(5) 0.0469(11) Uani 1 1 d . . . N5 N 0.20313(14) 0.02120(14) 0.2483(5) 0.0407(9) Uani 1 1 d . . . N6 N 0.16720(16) -0.01522(14) 0.1750(4) 0.0420(10) Uani 1 1 d . . . N7 N 0.06612(19) 0.26044(17) -0.4224(5) 0.0569(12) Uani 1 1 d . . . N8 N 0.1556(3) 0.2397(3) -0.5653(9) 0.151(3) Uani 1 1 d . . . N9 N 0.2562(3) 0.2575(2) -0.5066(10) 0.133(2) Uani 1 1 d . . . C1 C 0.1068(2) 0.39822(17) 0.0736(5) 0.0415(12) Uani 1 1 d . . . C2 C 0.1351(2) 0.35509(17) 0.0017(6) 0.0490(13) Uani 1 1 d . . . H2 H 0.1752 0.3511 0.0145 0.059 Uiso 1 1 calc R . . C3 C 0.1047(2) 0.31825(18) -0.0880(6) 0.0505(13) Uani 1 1 d . . . H3 H 0.1255 0.2901 -0.1354 0.061 Uiso 1 1 calc R . . C4 C 0.0192(2) 0.36101(18) -0.0377(6) 0.0544(15) Uani 1 1 d . . . H4 H -0.0212 0.3631 -0.0482 0.065 Uiso 1 1 calc R . . C5 C 0.0468(2) 0.39969(18) 0.0523(6) 0.0516(14) Uani 1 1 d . . . H5 H 0.0251 0.4272 0.0996 0.062 Uiso 1 1 calc R . . C6 C 0.13806(19) 0.44030(17) 0.1640(5) 0.0385(12) Uani 1 1 d . . . C7 C 0.1282(2) 0.49690(18) 0.1605(5) 0.0407(12) Uani 1 1 d . . . C8 C 0.0833(2) 0.52914(18) 0.0740(6) 0.0566(15) Uani 1 1 d . . . H8A H 0.0477 0.5292 0.1347 0.085 Uiso 1 1 calc R . . H8B H 0.0763 0.5133 -0.0295 0.085 Uiso 1 1 calc R . . H8C H 0.0969 0.5657 0.0608 0.085 Uiso 1 1 calc R . . C9 C 0.18545(19) 0.43324(17) 0.2649(6) 0.0430(12) Uani 1 1 d . . . C10 C 0.2151(2) 0.38325(17) 0.3256(6) 0.0621(15) Uani 1 1 d . . . H10A H 0.2535 0.3809 0.2804 0.093 Uiso 1 1 calc R . . H10B H 0.1929 0.3519 0.2950 0.093 Uiso 1 1 calc R . . H10C H 0.2179 0.3848 0.4405 0.093 Uiso 1 1 calc R . . C11 C 0.2500 0.5000 0.4118(8) 0.0483(18) Uani 1 2 d S . . H11A H 0.2616 0.4701 0.4803 0.058 Uiso 0.50 1 calc PR . . H11B H 0.2384 0.5299 0.4803 0.058 Uiso 0.50 1 calc PR . . C12 C 0.1097(2) 0.11555(18) 0.0369(6) 0.0458(13) Uani 1 1 d . . . C13 C 0.0861(2) 0.15820(19) 0.1201(6) 0.0564(15) Uani 1 1 d . . . H13 H 0.0909 0.1604 0.2307 0.068 Uiso 1 1 calc R . . C14 C 0.0549(2) 0.1983(2) 0.0388(7) 0.0596(15) Uani 1 1 d . . . H14 H 0.0391 0.2266 0.0981 0.072 Uiso 1 1 calc R . . C15 C 0.0704(2) 0.15701(18) -0.1993(6) 0.0524(14) Uani 1 1 d . . . H15 H 0.0658 0.1561 -0.3101 0.063 Uiso 1 1 calc R . . C16 C 0.1016(2) 0.11565(18) -0.1277(6) 0.0505(14) Uani 1 1 d . . . H16 H 0.1172 0.0879 -0.1899 0.061 Uiso 1 1 calc R . . C17 C 0.1420(2) 0.07056(17) 0.1135(6) 0.0428(12) Uani 1 1 d . . . C18 C 0.1889(2) 0.07306(17) 0.2156(6) 0.0449(13) Uani 1 1 d . . . C19 C 0.2225(2) 0.12072(17) 0.2770(6) 0.0635(16) Uani 1 1 d . . . H19A H 0.2175 0.1235 0.3911 0.095 Uiso 1 1 calc R . . H19B H 0.2084 0.1532 0.2267 0.095 Uiso 1 1 calc R . . H19C H 0.2631 0.1161 0.2527 0.095 Uiso 1 1 calc R . . C20 C 0.12997(19) 0.01459(18) 0.0926(6) 0.0419(12) Uani 1 1 d . . . C21 C 0.0811(2) -0.01228(19) 0.0048(6) 0.0583(15) Uani 1 1 d . . . H21A H 0.0959 -0.0289 -0.0912 0.087 Uiso 1 1 calc R . . H21B H 0.0522 0.0142 -0.0230 0.087 Uiso 1 1 calc R . . H21C H 0.0639 -0.0395 0.0720 0.087 Uiso 1 1 calc R . . C22 C 0.2500 0.0000 0.3458(8) 0.0424(17) Uani 1 2 d S . . H22A H 0.2350 -0.0286 0.4143 0.051 Uiso 0.50 1 calc PR . . H22B H 0.2650 0.0286 0.4143 0.051 Uiso 0.50 1 calc PR . . C23 C 0.1098(3) 0.2526(2) -0.4828(8) 0.0680(17) Uani 1 1 d . . . C24 C 0.2091(3) 0.2502(2) -0.5245(9) 0.088(2) 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 Co1 0.0463(6) 0.0276(4) 0.0595(6) 0.000 -0.0109(5) 0.000 N1 0.042(3) 0.037(2) 0.062(3) -0.006(2) -0.011(2) 0.0061(19) N2 0.041(3) 0.045(2) 0.041(3) -0.003(2) -0.0063(19) -0.009(2) N3 0.043(2) 0.040(2) 0.047(2) -0.008(2) 0.001(2) -0.0022(18) N4 0.054(3) 0.032(2) 0.054(3) -0.006(2) -0.007(2) 0.0096(19) N5 0.035(2) 0.041(2) 0.046(2) 0.000(2) -0.005(2) 0.0087(17) N6 0.039(2) 0.042(2) 0.045(2) 0.002(2) -0.001(2) 0.002(2) N7 0.051(3) 0.051(3) 0.068(3) 0.000(2) -0.003(2) -0.001(2) N8 0.072(4) 0.208(8) 0.173(7) -0.098(6) 0.038(5) -0.024(5) N9 0.073(4) 0.137(5) 0.189(7) 0.027(5) 0.002(5) -0.018(4) C1 0.043(3) 0.039(3) 0.043(3) -0.002(2) -0.009(3) 0.001(2) C2 0.035(3) 0.042(3) 0.071(4) -0.008(3) -0.012(3) 0.000(2) C3 0.050(3) 0.040(3) 0.061(4) -0.009(3) -0.007(3) 0.003(2) C4 0.041(3) 0.042(3) 0.080(4) -0.012(3) -0.008(3) 0.004(2) C5 0.046(3) 0.038(3) 0.071(4) -0.008(3) -0.007(3) 0.007(2) C6 0.040(3) 0.035(3) 0.040(3) 0.002(2) -0.002(2) -0.001(2) C7 0.041(3) 0.039(3) 0.041(3) -0.005(2) 0.006(2) -0.001(2) C8 0.052(3) 0.055(3) 0.062(4) 0.002(3) -0.009(3) 0.010(3) C9 0.045(3) 0.040(3) 0.045(3) 0.001(3) -0.001(3) -0.005(2) C10 0.066(4) 0.050(3) 0.070(4) 0.012(3) -0.022(3) -0.001(3) C11 0.054(5) 0.055(4) 0.036(4) 0.000 0.000 -0.010(4) C12 0.048(3) 0.037(3) 0.052(3) -0.001(3) -0.004(3) 0.010(2) C13 0.071(4) 0.054(3) 0.044(3) 0.000(3) -0.004(3) 0.023(3) C14 0.071(4) 0.052(3) 0.057(4) -0.010(3) -0.009(3) 0.019(3) C15 0.067(4) 0.037(3) 0.053(4) -0.004(3) -0.012(3) 0.010(2) C16 0.064(4) 0.039(3) 0.048(4) -0.004(3) -0.001(3) 0.019(3) C17 0.045(3) 0.035(3) 0.048(3) 0.000(2) 0.004(3) 0.010(2) C18 0.048(3) 0.036(3) 0.051(4) -0.004(2) 0.002(3) 0.013(2) C19 0.069(4) 0.045(3) 0.076(4) -0.015(3) -0.014(3) 0.007(3) C20 0.032(3) 0.042(3) 0.051(3) 0.002(2) 0.002(2) 0.003(2) C21 0.041(3) 0.067(4) 0.067(4) 0.010(3) -0.005(3) -0.003(3) C22 0.045(4) 0.042(4) 0.040(4) 0.000 0.000 0.012(3) C23 0.067(4) 0.058(4) 0.079(5) -0.010(3) -0.004(4) -0.011(3) C24 0.066(5) 0.064(4) 0.134(6) -0.002(4) 0.015(5) -0.014(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 Co1 N7 2.088(5) . ? Co1 N7 2.088(5) 4_554 ? Co1 N1 2.157(4) . ? Co1 N1 2.157(4) 4_554 ? Co1 N4 2.171(4) 4_554 ? Co1 N4 2.171(4) . ? N1 C3 1.335(5) . ? N1 C4 1.347(5) . ? N2 C9 1.356(5) . ? N2 N3 1.363(5) . ? N2 C11 1.445(5) . ? N3 C7 1.332(5) . ? N4 C15 1.327(5) . ? N4 C14 1.333(6) . ? N5 C18 1.349(5) . ? N5 N6 1.364(5) . ? N5 C22 1.445(5) . ? N6 C20 1.320(5) . ? N7 C23 1.137(6) . ? N8 C23 1.294(8) . ? N8 C24 1.299(9) . ? N9 C24 1.104(7) . ? C1 C2 1.383(6) . ? C1 C5 1.388(6) . ? C1 C6 1.470(6) . ? C2 C3 1.368(6) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.369(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C9 1.385(6) . ? C6 C7 1.416(6) . ? C7 C8 1.487(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.496(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.445(5) 2_565 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.371(6) . ? C12 C16 1.384(6) . ? C12 C17 1.480(6) . ? C13 C14 1.396(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.382(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.372(6) . ? C17 C20 1.419(6) . ? C18 C19 1.496(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.493(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N5 1.445(5) 2 ? C22 H22A 0.9700 . ? C22 H22B 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 N7 Co1 N7 179.9(2) . 4_554 ? N7 Co1 N1 90.23(15) . . ? N7 Co1 N1 89.87(15) 4_554 . ? N7 Co1 N1 89.87(15) . 4_554 ? N7 Co1 N1 90.23(15) 4_554 4_554 ? N1 Co1 N1 94.1(2) . 4_554 ? N7 Co1 N4 90.74(16) . 4_554 ? N7 Co1 N4 89.15(16) 4_554 4_554 ? N1 Co1 N4 177.43(15) . 4_554 ? N1 Co1 N4 88.26(14) 4_554 4_554 ? N7 Co1 N4 89.15(16) . . ? N7 Co1 N4 90.74(16) 4_554 . ? N1 Co1 N4 88.26(14) . . ? N1 Co1 N4 177.43(15) 4_554 . ? N4 Co1 N4 89.4(2) 4_554 . ? C3 N1 C4 115.3(4) . . ? C3 N1 Co1 123.5(3) . . ? C4 N1 Co1 121.1(3) . . ? C9 N2 N3 113.0(4) . . ? C9 N2 C11 129.2(4) . . ? N3 N2 C11 117.6(3) . . ? C7 N3 N2 104.5(3) . . ? C15 N4 C14 116.3(4) . . ? C15 N4 Co1 119.6(3) . . ? C14 N4 Co1 124.2(3) . . ? C18 N5 N6 112.9(4) . . ? C18 N5 C22 129.6(4) . . ? N6 N5 C22 117.5(3) . . ? C20 N6 N5 104.8(3) . . ? C23 N7 Co1 160.7(5) . . ? C23 N8 C24 125.3(7) . . ? C2 C1 C5 115.4(4) . . ? C2 C1 C6 122.6(4) . . ? C5 C1 C6 122.0(4) . . ? C3 C2 C1 120.7(5) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? N1 C3 C2 124.2(4) . . ? N1 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? N1 C4 C5 123.6(5) . . ? N1 C4 H4 118.2 . . ? C5 C4 H4 118.2 . . ? C4 C5 C1 120.7(4) . . ? C4 C5 H5 119.7 . . ? C1 C5 H5 119.7 . . ? C9 C6 C7 105.2(4) . . ? C9 C6 C1 127.2(4) . . ? C7 C6 C1 127.5(4) . . ? N3 C7 C6 111.3(4) . . ? N3 C7 C8 118.2(4) . . ? C6 C7 C8 130.5(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C6 106.0(4) . . ? N2 C9 C10 122.2(4) . . ? C6 C9 C10 131.7(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 N2 111.8(5) . 2_565 ? N2 C11 H11A 109.3 . . ? N2 C11 H11A 109.3 2_565 . ? N2 C11 H11B 109.3 . . ? N2 C11 H11B 109.3 2_565 . ? H11A C11 H11B 107.9 . . ? C13 C12 C16 116.6(4) . . ? C13 C12 C17 123.7(5) . . ? C16 C12 C17 119.7(4) . . ? C12 C13 C14 120.0(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? N4 C14 C13 123.3(5) . . ? N4 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? N4 C15 C16 124.0(5) . . ? N4 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? C15 C16 C12 119.9(4) . . ? C15 C16 H16 120.1 . . ? C12 C16 H16 120.1 . . ? C18 C17 C20 105.8(4) . . ? C18 C17 C12 128.8(4) . . ? C20 C17 C12 125.5(5) . . ? N5 C18 C17 105.8(4) . . ? N5 C18 C19 123.5(4) . . ? C17 C18 C19 130.6(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N6 C20 C17 110.7(4) . . ? N6 C20 C21 119.5(4) . . ? C17 C20 C21 129.7(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 N5 111.6(5) . 2 ? N5 C22 H22A 109.3 . . ? N5 C22 H22A 109.3 2 . ? N5 C22 H22B 109.3 . . ? N5 C22 H22B 109.3 2 . ? H22A C22 H22B 108.0 . . ? N7 C23 N8 172.3(7) . . ? N9 C24 N8 172.2(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Co1 N1 C3 -42.3(4) . . . . ? N7 Co1 N1 C3 137.6(4) 4_554 . . . ? N1 Co1 N1 C3 -132.2(4) 4_554 . . . ? N4 Co1 N1 C3 46.8(4) . . . . ? N7 Co1 N1 C4 140.5(4) . . . . ? N7 Co1 N1 C4 -39.6(4) 4_554 . . . ? N1 Co1 N1 C4 50.6(3) 4_554 . . . ? N4 Co1 N1 C4 -130.4(4) . . . . ? C9 N2 N3 C7 1.5(5) . . . . ? C11 N2 N3 C7 176.3(4) . . . . ? N7 Co1 N4 C15 -43.1(4) . . . . ? N7 Co1 N4 C15 136.8(4) 4_554 . . . ? N1 Co1 N4 C15 -133.3(4) . . . . ? N4 Co1 N4 C15 47.7(3) 4_554 . . . ? N7 Co1 N4 C14 135.2(4) . . . . ? N7 Co1 N4 C14 -44.9(4) 4_554 . . . ? N1 Co1 N4 C14 45.0(4) . . . . ? N4 Co1 N4 C14 -134.0(5) 4_554 . . . ? C18 N5 N6 C20 0.9(5) . . . . ? C22 N5 N6 C20 -178.6(4) . . . . ? N1 Co1 N7 C23 73.7(13) . . . . ? N1 Co1 N7 C23 167.9(13) 4_554 . . . ? N4 Co1 N7 C23 -103.9(14) 4_554 . . . ? N4 Co1 N7 C23 -14.5(13) . . . . ? C5 C1 C2 C3 2.2(7) . . . . ? C6 C1 C2 C3 -176.8(4) . . . . ? C4 N1 C3 C2 -1.4(7) . . . . ? Co1 N1 C3 C2 -178.7(4) . . . . ? C1 C2 C3 N1 -0.8(8) . . . . ? C3 N1 C4 C5 2.1(7) . . . . ? Co1 N1 C4 C5 179.5(4) . . . . ? N1 C4 C5 C1 -0.7(8) . . . . ? C2 C1 C5 C4 -1.4(7) . . . . ? C6 C1 C5 C4 177.5(5) . . . . ? C2 C1 C6 C9 -38.3(7) . . . . ? C5 C1 C6 C9 142.8(5) . . . . ? C2 C1 C6 C7 138.2(5) . . . . ? C5 C1 C6 C7 -40.7(7) . . . . ? N2 N3 C7 C6 -1.5(5) . . . . ? N2 N3 C7 C8 179.1(4) . . . . ? C9 C6 C7 N3 0.9(5) . . . . ? C1 C6 C7 N3 -176.1(4) . . . . ? C9 C6 C7 C8 -179.7(5) . . . . ? C1 C6 C7 C8 3.3(8) . . . . ? N3 N2 C9 C6 -0.9(5) . . . . ? C11 N2 C9 C6 -175.0(4) . . . . ? N3 N2 C9 C10 -177.4(4) . . . . ? C11 N2 C9 C10 8.5(7) . . . . ? C7 C6 C9 N2 0.0(5) . . . . ? C1 C6 C9 N2 177.1(4) . . . . ? C7 C6 C9 C10 176.0(5) . . . . ? C1 C6 C9 C10 -6.9(9) . . . . ? C9 N2 C11 N2 94.4(5) . . . 2_565 ? N3 N2 C11 N2 -79.4(3) . . . 2_565 ? C16 C12 C13 C14 1.2(8) . . . . ? C17 C12 C13 C14 -178.4(5) . . . . ? C15 N4 C14 C13 -0.4(8) . . . . ? Co1 N4 C14 C13 -178.7(4) . . . . ? C12 C13 C14 N4 -0.6(8) . . . . ? C14 N4 C15 C16 0.7(7) . . . . ? Co1 N4 C15 C16 179.2(4) . . . . ? N4 C15 C16 C12 -0.1(8) . . . . ? C13 C12 C16 C15 -0.9(8) . . . . ? C17 C12 C16 C15 178.7(4) . . . . ? C13 C12 C17 C18 -53.3(8) . . . . ? C16 C12 C17 C18 127.1(6) . . . . ? C13 C12 C17 C20 127.3(6) . . . . ? C16 C12 C17 C20 -52.3(7) . . . . ? N6 N5 C18 C17 -1.2(5) . . . . ? C22 N5 C18 C17 178.2(4) . . . . ? N6 N5 C18 C19 -178.1(4) . . . . ? C22 N5 C18 C19 1.4(8) . . . . ? C20 C17 C18 N5 1.0(5) . . . . ? C12 C17 C18 N5 -178.5(4) . . . . ? C20 C17 C18 C19 177.6(5) . . . . ? C12 C17 C18 C19 -2.0(9) . . . . ? N5 N6 C20 C17 -0.1(5) . . . . ? N5 N6 C20 C21 -176.0(4) . . . . ? C18 C17 C20 N6 -0.6(5) . . . . ? C12 C17 C20 N6 179.0(4) . . . . ? C18 C17 C20 C21 174.7(5) . . . . ? C12 C17 C20 C21 -5.7(8) . . . . ? C18 N5 C22 N5 -104.2(5) . . . 2 ? N6 N5 C22 N5 75.2(3) . . . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.279 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.059 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 296386' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 Co N18 O' _chemical_formula_weight 925.94 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 24.958(4) _cell_length_b 24.637(4) _cell_length_c 8.1686(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5022.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4756 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 23.82 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1932 _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.858155 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'APEX II 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 25804 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4435 _reflns_number_gt 3269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0994P)^2^+2.7475P] 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 4435 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1717 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.0000 0.23222(2) 0.2500 0.0387(2) Uani 1 2 d S . . N1 N 0.45183(11) -0.20519(10) 0.1475(3) 0.0474(7) Uani 1 1 d . . . N2 N 0.33959(10) 0.01366(10) -0.1211(3) 0.0399(6) Uani 1 1 d . . . N3 N 0.30674(10) -0.02354(10) -0.1943(3) 0.0404(6) Uani 1 1 d . . . N4 N 0.21577(10) 0.00928(10) -0.2003(3) 0.0398(6) Uani 1 1 d . . . N5 N 0.18385(11) -0.03151(10) -0.1452(3) 0.0445(6) Uani 1 1 d . . . N6 N 0.04963(10) 0.17165(10) 0.1426(4) 0.0472(7) Uani 1 1 d . . . N7 N 0.04641(12) 0.23023(11) 0.4580(4) 0.0548(7) Uani 1 1 d . . . N8 N 0.1011(2) 0.2025(2) 0.6909(6) 0.1150(17) Uani 1 1 d . . . N9 N 0.1830(3) 0.24191(18) 0.7937(9) 0.133(2) Uani 1 1 d . . . C1 C 0.40355(14) -0.12222(13) 0.1804(4) 0.0526(8) Uani 1 1 d . . . H1 H 0.3904 -0.0958 0.2512 0.063 Uiso 1 1 calc R . . C2 C 0.43153(15) -0.16567(13) 0.2410(4) 0.0528(9) Uani 1 1 d . . . H2 H 0.4367 -0.1678 0.3536 0.063 Uiso 1 1 calc R . . C3 C 0.44258(15) -0.20151(14) -0.0116(4) 0.0573(10) Uani 1 1 d . . . H3 H 0.4555 -0.2290 -0.0790 0.069 Uiso 1 1 calc R . . C4 C 0.41497(15) -0.15932(14) -0.0830(4) 0.0579(10) Uani 1 1 d . . . H4 H 0.4098 -0.1588 -0.1958 0.069 Uiso 1 1 calc R . . C5 C 0.39493(13) -0.11767(12) 0.0124(4) 0.0442(7) Uani 1 1 d . . . C6 C 0.36472(13) -0.07189(12) -0.0573(4) 0.0423(7) Uani 1 1 d . . . C7 C 0.32042(13) -0.07530(12) -0.1593(4) 0.0452(8) Uani 1 1 d . . . C8 C 0.28997(18) -0.12254(15) -0.2211(6) 0.0736(13) Uani 1 1 d . . . H8A H 0.2524 -0.1168 -0.2026 0.110 Uiso 1 1 calc R . . H8B H 0.3013 -0.1547 -0.1645 0.110 Uiso 1 1 calc R . . H8C H 0.2964 -0.1267 -0.3362 0.110 Uiso 1 1 calc R . . C9 C 0.37483(12) -0.01599(12) -0.0385(4) 0.0394(7) Uani 1 1 d . . . C10 C 0.41976(13) 0.01109(15) 0.0494(4) 0.0526(8) Uani 1 1 d . . . H10A H 0.4492 0.0164 -0.0246 0.079 Uiso 1 1 d R . . H10B H 0.4311 -0.0113 0.1391 0.079 Uiso 1 1 d R . . H10C H 0.4079 0.0456 0.0904 0.079 Uiso 1 1 d R . . C11 C 0.26279(12) -0.00456(14) -0.2954(4) 0.0432(7) Uani 1 1 d . . . H11A H 0.2743 0.0271 -0.3564 0.052 Uiso 1 1 calc R . . H11B H 0.2535 -0.0326 -0.3737 0.052 Uiso 1 1 calc R . . C12 C 0.14430(12) -0.00672(12) -0.0683(4) 0.0415(7) Uani 1 1 d . . . C13 C 0.10054(15) -0.03963(15) 0.0070(5) 0.0627(10) Uani 1 1 d . . . H13A H 0.0718 -0.0437 -0.0701 0.094 Uiso 1 1 calc R . . H13B H 0.0876 -0.0216 0.1034 0.094 Uiso 1 1 calc R . . H13C H 0.1141 -0.0748 0.0360 0.094 Uiso 1 1 calc R . . C14 C 0.15126(12) 0.05048(12) -0.0697(4) 0.0397(7) Uani 1 1 d . . . C15 C 0.19810(12) 0.05905(12) -0.1574(4) 0.0410(7) Uani 1 1 d . . . C16 C 0.22599(15) 0.10915(14) -0.2096(5) 0.0614(10) Uani 1 1 d . . . H16A H 0.2616 0.1095 -0.1651 0.092 Uiso 1 1 calc R . . H16B H 0.2067 0.1402 -0.1705 0.092 Uiso 1 1 calc R . . H16C H 0.2278 0.1102 -0.3269 0.092 Uiso 1 1 calc R . . C17 C 0.11633(12) 0.09210(12) 0.0036(4) 0.0410(7) Uani 1 1 d . . . C18 C 0.06069(13) 0.09019(13) -0.0115(5) 0.0522(9) Uani 1 1 d . . . H18 H 0.0446 0.0621 -0.0696 0.063 Uiso 1 1 calc R . . C19 C 0.02978(13) 0.12975(13) 0.0596(5) 0.0545(9) Uani 1 1 d . . . H19 H -0.0072 0.1271 0.0491 0.065 Uiso 1 1 calc R . . C20 C 0.10281(12) 0.17367(13) 0.1569(4) 0.0483(8) Uani 1 1 d . . . H20 H 0.1179 0.2026 0.2137 0.058 Uiso 1 1 calc R . . C21 C 0.13651(12) 0.13518(13) 0.0919(4) 0.0472(8) Uani 1 1 d . . . H21 H 0.1733 0.1382 0.1077 0.057 Uiso 1 1 calc R . . C22 C 0.07403(18) 0.22027(16) 0.5647(6) 0.0641(10) Uani 1 1 d . . . C23 C 0.1446(3) 0.22555(19) 0.7390(7) 0.0872(15) Uani 1 1 d . . . O1 O 0.2962(4) 0.2381(5) 0.6676(15) 0.170(4) Uani 0.50 1 d P . . 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 0.0335(3) 0.0250(3) 0.0575(4) 0.000 0.0160(3) 0.000 N1 0.0481(16) 0.0366(14) 0.0575(18) -0.0062(12) -0.0174(13) 0.0056(12) N2 0.0398(14) 0.0381(13) 0.0417(14) 0.0021(11) 0.0044(11) 0.0041(11) N3 0.0403(14) 0.0406(14) 0.0401(14) 0.0006(11) -0.0022(11) 0.0135(11) N4 0.0406(14) 0.0384(14) 0.0405(14) -0.0015(11) 0.0024(11) 0.0114(11) N5 0.0484(16) 0.0382(14) 0.0469(15) -0.0035(11) -0.0006(12) 0.0045(12) N6 0.0358(14) 0.0345(13) 0.0715(19) -0.0068(12) 0.0134(13) -0.0013(11) N7 0.0463(17) 0.0456(16) 0.072(2) 0.0031(14) 0.0115(16) 0.0010(13) N8 0.140(4) 0.105(3) 0.100(3) 0.035(3) -0.042(3) -0.031(3) N9 0.112(4) 0.072(3) 0.216(6) 0.007(3) -0.059(4) 0.005(3) C1 0.063(2) 0.0427(18) 0.052(2) -0.0048(15) -0.0087(17) 0.0133(16) C2 0.062(2) 0.0441(18) 0.052(2) -0.0026(15) -0.0132(16) 0.0147(16) C3 0.066(2) 0.0458(19) 0.060(2) -0.0135(16) -0.0193(18) 0.0199(17) C4 0.068(2) 0.055(2) 0.051(2) -0.0074(16) -0.0189(17) 0.0249(18) C5 0.0412(18) 0.0401(16) 0.0513(19) -0.0001(14) -0.0087(14) 0.0082(13) C6 0.0449(18) 0.0384(16) 0.0435(17) 0.0006(13) -0.0027(14) 0.0102(13) C7 0.0466(18) 0.0369(16) 0.0520(19) -0.0031(14) -0.0079(15) 0.0131(14) C8 0.074(3) 0.046(2) 0.101(3) -0.017(2) -0.032(2) 0.0123(19) C9 0.0379(17) 0.0418(16) 0.0384(16) 0.0030(13) 0.0041(13) 0.0053(13) C10 0.0428(19) 0.057(2) 0.058(2) 0.0030(17) 0.0003(16) -0.0042(15) C11 0.0424(17) 0.0524(17) 0.0347(16) 0.0010(13) -0.0006(13) 0.0164(15) C12 0.0438(17) 0.0398(16) 0.0409(17) -0.0044(13) -0.0013(14) 0.0034(13) C13 0.062(2) 0.051(2) 0.075(3) -0.0022(18) 0.011(2) -0.0034(17) C14 0.0369(16) 0.0380(15) 0.0443(17) -0.0015(13) -0.0002(13) 0.0078(13) C15 0.0387(17) 0.0398(16) 0.0447(17) -0.0009(13) -0.0003(13) 0.0097(13) C16 0.054(2) 0.0455(19) 0.084(3) 0.0096(18) 0.0176(19) 0.0085(16) C17 0.0396(17) 0.0364(15) 0.0471(17) -0.0018(13) 0.0059(13) 0.0054(13) C18 0.0401(19) 0.0391(17) 0.077(2) -0.0139(16) 0.0009(16) 0.0020(14) C19 0.0324(18) 0.0429(18) 0.088(3) -0.0115(17) 0.0084(16) 0.0001(14) C20 0.0388(18) 0.0417(17) 0.064(2) -0.0117(15) 0.0068(15) -0.0026(13) C21 0.0325(16) 0.0456(17) 0.063(2) -0.0075(16) 0.0040(14) 0.0048(13) C22 0.069(3) 0.052(2) 0.071(3) 0.001(2) 0.010(2) -0.0016(19) C23 0.089(4) 0.060(3) 0.113(4) 0.005(3) -0.018(3) 0.007(3) O1 0.102(7) 0.221(11) 0.188(10) -0.001(8) 0.047(7) -0.077(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N7 2.057(4) 3 ? Co1 N7 2.057(4) . ? Co1 N1 2.127(3) 6_566 ? Co1 N1 2.127(3) 8_665 ? Co1 N6 2.129(2) . ? Co1 N6 2.129(2) 3 ? N1 C3 1.323(4) . ? N1 C2 1.337(4) . ? N1 Co1 2.127(3) 6_656 ? N2 C9 1.328(4) . ? N2 N3 1.367(4) . ? N3 C7 1.351(4) . ? N3 C11 1.450(4) . ? N4 C15 1.350(4) . ? N4 N5 1.359(4) . ? N4 C11 1.448(4) . ? N5 C12 1.320(4) . ? N6 C19 1.331(4) . ? N6 C20 1.333(4) . ? N7 C22 1.138(5) . ? N8 C23 1.287(7) . ? N8 C22 1.308(6) . ? N9 C23 1.130(7) . ? C1 C2 1.371(5) . ? C1 C5 1.394(5) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.377(5) . ? C3 H3 0.9300 . ? C4 C5 1.382(5) . ? C4 H4 0.9300 . ? C5 C6 1.471(4) . ? C6 C7 1.387(4) . ? C6 C9 1.408(4) . ? C7 C8 1.479(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.489(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C14 1.420(4) . ? C12 C13 1.493(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.387(4) . ? C14 C17 1.473(4) . ? C15 C16 1.480(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C21 1.378(4) . ? C17 C18 1.395(5) . ? C18 C19 1.372(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.374(4) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? 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 N7 Co1 N7 177.26(15) 3 . ? N7 Co1 N1 91.39(11) 3 6_566 ? N7 Co1 N1 90.60(11) . 6_566 ? N7 Co1 N1 90.60(11) 3 8_665 ? N7 Co1 N1 91.39(11) . 8_665 ? N1 Co1 N1 87.06(14) 6_566 8_665 ? N7 Co1 N6 88.30(11) 3 . ? N7 Co1 N6 89.78(11) . . ? N1 Co1 N6 178.01(10) 6_566 . ? N1 Co1 N6 90.98(10) 8_665 . ? N7 Co1 N6 89.78(11) 3 3 ? N7 Co1 N6 88.30(11) . 3 ? N1 Co1 N6 90.98(10) 6_566 3 ? N1 Co1 N6 178.01(10) 8_665 3 ? N6 Co1 N6 90.98(14) . 3 ? C3 N1 C2 116.4(3) . . ? C3 N1 Co1 122.3(2) . 6_656 ? C2 N1 Co1 121.2(2) . 6_656 ? C9 N2 N3 104.5(2) . . ? C7 N3 N2 112.9(2) . . ? C7 N3 C11 128.1(3) . . ? N2 N3 C11 119.1(2) . . ? C15 N4 N5 113.2(2) . . ? C15 N4 C11 128.2(3) . . ? N5 N4 C11 118.6(2) . . ? C12 N5 N4 104.7(2) . . ? C19 N6 C20 116.4(3) . . ? C19 N6 Co1 122.5(2) . . ? C20 N6 Co1 121.1(2) . . ? C22 N7 Co1 168.2(3) . . ? C23 N8 C22 121.9(5) . . ? C2 C1 C5 119.8(3) . . ? C2 C1 H1 120.1 . . ? C5 C1 H1 120.1 . . ? N1 C2 C1 123.8(3) . . ? N1 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? N1 C3 C4 123.7(3) . . ? N1 C3 H3 118.1 . . ? C4 C3 H3 118.1 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C1 116.1(3) . . ? C4 C5 C6 122.5(3) . . ? C1 C5 C6 121.4(3) . . ? C7 C6 C9 105.5(3) . . ? C7 C6 C5 126.5(3) . . ? C9 C6 C5 128.0(3) . . ? N3 C7 C6 105.8(3) . . ? N3 C7 C8 122.7(3) . . ? C6 C7 C8 131.5(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C6 111.3(3) . . ? N2 C9 C10 119.8(3) . . ? C6 C9 C10 128.7(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 N3 112.5(2) . . ? N4 C11 H11A 109.1 . . ? N3 C11 H11A 109.1 . . ? N4 C11 H11B 109.1 . . ? N3 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N5 C12 C14 111.4(3) . . ? N5 C12 C13 119.5(3) . . ? C14 C12 C13 129.2(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C12 105.0(3) . . ? C15 C14 C17 127.1(3) . . ? C12 C14 C17 128.0(3) . . ? N4 C15 C14 105.7(3) . . ? N4 C15 C16 122.0(3) . . ? C14 C15 C16 132.2(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C21 C17 C18 115.8(3) . . ? C21 C17 C14 122.2(3) . . ? C18 C17 C14 122.0(3) . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? N6 C19 C18 123.9(3) . . ? N6 C19 H19 118.1 . . ? C18 C19 H19 118.1 . . ? N6 C20 C21 123.3(3) . . ? N6 C20 H20 118.3 . . ? C21 C20 H20 118.3 . . ? C20 C21 C17 120.7(3) . . ? C20 C21 H21 119.7 . . ? C17 C21 H21 119.7 . . ? N7 C22 N8 171.3(5) . . ? N9 C23 N8 172.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 N2 N3 C7 0.2(3) . . . . ? C9 N2 N3 C11 179.7(3) . . . . ? C15 N4 N5 C12 1.3(3) . . . . ? C11 N4 N5 C12 -178.3(3) . . . . ? N7 Co1 N6 C19 -41.3(3) 3 . . . ? N7 Co1 N6 C19 136.7(3) . . . . ? N1 Co1 N6 C19 -131.9(3) 8_665 . . . ? N6 Co1 N6 C19 48.4(2) 3 . . . ? N7 Co1 N6 C20 139.3(3) 3 . . . ? N7 Co1 N6 C20 -42.6(3) . . . . ? N1 Co1 N6 C20 48.8(3) 8_665 . . . ? N6 Co1 N6 C20 -130.9(3) 3 . . . ? N1 Co1 N7 C22 156.3(16) 6_566 . . . ? N1 Co1 N7 C22 -116.6(16) 8_665 . . . ? N6 Co1 N7 C22 -25.6(16) . . . . ? N6 Co1 N7 C22 65.4(16) 3 . . . ? C3 N1 C2 C1 -1.6(5) . . . . ? Co1 N1 C2 C1 175.1(3) 6_656 . . . ? C5 C1 C2 N1 0.1(6) . . . . ? C2 N1 C3 C4 1.7(6) . . . . ? Co1 N1 C3 C4 -175.0(3) 6_656 . . . ? N1 C3 C4 C5 -0.2(6) . . . . ? C3 C4 C5 C1 -1.3(5) . . . . ? C3 C4 C5 C6 -179.4(3) . . . . ? C2 C1 C5 C4 1.3(5) . . . . ? C2 C1 C5 C6 179.5(3) . . . . ? C4 C5 C6 C7 52.4(5) . . . . ? C1 C5 C6 C7 -125.6(4) . . . . ? C4 C5 C6 C9 -126.1(4) . . . . ? C1 C5 C6 C9 55.8(5) . . . . ? C11 N3 C7 C6 -179.5(3) . . . . ? N2 N3 C7 C8 178.5(3) . . . . ? C11 N3 C7 C8 -1.1(5) . . . . ? C9 C6 C7 N3 -0.2(4) . . . . ? C5 C6 C7 N3 -179.0(3) . . . . ? C9 C6 C7 C8 -178.4(4) . . . . ? C5 C6 C7 C8 2.8(6) . . . . ? N3 N2 C9 C6 -0.3(3) . . . . ? N3 N2 C9 C10 176.1(3) . . . . ? C7 C6 C9 N2 0.3(4) . . . . ? C5 C6 C9 N2 179.1(3) . . . . ? C7 C6 C9 C10 -175.6(3) . . . . ? C5 C6 C9 C10 3.1(6) . . . . ? C15 N4 C11 N3 102.4(4) . . . . ? N5 N4 C11 N3 -78.1(3) . . . . ? C7 N3 C11 N4 96.1(4) . . . . ? N2 N3 C11 N4 -83.4(3) . . . . ? N4 N5 C12 C14 -1.5(3) . . . . ? N4 N5 C12 C13 179.1(3) . . . . ? N5 C12 C14 C15 1.2(4) . . . . ? C13 C12 C14 C15 -179.5(3) . . . . ? N5 C12 C14 C17 -179.5(3) . . . . ? C13 C12 C14 C17 -0.2(6) . . . . ? N5 N4 C15 C14 -0.6(3) . . . . ? C11 N4 C15 C14 179.0(3) . . . . ? N5 N4 C15 C16 -178.0(3) . . . . ? C11 N4 C15 C16 1.6(5) . . . . ? C12 C14 C15 N4 -0.4(3) . . . . ? C17 C14 C15 N4 -179.7(3) . . . . ? C12 C14 C15 C16 176.6(4) . . . . ? C17 C14 C15 C16 -2.7(6) . . . . ? C15 C14 C17 C21 -45.2(5) . . . . ? C12 C14 C17 C21 135.6(3) . . . . ? C15 C14 C17 C18 135.1(4) . . . . ? C12 C14 C17 C18 -44.1(5) . . . . ? C14 C17 C18 C19 179.7(3) . . . . ? C20 N6 C19 C18 -0.9(5) . . . . ? Co1 N6 C19 C18 179.8(3) . . . . ? C17 C18 C19 N6 1.1(6) . . . . ? C19 N6 C20 C21 -0.4(5) . . . . ? Co1 N6 C20 C21 179.0(3) . . . . ? N6 C20 C21 C17 1.4(5) . . . . ? C18 C17 C21 C20 -1.1(5) . . . . ? C14 C17 C21 C20 179.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.862 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.075 #===END