data_1cooling303K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.8533(13) _cell_length_b 25.995(3) _cell_length_c 8.1782(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.741(2) _cell_angle_gamma 90.00 _cell_volume 2058.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 303(2) _cell_measurement_reflns_used 3810 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7752 _exptl_absorpt_correction_T_max 0.9159 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 303(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17031 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3810 _reflns_number_gt 3671 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+0.3933P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3810 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.1663 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.310 _refine_ls_restrained_S_all 1.310 _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 0.56096(3) 0.124997(12) 0.20058(4) 0.03678(19) Uani 1 1 d . . . C1 C 0.4078(4) 0.02220(12) 0.3034(4) 0.0537(7) Uani 1 1 d . . . H1A H 0.4651 -0.0025 0.2693 0.064 Uiso 1 1 calc R . . C2 C 0.2928(4) 0.01073(12) 0.3736(4) 0.0554(8) Uani 1 1 d . . . H2A H 0.2605 -0.0217 0.3955 0.066 Uiso 1 1 calc R . . C3 C 0.2384(3) 0.05683(11) 0.4033(4) 0.0470(6) Uani 1 1 d . . . H3A H 0.1601 0.0622 0.4491 0.056 Uiso 1 1 calc R . . C4 C 0.3094(3) 0.14750(10) 0.3537(3) 0.0342(5) Uani 1 1 d . . . C5 C 0.2045(3) 0.17462(10) 0.4056(3) 0.0389(6) Uani 1 1 d . . . H5A H 0.1347 0.1581 0.4477 0.047 Uiso 1 1 calc R . . C6 C 0.2083(3) 0.22780(10) 0.3917(3) 0.0382(5) Uani 1 1 d . . . C7 C 0.0927(3) 0.25840(11) 0.4436(4) 0.0455(6) Uani 1 1 d . . . C8 C 0.3142(3) 0.25237(10) 0.3318(3) 0.0371(5) Uani 1 1 d . . . H8A H 0.3175 0.2880 0.3226 0.045 Uiso 1 1 calc R . . C9 C 0.4140(3) 0.22127(10) 0.2866(3) 0.0329(5) Uani 1 1 d . . . C10 C 0.5646(3) 0.28878(11) 0.1915(3) 0.0425(6) Uani 1 1 d . . . H10A H 0.5142 0.3185 0.2013 0.051 Uiso 1 1 calc R . . C11 C 0.6872(3) 0.28592(12) 0.1399(4) 0.0490(7) Uani 1 1 d . . . H11A H 0.7380 0.3130 0.1080 0.059 Uiso 1 1 calc R . . C12 C 0.7213(3) 0.23393(13) 0.1445(4) 0.0515(7) Uani 1 1 d . . . H12A H 0.8009 0.2207 0.1145 0.062 Uiso 1 1 calc R . . C13 C -0.0020(4) 0.34174(14) 0.4590(6) 0.0698(10) Uani 1 1 d . . . H13A H 0.0147 0.3487 0.5775 0.084 Uiso 1 1 calc R A 1 H13B H -0.0908 0.3247 0.4293 0.084 Uiso 1 1 calc R A 1 C16 C 0.1281(8) 0.4739(2) 0.3360(9) 0.123(2) Uani 1 1 d . . . H16A H 0.2100 0.4926 0.3829 0.148 Uiso 1 1 calc R B 1 H16B H 0.0482 0.4946 0.3408 0.148 Uiso 1 1 calc R B 1 H16C H 0.1303 0.4655 0.2222 0.148 Uiso 1 1 calc R B 1 N1 N 0.4254(2) 0.07201(9) 0.2910(3) 0.0430(6) Uani 1 1 d . . . N2 N 0.3193(2) 0.09373(8) 0.3537(3) 0.0365(5) Uani 1 1 d . . . N3 N 0.4112(2) 0.17016(8) 0.2951(2) 0.0320(4) Uani 1 1 d . . . N4 N 0.5292(2) 0.24008(8) 0.2262(3) 0.0343(4) Uani 1 1 d . . . N5 N 0.6259(2) 0.20545(9) 0.1972(3) 0.0433(5) Uani 1 1 d . . . N6 N 0.4733(3) 0.09845(10) -0.1113(3) 0.0529(6) Uani 1 1 d . . . N7 N 0.8111(3) 0.10518(11) 0.3381(4) 0.0584(7) Uani 1 1 d . . . O1 O 0.4495(2) 0.14029(8) -0.0418(3) 0.0532(5) Uani 1 1 d . . . O2 O 0.4368(4) 0.09253(11) -0.2615(3) 0.0832(9) Uani 1 1 d . . . O3 O 0.5381(3) 0.06564(10) -0.0182(3) 0.0804(8) Uani 1 1 d . . . O4 O 0.7739(3) 0.11034(12) 0.1831(4) 0.0733(7) Uani 1 1 d . . . O5 O 0.9301(3) 0.09718(14) 0.4030(6) 0.1105(13) Uani 1 1 d . . . O6 O 0.7150(2) 0.10736(9) 0.4203(3) 0.0578(5) Uani 1 1 d . . . O7 O 0.1069(2) 0.30809(8) 0.4195(3) 0.0600(6) Uani 1 1 d . C . O8 O 0.0021(3) 0.23937(9) 0.5013(4) 0.0724(7) Uani 1 1 d . . . C14 C -0.0043(8) 0.3918(3) 0.3639(10) 0.060(2) Uani 0.551(14) 1 d P C 1 H14A H -0.0039 0.3847 0.2475 0.072 Uiso 0.551(14) 1 calc PR C 1 H14B H -0.0876 0.4108 0.3710 0.072 Uiso 0.551(14) 1 calc PR C 1 C15 C 0.1211(10) 0.4232(4) 0.4371(15) 0.079(3) Uani 0.551(14) 1 d P C 1 H15A H 0.2039 0.4031 0.4365 0.095 Uiso 0.551(14) 1 calc PR C 1 H15B H 0.1176 0.4317 0.5517 0.095 Uiso 0.551(14) 1 calc PR C 1 C14' C 0.0651(11) 0.3975(4) 0.4742(13) 0.065(3) Uani 0.449(14) 1 d P C 2 H14C H 0.0075 0.4206 0.5245 0.077 Uiso 0.449(14) 1 calc PR C 2 H14D H 0.1551 0.3960 0.5462 0.077 Uiso 0.449(14) 1 calc PR C 2 C15' C 0.0799(19) 0.4173(4) 0.3127(17) 0.100(5) Uani 0.449(14) 1 d P C 2 H15C H -0.0077 0.4154 0.2357 0.121 Uiso 0.449(14) 1 calc PR C 2 H15D H 0.1473 0.3972 0.2678 0.121 Uiso 0.449(14) 1 calc PR C 2 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 0.0344(3) 0.0349(3) 0.0432(3) 0.00084(12) 0.01275(18) 0.00556(12) C1 0.0578(17) 0.0341(15) 0.071(2) 0.0011(12) 0.0176(14) 0.0035(13) C2 0.0627(19) 0.0359(15) 0.0676(19) 0.0060(13) 0.0121(15) -0.0080(13) C3 0.0456(15) 0.0407(15) 0.0565(16) 0.0068(12) 0.0141(12) -0.0091(12) C4 0.0332(12) 0.0329(13) 0.0367(12) -0.0023(9) 0.0067(9) -0.0016(9) C5 0.0332(12) 0.0380(13) 0.0488(14) -0.0014(10) 0.0160(10) -0.0032(10) C6 0.0334(12) 0.0384(13) 0.0451(13) -0.0045(10) 0.0136(10) 0.0034(10) C7 0.0344(13) 0.0459(15) 0.0589(17) -0.0062(12) 0.0155(12) 0.0046(11) C8 0.0356(13) 0.0328(12) 0.0443(13) -0.0037(10) 0.0107(10) -0.0004(9) C9 0.0329(12) 0.0317(13) 0.0357(12) -0.0012(9) 0.0103(9) -0.0024(9) C10 0.0468(16) 0.0358(14) 0.0466(15) 0.0005(10) 0.0129(12) -0.0053(10) C11 0.0469(16) 0.0520(16) 0.0515(15) 0.0033(12) 0.0178(12) -0.0147(12) C12 0.0393(15) 0.0562(18) 0.0650(18) -0.0011(14) 0.0248(13) -0.0091(13) C13 0.062(2) 0.0518(19) 0.104(3) -0.0057(18) 0.037(2) 0.0176(16) C16 0.168(6) 0.059(3) 0.161(5) 0.012(3) 0.079(5) 0.008(3) N1 0.0416(13) 0.0338(12) 0.0564(14) -0.0004(9) 0.0167(10) 0.0045(9) N2 0.0364(11) 0.0306(11) 0.0442(11) -0.0008(8) 0.0118(9) -0.0016(8) N3 0.0312(9) 0.0301(11) 0.0368(11) -0.0006(7) 0.0120(8) -0.0007(8) N4 0.0320(10) 0.0321(10) 0.0412(11) -0.0007(8) 0.0131(8) -0.0004(8) N5 0.0337(11) 0.0415(12) 0.0591(14) -0.0001(10) 0.0197(10) 0.0005(9) N6 0.0697(17) 0.0433(14) 0.0466(14) -0.0022(10) 0.0131(12) 0.0010(12) N7 0.0367(13) 0.0469(14) 0.090(2) 0.0041(13) 0.0090(13) 0.0043(11) O1 0.0724(15) 0.0385(10) 0.0501(11) -0.0013(9) 0.0151(10) 0.0100(10) O2 0.127(3) 0.0731(17) 0.0457(14) -0.0124(12) 0.0067(14) -0.0055(16) O3 0.120(2) 0.0596(15) 0.0657(15) 0.0095(12) 0.0266(15) 0.0365(15) O4 0.0694(17) 0.0754(16) 0.0838(18) 0.0113(14) 0.0368(14) 0.0263(14) O5 0.0398(14) 0.100(3) 0.177(4) 0.004(2) -0.0171(18) 0.0087(14) O6 0.0517(13) 0.0576(13) 0.0637(13) 0.0101(11) 0.0093(10) 0.0030(10) O7 0.0556(13) 0.0413(11) 0.0924(16) -0.0048(11) 0.0382(12) 0.0083(9) O8 0.0522(13) 0.0541(14) 0.124(2) 0.0030(13) 0.0518(14) 0.0063(10) C14 0.056(4) 0.062(4) 0.061(4) -0.006(3) 0.006(4) 0.018(3) C15 0.072(5) 0.060(5) 0.102(8) 0.004(5) 0.006(5) 0.002(4) C14' 0.065(6) 0.056(6) 0.076(7) -0.004(4) 0.021(5) 0.016(5) C15' 0.168(14) 0.068(6) 0.074(8) 0.002(5) 0.042(8) 0.026(8) _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 O1 2.117(2) . ? Co1 N3 2.139(2) . ? Co1 N1 2.144(2) . ? Co1 O4 2.163(3) . ? Co1 O6 2.174(2) . ? Co1 N5 2.189(2) . ? Co1 O3 2.342(3) . ? C1 N1 1.313(4) . ? C1 C2 1.395(5) . ? C1 H1A 0.9300 . ? C2 C3 1.353(5) . ? C2 H2A 0.9300 . ? C3 N2 1.357(3) . ? C3 H3A 0.9300 . ? C4 N3 1.328(3) . ? C4 C5 1.382(4) . ? C4 N2 1.401(4) . ? C5 C6 1.388(4) . ? C5 H5A 0.9300 . ? C6 C8 1.388(4) . ? C6 C7 1.514(4) . ? C7 O8 1.192(4) . ? C7 O7 1.318(4) . ? C8 C9 1.376(4) . ? C8 H8A 0.9300 . ? C9 N3 1.331(3) . ? C9 N4 1.408(3) . ? C10 C11 1.353(4) . ? C10 N4 1.357(4) . ? C10 H10A 0.9300 . ? C11 C12 1.391(5) . ? C11 H11A 0.9300 . ? C12 N5 1.330(4) . ? C12 H12A 0.9300 . ? C13 O7 1.466(4) . ? C13 C14 1.514(9) . ? C13 C14' 1.588(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C16 C15' 1.545(14) . ? C16 C15 1.562(11) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 N2 1.369(3) . ? N4 N5 1.363(3) . ? N6 O2 1.223(4) . ? N6 O3 1.238(3) . ? N6 O1 1.269(3) . ? N7 O5 1.212(4) . ? N7 O4 1.259(4) . ? N7 O6 1.260(4) . ? C14 C15 1.509(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C14' C15' 1.451(19) . ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' H15C 0.9700 . ? C15' H15D 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 O1 Co1 N3 87.87(8) . . ? O1 Co1 N1 101.30(9) . . ? N3 Co1 N1 73.27(9) . . ? O1 Co1 O4 108.14(10) . . ? N3 Co1 O4 149.67(10) . . ? N1 Co1 O4 125.73(10) . . ? O1 Co1 O6 166.88(9) . . ? N3 Co1 O6 103.85(8) . . ? N1 Co1 O6 87.89(9) . . ? O4 Co1 O6 58.74(10) . . ? O1 Co1 N5 84.87(9) . . ? N3 Co1 N5 72.73(8) . . ? N1 Co1 N5 145.15(9) . . ? O4 Co1 N5 82.99(10) . . ? O6 Co1 N5 92.93(9) . . ? O1 Co1 O3 56.56(8) . . ? N3 Co1 O3 131.52(9) . . ? N1 Co1 O3 82.11(10) . . ? O4 Co1 O3 77.88(12) . . ? O6 Co1 O3 116.46(9) . . ? N5 Co1 O3 127.35(9) . . ? N1 C1 C2 111.8(3) . . ? N1 C1 H1A 124.1 . . ? C2 C1 H1A 124.1 . . ? C3 C2 C1 105.3(3) . . ? C3 C2 H2A 127.4 . . ? C1 C2 H2A 127.4 . . ? C2 C3 N2 107.4(3) . . ? C2 C3 H3A 126.3 . . ? N2 C3 H3A 126.3 . . ? N3 C4 C5 122.9(2) . . ? N3 C4 N2 112.7(2) . . ? C5 C4 N2 124.4(2) . . ? C4 C5 C6 116.7(2) . . ? C4 C5 H5A 121.6 . . ? C6 C5 H5A 121.6 . . ? C5 C6 C8 121.4(2) . . ? C5 C6 C7 117.9(2) . . ? C8 C6 C7 120.8(2) . . ? O8 C7 O7 125.0(3) . . ? O8 C7 C6 123.4(3) . . ? O7 C7 C6 111.5(2) . . ? C9 C8 C6 116.5(2) . . ? C9 C8 H8A 121.7 . . ? C6 C8 H8A 121.7 . . ? N3 C9 C8 123.4(2) . . ? N3 C9 N4 113.0(2) . . ? C8 C9 N4 123.6(2) . . ? C11 C10 N4 107.0(3) . . ? C11 C10 H10A 126.5 . . ? N4 C10 H10A 126.5 . . ? C10 C11 C12 105.7(3) . . ? C10 C11 H11A 127.2 . . ? C12 C11 H11A 127.2 . . ? N5 C12 C11 111.6(3) . . ? N5 C12 H12A 124.2 . . ? C11 C12 H12A 124.2 . . ? O7 C13 C14 109.9(4) . . ? O7 C13 C14' 104.5(4) . . ? C14 C13 C14' 38.9(4) . . ? O7 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? C14' C13 H13A 76.2 . . ? O7 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? C14' C13 H13B 141.1 . . ? H13A C13 H13B 108.2 . . ? C15' C16 C15 38.9(5) . . ? C15' C16 H16A 138.5 . . ? C15 C16 H16A 109.5 . . ? C15' C16 H16B 107.6 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15' C16 H16C 74.1 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 N2 104.9(2) . . ? C1 N1 Co1 139.5(2) . . ? N2 N1 Co1 115.62(17) . . ? C3 N2 N1 110.6(2) . . ? C3 N2 C4 131.3(2) . . ? N1 N2 C4 118.0(2) . . ? C4 N3 C9 119.1(2) . . ? C4 N3 Co1 120.34(17) . . ? C9 N3 Co1 120.46(16) . . ? C10 N4 N5 111.4(2) . . ? C10 N4 C9 130.8(2) . . ? N5 N4 C9 117.8(2) . . ? C12 N5 N4 104.3(2) . . ? C12 N5 Co1 139.7(2) . . ? N4 N5 Co1 114.41(15) . . ? O2 N6 O3 123.5(3) . . ? O2 N6 O1 120.9(3) . . ? O3 N6 O1 115.6(2) . . ? O5 N7 O4 122.3(4) . . ? O5 N7 O6 122.4(4) . . ? O4 N7 O6 115.2(3) . . ? N6 O1 Co1 98.70(17) . . ? N6 O3 Co1 88.92(18) . . ? N7 O4 Co1 93.20(18) . . ? N7 O6 Co1 92.65(18) . . ? C7 O7 C13 116.7(2) . . ? C15 C14 C13 109.2(7) . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C14 C15 C16 111.1(8) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15' C14' C13 111.4(10) . . ? C15' C14' H14C 109.3 . . ? C13 C14' H14C 109.3 . . ? C15' C14' H14D 109.3 . . ? C13 C14' H14D 109.3 . . ? H14C C14' H14D 108.0 . . ? C14' C15' C16 107.9(10) . . ? C14' C15' H15C 110.1 . . ? C16 C15' H15C 110.1 . . ? C14' C15' H15D 110.1 . . ? C16 C15' H15D 110.1 . . ? H15C C15' H15D 108.4 . . ? 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 N1 C1 C2 C3 0.6(4) . . . . ? C1 C2 C3 N2 -0.6(4) . . . . ? N3 C4 C5 C6 0.9(4) . . . . ? N2 C4 C5 C6 -177.8(2) . . . . ? C4 C5 C6 C8 -1.3(4) . . . . ? C4 C5 C6 C7 178.5(2) . . . . ? C5 C6 C7 O8 2.9(5) . . . . ? C8 C6 C7 O8 -177.3(3) . . . . ? C5 C6 C7 O7 -178.1(3) . . . . ? C8 C6 C7 O7 1.7(4) . . . . ? C5 C6 C8 C9 0.3(4) . . . . ? C7 C6 C8 C9 -179.5(2) . . . . ? C6 C8 C9 N3 1.3(4) . . . . ? C6 C8 C9 N4 -178.9(2) . . . . ? N4 C10 C11 C12 0.5(3) . . . . ? C10 C11 C12 N5 -0.4(4) . . . . ? C2 C1 N1 N2 -0.3(4) . . . . ? C2 C1 N1 Co1 -178.3(2) . . . . ? O1 Co1 N1 C1 95.0(3) . . . . ? N3 Co1 N1 C1 179.3(3) . . . . ? O4 Co1 N1 C1 -27.4(4) . . . . ? O6 Co1 N1 C1 -75.6(3) . . . . ? N5 Co1 N1 C1 -167.7(3) . . . . ? O3 Co1 N1 C1 41.5(3) . . . . ? O1 Co1 N1 N2 -82.81(18) . . . . ? N3 Co1 N1 N2 1.48(17) . . . . ? O4 Co1 N1 N2 154.86(17) . . . . ? O6 Co1 N1 N2 106.62(19) . . . . ? N5 Co1 N1 N2 14.5(3) . . . . ? O3 Co1 N1 N2 -136.30(19) . . . . ? C2 C3 N2 N1 0.4(3) . . . . ? C2 C3 N2 C4 178.9(3) . . . . ? C1 N1 N2 C3 0.0(3) . . . . ? Co1 N1 N2 C3 178.47(18) . . . . ? C1 N1 N2 C4 -178.7(2) . . . . ? Co1 N1 N2 C4 -0.2(3) . . . . ? N3 C4 N2 C3 179.6(3) . . . . ? C5 C4 N2 C3 -1.6(4) . . . . ? N3 C4 N2 N1 -2.0(3) . . . . ? C5 C4 N2 N1 176.8(2) . . . . ? C5 C4 N3 C9 0.5(4) . . . . ? N2 C4 N3 C9 179.4(2) . . . . ? C5 C4 N3 Co1 -175.40(19) . . . . ? N2 C4 N3 Co1 3.5(3) . . . . ? C8 C9 N3 C4 -1.7(4) . . . . ? N4 C9 N3 C4 178.5(2) . . . . ? C8 C9 N3 Co1 174.25(19) . . . . ? N4 C9 N3 Co1 -5.6(3) . . . . ? O1 Co1 N3 C4 99.68(19) . . . . ? N1 Co1 N3 C4 -2.79(18) . . . . ? O4 Co1 N3 C4 -136.7(2) . . . . ? O6 Co1 N3 C4 -86.26(19) . . . . ? N5 Co1 N3 C4 -175.0(2) . . . . ? O3 Co1 N3 C4 60.0(2) . . . . ? O1 Co1 N3 C9 -76.20(19) . . . . ? N1 Co1 N3 C9 -178.67(19) . . . . ? O4 Co1 N3 C9 47.4(3) . . . . ? O6 Co1 N3 C9 97.86(19) . . . . ? N5 Co1 N3 C9 9.09(18) . . . . ? O3 Co1 N3 C9 -115.90(19) . . . . ? C11 C10 N4 N5 -0.4(3) . . . . ? C11 C10 N4 C9 178.8(2) . . . . ? N3 C9 N4 C10 176.0(2) . . . . ? C8 C9 N4 C10 -3.8(4) . . . . ? N3 C9 N4 N5 -4.8(3) . . . . ? C8 C9 N4 N5 175.3(2) . . . . ? C11 C12 N5 N4 0.1(3) . . . . ? C11 C12 N5 Co1 163.9(2) . . . . ? C10 N4 N5 C12 0.2(3) . . . . ? C9 N4 N5 C12 -179.1(2) . . . . ? C10 N4 N5 Co1 -168.33(17) . . . . ? C9 N4 N5 Co1 12.4(3) . . . . ? O1 Co1 N5 C12 -84.2(3) . . . . ? N3 Co1 N5 C12 -173.6(4) . . . . ? N1 Co1 N5 C12 173.4(3) . . . . ? O4 Co1 N5 C12 24.8(3) . . . . ? O6 Co1 N5 C12 82.8(3) . . . . ? O3 Co1 N5 C12 -44.1(4) . . . . ? O1 Co1 N5 N4 78.46(18) . . . . ? N3 Co1 N5 N4 -10.90(17) . . . . ? N1 Co1 N5 N4 -24.0(3) . . . . ? O4 Co1 N5 N4 -172.5(2) . . . . ? O6 Co1 N5 N4 -114.50(19) . . . . ? O3 Co1 N5 N4 118.60(18) . . . . ? O2 N6 O1 Co1 -173.4(3) . . . . ? O3 N6 O1 Co1 4.7(3) . . . . ? N3 Co1 O1 N6 -147.72(19) . . . . ? N1 Co1 O1 N6 -75.25(19) . . . . ? O4 Co1 O1 N6 58.6(2) . . . . ? O6 Co1 O1 N6 58.6(5) . . . . ? N5 Co1 O1 N6 139.44(19) . . . . ? O3 Co1 O1 N6 -2.68(18) . . . . ? O2 N6 O3 Co1 173.8(3) . . . . ? O1 N6 O3 Co1 -4.2(3) . . . . ? O1 Co1 O3 N6 2.72(19) . . . . ? N3 Co1 O3 N6 52.6(2) . . . . ? N1 Co1 O3 N6 111.9(2) . . . . ? O4 Co1 O3 N6 -118.8(2) . . . . ? O6 Co1 O3 N6 -164.44(19) . . . . ? N5 Co1 O3 N6 -47.6(3) . . . . ? O5 N7 O4 Co1 -178.0(3) . . . . ? O6 N7 O4 Co1 4.1(3) . . . . ? O1 Co1 O4 N7 177.48(19) . . . . ? N3 Co1 O4 N7 58.6(3) . . . . ? N1 Co1 O4 N7 -63.2(2) . . . . ? O6 Co1 O4 N7 -2.51(18) . . . . ? N5 Co1 O4 N7 95.2(2) . . . . ? O3 Co1 O4 N7 -134.1(2) . . . . ? O5 N7 O6 Co1 178.0(3) . . . . ? O4 N7 O6 Co1 -4.1(3) . . . . ? O1 Co1 O6 N7 2.5(5) . . . . ? N3 Co1 O6 N7 -150.40(18) . . . . ? N1 Co1 O6 N7 137.41(19) . . . . ? O4 Co1 O6 N7 2.51(18) . . . . ? N5 Co1 O6 N7 -77.47(19) . . . . ? O3 Co1 O6 N7 57.3(2) . . . . ? O8 C7 O7 C13 -3.4(5) . . . . ? C6 C7 O7 C13 177.6(3) . . . . ? C14 C13 O7 C7 -157.2(4) . . . . ? C14' C13 O7 C7 162.4(5) . . . . ? O7 C13 C14 C15 -71.6(7) . . . . ? C14' C13 C14 C15 17.0(7) . . . . ? C13 C14 C15 C16 176.5(6) . . . . ? C15' C16 C15 C14 -32.5(10) . . . . ? O7 C13 C14' C15' 71.8(10) . . . . ? C14 C13 C14' C15' -32.1(8) . . . . ? C13 C14' C15' C16 172.9(7) . . . . ? C15 C16 C15' C14' 19.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.706 _refine_diff_density_min -1.355 _refine_diff_density_rms 0.265 data_1cooling273K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.8490(11) _cell_length_b 25.942(3) _cell_length_c 8.1610(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.764(2) _cell_angle_gamma 90.00 _cell_volume 2048.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3763 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7743 _exptl_absorpt_correction_T_max 0.9155 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16941 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3763 _reflns_number_gt 3648 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.9698P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3763 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.44125(3) 0.375138(9) 0.79981(3) 0.03545(11) Uani 1 1 d . . . C1 C 0.5935(2) 0.47816(8) 0.6967(3) 0.0502(5) Uani 1 1 d . . . H1A H 0.5361 0.5028 0.7307 0.060 Uiso 1 1 calc R . . C2 C 0.7083(2) 0.48969(8) 0.6267(3) 0.0517(5) Uani 1 1 d . . . H2A H 0.7405 0.5222 0.6053 0.062 Uiso 1 1 calc R . . C3 C 0.7632(2) 0.44369(8) 0.5963(3) 0.0437(5) Uani 1 1 d . . . H3A H 0.8414 0.4385 0.5499 0.052 Uiso 1 1 calc R . . C4 C 0.69292(18) 0.35283(7) 0.6460(2) 0.0323(4) Uani 1 1 d . . . C5 C 0.79813(19) 0.32558(7) 0.5947(2) 0.0369(4) Uani 1 1 d . . . H5A H 0.8681 0.3422 0.5529 0.044 Uiso 1 1 calc R . . C6 C 0.79467(19) 0.27228(7) 0.6085(2) 0.0360(4) Uani 1 1 d . . . C7 C 0.9100(2) 0.24169(8) 0.5567(3) 0.0433(5) Uani 1 1 d . . . C8 C 0.68889(19) 0.24762(7) 0.6689(2) 0.0349(4) Uani 1 1 d . . . H8A H 0.6859 0.2119 0.6782 0.042 Uiso 1 1 calc R . . C9 C 0.58867(18) 0.27862(7) 0.7142(2) 0.0315(4) Uani 1 1 d . . . C10 C 0.4381(2) 0.21096(8) 0.8088(2) 0.0398(4) Uani 1 1 d . . . H10A H 0.4884 0.1812 0.7983 0.048 Uiso 1 1 calc R . . C11 C 0.3157(2) 0.21382(8) 0.8610(3) 0.0464(5) Uani 1 1 d . . . H11A H 0.2653 0.1867 0.8938 0.056 Uiso 1 1 calc R . . C12 C 0.2811(2) 0.26600(9) 0.8551(3) 0.0478(5) Uani 1 1 d . . . H12A H 0.2011 0.2792 0.8843 0.057 Uiso 1 1 calc R . . C13 C 1.0057(3) 0.15838(9) 0.5420(4) 0.0655(7) Uani 1 1 d . . . H13A H 1.0947 0.1753 0.5732 0.079 Uiso 1 1 calc R A 1 H13B H 0.9898 0.1517 0.4230 0.079 Uiso 1 1 calc R A 1 C14 C 1.0062(5) 0.10779(19) 0.6367(7) 0.0587(17) Uani 0.588(10) 1 d P B 1 H14A H 1.0890 0.0884 0.6292 0.070 Uiso 0.588(10) 1 calc PR B 1 H14B H 1.0061 0.1147 0.7535 0.070 Uiso 0.588(10) 1 calc PR B 1 C15 C 0.8805(7) 0.0771(2) 0.5631(10) 0.077(2) Uani 0.588(10) 1 d P B 1 H15A H 0.8835 0.0687 0.4479 0.093 Uiso 0.588(10) 1 calc PR B 1 H15B H 0.7982 0.0975 0.5645 0.093 Uiso 0.588(10) 1 calc PR B 1 C14' C 0.9380(9) 0.1025(3) 0.5250(10) 0.057(2) Uani 0.412(10) 1 d P B 2 H14C H 0.8474 0.1042 0.4538 0.069 Uiso 0.412(10) 1 calc PR B 2 H14D H 0.9951 0.0793 0.4738 0.069 Uiso 0.412(10) 1 calc PR B 2 C15' C 0.9248(13) 0.0828(3) 0.6896(12) 0.086(3) Uani 0.412(10) 1 d P B 2 H15C H 0.8592 0.1034 0.7363 0.103 Uiso 0.412(10) 1 calc PR B 2 H15D H 1.0134 0.0840 0.7650 0.103 Uiso 0.412(10) 1 calc PR B 2 C16 C 0.8730(5) 0.02578(13) 0.6643(5) 0.1144(14) Uani 1 1 d . . . H16A H 0.7921 0.0067 0.6152 0.137 Uiso 1 1 calc R B 1 H16B H 0.8684 0.0340 0.7778 0.137 Uiso 1 1 calc R B 1 H16C H 0.9538 0.0054 0.6616 0.137 Uiso 1 1 calc R B 1 N1 N 0.57607(16) 0.42807(6) 0.7089(2) 0.0407(4) Uani 1 1 d . . . N2 N 0.68267(16) 0.40649(6) 0.64613(19) 0.0349(3) Uani 1 1 d . . . N3 N 0.59072(15) 0.32993(6) 0.70531(18) 0.0312(3) Uani 1 1 d . . . N4 N 0.47357(16) 0.25992(6) 0.77460(19) 0.0334(3) Uani 1 1 d . . . N5 N 0.37602(17) 0.29442(6) 0.8031(2) 0.0413(4) Uani 1 1 d . . . N6 N 0.5300(2) 0.40168(7) 1.1124(2) 0.0497(4) Uani 1 1 d . . . N7 N 0.19063(19) 0.39510(7) 0.6634(3) 0.0551(5) Uani 1 1 d . . . O1 O 0.55312(17) 0.35963(6) 1.04282(18) 0.0501(4) Uani 1 1 d . . . O2 O 0.5674(2) 0.40763(8) 1.2624(2) 0.0766(6) Uani 1 1 d . . . O3 O 0.4651(2) 0.43465(7) 1.0186(2) 0.0750(6) Uani 1 1 d . . . O4 O 0.22888(19) 0.38969(7) 0.8188(2) 0.0675(5) Uani 1 1 d . . . O5 O 0.07125(19) 0.40276(9) 0.5983(4) 0.1008(8) Uani 1 1 d . . . O6 O 0.28654(16) 0.39253(6) 0.5802(2) 0.0535(4) Uani 1 1 d . . . O7 O 0.89650(16) 0.19192(6) 0.5814(2) 0.0566(4) Uani 1 1 d . B . O8 O 1.00092(17) 0.26104(7) 0.4997(3) 0.0674(5) 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 0.03489(16) 0.03331(16) 0.03980(17) 0.00080(10) 0.01127(11) 0.00505(10) C1 0.0583(13) 0.0306(10) 0.0624(14) -0.0012(9) 0.0132(11) 0.0051(9) C2 0.0596(14) 0.0333(11) 0.0618(14) 0.0051(9) 0.0105(11) -0.0066(9) C3 0.0440(11) 0.0394(11) 0.0496(11) 0.0060(9) 0.0133(9) -0.0077(9) C4 0.0329(9) 0.0318(9) 0.0321(9) -0.0018(7) 0.0060(7) -0.0020(7) C5 0.0339(9) 0.0378(10) 0.0414(10) -0.0015(8) 0.0129(8) -0.0030(8) C6 0.0333(9) 0.0369(10) 0.0386(10) -0.0042(8) 0.0087(8) 0.0014(8) C7 0.0370(10) 0.0431(11) 0.0512(12) -0.0063(9) 0.0117(9) 0.0025(8) C8 0.0362(10) 0.0302(9) 0.0389(10) -0.0020(7) 0.0084(8) 0.0001(7) C9 0.0322(9) 0.0318(9) 0.0308(9) -0.0010(7) 0.0065(7) -0.0035(7) C10 0.0470(11) 0.0323(10) 0.0411(10) 0.0021(8) 0.0112(9) -0.0043(8) C11 0.0484(12) 0.0466(12) 0.0465(11) 0.0046(9) 0.0148(9) -0.0121(9) C12 0.0388(11) 0.0505(12) 0.0588(13) -0.0011(10) 0.0213(10) -0.0056(9) C13 0.0620(15) 0.0469(13) 0.096(2) -0.0048(13) 0.0373(14) 0.0160(11) C14 0.060(3) 0.058(3) 0.057(3) -0.003(2) 0.006(3) 0.019(2) C15 0.071(3) 0.055(3) 0.104(6) 0.003(3) 0.009(3) 0.006(3) C14' 0.066(5) 0.047(4) 0.063(5) -0.005(3) 0.021(4) 0.013(3) C15' 0.143(9) 0.060(5) 0.063(6) 0.006(4) 0.040(6) 0.027(5) C16 0.159(4) 0.0549(19) 0.147(4) 0.010(2) 0.073(3) 0.008(2) N1 0.0416(9) 0.0330(9) 0.0495(10) -0.0009(7) 0.0139(8) 0.0040(7) N2 0.0352(8) 0.0307(8) 0.0397(8) 0.0006(6) 0.0097(7) -0.0009(6) N3 0.0313(7) 0.0302(8) 0.0332(8) -0.0009(6) 0.0089(6) -0.0004(6) N4 0.0336(8) 0.0309(8) 0.0376(8) -0.0006(6) 0.0112(6) -0.0013(6) N5 0.0341(8) 0.0387(9) 0.0544(10) -0.0004(7) 0.0168(7) 0.0014(7) N6 0.0656(12) 0.0406(10) 0.0438(10) -0.0011(8) 0.0123(9) 0.0019(8) N7 0.0379(10) 0.0425(10) 0.0829(15) 0.0033(10) 0.0066(10) 0.0029(8) O1 0.0687(10) 0.0372(8) 0.0452(8) -0.0012(6) 0.0124(7) 0.0099(7) O2 0.1157(16) 0.0705(12) 0.0402(9) -0.0110(8) 0.0058(9) -0.0057(11) O3 0.1142(16) 0.0538(10) 0.0607(11) 0.0082(8) 0.0260(10) 0.0342(10) O4 0.0676(11) 0.0679(11) 0.0749(12) 0.0088(9) 0.0340(10) 0.0220(9) O5 0.0380(10) 0.0921(16) 0.160(2) 0.0014(16) -0.0126(12) 0.0076(10) O6 0.0504(9) 0.0527(9) 0.0570(9) 0.0071(7) 0.0091(7) 0.0027(7) O7 0.0546(9) 0.0377(8) 0.0864(12) -0.0050(8) 0.0361(8) 0.0068(7) O8 0.0514(9) 0.0530(10) 0.1094(14) 0.0019(9) 0.0452(10) 0.0048(8) _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 O1 2.1196(15) . ? Co1 N3 2.1358(15) . ? Co1 N1 2.1372(16) . ? Co1 O4 2.1593(18) . ? Co1 O6 2.1722(16) . ? Co1 N5 2.1919(17) . ? Co1 O3 2.3389(19) . ? C1 N1 1.317(3) . ? C1 C2 1.391(3) . ? C1 H1A 0.9300 . ? C2 C3 1.352(3) . ? C2 H2A 0.9300 . ? C3 N2 1.358(2) . ? C3 H3A 0.9300 . ? C4 N3 1.335(2) . ? C4 C5 1.382(3) . ? C4 N2 1.396(2) . ? C5 C6 1.388(3) . ? C5 H5A 0.9300 . ? C6 C8 1.389(3) . ? C6 C7 1.509(3) . ? C7 O8 1.194(3) . ? C7 O7 1.317(3) . ? C8 C9 1.376(3) . ? C8 H8A 0.9300 . ? C9 N3 1.334(2) . ? C9 N4 1.404(2) . ? C10 C11 1.353(3) . ? C10 N4 1.360(2) . ? C10 H10A 0.9300 . ? C11 C12 1.395(3) . ? C11 H11A 0.9300 . ? C12 N5 1.321(3) . ? C12 H12A 0.9300 . ? C13 O7 1.465(3) . ? C13 C14 1.523(6) . ? C13 C14' 1.591(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.501(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.575(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C14' C15' 1.465(13) . ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' C16 1.565(10) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 N2 1.371(2) . ? N4 N5 1.365(2) . ? N6 O2 1.220(3) . ? N6 O3 1.243(2) . ? N6 O1 1.270(2) . ? N7 O5 1.213(3) . ? N7 O4 1.261(3) . ? N7 O6 1.264(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N3 87.75(6) . . ? O1 Co1 N1 101.46(6) . . ? N3 Co1 N1 73.30(6) . . ? O1 Co1 O4 107.90(7) . . ? N3 Co1 O4 149.78(7) . . ? N1 Co1 O4 125.84(7) . . ? O1 Co1 O6 166.78(6) . . ? N3 Co1 O6 103.93(6) . . ? N1 Co1 O6 88.03(6) . . ? O4 Co1 O6 58.88(7) . . ? O1 Co1 N5 84.80(6) . . ? N3 Co1 N5 72.74(6) . . ? N1 Co1 N5 145.15(6) . . ? O4 Co1 N5 82.88(7) . . ? O6 Co1 N5 92.67(6) . . ? O1 Co1 O3 56.67(6) . . ? N3 Co1 O3 131.34(7) . . ? N1 Co1 O3 81.99(7) . . ? O4 Co1 O3 77.89(8) . . ? O6 Co1 O3 116.60(6) . . ? N5 Co1 O3 127.51(7) . . ? N1 C1 C2 111.78(19) . . ? N1 C1 H1A 124.1 . . ? C2 C1 H1A 124.1 . . ? C3 C2 C1 105.59(19) . . ? C3 C2 H2A 127.2 . . ? C1 C2 H2A 127.2 . . ? C2 C3 N2 107.25(19) . . ? C2 C3 H3A 126.4 . . ? N2 C3 H3A 126.4 . . ? N3 C4 C5 122.75(17) . . ? N3 C4 N2 112.58(15) . . ? C5 C4 N2 124.66(16) . . ? C4 C5 C6 116.98(17) . . ? C4 C5 H5A 121.5 . . ? C6 C5 H5A 121.5 . . ? C5 C6 C8 121.26(17) . . ? C5 C6 C7 118.02(17) . . ? C8 C6 C7 120.72(17) . . ? O8 C7 O7 125.17(19) . . ? O8 C7 C6 123.1(2) . . ? O7 C7 C6 111.70(17) . . ? C9 C8 C6 116.70(17) . . ? C9 C8 H8A 121.7 . . ? C6 C8 H8A 121.7 . . ? N3 C9 C8 123.35(16) . . ? N3 C9 N4 112.67(15) . . ? C8 C9 N4 123.98(16) . . ? C11 C10 N4 106.94(18) . . ? C11 C10 H10A 126.5 . . ? N4 C10 H10A 126.5 . . ? C10 C11 C12 105.59(18) . . ? C10 C11 H11A 127.2 . . ? C12 C11 H11A 127.2 . . ? N5 C12 C11 111.70(19) . . ? N5 C12 H12A 124.2 . . ? C11 C12 H12A 124.2 . . ? O7 C13 C14 109.5(3) . . ? O7 C13 C14' 104.3(3) . . ? C14 C13 C14' 38.8(3) . . ? O7 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? C14' C13 H13A 141.0 . . ? O7 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? C14' C13 H13B 76.3 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C13 109.3(5) . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C14 C15 C16 110.8(5) . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15' C14' C13 110.3(7) . . ? C15' C14' H14C 109.6 . . ? C13 C14' H14C 109.6 . . ? C15' C14' H14D 109.6 . . ? C13 C14' H14D 109.6 . . ? H14C C14' H14D 108.1 . . ? C14' C15' C16 107.0(7) . . ? C14' C15' H15C 110.3 . . ? C16 C15' H15C 110.3 . . ? C14' C15' H15D 110.3 . . ? C16 C15' H15D 110.3 . . ? H15C C15' H15D 108.6 . . ? C15' C16 C15 39.2(3) . . ? C15' C16 H16A 140.1 . . ? C15 C16 H16A 109.5 . . ? C15' C16 H16B 74.7 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15' C16 H16C 105.8 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 N2 104.76(16) . . ? C1 N1 Co1 139.35(15) . . ? N2 N1 Co1 115.86(11) . . ? C3 N2 N1 110.62(16) . . ? C3 N2 C4 131.45(16) . . ? N1 N2 C4 117.92(14) . . ? C9 N3 C4 118.94(15) . . ? C9 N3 Co1 120.67(12) . . ? C4 N3 Co1 120.26(12) . . ? C10 N4 N5 111.21(15) . . ? C10 N4 C9 130.52(16) . . ? N5 N4 C9 118.26(15) . . ? C12 N5 N4 104.56(16) . . ? C12 N5 Co1 139.80(14) . . ? N4 N5 Co1 114.03(11) . . ? O2 N6 O3 123.7(2) . . ? O2 N6 O1 120.77(19) . . ? O3 N6 O1 115.49(18) . . ? O5 N7 O4 122.8(2) . . ? O5 N7 O6 122.3(3) . . ? O4 N7 O6 114.93(18) . . ? N6 O1 Co1 98.63(12) . . ? N6 O3 Co1 89.01(13) . . ? N7 O4 Co1 93.37(12) . . ? N7 O6 Co1 92.69(13) . . ? C7 O7 C13 116.71(17) . . ? 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 N1 C1 C2 C3 -0.4(3) . . . . ? C1 C2 C3 N2 0.3(2) . . . . ? N3 C4 C5 C6 -0.5(3) . . . . ? N2 C4 C5 C6 177.78(16) . . . . ? C4 C5 C6 C8 0.9(3) . . . . ? C4 C5 C6 C7 -178.75(17) . . . . ? C5 C6 C7 O8 -2.5(3) . . . . ? C8 C6 C7 O8 177.8(2) . . . . ? C5 C6 C7 O7 177.86(18) . . . . ? C8 C6 C7 O7 -1.8(3) . . . . ? C5 C6 C8 C9 -0.1(3) . . . . ? C7 C6 C8 C9 179.55(17) . . . . ? C6 C8 C9 N3 -1.2(3) . . . . ? C6 C8 C9 N4 178.80(16) . . . . ? N4 C10 C11 C12 0.3(2) . . . . ? C10 C11 C12 N5 -0.2(3) . . . . ? O7 C13 C14 C15 70.9(5) . . . . ? C14' C13 C14 C15 -17.9(5) . . . . ? C13 C14 C15 C16 -176.8(4) . . . . ? O7 C13 C14' C15' -72.5(7) . . . . ? C14 C13 C14' C15' 30.9(6) . . . . ? C13 C14' C15' C16 -173.9(5) . . . . ? C14' C15' C16 C15 -19.3(5) . . . . ? C14 C15 C16 C15' 31.4(6) . . . . ? C2 C1 N1 N2 0.3(2) . . . . ? C2 C1 N1 Co1 177.96(16) . . . . ? O1 Co1 N1 C1 -94.9(2) . . . . ? N3 Co1 N1 C1 -179.1(2) . . . . ? O4 Co1 N1 C1 27.3(3) . . . . ? O6 Co1 N1 C1 75.8(2) . . . . ? N5 Co1 N1 C1 167.6(2) . . . . ? O3 Co1 N1 C1 -41.4(2) . . . . ? O1 Co1 N1 N2 82.50(13) . . . . ? N3 Co1 N1 N2 -1.61(12) . . . . ? O4 Co1 N1 N2 -155.27(12) . . . . ? O6 Co1 N1 N2 -106.78(13) . . . . ? N5 Co1 N1 N2 -14.9(2) . . . . ? O3 Co1 N1 N2 136.01(14) . . . . ? C2 C3 N2 N1 -0.1(2) . . . . ? C2 C3 N2 C4 -178.79(19) . . . . ? C1 N1 N2 C3 -0.1(2) . . . . ? Co1 N1 N2 C3 -178.42(13) . . . . ? C1 N1 N2 C4 178.74(16) . . . . ? Co1 N1 N2 C4 0.5(2) . . . . ? N3 C4 N2 C3 -179.57(19) . . . . ? C5 C4 N2 C3 2.0(3) . . . . ? N3 C4 N2 N1 1.8(2) . . . . ? C5 C4 N2 N1 -176.65(17) . . . . ? C8 C9 N3 C4 1.6(3) . . . . ? N4 C9 N3 C4 -178.39(15) . . . . ? C8 C9 N3 Co1 -174.18(13) . . . . ? N4 C9 N3 Co1 5.81(19) . . . . ? C5 C4 N3 C9 -0.7(3) . . . . ? N2 C4 N3 C9 -179.19(15) . . . . ? C5 C4 N3 Co1 175.12(14) . . . . ? N2 C4 N3 Co1 -3.4(2) . . . . ? O1 Co1 N3 C9 75.86(13) . . . . ? N1 Co1 N3 C9 178.54(14) . . . . ? O4 Co1 N3 C9 -47.1(2) . . . . ? O6 Co1 N3 C9 -97.86(13) . . . . ? N5 Co1 N3 C9 -9.39(13) . . . . ? O3 Co1 N3 C9 115.78(14) . . . . ? O1 Co1 N3 C4 -99.88(13) . . . . ? N1 Co1 N3 C4 2.80(13) . . . . ? O4 Co1 N3 C4 137.19(15) . . . . ? O6 Co1 N3 C4 86.40(14) . . . . ? N5 Co1 N3 C4 174.87(14) . . . . ? O3 Co1 N3 C4 -59.96(15) . . . . ? C11 C10 N4 N5 -0.2(2) . . . . ? C11 C10 N4 C9 -178.81(18) . . . . ? N3 C9 N4 C10 -176.55(17) . . . . ? C8 C9 N4 C10 3.4(3) . . . . ? N3 C9 N4 N5 5.0(2) . . . . ? C8 C9 N4 N5 -175.05(17) . . . . ? C11 C12 N5 N4 0.1(2) . . . . ? C11 C12 N5 Co1 -163.48(17) . . . . ? C10 N4 N5 C12 0.1(2) . . . . ? C9 N4 N5 C12 178.85(16) . . . . ? C10 N4 N5 Co1 168.56(12) . . . . ? C9 N4 N5 Co1 -12.7(2) . . . . ? O1 Co1 N5 C12 84.5(2) . . . . ? N3 Co1 N5 C12 173.7(2) . . . . ? N1 Co1 N5 C12 -172.9(2) . . . . ? O4 Co1 N5 C12 -24.3(2) . . . . ? O6 Co1 N5 C12 -82.5(2) . . . . ? O3 Co1 N5 C12 44.4(3) . . . . ? O1 Co1 N5 N4 -78.10(13) . . . . ? N3 Co1 N5 N4 11.15(12) . . . . ? N1 Co1 N5 N4 24.5(2) . . . . ? O4 Co1 N5 N4 173.09(14) . . . . ? O6 Co1 N5 N4 114.91(13) . . . . ? O3 Co1 N5 N4 -118.16(13) . . . . ? O2 N6 O1 Co1 173.7(2) . . . . ? O3 N6 O1 Co1 -4.6(2) . . . . ? N3 Co1 O1 N6 147.42(13) . . . . ? N1 Co1 O1 N6 74.96(13) . . . . ? O4 Co1 O1 N6 -58.93(14) . . . . ? O6 Co1 O1 N6 -60.2(3) . . . . ? N5 Co1 O1 N6 -139.71(13) . . . . ? O3 Co1 O1 N6 2.63(13) . . . . ? O2 N6 O3 Co1 -174.1(2) . . . . ? O1 N6 O3 Co1 4.1(2) . . . . ? O1 Co1 O3 N6 -2.65(13) . . . . ? N3 Co1 O3 N6 -52.77(17) . . . . ? N1 Co1 O3 N6 -112.08(15) . . . . ? O4 Co1 O3 N6 118.50(15) . . . . ? O6 Co1 O3 N6 164.19(13) . . . . ? N5 Co1 O3 N6 47.44(17) . . . . ? O5 N7 O4 Co1 177.4(2) . . . . ? O6 N7 O4 Co1 -3.42(19) . . . . ? O1 Co1 O4 N7 -177.55(12) . . . . ? N3 Co1 O4 N7 -59.34(19) . . . . ? N1 Co1 O4 N7 63.05(16) . . . . ? O6 Co1 O4 N7 2.11(12) . . . . ? N5 Co1 O4 N7 -95.38(14) . . . . ? O3 Co1 O4 N7 133.74(14) . . . . ? O5 N7 O6 Co1 -177.4(2) . . . . ? O4 N7 O6 Co1 3.40(19) . . . . ? O1 Co1 O6 N7 -0.7(3) . . . . ? N3 Co1 O6 N7 150.80(12) . . . . ? N1 Co1 O6 N7 -136.94(12) . . . . ? O4 Co1 O6 N7 -2.10(12) . . . . ? N5 Co1 O6 N7 77.93(12) . . . . ? O3 Co1 O6 N7 -56.91(14) . . . . ? O8 C7 O7 C13 2.8(4) . . . . ? C6 C7 O7 C13 -177.6(2) . . . . ? C14 C13 O7 C7 158.1(3) . . . . ? C14' C13 O7 C7 -161.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.255 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.047 data_1cooling238K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.8458(15) _cell_length_b 25.898(4) _cell_length_c 8.1434(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.839(3) _cell_angle_gamma 90.00 _cell_volume 2039.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used 3742 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7735 _exptl_absorpt_correction_T_max 0.9152 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16901 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3742 _reflns_number_gt 3639 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.9547P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3742 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.44336(2) 0.375290(9) 0.80030(3) 0.03049(10) Uani 1 1 d . . . C1 C 0.5947(2) 0.47859(7) 0.6962(3) 0.0434(5) Uani 1 1 d . . . H1A H 0.5364 0.5035 0.7303 0.052 Uiso 1 1 calc R . . C2 C 0.7098(2) 0.49032(8) 0.6260(3) 0.0449(5) Uani 1 1 d . . . H2A H 0.7422 0.5233 0.6041 0.054 Uiso 1 1 calc R . . C3 C 0.7649(2) 0.44410(7) 0.5960(2) 0.0379(4) Uani 1 1 d . . . H3A H 0.8442 0.4388 0.5493 0.045 Uiso 1 1 calc R . . C4 C 0.69517(17) 0.35300(6) 0.6463(2) 0.0279(3) Uani 1 1 d . . . C5 C 0.80065(18) 0.32583(7) 0.5950(2) 0.0322(4) Uani 1 1 d . . . H5A H 0.8712 0.3427 0.5526 0.039 Uiso 1 1 calc R . . C6 C 0.79764(18) 0.27233(7) 0.6091(2) 0.0319(4) Uani 1 1 d . . . C7 C 0.91295(19) 0.24183(7) 0.5572(2) 0.0373(4) Uani 1 1 d . . . C8 C 0.69163(17) 0.24755(7) 0.6696(2) 0.0303(4) Uani 1 1 d . . . H8A H 0.6887 0.2114 0.6791 0.036 Uiso 1 1 calc R . . C9 C 0.59130(17) 0.27864(6) 0.71494(19) 0.0270(3) Uani 1 1 d . . . C10 C 0.44071(19) 0.21073(7) 0.8099(2) 0.0346(4) Uani 1 1 d . . . H10A H 0.4917 0.1806 0.7997 0.042 Uiso 1 1 calc R . . C11 C 0.3181(2) 0.21368(8) 0.8619(2) 0.0404(4) Uani 1 1 d . . . H11A H 0.2670 0.1862 0.8954 0.049 Uiso 1 1 calc R . . C12 C 0.2833(2) 0.26592(8) 0.8553(3) 0.0412(4) Uani 1 1 d . . . H12A H 0.2023 0.2793 0.8845 0.049 Uiso 1 1 calc R . . C13 C 1.0091(2) 0.15836(9) 0.5424(3) 0.0574(6) Uani 1 1 d . . . H13A H 1.0991 0.1753 0.5749 0.069 Uiso 1 1 calc R A 1 H13B H 0.9934 0.1518 0.4218 0.069 Uiso 1 1 calc R A 1 C14 C 1.0088(4) 0.10743(15) 0.6366(6) 0.0475(13) Uani 0.602(8) 1 d P B 1 H14A H 1.0920 0.0876 0.6285 0.057 Uiso 0.602(8) 1 calc PR B 1 H14B H 1.0092 0.1143 0.7550 0.057 Uiso 0.602(8) 1 calc PR B 1 C15 C 0.8812(5) 0.07655(19) 0.5624(8) 0.0635(15) Uani 0.602(8) 1 d P B 1 H15A H 0.8837 0.0681 0.4457 0.076 Uiso 0.602(8) 1 calc PR B 1 H15B H 0.7984 0.0973 0.5643 0.076 Uiso 0.602(8) 1 calc PR B 1 C14' C 0.9393(8) 0.1019(3) 0.5252(9) 0.050(2) Uani 0.398(8) 1 d P B 2 H14C H 0.8475 0.1037 0.4538 0.060 Uiso 0.398(8) 1 calc PR B 2 H14D H 0.9962 0.0781 0.4734 0.060 Uiso 0.398(8) 1 calc PR B 2 C15' C 0.9273(11) 0.0829(3) 0.6899(11) 0.076(3) Uani 0.398(8) 1 d P B 2 H15C H 0.8617 0.1040 0.7375 0.092 Uiso 0.398(8) 1 calc PR B 2 H15D H 1.0173 0.0840 0.7657 0.092 Uiso 0.398(8) 1 calc PR B 2 C16 C 0.8737(4) 0.02547(11) 0.6634(5) 0.0992(12) Uani 1 1 d . . . H16A H 0.7914 0.0063 0.6142 0.149 Uiso 1 1 calc R B 1 H16B H 0.8700 0.0338 0.7786 0.149 Uiso 1 1 calc R B 1 H16C H 0.9550 0.0046 0.6599 0.149 Uiso 1 1 calc R B 1 N1 N 0.57754(15) 0.42837(6) 0.70892(19) 0.0353(3) Uani 1 1 d . . . N2 N 0.68450(15) 0.40678(5) 0.64600(18) 0.0301(3) Uani 1 1 d . . . N3 N 0.59298(14) 0.33009(5) 0.70583(17) 0.0273(3) Uani 1 1 d . . . N4 N 0.47597(15) 0.25982(5) 0.77510(18) 0.0291(3) Uani 1 1 d . . . N5 N 0.37831(16) 0.29440(6) 0.8031(2) 0.0360(3) Uani 1 1 d . . . N6 N 0.53266(18) 0.40187(6) 1.1132(2) 0.0425(4) Uani 1 1 d . . . N7 N 0.19265(17) 0.39530(7) 0.6649(3) 0.0477(4) Uani 1 1 d . . . O1 O 0.55558(15) 0.35956(5) 1.04329(17) 0.0433(3) Uani 1 1 d . . . O2 O 0.5707(2) 0.40788(7) 1.26370(19) 0.0659(5) Uani 1 1 d . . . O3 O 0.4680(2) 0.43504(6) 1.0192(2) 0.0641(5) Uani 1 1 d . . . O4 O 0.23136(17) 0.38974(6) 0.8207(2) 0.0581(4) Uani 1 1 d . . . O5 O 0.07248(17) 0.40292(8) 0.6008(3) 0.0872(7) Uani 1 1 d . . . O6 O 0.28769(15) 0.39260(6) 0.58041(18) 0.0456(3) Uani 1 1 d . . . O7 O 0.89963(15) 0.19184(5) 0.5822(2) 0.0497(4) Uani 1 1 d . B . O8 O 1.00360(16) 0.26117(6) 0.4998(2) 0.0585(4) 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 0.03020(15) 0.02850(15) 0.03435(15) 0.00072(9) 0.01010(10) 0.00436(9) C1 0.0497(11) 0.0268(9) 0.0546(12) -0.0011(8) 0.0118(9) 0.0047(8) C2 0.0530(12) 0.0288(10) 0.0524(12) 0.0044(8) 0.0089(10) -0.0053(8) C3 0.0388(10) 0.0343(10) 0.0420(10) 0.0051(8) 0.0114(8) -0.0070(8) C4 0.0277(8) 0.0278(8) 0.0283(8) -0.0013(6) 0.0056(6) -0.0020(7) C5 0.0296(9) 0.0325(9) 0.0363(9) -0.0009(7) 0.0108(7) -0.0026(7) C6 0.0300(9) 0.0324(9) 0.0336(9) -0.0039(7) 0.0068(7) 0.0016(7) C7 0.0321(9) 0.0378(10) 0.0431(10) -0.0046(8) 0.0096(8) 0.0022(8) C8 0.0312(9) 0.0262(8) 0.0342(9) -0.0018(7) 0.0077(7) 0.0004(7) C9 0.0276(8) 0.0272(8) 0.0264(8) -0.0006(6) 0.0059(6) -0.0028(7) C10 0.0412(10) 0.0289(9) 0.0347(9) 0.0013(7) 0.0098(8) -0.0035(7) C11 0.0413(10) 0.0418(11) 0.0403(10) 0.0035(8) 0.0130(8) -0.0113(8) C12 0.0332(10) 0.0443(11) 0.0499(11) -0.0011(9) 0.0178(8) -0.0044(8) C13 0.0541(13) 0.0417(12) 0.0848(17) -0.0043(11) 0.0342(12) 0.0133(10) C14 0.048(2) 0.046(2) 0.047(3) -0.0021(17) 0.006(2) 0.0152(18) C15 0.058(3) 0.043(2) 0.088(4) 0.002(2) 0.010(3) 0.000(2) C14' 0.056(4) 0.041(4) 0.055(4) -0.007(3) 0.015(3) 0.013(3) C15' 0.124(7) 0.049(4) 0.063(5) 0.003(3) 0.036(5) 0.023(4) C16 0.136(3) 0.0469(16) 0.130(3) 0.0072(17) 0.063(3) 0.0059(17) N1 0.0363(8) 0.0285(8) 0.0429(9) -0.0017(6) 0.0119(7) 0.0039(6) N2 0.0304(7) 0.0265(7) 0.0344(8) 0.0012(6) 0.0084(6) -0.0005(6) N3 0.0273(7) 0.0259(7) 0.0294(7) -0.0012(5) 0.0072(5) 0.0000(6) N4 0.0295(7) 0.0266(7) 0.0327(7) -0.0010(6) 0.0098(6) -0.0005(6) N5 0.0304(8) 0.0332(8) 0.0472(9) -0.0004(7) 0.0143(7) 0.0017(6) N6 0.0555(10) 0.0354(9) 0.0379(9) -0.0014(7) 0.0116(8) 0.0005(7) N7 0.0328(9) 0.0358(9) 0.0728(13) 0.0017(8) 0.0058(9) 0.0026(7) O1 0.0593(9) 0.0322(7) 0.0392(7) -0.0012(6) 0.0110(6) 0.0088(6) O2 0.0978(14) 0.0617(10) 0.0352(8) -0.0104(7) 0.0051(8) -0.0047(9) O3 0.0978(13) 0.0461(9) 0.0516(9) 0.0071(7) 0.0225(9) 0.0296(9) O4 0.0579(10) 0.0588(10) 0.0643(11) 0.0074(8) 0.0290(8) 0.0185(8) O5 0.0314(9) 0.0774(13) 0.142(2) 0.0008(13) -0.0103(10) 0.0073(8) O6 0.0432(8) 0.0449(8) 0.0480(8) 0.0064(6) 0.0071(6) 0.0024(6) O7 0.0487(8) 0.0325(7) 0.0763(10) -0.0042(7) 0.0332(8) 0.0064(6) O8 0.0451(8) 0.0458(8) 0.0949(12) 0.0023(8) 0.0395(8) 0.0042(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 O1 2.1166(14) . ? Co1 N1 2.1350(16) . ? Co1 N3 2.1351(14) . ? Co1 O4 2.1576(16) . ? Co1 O6 2.1736(14) . ? Co1 N5 2.1921(16) . ? Co1 O3 2.3386(17) . ? C1 N1 1.318(2) . ? C1 C2 1.395(3) . ? C1 H1A 0.9400 . ? C2 C3 1.355(3) . ? C2 H2A 0.9400 . ? C3 N2 1.359(2) . ? C3 H3A 0.9400 . ? C4 N3 1.335(2) . ? C4 C5 1.383(2) . ? C4 N2 1.397(2) . ? C5 C6 1.391(2) . ? C5 H5A 0.9400 . ? C6 C8 1.392(2) . ? C6 C7 1.507(2) . ? C7 O8 1.193(2) . ? C7 O7 1.321(2) . ? C8 C9 1.377(2) . ? C8 H8A 0.9400 . ? C9 N3 1.335(2) . ? C9 N4 1.406(2) . ? C10 C11 1.355(3) . ? C10 N4 1.362(2) . ? C10 H10A 0.9400 . ? C11 C12 1.394(3) . ? C11 H11A 0.9400 . ? C12 N5 1.323(2) . ? C12 H12A 0.9400 . ? C13 O7 1.467(2) . ? C13 C14 1.526(5) . ? C13 C14' 1.612(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.515(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.567(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C14' C15' 1.453(12) . ? C14' H14C 0.9800 . ? C14' H14D 0.9800 . ? C15' C16 1.581(9) . ? C15' H15C 0.9800 . ? C15' H15D 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? N1 N2 1.374(2) . ? N4 N5 1.364(2) . ? N6 O2 1.222(2) . ? N6 O3 1.243(2) . ? N6 O1 1.274(2) . ? N7 O5 1.216(2) . ? N7 O4 1.263(2) . ? N7 O6 1.263(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N1 101.62(6) . . ? O1 Co1 N3 87.54(5) . . ? N1 Co1 N3 73.34(6) . . ? O1 Co1 O4 107.68(6) . . ? N1 Co1 O4 125.89(6) . . ? N3 Co1 O4 149.99(6) . . ? O1 Co1 O6 166.69(6) . . ? N1 Co1 O6 88.10(6) . . ? N3 Co1 O6 104.10(5) . . ? O4 Co1 O6 59.02(6) . . ? O1 Co1 N5 84.75(6) . . ? N1 Co1 N5 145.09(6) . . ? N3 Co1 N5 72.69(5) . . ? O4 Co1 N5 82.89(6) . . ? O6 Co1 N5 92.49(6) . . ? O1 Co1 O3 56.88(5) . . ? N1 Co1 O3 81.80(6) . . ? N3 Co1 O3 131.14(6) . . ? O4 Co1 O3 77.85(7) . . ? O6 Co1 O3 116.59(6) . . ? N5 Co1 O3 127.81(6) . . ? N1 C1 C2 111.92(18) . . ? N1 C1 H1A 124.0 . . ? C2 C1 H1A 124.0 . . ? C3 C2 C1 105.37(17) . . ? C3 C2 H2A 127.3 . . ? C1 C2 H2A 127.3 . . ? C2 C3 N2 107.36(17) . . ? C2 C3 H3A 126.3 . . ? N2 C3 H3A 126.3 . . ? N3 C4 C5 122.93(16) . . ? N3 C4 N2 112.48(14) . . ? C5 C4 N2 124.57(15) . . ? C4 C5 C6 116.95(16) . . ? C4 C5 H5A 121.5 . . ? C6 C5 H5A 121.5 . . ? C5 C6 C8 121.16(16) . . ? C5 C6 C7 118.04(16) . . ? C8 C6 C7 120.80(16) . . ? O8 C7 O7 125.12(18) . . ? O8 C7 C6 123.25(18) . . ? O7 C7 C6 111.63(16) . . ? C9 C8 C6 116.65(16) . . ? C9 C8 H8A 121.7 . . ? C6 C8 H8A 121.7 . . ? N3 C9 C8 123.48(15) . . ? N3 C9 N4 112.62(14) . . ? C8 C9 N4 123.90(15) . . ? C11 C10 N4 106.83(16) . . ? C11 C10 H10A 126.6 . . ? N4 C10 H10A 126.6 . . ? C10 C11 C12 105.64(17) . . ? C10 C11 H11A 127.2 . . ? C12 C11 H11A 127.2 . . ? N5 C12 C11 111.70(17) . . ? N5 C12 H12A 124.1 . . ? C11 C12 H12A 124.1 . . ? O7 C13 C14 109.2(2) . . ? O7 C13 C14' 103.7(3) . . ? C14 C13 C14' 38.5(3) . . ? O7 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? C14' C13 H13A 141.3 . . ? O7 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? C14' C13 H13B 76.8 . . ? H13A C13 H13B 108.3 . . ? C15 C14 C13 109.6(4) . . ? C15 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C14 C15 C16 110.7(4) . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15' C14' C13 109.5(6) . . ? C15' C14' H14C 109.8 . . ? C13 C14' H14C 109.8 . . ? C15' C14' H14D 109.8 . . ? C13 C14' H14D 109.8 . . ? H14C C14' H14D 108.2 . . ? C14' C15' C16 105.9(7) . . ? C14' C15' H15C 110.6 . . ? C16 C15' H15C 110.6 . . ? C14' C15' H15D 110.6 . . ? C16 C15' H15D 110.6 . . ? H15C C15' H15D 108.7 . . ? C15 C16 C15' 39.6(3) . . ? C15 C16 H16A 109.5 . . ? C15' C16 H16A 140.3 . . ? C15 C16 H16B 109.5 . . ? C15' C16 H16B 74.3 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? C15' C16 H16C 105.7 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 N2 104.69(15) . . ? C1 N1 Co1 139.43(14) . . ? N2 N1 Co1 115.84(11) . . ? C3 N2 N1 110.66(15) . . ? C3 N2 C4 131.43(15) . . ? N1 N2 C4 117.89(13) . . ? C9 N3 C4 118.81(14) . . ? C9 N3 Co1 120.71(11) . . ? C4 N3 Co1 120.34(11) . . ? C10 N4 N5 111.27(14) . . ? C10 N4 C9 130.57(15) . . ? N5 N4 C9 118.15(14) . . ? C12 N5 N4 104.55(15) . . ? C12 N5 Co1 139.62(13) . . ? N4 N5 Co1 114.15(11) . . ? O2 N6 O3 123.63(18) . . ? O2 N6 O1 120.71(17) . . ? O3 N6 O1 115.64(16) . . ? O5 N7 O4 122.4(2) . . ? O5 N7 O6 122.4(2) . . ? O4 N7 O6 115.25(16) . . ? N6 O1 Co1 98.45(11) . . ? N6 O3 Co1 88.83(11) . . ? N7 O4 Co1 93.20(11) . . ? N7 O6 Co1 92.44(12) . . ? C7 O7 C13 116.55(16) . . ? 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 N1 C1 C2 C3 -0.4(2) . . . . ? C1 C2 C3 N2 0.4(2) . . . . ? N3 C4 C5 C6 -0.6(3) . . . . ? N2 C4 C5 C6 177.85(15) . . . . ? C4 C5 C6 C8 1.0(3) . . . . ? C4 C5 C6 C7 -178.83(16) . . . . ? C5 C6 C7 O8 -2.6(3) . . . . ? C8 C6 C7 O8 177.6(2) . . . . ? C5 C6 C7 O7 177.91(16) . . . . ? C8 C6 C7 O7 -1.9(2) . . . . ? C5 C6 C8 C9 -0.2(3) . . . . ? C7 C6 C8 C9 179.60(16) . . . . ? C6 C8 C9 N3 -1.1(3) . . . . ? C6 C8 C9 N4 178.68(15) . . . . ? N4 C10 C11 C12 0.3(2) . . . . ? C10 C11 C12 N5 -0.3(2) . . . . ? O7 C13 C14 C15 70.4(4) . . . . ? C14' C13 C14 C15 -17.6(4) . . . . ? C13 C14 C15 C16 -176.7(3) . . . . ? O7 C13 C14' C15' -72.6(6) . . . . ? C14 C13 C14' C15' 31.1(5) . . . . ? C13 C14' C15' C16 -173.9(4) . . . . ? C14 C15 C16 C15' 31.3(5) . . . . ? C14' C15' C16 C15 -19.4(4) . . . . ? C2 C1 N1 N2 0.2(2) . . . . ? C2 C1 N1 Co1 177.89(15) . . . . ? O1 Co1 N1 C1 -95.3(2) . . . . ? N3 Co1 N1 C1 -179.1(2) . . . . ? O4 Co1 N1 C1 26.9(2) . . . . ? O6 Co1 N1 C1 75.6(2) . . . . ? N5 Co1 N1 C1 167.20(19) . . . . ? O3 Co1 N1 C1 -41.6(2) . . . . ? O1 Co1 N1 N2 82.22(12) . . . . ? N3 Co1 N1 N2 -1.63(11) . . . . ? O4 Co1 N1 N2 -155.68(11) . . . . ? O6 Co1 N1 N2 -106.96(12) . . . . ? N5 Co1 N1 N2 -15.34(18) . . . . ? O3 Co1 N1 N2 135.83(12) . . . . ? C2 C3 N2 N1 -0.2(2) . . . . ? C2 C3 N2 C4 -178.74(17) . . . . ? C1 N1 N2 C3 0.0(2) . . . . ? Co1 N1 N2 C3 -178.31(12) . . . . ? C1 N1 N2 C4 178.73(15) . . . . ? Co1 N1 N2 C4 0.43(18) . . . . ? N3 C4 N2 C3 -179.66(17) . . . . ? C5 C4 N2 C3 1.8(3) . . . . ? N3 C4 N2 N1 1.9(2) . . . . ? C5 C4 N2 N1 -176.65(16) . . . . ? C8 C9 N3 C4 1.6(2) . . . . ? N4 C9 N3 C4 -178.24(14) . . . . ? C8 C9 N3 Co1 -174.20(12) . . . . ? N4 C9 N3 Co1 6.01(18) . . . . ? C5 C4 N3 C9 -0.7(2) . . . . ? N2 C4 N3 C9 -179.27(14) . . . . ? C5 C4 N3 Co1 175.10(13) . . . . ? N2 C4 N3 Co1 -3.50(18) . . . . ? O1 Co1 N3 C9 75.68(13) . . . . ? N1 Co1 N3 C9 178.57(13) . . . . ? O4 Co1 N3 C9 -46.56(18) . . . . ? O6 Co1 N3 C9 -97.79(13) . . . . ? N5 Co1 N3 C9 -9.59(12) . . . . ? O3 Co1 N3 C9 115.89(13) . . . . ? O1 Co1 N3 C4 -100.01(13) . . . . ? N1 Co1 N3 C4 2.88(12) . . . . ? O4 Co1 N3 C4 137.74(14) . . . . ? O6 Co1 N3 C4 86.52(13) . . . . ? N5 Co1 N3 C4 174.72(13) . . . . ? O3 Co1 N3 C4 -59.80(14) . . . . ? C11 C10 N4 N5 -0.2(2) . . . . ? C11 C10 N4 C9 -178.97(16) . . . . ? N3 C9 N4 C10 -176.38(16) . . . . ? C8 C9 N4 C10 3.8(3) . . . . ? N3 C9 N4 N5 4.9(2) . . . . ? C8 C9 N4 N5 -174.88(16) . . . . ? C11 C12 N5 N4 0.1(2) . . . . ? C11 C12 N5 Co1 -163.14(15) . . . . ? C10 N4 N5 C12 0.0(2) . . . . ? C9 N4 N5 C12 178.98(15) . . . . ? C10 N4 N5 Co1 168.25(11) . . . . ? C9 N4 N5 Co1 -12.80(19) . . . . ? O1 Co1 N5 C12 84.5(2) . . . . ? N1 Co1 N5 C12 -172.69(19) . . . . ? N3 Co1 N5 C12 173.6(2) . . . . ? O4 Co1 N5 C12 -24.1(2) . . . . ? O6 Co1 N5 C12 -82.4(2) . . . . ? O3 Co1 N5 C12 44.5(2) . . . . ? O1 Co1 N5 N4 -77.73(12) . . . . ? N1 Co1 N5 N4 25.08(18) . . . . ? N3 Co1 N5 N4 11.33(11) . . . . ? O4 Co1 N5 N4 173.68(13) . . . . ? O6 Co1 N5 N4 115.33(12) . . . . ? O3 Co1 N5 N4 -117.75(12) . . . . ? O2 N6 O1 Co1 173.86(18) . . . . ? O3 N6 O1 Co1 -4.7(2) . . . . ? N1 Co1 O1 N6 74.77(12) . . . . ? N3 Co1 O1 N6 147.21(12) . . . . ? O4 Co1 O1 N6 -59.15(13) . . . . ? O6 Co1 O1 N6 -61.4(3) . . . . ? N5 Co1 O1 N6 -139.95(12) . . . . ? O3 Co1 O1 N6 2.71(11) . . . . ? O2 N6 O3 Co1 -174.3(2) . . . . ? O1 N6 O3 Co1 4.24(18) . . . . ? O1 Co1 O3 N6 -2.74(11) . . . . ? N1 Co1 O3 N6 -112.43(13) . . . . ? N3 Co1 O3 N6 -53.11(15) . . . . ? O4 Co1 O3 N6 118.01(13) . . . . ? O6 Co1 O3 N6 163.86(12) . . . . ? N5 Co1 O3 N6 47.12(15) . . . . ? O5 N7 O4 Co1 177.23(19) . . . . ? O6 N7 O4 Co1 -3.05(17) . . . . ? O1 Co1 O4 N7 -177.52(11) . . . . ? N1 Co1 O4 N7 63.04(14) . . . . ? N3 Co1 O4 N7 -60.01(17) . . . . ? O6 Co1 O4 N7 1.87(11) . . . . ? N5 Co1 O4 N7 -95.37(12) . . . . ? O3 Co1 O4 N7 133.42(13) . . . . ? O5 N7 O6 Co1 -177.26(19) . . . . ? O4 N7 O6 Co1 3.03(17) . . . . ? O1 Co1 O6 N7 0.6(3) . . . . ? N1 Co1 O6 N7 -136.62(11) . . . . ? N3 Co1 O6 N7 151.07(11) . . . . ? O4 Co1 O6 N7 -1.87(11) . . . . ? N5 Co1 O6 N7 78.30(11) . . . . ? O3 Co1 O6 N7 -56.77(13) . . . . ? O8 C7 O7 C13 2.8(3) . . . . ? C6 C7 O7 C13 -177.67(18) . . . . ? C14 C13 O7 C7 158.7(2) . . . . ? C14' C13 O7 C7 -161.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.276 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.044 data_1cooling228K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.7984(18) _cell_length_b 27.410(5) _cell_length_c 7.6404(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.082(4) _cell_angle_gamma 90.00 _cell_volume 2020.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 228(2) _cell_measurement_reflns_used 3723 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7717 _exptl_absorpt_correction_T_max 0.9144 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 228(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16695 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3723 _reflns_number_gt 3612 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+1.0394P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3723 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36420(2) 0.873757(8) 0.84050(3) 0.02673(9) Uani 1 1 d . . . C1 C 0.5474(2) 0.96692(7) 0.7444(3) 0.0408(5) Uani 1 1 d . . . H1A H 0.4914 0.9924 0.7742 0.049 Uiso 1 1 calc R . . C2 C 0.6729(2) 0.97384(7) 0.6835(3) 0.0455(5) Uani 1 1 d . . . H2A H 0.7150 1.0037 0.6647 0.055 Uiso 1 1 calc R . . C3 C 0.7210(2) 0.92858(7) 0.6571(3) 0.0373(4) Uani 1 1 d . . . H3A H 0.8037 0.9209 0.6167 0.045 Uiso 1 1 calc R . . C4 C 0.62374(17) 0.84522(6) 0.6970(2) 0.0253(3) Uani 1 1 d . . . C5 C 0.72613(18) 0.81654(6) 0.6459(2) 0.0288(4) Uani 1 1 d . . . H5A H 0.8030 0.8303 0.6059 0.035 Uiso 1 1 calc R . . C6 C 0.70948(17) 0.76623(6) 0.6567(2) 0.0271(4) Uani 1 1 d . . . C7 C 0.81977(18) 0.73341(7) 0.6076(2) 0.0310(4) Uani 1 1 d . . . C8 C 0.59446(17) 0.74605(6) 0.7140(2) 0.0263(3) Uani 1 1 d . . . H8A H 0.5827 0.7121 0.7216 0.032 Uiso 1 1 calc R . . C9 C 0.49871(17) 0.77853(6) 0.7591(2) 0.0245(3) Uani 1 1 d . . . C10 C 0.32827(18) 0.71856(6) 0.8461(2) 0.0298(4) Uani 1 1 d . . . H10A H 0.3719 0.6887 0.8313 0.036 Uiso 1 1 calc R . . C11 C 0.20423(19) 0.72492(7) 0.8993(2) 0.0330(4) Uani 1 1 d . . . H11A H 0.1448 0.7005 0.9288 0.040 Uiso 1 1 calc R . . C12 C 0.18337(18) 0.77535(7) 0.9009(2) 0.0331(4) Uani 1 1 d . . . H12A H 0.1049 0.7903 0.9327 0.040 Uiso 1 1 calc R . . C13 C 0.8929(2) 0.65028(7) 0.6065(3) 0.0382(4) Uani 1 1 d . . . H13A H 0.9821 0.6569 0.6830 0.046 Uiso 1 1 calc R . . H13B H 0.9064 0.6503 0.4824 0.046 Uiso 1 1 calc R . . C14 C 0.8365(2) 0.60180(7) 0.6535(3) 0.0384(4) Uani 1 1 d . . . H14A H 0.7530 0.5941 0.5672 0.046 Uiso 1 1 calc R . . H14B H 0.8100 0.6041 0.7711 0.046 Uiso 1 1 calc R . . C15 C 0.9412(3) 0.56090(8) 0.6549(3) 0.0538(6) Uani 1 1 d . . . H15A H 0.9636 0.5574 0.5355 0.065 Uiso 1 1 calc R . . H15B H 1.0267 0.5696 0.7359 0.065 Uiso 1 1 calc R . . C16 C 0.8888(4) 0.51269(10) 0.7122(5) 0.0794(9) Uani 1 1 d . . . H16A H 0.9594 0.4879 0.7118 0.119 Uiso 1 1 calc R . . H16B H 0.8056 0.5034 0.6305 0.119 Uiso 1 1 calc R . . H16C H 0.8678 0.5158 0.8311 0.119 Uiso 1 1 calc R . . N1 N 0.51798(15) 0.92004(5) 0.7547(2) 0.0308(3) Uani 1 1 d . . . N2 N 0.62628(15) 0.89621(5) 0.7004(2) 0.0280(3) Uani 1 1 d . . . N3 N 0.51234(14) 0.82681(5) 0.75163(18) 0.0245(3) Uani 1 1 d . . . N4 N 0.37723(14) 0.76390(5) 0.81825(18) 0.0253(3) Uani 1 1 d . . . N5 N 0.28734(15) 0.79933(5) 0.8524(2) 0.0300(3) Uani 1 1 d . . . N6 N 0.44034(18) 0.90178(6) 1.1658(2) 0.0375(4) Uani 1 1 d . . . N7 N 0.12232(17) 0.88480(6) 0.6508(2) 0.0391(4) Uani 1 1 d . . . O1 O 0.46942(15) 0.86015(5) 1.10887(18) 0.0381(3) Uani 1 1 d . . . O2 O 0.4767(2) 0.91376(7) 1.3198(2) 0.0662(5) Uani 1 1 d . . . O3 O 0.37106(16) 0.92928(5) 1.05078(19) 0.0466(4) Uani 1 1 d . . . O4 O 0.13783(16) 0.88697(6) 0.8172(2) 0.0485(4) Uani 1 1 d . . . O5 O 0.00809(16) 0.88259(7) 0.5549(3) 0.0635(5) Uani 1 1 d . . . O6 O 0.23209(14) 0.88403(5) 0.5861(2) 0.0426(3) Uani 1 1 d . . . O7 O 0.79110(14) 0.68703(5) 0.6333(2) 0.0407(3) Uani 1 1 d . . . O8 O 0.91912(14) 0.74804(5) 0.5517(2) 0.0453(4) 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 0.02536(15) 0.02423(14) 0.03121(15) -0.00159(9) 0.00667(10) 0.00234(8) C1 0.0420(11) 0.0258(9) 0.0564(13) -0.0037(8) 0.0138(9) -0.0008(8) C2 0.0493(12) 0.0282(10) 0.0618(14) -0.0008(9) 0.0179(10) -0.0096(9) C3 0.0367(10) 0.0334(10) 0.0443(11) -0.0010(8) 0.0138(8) -0.0089(8) C4 0.0249(8) 0.0272(9) 0.0236(8) -0.0008(6) 0.0033(6) -0.0019(7) C5 0.0253(8) 0.0310(9) 0.0312(9) -0.0016(7) 0.0079(7) -0.0027(7) C6 0.0242(8) 0.0314(9) 0.0258(8) -0.0031(7) 0.0048(7) 0.0016(7) C7 0.0273(9) 0.0337(10) 0.0323(9) -0.0039(7) 0.0054(7) 0.0013(7) C8 0.0263(8) 0.0248(8) 0.0275(8) -0.0021(6) 0.0042(7) -0.0003(6) C9 0.0235(8) 0.0266(8) 0.0233(8) -0.0009(6) 0.0037(6) -0.0014(6) C10 0.0321(9) 0.0258(9) 0.0312(9) 0.0004(7) 0.0044(7) -0.0036(7) C11 0.0310(9) 0.0367(10) 0.0320(9) 0.0008(7) 0.0076(7) -0.0095(8) C12 0.0254(9) 0.0385(10) 0.0371(10) -0.0010(8) 0.0102(7) -0.0038(7) C13 0.0318(10) 0.0346(10) 0.0491(11) -0.0059(9) 0.0095(9) 0.0089(8) C14 0.0391(11) 0.0353(10) 0.0410(11) -0.0046(8) 0.0071(8) 0.0036(8) C15 0.0625(15) 0.0378(12) 0.0634(15) -0.0028(10) 0.0175(12) 0.0136(10) C16 0.110(2) 0.0384(14) 0.096(2) 0.0040(14) 0.0346(19) 0.0142(14) N1 0.0292(8) 0.0258(7) 0.0384(8) -0.0031(6) 0.0086(6) 0.0011(6) N2 0.0265(7) 0.0261(8) 0.0321(8) 0.0001(6) 0.0073(6) -0.0028(6) N3 0.0230(7) 0.0246(7) 0.0260(7) -0.0022(5) 0.0049(5) -0.0013(5) N4 0.0232(7) 0.0242(7) 0.0292(7) -0.0008(6) 0.0065(6) -0.0002(5) N5 0.0252(7) 0.0293(8) 0.0372(8) -0.0032(6) 0.0099(6) 0.0014(6) N6 0.0469(10) 0.0319(8) 0.0333(8) -0.0020(7) 0.0061(7) -0.0010(7) N7 0.0310(9) 0.0352(9) 0.0498(11) 0.0044(7) 0.0039(8) 0.0033(7) O1 0.0475(8) 0.0278(7) 0.0384(7) 0.0000(6) 0.0064(6) 0.0049(6) O2 0.1010(14) 0.0620(11) 0.0302(8) -0.0121(7) -0.0036(8) 0.0054(10) O3 0.0648(10) 0.0357(8) 0.0384(8) 0.0004(6) 0.0064(7) 0.0163(7) O4 0.0531(9) 0.0440(8) 0.0501(9) -0.0002(7) 0.0139(7) 0.0144(7) O5 0.0298(8) 0.0825(13) 0.0728(12) 0.0109(10) -0.0062(8) 0.0005(8) O6 0.0309(7) 0.0491(8) 0.0471(8) 0.0079(7) 0.0047(6) -0.0007(6) O7 0.0335(7) 0.0301(7) 0.0625(9) -0.0035(6) 0.0194(7) 0.0053(5) O8 0.0332(7) 0.0410(8) 0.0680(10) -0.0013(7) 0.0259(7) 0.0027(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.1374(14) . ? Co1 O6 2.1566(15) . ? Co1 N1 2.1577(15) . ? Co1 O1 2.1602(14) . ? Co1 N5 2.1820(16) . ? Co1 O3 2.2054(15) . ? Co1 O4 2.2235(16) . ? C1 N1 1.322(2) . ? C1 C2 1.401(3) . ? C1 H1A 0.9400 . ? C2 C3 1.355(3) . ? C2 H2A 0.9400 . ? C3 N2 1.366(2) . ? C3 H3A 0.9400 . ? C4 N3 1.334(2) . ? C4 C5 1.384(2) . ? C4 N2 1.398(2) . ? C5 C6 1.393(2) . ? C5 H5A 0.9400 . ? C6 C8 1.393(2) . ? C6 C7 1.503(2) . ? C7 O8 1.199(2) . ? C7 O7 1.324(2) . ? C8 C9 1.380(2) . ? C8 H8A 0.9400 . ? C9 N3 1.333(2) . ? C9 N4 1.404(2) . ? C10 C11 1.359(3) . ? C10 N4 1.362(2) . ? C10 H10A 0.9400 . ? C11 C12 1.398(3) . ? C11 H11A 0.9400 . ? C12 N5 1.319(2) . ? C12 H12A 0.9400 . ? C13 O7 1.457(2) . ? C13 C14 1.507(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.519(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.510(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? N1 N2 1.371(2) . ? N4 N5 1.366(2) . ? N6 O2 1.213(2) . ? N6 O3 1.262(2) . ? N6 O1 1.271(2) . ? N7 O5 1.227(2) . ? N7 O4 1.255(2) . ? N7 O6 1.260(2) . ? 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 N3 Co1 O6 97.25(6) . . ? N3 Co1 N1 73.03(6) . . ? O6 Co1 N1 89.45(6) . . ? N3 Co1 O1 87.69(5) . . ? O6 Co1 O1 171.64(5) . . ? N1 Co1 O1 98.47(6) . . ? N3 Co1 N5 73.08(5) . . ? O6 Co1 N5 90.14(6) . . ? N1 Co1 N5 145.77(6) . . ? O1 Co1 N5 84.83(5) . . ? N3 Co1 O3 135.32(6) . . ? O6 Co1 O3 120.22(6) . . ? N1 Co1 O3 83.21(6) . . ? O1 Co1 O3 58.60(5) . . ? N5 Co1 O3 125.56(6) . . ? N3 Co1 O4 142.74(6) . . ? O6 Co1 O4 58.23(6) . . ? N1 Co1 O4 128.30(6) . . ? O1 Co1 O4 114.07(6) . . ? N5 Co1 O4 78.99(6) . . ? O3 Co1 O4 81.30(6) . . ? N1 C1 C2 111.37(18) . . ? N1 C1 H1A 124.3 . . ? C2 C1 H1A 124.3 . . ? C3 C2 C1 105.89(17) . . ? C3 C2 H2A 127.1 . . ? C1 C2 H2A 127.1 . . ? C2 C3 N2 106.86(17) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? N3 C4 C5 123.16(16) . . ? N3 C4 N2 112.65(14) . . ? C5 C4 N2 124.19(15) . . ? C4 C5 C6 116.60(16) . . ? C4 C5 H5A 121.7 . . ? C6 C5 H5A 121.7 . . ? C5 C6 C8 121.41(16) . . ? C5 C6 C7 118.75(16) . . ? C8 C6 C7 119.83(16) . . ? O8 C7 O7 125.50(17) . . ? O8 C7 C6 123.56(17) . . ? O7 C7 C6 110.93(15) . . ? C9 C8 C6 116.45(16) . . ? C9 C8 H8A 121.8 . . ? C6 C8 H8A 121.8 . . ? N3 C9 C8 123.52(15) . . ? N3 C9 N4 113.23(14) . . ? C8 C9 N4 123.24(15) . . ? C11 C10 N4 106.71(16) . . ? C11 C10 H10A 126.6 . . ? N4 C10 H10A 126.6 . . ? C10 C11 C12 105.63(16) . . ? C10 C11 H11A 127.2 . . ? C12 C11 H11A 127.2 . . ? N5 C12 C11 111.65(16) . . ? N5 C12 H12A 124.2 . . ? C11 C12 H12A 124.2 . . ? O7 C13 C14 106.72(15) . . ? O7 C13 H13A 110.4 . . ? C14 C13 H13A 110.4 . . ? O7 C13 H13B 110.4 . . ? C14 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? C13 C14 C15 112.16(18) . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 112.6(2) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? 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 . . ? C1 N1 N2 104.87(15) . . ? C1 N1 Co1 139.52(13) . . ? N2 N1 Co1 115.50(11) . . ? C3 N2 N1 111.00(15) . . ? C3 N2 C4 130.97(15) . . ? N1 N2 C4 118.02(13) . . ? C9 N3 C4 118.86(14) . . ? C9 N3 Co1 120.37(11) . . ? C4 N3 Co1 120.67(11) . . ? C10 N4 N5 111.24(14) . . ? C10 N4 C9 130.73(15) . . ? N5 N4 C9 118.02(14) . . ? C12 N5 N4 104.77(15) . . ? C12 N5 Co1 140.06(13) . . ? N4 N5 Co1 114.70(10) . . ? O2 N6 O3 122.99(17) . . ? O2 N6 O1 121.97(17) . . ? O3 N6 O1 115.04(15) . . ? O5 N7 O4 122.90(18) . . ? O5 N7 O6 121.12(19) . . ? O4 N7 O6 115.96(16) . . ? N6 O1 Co1 94.10(10) . . ? N6 O3 Co1 92.26(10) . . ? N7 O4 Co1 90.90(11) . . ? N7 O6 Co1 93.88(11) . . ? C7 O7 C13 118.35(15) . . ? 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 N1 C1 C2 C3 -0.4(3) . . . . ? C1 C2 C3 N2 0.3(2) . . . . ? N3 C4 C5 C6 -1.1(3) . . . . ? N2 C4 C5 C6 177.71(15) . . . . ? C4 C5 C6 C8 0.8(3) . . . . ? C4 C5 C6 C7 -178.30(15) . . . . ? C5 C6 C7 O8 -3.5(3) . . . . ? C8 C6 C7 O8 177.41(18) . . . . ? C5 C6 C7 O7 177.03(16) . . . . ? C8 C6 C7 O7 -2.1(2) . . . . ? C5 C6 C8 C9 0.0(2) . . . . ? C7 C6 C8 C9 179.08(15) . . . . ? C6 C8 C9 N3 -0.6(2) . . . . ? C6 C8 C9 N4 179.66(15) . . . . ? N4 C10 C11 C12 0.1(2) . . . . ? C10 C11 C12 N5 -0.1(2) . . . . ? O7 C13 C14 C15 -172.40(17) . . . . ? C13 C14 C15 C16 176.7(2) . . . . ? C2 C1 N1 N2 0.3(2) . . . . ? C2 C1 N1 Co1 176.07(16) . . . . ? N3 Co1 N1 C1 -178.5(2) . . . . ? O6 Co1 N1 C1 83.8(2) . . . . ? O1 Co1 N1 C1 -93.5(2) . . . . ? N5 Co1 N1 C1 173.22(19) . . . . ? O3 Co1 N1 C1 -36.8(2) . . . . ? O4 Co1 N1 C1 36.5(2) . . . . ? N3 Co1 N1 N2 -2.97(11) . . . . ? O6 Co1 N1 N2 -100.72(12) . . . . ? O1 Co1 N1 N2 81.98(12) . . . . ? N5 Co1 N1 N2 -11.28(18) . . . . ? O3 Co1 N1 N2 138.74(12) . . . . ? O4 Co1 N1 N2 -148.00(11) . . . . ? C2 C3 N2 N1 -0.1(2) . . . . ? C2 C3 N2 C4 179.64(18) . . . . ? C1 N1 N2 C3 -0.1(2) . . . . ? Co1 N1 N2 C3 -177.07(12) . . . . ? C1 N1 N2 C4 -179.89(16) . . . . ? Co1 N1 N2 C4 3.13(18) . . . . ? N3 C4 N2 C3 179.42(18) . . . . ? C5 C4 N2 C3 0.5(3) . . . . ? N3 C4 N2 N1 -0.8(2) . . . . ? C5 C4 N2 N1 -179.74(16) . . . . ? C8 C9 N3 C4 0.3(2) . . . . ? N4 C9 N3 C4 -179.90(14) . . . . ? C8 C9 N3 Co1 -176.05(12) . . . . ? N4 C9 N3 Co1 3.71(19) . . . . ? C5 C4 N3 C9 0.6(2) . . . . ? N2 C4 N3 C9 -178.37(14) . . . . ? C5 C4 N3 Co1 176.93(13) . . . . ? N2 C4 N3 Co1 -1.99(18) . . . . ? O6 Co1 N3 C9 -93.73(13) . . . . ? N1 Co1 N3 C9 179.08(14) . . . . ? O1 Co1 N3 C9 79.50(13) . . . . ? N5 Co1 N3 C9 -5.80(12) . . . . ? O3 Co1 N3 C9 118.04(13) . . . . ? O4 Co1 N3 C9 -48.92(17) . . . . ? O6 Co1 N3 C4 89.95(13) . . . . ? N1 Co1 N3 C4 2.75(12) . . . . ? O1 Co1 N3 C4 -96.82(13) . . . . ? N5 Co1 N3 C4 177.88(14) . . . . ? O3 Co1 N3 C4 -58.29(15) . . . . ? O4 Co1 N3 C4 134.76(12) . . . . ? C11 C10 N4 N5 -0.02(19) . . . . ? C11 C10 N4 C9 -178.52(16) . . . . ? N3 C9 N4 C10 -178.80(16) . . . . ? C8 C9 N4 C10 1.0(3) . . . . ? N3 C9 N4 N5 2.8(2) . . . . ? C8 C9 N4 N5 -177.45(15) . . . . ? C11 C12 N5 N4 0.1(2) . . . . ? C11 C12 N5 Co1 -171.01(14) . . . . ? C10 N4 N5 C12 -0.05(19) . . . . ? C9 N4 N5 C12 178.66(15) . . . . ? C10 N4 N5 Co1 173.68(11) . . . . ? C9 N4 N5 Co1 -7.60(18) . . . . ? N3 Co1 N5 C12 177.4(2) . . . . ? O6 Co1 N5 C12 -85.1(2) . . . . ? N1 Co1 N5 C12 -174.34(17) . . . . ? O1 Co1 N5 C12 88.2(2) . . . . ? O3 Co1 N5 C12 43.2(2) . . . . ? O4 Co1 N5 C12 -27.6(2) . . . . ? N3 Co1 N5 N4 6.81(11) . . . . ? O6 Co1 N5 N4 104.34(12) . . . . ? N1 Co1 N5 N4 15.12(18) . . . . ? O1 Co1 N5 N4 -82.35(12) . . . . ? O3 Co1 N5 N4 -127.30(11) . . . . ? O4 Co1 N5 N4 161.87(12) . . . . ? O2 N6 O1 Co1 179.45(18) . . . . ? O3 N6 O1 Co1 -0.37(17) . . . . ? N3 Co1 O1 N6 149.35(11) . . . . ? O6 Co1 O1 N6 -84.2(4) . . . . ? N1 Co1 O1 N6 76.88(11) . . . . ? N5 Co1 O1 N6 -137.45(11) . . . . ? O3 Co1 O1 N6 0.23(10) . . . . ? O4 Co1 O1 N6 -61.95(12) . . . . ? O2 N6 O3 Co1 -179.45(19) . . . . ? O1 N6 O3 Co1 0.37(17) . . . . ? N3 Co1 O3 N6 -47.06(15) . . . . ? O6 Co1 O3 N6 170.13(10) . . . . ? N1 Co1 O3 N6 -104.49(12) . . . . ? O1 Co1 O3 N6 -0.23(10) . . . . ? N5 Co1 O3 N6 55.30(14) . . . . ? O4 Co1 O3 N6 125.00(12) . . . . ? O5 N7 O4 Co1 168.94(18) . . . . ? O6 N7 O4 Co1 -9.68(17) . . . . ? N3 Co1 O4 N7 -49.36(15) . . . . ? O6 Co1 O4 N7 5.96(10) . . . . ? N1 Co1 O4 N7 65.73(13) . . . . ? O1 Co1 O4 N7 -170.33(10) . . . . ? N5 Co1 O4 N7 -91.13(12) . . . . ? O3 Co1 O4 N7 139.88(12) . . . . ? O5 N7 O6 Co1 -168.65(17) . . . . ? O4 N7 O6 Co1 10.00(17) . . . . ? N3 Co1 O6 N7 143.93(11) . . . . ? N1 Co1 O6 N7 -143.25(11) . . . . ? O1 Co1 O6 N7 18.0(4) . . . . ? N5 Co1 O6 N7 70.98(11) . . . . ? O3 Co1 O6 N7 -61.44(13) . . . . ? O4 Co1 O6 N7 -5.95(10) . . . . ? O8 C7 O7 C13 5.5(3) . . . . ? C6 C7 O7 C13 -175.02(15) . . . . ? C14 C13 O7 C7 177.22(16) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.283 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.046 data_1cooling183K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.7948(18) _cell_length_b 27.435(5) _cell_length_c 7.5979(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.265(5) _cell_angle_gamma 90.00 _cell_volume 2009.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 3656 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 25.49 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7706 _exptl_absorpt_correction_T_max 0.9140 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15678 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3656 _reflns_number_gt 3447 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1325P)^2^+2.5933P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3656 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.2094 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36339(5) 0.373781(17) 0.84214(6) 0.0217(3) Uani 1 1 d . . . C1 C 0.5479(4) 0.46688(14) 0.7458(6) 0.0334(9) Uani 1 1 d . . . H1A H 0.4908 0.4926 0.7742 0.040 Uiso 1 1 calc R . . C2 C 0.6753(5) 0.47352(16) 0.6862(6) 0.0368(9) Uani 1 1 d . . . H2A H 0.7186 0.5036 0.6681 0.044 Uiso 1 1 calc R . . C3 C 0.7232(4) 0.42808(15) 0.6599(5) 0.0315(8) Uani 1 1 d . . . H3A H 0.8070 0.4201 0.6200 0.038 Uiso 1 1 calc R . . C4 C 0.6230(4) 0.34456(13) 0.6999(5) 0.0221(7) Uani 1 1 d . . . C5 C 0.7261(4) 0.31614(13) 0.6476(5) 0.0230(7) Uani 1 1 d . . . H5A H 0.8036 0.3300 0.6066 0.028 Uiso 1 1 calc R . . C6 C 0.7083(3) 0.26584(13) 0.6591(5) 0.0227(7) Uani 1 1 d . . . C7 C 0.8179(4) 0.23277(13) 0.6097(5) 0.0256(8) Uani 1 1 d . . . C8 C 0.5925(3) 0.24582(13) 0.7162(5) 0.0221(7) Uani 1 1 d . . . H8A H 0.5802 0.2116 0.7236 0.027 Uiso 1 1 calc R . . C9 C 0.4976(4) 0.27815(13) 0.7610(5) 0.0211(7) Uani 1 1 d . . . C10 C 0.3253(4) 0.21863(13) 0.8478(5) 0.0260(8) Uani 1 1 d . . . H10A H 0.3690 0.1884 0.8328 0.031 Uiso 1 1 calc R . . C11 C 0.2013(4) 0.22509(14) 0.9010(5) 0.0289(8) Uani 1 1 d . . . H11A H 0.1410 0.2005 0.9306 0.035 Uiso 1 1 calc R . . C12 C 0.1806(4) 0.27587(14) 0.9030(5) 0.0255(8) Uani 1 1 d . . . H12A H 0.1015 0.2912 0.9349 0.031 Uiso 1 1 calc R . . C13 C 0.8920(4) 0.14961(14) 0.6062(6) 0.0320(9) Uani 1 1 d . . . H13A H 0.9828 0.1563 0.6831 0.038 Uiso 1 1 calc R . . H13B H 0.9044 0.1496 0.4797 0.038 Uiso 1 1 calc R . . C14 C 0.8345(4) 0.10121(14) 0.6548(5) 0.0309(8) Uani 1 1 d . . . H14A H 0.7502 0.0933 0.5668 0.037 Uiso 1 1 calc R . . H14B H 0.8075 0.1039 0.7739 0.037 Uiso 1 1 calc R . . C15 C 0.9391(5) 0.06007(16) 0.6585(7) 0.0448(11) Uani 1 1 d . . . H15A H 0.9621 0.0564 0.5376 0.054 Uiso 1 1 calc R . . H15B H 1.0254 0.0690 0.7412 0.054 Uiso 1 1 calc R . . C16 C 0.8877(7) 0.01160(19) 0.7167(9) 0.0642(16) Uani 1 1 d . . . H16A H 0.9594 -0.0133 0.7159 0.077 Uiso 1 1 calc R . . H16B H 0.8034 0.0021 0.6340 0.077 Uiso 1 1 calc R . . H16C H 0.8670 0.0147 0.8377 0.077 Uiso 1 1 calc R . . N1 N 0.5187(3) 0.41976(11) 0.7568(4) 0.0263(7) Uani 1 1 d . . . N2 N 0.6263(3) 0.39575(11) 0.7027(4) 0.0235(6) Uani 1 1 d . . . N3 N 0.5115(3) 0.32678(11) 0.7533(4) 0.0208(6) Uani 1 1 d . . . N4 N 0.3753(3) 0.26404(11) 0.8200(4) 0.0220(6) Uani 1 1 d . . . N5 N 0.2866(3) 0.29963(11) 0.8544(4) 0.0253(7) Uani 1 1 d . . . N6 N 0.4401(4) 0.40254(12) 1.1677(4) 0.0299(7) Uani 1 1 d . . . N7 N 0.1209(3) 0.38455(13) 0.6507(5) 0.0313(8) Uani 1 1 d . . . O1 O 0.4691(3) 0.36046(10) 1.1126(4) 0.0311(6) Uani 1 1 d . . . O2 O 0.4761(4) 0.41481(13) 1.3233(4) 0.0540(10) Uani 1 1 d . . . O3 O 0.3702(3) 0.42966(10) 1.0522(4) 0.0375(7) Uani 1 1 d . . . O4 O 0.1370(3) 0.38687(11) 0.8172(4) 0.0385(7) Uani 1 1 d . . . O5 O 0.0080(3) 0.38192(13) 0.5538(5) 0.0481(9) Uani 1 1 d . . . O6 O 0.2330(3) 0.38346(11) 0.5853(4) 0.0336(7) Uani 1 1 d . . . O7 O 0.7897(3) 0.18624(10) 0.6350(4) 0.0341(7) Uani 1 1 d . . . O8 O 0.9184(3) 0.24751(11) 0.5535(4) 0.0369(7) 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 0.0209(4) 0.0189(4) 0.0256(4) -0.00108(16) 0.0046(2) 0.00141(15) C1 0.039(2) 0.0176(18) 0.044(2) -0.0040(15) 0.0104(18) -0.0034(15) C2 0.035(2) 0.026(2) 0.051(2) -0.0019(17) 0.0125(19) -0.0072(17) C3 0.0302(19) 0.0266(19) 0.038(2) 0.0009(16) 0.0060(16) -0.0064(15) C4 0.0221(16) 0.0231(18) 0.0215(16) 0.0003(13) 0.0050(13) -0.0034(13) C5 0.0175(16) 0.0263(18) 0.0261(17) -0.0016(14) 0.0063(13) -0.0015(13) C6 0.0192(17) 0.0250(18) 0.0241(17) -0.0055(13) 0.0044(13) 0.0035(13) C7 0.0238(18) 0.0243(18) 0.0284(18) -0.0043(14) 0.0039(14) 0.0037(14) C8 0.0230(17) 0.0199(17) 0.0234(16) -0.0040(13) 0.0039(13) 0.0001(13) C9 0.0193(16) 0.0241(17) 0.0196(16) -0.0010(13) 0.0026(12) -0.0028(13) C10 0.0300(18) 0.0197(18) 0.0264(18) -0.0021(13) -0.0001(14) -0.0015(14) C11 0.0249(18) 0.031(2) 0.031(2) 0.0029(15) 0.0063(15) -0.0083(15) C12 0.0191(16) 0.0308(19) 0.0270(18) -0.0031(14) 0.0053(13) -0.0062(14) C13 0.033(2) 0.0242(19) 0.040(2) -0.0046(16) 0.0093(16) 0.0035(15) C14 0.030(2) 0.029(2) 0.033(2) -0.0012(16) 0.0058(16) -0.0032(16) C15 0.058(3) 0.028(2) 0.049(3) -0.0041(18) 0.010(2) 0.0083(19) C16 0.090(4) 0.029(3) 0.075(4) -0.001(2) 0.019(3) 0.013(3) N1 0.0282(16) 0.0195(15) 0.0317(16) -0.0035(12) 0.0069(13) 0.0017(12) N2 0.0211(15) 0.0212(16) 0.0273(15) 0.0021(12) 0.0022(12) -0.0038(11) N3 0.0203(14) 0.0215(14) 0.0206(14) -0.0020(11) 0.0037(11) -0.0019(11) N4 0.0203(14) 0.0201(15) 0.0258(15) 0.0011(11) 0.0049(11) -0.0016(11) N5 0.0232(15) 0.0224(15) 0.0312(16) -0.0036(12) 0.0069(12) 0.0020(12) N6 0.0378(18) 0.0245(16) 0.0268(16) -0.0016(13) 0.0043(13) -0.0003(13) N7 0.0264(18) 0.0263(16) 0.040(2) 0.0033(13) 0.0033(15) 0.0033(13) O1 0.0370(15) 0.0227(13) 0.0327(14) -0.0005(11) 0.0040(12) 0.0026(11) O2 0.084(3) 0.049(2) 0.0236(15) -0.0091(13) -0.0050(16) 0.0046(18) O3 0.0563(18) 0.0265(14) 0.0283(14) -0.0014(11) 0.0039(13) 0.0126(13) O4 0.0409(17) 0.0343(16) 0.0420(18) 0.0007(13) 0.0122(13) 0.0099(13) O5 0.0273(17) 0.056(2) 0.057(2) 0.0076(16) -0.0023(15) 0.0007(14) O6 0.0260(15) 0.0378(15) 0.0371(16) 0.0044(12) 0.0061(12) -0.0021(11) O7 0.0322(15) 0.0219(14) 0.0507(17) -0.0007(12) 0.0142(13) 0.0022(11) O8 0.0283(14) 0.0311(15) 0.0555(18) 0.0003(13) 0.0189(13) 0.0014(11) _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 N3 2.138(3) . ? Co1 O6 2.150(3) . ? Co1 O1 2.161(3) . ? Co1 N1 2.163(3) . ? Co1 N5 2.177(3) . ? Co1 O3 2.205(3) . ? Co1 O4 2.220(3) . ? C1 N1 1.330(5) . ? C1 C2 1.412(6) . ? C1 H1A 0.9500 . ? C2 C3 1.359(6) . ? C2 H2A 0.9500 . ? C3 N2 1.379(5) . ? C3 H3A 0.9500 . ? C4 N3 1.325(5) . ? C4 C5 1.388(5) . ? C4 N2 1.405(5) . ? C5 C6 1.396(5) . ? C5 H5A 0.9500 . ? C6 C8 1.396(5) . ? C6 C7 1.503(5) . ? C7 O8 1.211(5) . ? C7 O7 1.327(5) . ? C8 C9 1.371(5) . ? C8 H8A 0.9500 . ? C9 N3 1.343(4) . ? C9 N4 1.406(5) . ? C10 C11 1.358(6) . ? C10 N4 1.369(5) . ? C10 H10A 0.9500 . ? C11 C12 1.408(6) . ? C11 H11A 0.9500 . ? C12 N5 1.332(5) . ? C12 H12A 0.9500 . ? C13 O7 1.463(5) . ? C13 C14 1.514(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.521(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.515(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N1 N2 1.366(5) . ? N4 N5 1.363(4) . ? N6 O2 1.219(4) . ? N6 O3 1.256(4) . ? N6 O1 1.277(4) . ? N7 O5 1.217(5) . ? N7 O4 1.248(5) . ? N7 O6 1.283(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 O6 96.59(12) . . ? N3 Co1 O1 87.76(11) . . ? O6 Co1 O1 172.12(11) . . ? N3 Co1 N1 72.79(12) . . ? O6 Co1 N1 89.52(12) . . ? O1 Co1 N1 98.06(12) . . ? N3 Co1 N5 73.08(11) . . ? O6 Co1 N5 90.02(12) . . ? O1 Co1 N5 84.95(11) . . ? N1 Co1 N5 145.57(12) . . ? N3 Co1 O3 135.48(11) . . ? O6 Co1 O3 120.49(11) . . ? O1 Co1 O3 58.80(10) . . ? N1 Co1 O3 83.08(12) . . ? N5 Co1 O3 125.78(12) . . ? N3 Co1 O4 142.55(12) . . ? O6 Co1 O4 58.66(11) . . ? O1 Co1 O4 114.25(11) . . ? N1 Co1 O4 128.68(12) . . ? N5 Co1 O4 78.89(12) . . ? O3 Co1 O4 81.38(12) . . ? N1 C1 C2 110.9(4) . . ? N1 C1 H1A 124.5 . . ? C2 C1 H1A 124.5 . . ? C3 C2 C1 106.1(4) . . ? C3 C2 H2A 127.0 . . ? C1 C2 H2A 127.0 . . ? C2 C3 N2 106.6(4) . . ? C2 C3 H3A 126.7 . . ? N2 C3 H3A 126.7 . . ? N3 C4 C5 124.2(3) . . ? N3 C4 N2 112.4(3) . . ? C5 C4 N2 123.4(3) . . ? C4 C5 C6 115.6(3) . . ? C4 C5 H5A 122.2 . . ? C6 C5 H5A 122.2 . . ? C5 C6 C8 121.7(3) . . ? C5 C6 C7 118.6(3) . . ? C8 C6 C7 119.7(3) . . ? O8 C7 O7 125.1(3) . . ? O8 C7 C6 123.3(3) . . ? O7 C7 C6 111.6(3) . . ? C9 C8 C6 116.5(3) . . ? C9 C8 H8A 121.7 . . ? C6 C8 H8A 121.7 . . ? N3 C9 C8 123.6(3) . . ? N3 C9 N4 112.7(3) . . ? C8 C9 N4 123.7(3) . . ? C11 C10 N4 106.9(3) . . ? C11 C10 H10A 126.5 . . ? N4 C10 H10A 126.5 . . ? C10 C11 C12 105.7(3) . . ? C10 C11 H11A 127.2 . . ? C12 C11 H11A 127.2 . . ? N5 C12 C11 111.1(3) . . ? N5 C12 H12A 124.4 . . ? C11 C12 H12A 124.4 . . ? O7 C13 C14 105.8(3) . . ? O7 C13 H13A 110.6 . . ? C14 C13 H13A 110.6 . . ? O7 C13 H13B 110.6 . . ? C14 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? C13 C14 C15 112.2(4) . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 113.5(4) . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? 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 . . ? C1 N1 N2 105.3(3) . . ? C1 N1 Co1 139.1(3) . . ? N2 N1 Co1 115.5(2) . . ? N1 N2 C3 111.1(3) . . ? N1 N2 C4 118.0(3) . . ? C3 N2 C4 130.8(3) . . ? C4 N3 C9 118.3(3) . . ? C4 N3 Co1 121.2(2) . . ? C9 N3 Co1 120.4(2) . . ? N5 N4 C10 111.4(3) . . ? N5 N4 C9 118.2(3) . . ? C10 N4 C9 130.4(3) . . ? C12 N5 N4 104.9(3) . . ? C12 N5 Co1 139.6(3) . . ? N4 N5 Co1 115.1(2) . . ? O2 N6 O3 122.8(3) . . ? O2 N6 O1 121.6(3) . . ? O3 N6 O1 115.6(3) . . ? O5 N7 O4 123.6(4) . . ? O5 N7 O6 120.9(4) . . ? O4 N7 O6 115.5(3) . . ? N6 O1 Co1 93.5(2) . . ? N6 O3 Co1 92.1(2) . . ? N7 O4 Co1 91.3(2) . . ? N7 O6 Co1 93.6(2) . . ? C7 O7 C13 118.3(3) . . ? 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 N1 C1 C2 C3 0.3(5) . . . . ? C1 C2 C3 N2 0.1(5) . . . . ? N3 C4 C5 C6 -1.8(5) . . . . ? N2 C4 C5 C6 177.8(3) . . . . ? C4 C5 C6 C8 1.3(5) . . . . ? C4 C5 C6 C7 -178.3(3) . . . . ? C5 C6 C7 O8 -3.0(5) . . . . ? C8 C6 C7 O8 177.5(4) . . . . ? C5 C6 C7 O7 177.2(3) . . . . ? C8 C6 C7 O7 -2.4(5) . . . . ? C5 C6 C8 C9 -0.3(5) . . . . ? C7 C6 C8 C9 179.3(3) . . . . ? C6 C8 C9 N3 -0.4(5) . . . . ? C6 C8 C9 N4 179.7(3) . . . . ? N4 C10 C11 C12 0.1(4) . . . . ? C10 C11 C12 N5 -0.2(4) . . . . ? O7 C13 C14 C15 -171.5(3) . . . . ? C13 C14 C15 C16 176.8(4) . . . . ? C2 C1 N1 N2 -0.6(5) . . . . ? C2 C1 N1 Co1 176.0(3) . . . . ? N3 Co1 N1 C1 -179.2(5) . . . . ? O6 Co1 N1 C1 83.8(4) . . . . ? O1 Co1 N1 C1 -94.1(4) . . . . ? N5 Co1 N1 C1 173.1(4) . . . . ? O3 Co1 N1 C1 -37.0(4) . . . . ? O4 Co1 N1 C1 36.1(5) . . . . ? N3 Co1 N1 N2 -2.9(2) . . . . ? O6 Co1 N1 N2 -99.9(3) . . . . ? O1 Co1 N1 N2 82.3(3) . . . . ? N5 Co1 N1 N2 -10.6(4) . . . . ? O3 Co1 N1 N2 139.3(3) . . . . ? O4 Co1 N1 N2 -147.6(2) . . . . ? C1 N1 N2 C3 0.7(4) . . . . ? Co1 N1 N2 C3 -176.8(2) . . . . ? C1 N1 N2 C4 -179.7(3) . . . . ? Co1 N1 N2 C4 2.7(4) . . . . ? C2 C3 N2 N1 -0.5(4) . . . . ? C2 C3 N2 C4 180.0(3) . . . . ? N3 C4 N2 N1 -0.3(4) . . . . ? C5 C4 N2 N1 180.0(3) . . . . ? N3 C4 N2 C3 179.2(4) . . . . ? C5 C4 N2 C3 -0.5(5) . . . . ? C5 C4 N3 C9 1.3(5) . . . . ? N2 C4 N3 C9 -178.4(3) . . . . ? C5 C4 N3 Co1 177.3(3) . . . . ? N2 C4 N3 Co1 -2.4(4) . . . . ? C8 C9 N3 C4 -0.1(5) . . . . ? N4 C9 N3 C4 179.8(3) . . . . ? C8 C9 N3 Co1 -176.1(3) . . . . ? N4 C9 N3 Co1 3.8(4) . . . . ? O6 Co1 N3 C4 90.4(3) . . . . ? O1 Co1 N3 C4 -96.2(3) . . . . ? N1 Co1 N3 C4 2.9(3) . . . . ? N5 Co1 N3 C4 178.4(3) . . . . ? O3 Co1 N3 C4 -57.4(3) . . . . ? O4 Co1 N3 C4 135.1(3) . . . . ? O6 Co1 N3 C9 -93.7(3) . . . . ? O1 Co1 N3 C9 79.7(3) . . . . ? N1 Co1 N3 C9 178.8(3) . . . . ? N5 Co1 N3 C9 -5.7(3) . . . . ? O3 Co1 N3 C9 118.5(3) . . . . ? O4 Co1 N3 C9 -49.0(3) . . . . ? C11 C10 N4 N5 0.1(4) . . . . ? C11 C10 N4 C9 -178.6(3) . . . . ? N3 C9 N4 N5 2.4(4) . . . . ? C8 C9 N4 N5 -177.7(3) . . . . ? N3 C9 N4 C10 -179.0(3) . . . . ? C8 C9 N4 C10 1.0(6) . . . . ? C11 C12 N5 N4 0.3(4) . . . . ? C11 C12 N5 Co1 -171.6(3) . . . . ? C10 N4 N5 C12 -0.3(4) . . . . ? C9 N4 N5 C12 178.6(3) . . . . ? C10 N4 N5 Co1 173.9(2) . . . . ? C9 N4 N5 Co1 -7.2(4) . . . . ? N3 Co1 N5 C12 177.9(4) . . . . ? O6 Co1 N5 C12 -85.2(4) . . . . ? O1 Co1 N5 C12 88.7(4) . . . . ? N1 Co1 N5 C12 -174.4(3) . . . . ? O3 Co1 N5 C12 43.5(4) . . . . ? O4 Co1 N5 C12 -27.2(4) . . . . ? N3 Co1 N5 N4 6.5(2) . . . . ? O6 Co1 N5 N4 103.4(2) . . . . ? O1 Co1 N5 N4 -82.6(2) . . . . ? N1 Co1 N5 N4 14.3(4) . . . . ? O3 Co1 N5 N4 -127.8(2) . . . . ? O4 Co1 N5 N4 161.4(3) . . . . ? O2 N6 O1 Co1 178.9(4) . . . . ? O3 N6 O1 Co1 0.3(3) . . . . ? N3 Co1 O1 N6 148.9(2) . . . . ? O6 Co1 O1 N6 -87.4(8) . . . . ? N1 Co1 O1 N6 76.7(2) . . . . ? N5 Co1 O1 N6 -137.9(2) . . . . ? O3 Co1 O1 N6 -0.2(2) . . . . ? O4 Co1 O1 N6 -62.5(2) . . . . ? O2 N6 O3 Co1 -178.8(4) . . . . ? O1 N6 O3 Co1 -0.2(3) . . . . ? N3 Co1 O3 N6 -46.9(3) . . . . ? O6 Co1 O3 N6 171.0(2) . . . . ? O1 Co1 O3 N6 0.2(2) . . . . ? N1 Co1 O3 N6 -103.6(2) . . . . ? N5 Co1 O3 N6 55.9(3) . . . . ? O4 Co1 O3 N6 125.4(2) . . . . ? O5 N7 O4 Co1 168.5(4) . . . . ? O6 N7 O4 Co1 -9.3(3) . . . . ? N3 Co1 O4 N7 -49.1(3) . . . . ? O6 Co1 O4 N7 5.9(2) . . . . ? O1 Co1 O4 N7 -170.3(2) . . . . ? N1 Co1 O4 N7 65.8(3) . . . . ? N5 Co1 O4 N7 -91.0(2) . . . . ? O3 Co1 O4 N7 139.7(2) . . . . ? O5 N7 O6 Co1 -168.2(4) . . . . ? O4 N7 O6 Co1 9.6(4) . . . . ? N3 Co1 O6 N7 144.2(2) . . . . ? O1 Co1 O6 N7 21.0(9) . . . . ? N1 Co1 O6 N7 -143.2(2) . . . . ? N5 Co1 O6 N7 71.2(2) . . . . ? O3 Co1 O6 N7 -61.5(3) . . . . ? O4 Co1 O6 N7 -5.7(2) . . . . ? O8 C7 O7 C13 4.8(6) . . . . ? C6 C7 O7 C13 -175.3(3) . . . . ? C14 C13 O7 C7 177.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.761 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.205 data_1cooling123K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.794(3) _cell_length_b 27.475(9) _cell_length_c 7.548(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.433(8) _cell_angle_gamma 90.00 _cell_volume 1997.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3672 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7695 _exptl_absorpt_correction_T_max 0.9135 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16278 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3672 _reflns_number_gt 3537 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+1.5856P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3672 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.003 _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 0.36262(2) 0.873880(8) 0.84426(3) 0.01649(9) Uani 1 1 d . . . C1 C 0.5493(2) 0.96647(7) 0.7489(3) 0.0247(4) Uani 1 1 d . . . H1A H 0.4926 0.9923 0.7779 0.030 Uiso 1 1 calc R . . C2 C 0.6765(2) 0.97312(7) 0.6900(3) 0.0270(4) Uani 1 1 d . . . H2A H 0.7202 1.0032 0.6723 0.032 Uiso 1 1 calc R . . C3 C 0.72386(19) 0.92754(7) 0.6637(2) 0.0229(4) Uani 1 1 d . . . H3A H 0.8077 0.9195 0.6239 0.027 Uiso 1 1 calc R . . C4 C 0.62358(17) 0.84446(6) 0.7016(2) 0.0164(3) Uani 1 1 d . . . C5 C 0.72601(18) 0.81546(6) 0.6503(2) 0.0186(4) Uani 1 1 d . . . H5A H 0.8041 0.8291 0.6100 0.022 Uiso 1 1 calc R . . C6 C 0.70774(17) 0.76507(6) 0.6613(2) 0.0177(3) Uani 1 1 d . . . C7 C 0.81806(18) 0.73208(7) 0.6114(2) 0.0197(4) Uani 1 1 d . . . C8 C 0.59181(17) 0.74533(6) 0.7185(2) 0.0172(3) Uani 1 1 d . . . H8A H 0.5790 0.7112 0.7263 0.021 Uiso 1 1 calc R . . C9 C 0.49635(17) 0.77819(6) 0.7634(2) 0.0162(3) Uani 1 1 d . . . C10 C 0.32277(18) 0.71873(6) 0.8493(2) 0.0184(4) Uani 1 1 d . . . H10A H 0.3658 0.6884 0.8339 0.022 Uiso 1 1 calc R . . C11 C 0.19829(18) 0.72544(7) 0.9026(2) 0.0206(4) Uani 1 1 d . . . H11A H 0.1374 0.7010 0.9321 0.025 Uiso 1 1 calc R . . C12 C 0.17896(18) 0.77629(7) 0.9049(2) 0.0203(4) Uani 1 1 d . . . H12A H 0.1001 0.7918 0.9367 0.024 Uiso 1 1 calc R . . C13 C 0.89030(19) 0.64882(7) 0.6095(3) 0.0236(4) Uani 1 1 d . . . H13A H 0.9810 0.6555 0.6875 0.028 Uiso 1 1 calc R . . H13B H 0.9031 0.6489 0.4823 0.028 Uiso 1 1 calc R . . C14 C 0.83415(19) 0.60013(7) 0.6571(3) 0.0230(4) Uani 1 1 d . . . H14A H 0.7502 0.5920 0.5678 0.028 Uiso 1 1 calc R . . H14B H 0.8069 0.6024 0.7769 0.028 Uiso 1 1 calc R . . C15 C 0.9413(2) 0.55959(7) 0.6604(3) 0.0312(5) Uani 1 1 d . . . H15A H 0.9645 0.5561 0.5388 0.037 Uiso 1 1 calc R . . H15B H 1.0272 0.5687 0.7445 0.037 Uiso 1 1 calc R . . C16 C 0.8885(3) 0.51104(8) 0.7187(3) 0.0445(6) Uani 1 1 d . . . H16A H 0.9601 0.4861 0.7194 0.053 Uiso 1 1 calc R . . H16B H 0.8045 0.5016 0.6343 0.053 Uiso 1 1 calc R . . H16C H 0.8669 0.5142 0.8400 0.053 Uiso 1 1 calc R . . N1 N 0.51864(15) 0.91964(5) 0.7589(2) 0.0188(3) Uani 1 1 d . . . N2 N 0.62741(15) 0.89551(5) 0.70552(19) 0.0176(3) Uani 1 1 d . . . N3 N 0.51112(14) 0.82648(5) 0.75598(18) 0.0157(3) Uani 1 1 d . . . N4 N 0.37379(14) 0.76396(5) 0.82238(18) 0.0161(3) Uani 1 1 d . . . N5 N 0.28495(15) 0.79974(5) 0.8568(2) 0.0185(3) Uani 1 1 d . . . N6 N 0.43831(16) 0.90308(5) 1.1719(2) 0.0221(3) Uani 1 1 d . . . N7 N 0.12150(16) 0.88368(6) 0.6492(2) 0.0232(3) Uani 1 1 d . . . O1 O 0.46748(14) 0.86088(5) 1.11718(17) 0.0235(3) Uani 1 1 d . . . O2 O 0.47560(17) 0.91613(6) 1.32719(18) 0.0387(4) Uani 1 1 d . . . O3 O 0.36805(14) 0.93007(5) 1.05265(17) 0.0267(3) Uani 1 1 d . . . O4 O 0.13636(14) 0.88695(5) 0.81888(18) 0.0269(3) Uani 1 1 d . . . O5 O 0.00651(14) 0.88059(6) 0.5522(2) 0.0342(3) Uani 1 1 d . . . O6 O 0.23238(13) 0.88306(5) 0.58370(18) 0.0247(3) Uani 1 1 d . . . O7 O 0.78813(13) 0.68556(5) 0.63762(18) 0.0248(3) Uani 1 1 d . . . O8 O 0.91827(13) 0.74659(5) 0.55528(19) 0.0272(3) 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 0.01591(15) 0.01549(13) 0.01834(14) -0.00101(8) 0.00383(10) 0.00103(8) C1 0.0267(10) 0.0166(9) 0.0313(10) -0.0022(7) 0.0069(8) -0.0004(7) C2 0.0295(10) 0.0190(9) 0.0338(11) -0.0008(8) 0.0094(8) -0.0060(8) C3 0.0229(10) 0.0233(9) 0.0236(9) -0.0012(7) 0.0072(7) -0.0064(7) C4 0.0178(9) 0.0170(8) 0.0139(8) -0.0007(6) 0.0015(6) -0.0018(7) C5 0.0170(9) 0.0213(9) 0.0180(8) -0.0008(7) 0.0040(7) -0.0023(7) C6 0.0163(9) 0.0210(9) 0.0154(8) -0.0014(7) 0.0014(7) 0.0009(7) C7 0.0188(9) 0.0235(9) 0.0161(8) -0.0022(7) 0.0012(7) 0.0005(7) C8 0.0184(9) 0.0166(8) 0.0159(8) -0.0024(6) 0.0017(7) -0.0013(7) C9 0.0160(8) 0.0193(8) 0.0124(8) 0.0001(6) 0.0005(6) -0.0013(7) C10 0.0210(9) 0.0165(8) 0.0173(8) -0.0004(6) 0.0027(7) -0.0020(7) C11 0.0197(9) 0.0231(9) 0.0191(9) -0.0002(7) 0.0037(7) -0.0051(7) C12 0.0163(9) 0.0247(9) 0.0204(9) -0.0010(7) 0.0044(7) -0.0025(7) C13 0.0201(9) 0.0230(9) 0.0282(10) -0.0035(8) 0.0058(7) 0.0046(7) C14 0.0241(10) 0.0210(9) 0.0233(9) -0.0023(7) 0.0023(7) 0.0014(7) C15 0.0362(12) 0.0238(10) 0.0338(11) -0.0025(8) 0.0066(9) 0.0071(8) C16 0.0606(16) 0.0249(11) 0.0501(14) 0.0010(10) 0.0153(12) 0.0074(10) N1 0.0177(7) 0.0174(7) 0.0221(8) -0.0018(6) 0.0058(6) 0.0013(6) N2 0.0165(7) 0.0178(7) 0.0190(7) -0.0001(6) 0.0041(6) -0.0018(6) N3 0.0150(7) 0.0176(7) 0.0146(7) -0.0011(5) 0.0024(5) -0.0002(6) N4 0.0154(7) 0.0160(7) 0.0174(7) -0.0005(5) 0.0039(6) -0.0003(5) N5 0.0157(7) 0.0187(7) 0.0215(7) -0.0020(6) 0.0049(6) 0.0020(6) N6 0.0259(8) 0.0197(8) 0.0205(8) -0.0002(6) 0.0039(6) -0.0014(6) N7 0.0210(8) 0.0197(8) 0.0281(9) 0.0030(6) 0.0022(7) 0.0010(6) O1 0.0287(7) 0.0177(6) 0.0237(7) 0.0002(5) 0.0041(5) 0.0032(5) O2 0.0568(10) 0.0377(9) 0.0180(7) -0.0070(6) -0.0032(7) 0.0024(7) O3 0.0343(8) 0.0227(7) 0.0219(7) 0.0007(5) 0.0020(6) 0.0079(6) O4 0.0304(8) 0.0254(7) 0.0251(7) -0.0009(5) 0.0058(6) 0.0063(6) O5 0.0178(7) 0.0456(9) 0.0358(8) 0.0043(7) -0.0038(6) 0.0001(6) O6 0.0189(7) 0.0295(7) 0.0259(7) 0.0038(5) 0.0042(5) -0.0011(5) O7 0.0209(7) 0.0192(6) 0.0365(8) -0.0010(5) 0.0113(6) 0.0027(5) O8 0.0207(7) 0.0263(7) 0.0379(8) -0.0018(6) 0.0141(6) 0.0009(5) _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 N3 2.1462(15) . ? Co1 O6 2.1563(14) . ? Co1 O1 2.1585(14) . ? Co1 N1 2.1651(16) . ? Co1 N5 2.1824(16) . ? Co1 O3 2.1977(14) . ? Co1 O4 2.2188(16) . ? C1 N1 1.326(2) . ? C1 C2 1.409(3) . ? C1 H1A 0.9500 . ? C2 C3 1.363(3) . ? C2 H2A 0.9500 . ? C3 N2 1.369(2) . ? C3 H3A 0.9500 . ? C4 N3 1.338(2) . ? C4 C5 1.390(2) . ? C4 N2 1.403(2) . ? C5 C6 1.400(2) . ? C5 H5A 0.9500 . ? C6 C8 1.396(2) . ? C6 C7 1.509(2) . ? C7 O8 1.205(2) . ? C7 O7 1.334(2) . ? C8 C9 1.385(2) . ? C8 H8A 0.9500 . ? C9 N3 1.337(2) . ? C9 N4 1.409(2) . ? C10 C11 1.364(3) . ? C10 N4 1.368(2) . ? C10 H10A 0.9500 . ? C11 C12 1.411(3) . ? C11 H11A 0.9500 . ? C12 N5 1.327(2) . ? C12 H12A 0.9500 . ? C13 O7 1.464(2) . ? C13 C14 1.514(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.527(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.524(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N1 N2 1.375(2) . ? N4 N5 1.369(2) . ? N6 O2 1.217(2) . ? N6 O3 1.268(2) . ? N6 O1 1.280(2) . ? N7 O5 1.230(2) . ? N7 O4 1.266(2) . ? N7 O6 1.272(2) . ? 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 N3 Co1 O6 96.32(6) . . ? N3 Co1 O1 87.93(5) . . ? O6 Co1 O1 172.03(5) . . ? N3 Co1 N1 72.87(6) . . ? O6 Co1 N1 89.63(6) . . ? O1 Co1 N1 98.08(6) . . ? N3 Co1 N5 73.04(6) . . ? O6 Co1 N5 89.74(5) . . ? O1 Co1 N5 85.04(5) . . ? N1 Co1 N5 145.61(5) . . ? N3 Co1 O3 135.93(5) . . ? O6 Co1 O3 120.28(5) . . ? O1 Co1 O3 59.17(5) . . ? N1 Co1 O3 83.00(6) . . ? N5 Co1 O3 126.02(6) . . ? N3 Co1 O4 142.55(5) . . ? O6 Co1 O4 59.05(5) . . ? O1 Co1 O4 113.85(5) . . ? N1 Co1 O4 128.91(6) . . ? N5 Co1 O4 78.71(5) . . ? O3 Co1 O4 80.93(5) . . ? N1 C1 C2 111.46(17) . . ? N1 C1 H1A 124.3 . . ? C2 C1 H1A 124.3 . . ? C3 C2 C1 105.71(16) . . ? C3 C2 H2A 127.1 . . ? C1 C2 H2A 127.1 . . ? C2 C3 N2 106.83(16) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? N3 C4 C5 123.35(16) . . ? N3 C4 N2 112.51(14) . . ? C5 C4 N2 124.13(15) . . ? C4 C5 C6 116.35(16) . . ? C4 C5 H5A 121.8 . . ? C6 C5 H5A 121.8 . . ? C8 C6 C5 121.49(16) . . ? C8 C6 C7 120.21(16) . . ? C5 C6 C7 118.30(16) . . ? O8 C7 O7 125.72(16) . . ? O8 C7 C6 123.67(17) . . ? O7 C7 C6 110.61(15) . . ? C9 C8 C6 116.46(16) . . ? C9 C8 H8A 121.8 . . ? C6 C8 H8A 121.8 . . ? N3 C9 C8 123.60(16) . . ? N3 C9 N4 113.18(15) . . ? C8 C9 N4 123.22(15) . . ? C11 C10 N4 106.93(15) . . ? C11 C10 H10A 126.5 . . ? N4 C10 H10A 126.5 . . ? C10 C11 C12 105.45(15) . . ? C10 C11 H11A 127.3 . . ? C12 C11 H11A 127.3 . . ? N5 C12 C11 111.37(16) . . ? N5 C12 H12A 124.3 . . ? C11 C12 H12A 124.3 . . ? O7 C13 C14 106.71(15) . . ? O7 C13 H13A 110.4 . . ? C14 C13 H13A 110.4 . . ? O7 C13 H13B 110.4 . . ? C14 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? C13 C14 C15 111.72(16) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 112.02(18) . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? 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 . . ? C1 N1 N2 104.82(15) . . ? C1 N1 Co1 139.39(13) . . ? N2 N1 Co1 115.67(11) . . ? C3 N2 N1 111.18(14) . . ? C3 N2 C4 130.87(15) . . ? N1 N2 C4 117.95(13) . . ? C9 N3 C4 118.74(15) . . ? C9 N3 Co1 120.30(11) . . ? C4 N3 Co1 120.88(12) . . ? C10 N4 N5 111.24(14) . . ? C10 N4 C9 130.84(15) . . ? N5 N4 C9 117.90(14) . . ? C12 N5 N4 105.00(14) . . ? C12 N5 Co1 139.57(12) . . ? N4 N5 Co1 115.06(10) . . ? O2 N6 O3 122.74(16) . . ? O2 N6 O1 122.13(15) . . ? O3 N6 O1 115.13(14) . . ? O5 N7 O4 122.18(16) . . ? O5 N7 O6 121.43(16) . . ? O4 N7 O6 116.38(15) . . ? N6 O1 Co1 93.59(10) . . ? N6 O3 Co1 92.11(10) . . ? N7 O4 Co1 90.34(10) . . ? N7 O6 Co1 93.03(10) . . ? C7 O7 C13 117.70(14) . . ? 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 N1 C1 C2 C3 0.0(2) . . . . ? C1 C2 C3 N2 0.1(2) . . . . ? N3 C4 C5 C6 -1.2(2) . . . . ? N2 C4 C5 C6 177.55(15) . . . . ? C4 C5 C6 C8 0.8(2) . . . . ? C4 C5 C6 C7 -178.50(15) . . . . ? C8 C6 C7 O8 177.40(17) . . . . ? C5 C6 C7 O8 -3.3(3) . . . . ? C8 C6 C7 O7 -2.3(2) . . . . ? C5 C6 C7 O7 176.98(15) . . . . ? C5 C6 C8 C9 0.1(2) . . . . ? C7 C6 C8 C9 179.34(15) . . . . ? C6 C8 C9 N3 -0.6(2) . . . . ? C6 C8 C9 N4 179.59(15) . . . . ? N4 C10 C11 C12 0.21(19) . . . . ? C10 C11 C12 N5 -0.3(2) . . . . ? O7 C13 C14 C15 -171.44(15) . . . . ? C13 C14 C15 C16 176.74(17) . . . . ? C2 C1 N1 N2 -0.1(2) . . . . ? C2 C1 N1 Co1 175.52(14) . . . . ? N3 Co1 N1 C1 -178.3(2) . . . . ? O6 Co1 N1 C1 84.9(2) . . . . ? O1 Co1 N1 C1 -93.0(2) . . . . ? N5 Co1 N1 C1 173.92(17) . . . . ? O3 Co1 N1 C1 -35.66(19) . . . . ? O4 Co1 N1 C1 36.7(2) . . . . ? N3 Co1 N1 N2 -3.09(11) . . . . ? O6 Co1 N1 N2 -99.82(12) . . . . ? O1 Co1 N1 N2 82.20(12) . . . . ? N5 Co1 N1 N2 -10.83(17) . . . . ? O3 Co1 N1 N2 139.59(12) . . . . ? O4 Co1 N1 N2 -148.05(10) . . . . ? C2 C3 N2 N1 -0.1(2) . . . . ? C2 C3 N2 C4 179.68(17) . . . . ? C1 N1 N2 C3 0.12(19) . . . . ? Co1 N1 N2 C3 -176.69(11) . . . . ? C1 N1 N2 C4 -179.72(15) . . . . ? Co1 N1 N2 C4 3.47(18) . . . . ? N3 C4 N2 C3 178.95(17) . . . . ? C5 C4 N2 C3 0.1(3) . . . . ? N3 C4 N2 N1 -1.2(2) . . . . ? C5 C4 N2 N1 179.89(15) . . . . ? C8 C9 N3 C4 0.3(2) . . . . ? N4 C9 N3 C4 -179.90(14) . . . . ? C8 C9 N3 Co1 -176.25(12) . . . . ? N4 C9 N3 Co1 3.54(19) . . . . ? C5 C4 N3 C9 0.7(2) . . . . ? N2 C4 N3 C9 -178.21(14) . . . . ? C5 C4 N3 Co1 177.19(12) . . . . ? N2 C4 N3 Co1 -1.67(18) . . . . ? O6 Co1 N3 C9 -93.23(13) . . . . ? O1 Co1 N3 C9 80.01(13) . . . . ? N1 Co1 N3 C9 179.12(13) . . . . ? N5 Co1 N3 C9 -5.44(12) . . . . ? O3 Co1 N3 C9 119.24(12) . . . . ? O4 Co1 N3 C9 -48.17(16) . . . . ? O6 Co1 N3 C4 90.29(13) . . . . ? O1 Co1 N3 C4 -96.47(13) . . . . ? N1 Co1 N3 C4 2.64(12) . . . . ? N5 Co1 N3 C4 178.08(14) . . . . ? O3 Co1 N3 C4 -57.24(15) . . . . ? O4 Co1 N3 C4 135.35(12) . . . . ? C11 C10 N4 N5 -0.10(19) . . . . ? C11 C10 N4 C9 -178.48(16) . . . . ? N3 C9 N4 C10 -179.23(16) . . . . ? C8 C9 N4 C10 0.6(3) . . . . ? N3 C9 N4 N5 2.5(2) . . . . ? C8 C9 N4 N5 -177.73(15) . . . . ? C11 C12 N5 N4 0.21(19) . . . . ? C11 C12 N5 Co1 -172.00(13) . . . . ? C10 N4 N5 C12 -0.07(18) . . . . ? C9 N4 N5 C12 178.54(14) . . . . ? C10 N4 N5 Co1 174.36(11) . . . . ? C9 N4 N5 Co1 -7.03(18) . . . . ? N3 Co1 N5 C12 178.0(2) . . . . ? O6 Co1 N5 C12 -85.28(19) . . . . ? O1 Co1 N5 C12 88.69(19) . . . . ? N1 Co1 N5 C12 -174.24(16) . . . . ? O3 Co1 N5 C12 43.0(2) . . . . ? O4 Co1 N5 C12 -26.85(18) . . . . ? N3 Co1 N5 N4 6.34(10) . . . . ? O6 Co1 N5 N4 103.03(11) . . . . ? O1 Co1 N5 N4 -83.00(11) . . . . ? N1 Co1 N5 N4 14.07(17) . . . . ? O3 Co1 N5 N4 -128.65(11) . . . . ? O4 Co1 N5 N4 161.46(12) . . . . ? O2 N6 O1 Co1 -179.74(16) . . . . ? O3 N6 O1 Co1 0.25(15) . . . . ? N3 Co1 O1 N6 149.03(10) . . . . ? O6 Co1 O1 N6 -88.6(4) . . . . ? N1 Co1 O1 N6 76.67(10) . . . . ? N5 Co1 O1 N6 -137.81(10) . . . . ? O3 Co1 O1 N6 -0.15(9) . . . . ? O4 Co1 O1 N6 -62.48(11) . . . . ? O2 N6 O3 Co1 179.75(16) . . . . ? O1 N6 O3 Co1 -0.25(15) . . . . ? N3 Co1 O3 N6 -47.23(13) . . . . ? O6 Co1 O3 N6 170.92(9) . . . . ? O1 Co1 O3 N6 0.16(9) . . . . ? N1 Co1 O3 N6 -103.62(11) . . . . ? N5 Co1 O3 N6 56.22(12) . . . . ? O4 Co1 O3 N6 125.05(11) . . . . ? O5 N7 O4 Co1 168.53(15) . . . . ? O6 N7 O4 Co1 -10.53(15) . . . . ? N3 Co1 O4 N7 -48.65(14) . . . . ? O6 Co1 O4 N7 6.47(9) . . . . ? O1 Co1 O4 N7 -169.45(9) . . . . ? N1 Co1 O4 N7 66.88(12) . . . . ? N5 Co1 O4 N7 -90.09(10) . . . . ? O3 Co1 O4 N7 140.18(10) . . . . ? O5 N7 O6 Co1 -168.21(15) . . . . ? O4 N7 O6 Co1 10.85(15) . . . . ? N3 Co1 O6 N7 143.43(10) . . . . ? O1 Co1 O6 N7 21.5(4) . . . . ? N1 Co1 O6 N7 -143.85(10) . . . . ? N5 Co1 O6 N7 70.53(10) . . . . ? O3 Co1 O6 N7 -62.18(11) . . . . ? O4 Co1 O6 N7 -6.44(9) . . . . ? O8 C7 O7 C13 5.0(3) . . . . ? C6 C7 O7 C13 -175.23(14) . . . . ? C14 C13 O7 C7 177.16(15) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.299 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.052 data_1heating183K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.796(2) _cell_length_b 27.433(6) _cell_length_c 7.5962(17) _cell_angle_alpha 90.00 _cell_angle_beta 100.288(5) _cell_angle_gamma 90.00 _cell_volume 2008.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 3666 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7706 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15991 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3666 _reflns_number_gt 3520 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.3999P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3666 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36337(3) 0.873822(9) 0.84215(4) 0.02160(11) Uani 1 1 d . . . C1 C 0.5486(2) 0.96682(8) 0.7460(3) 0.0333(5) Uani 1 1 d . . . H1A H 0.4921 0.9927 0.7754 0.040 Uiso 1 1 calc R . . C2 C 0.6746(2) 0.97347(8) 0.6861(3) 0.0365(5) Uani 1 1 d . . . H2A H 0.7178 1.0036 0.6677 0.044 Uiso 1 1 calc R . . C3 C 0.7223(2) 0.92803(8) 0.6598(3) 0.0307(5) Uani 1 1 d . . . H3A H 0.8060 0.9201 0.6195 0.037 Uiso 1 1 calc R . . C4 C 0.62337(19) 0.84479(7) 0.6992(2) 0.0211(4) Uani 1 1 d . . . C5 C 0.7263(2) 0.81603(7) 0.6475(3) 0.0240(4) Uani 1 1 d . . . H5A H 0.8040 0.8298 0.6068 0.029 Uiso 1 1 calc R . . C6 C 0.70857(19) 0.76567(7) 0.6588(3) 0.0221(4) Uani 1 1 d . . . C7 C 0.8189(2) 0.73292(7) 0.6092(3) 0.0252(4) Uani 1 1 d . . . C8 C 0.59300(19) 0.74577(7) 0.7161(2) 0.0217(4) Uani 1 1 d . . . H8A H 0.5807 0.7115 0.7240 0.026 Uiso 1 1 calc R . . C9 C 0.49748(19) 0.77842(7) 0.7607(2) 0.0204(4) Uani 1 1 d . . . C10 C 0.3257(2) 0.71862(7) 0.8472(3) 0.0241(4) Uani 1 1 d . . . H10A H 0.3691 0.6884 0.8314 0.029 Uiso 1 1 calc R . . C11 C 0.2012(2) 0.72515(8) 0.9013(3) 0.0273(4) Uani 1 1 d . . . H11A H 0.1409 0.7006 0.9316 0.033 Uiso 1 1 calc R . . C12 C 0.1815(2) 0.77580(8) 0.9026(3) 0.0271(4) Uani 1 1 d . . . H12A H 0.1023 0.7911 0.9345 0.033 Uiso 1 1 calc R . . C13 C 0.8920(2) 0.64963(8) 0.6076(3) 0.0317(5) Uani 1 1 d . . . H13A H 0.9823 0.6563 0.6855 0.038 Uiso 1 1 calc R . . H13B H 0.9053 0.6497 0.4814 0.038 Uiso 1 1 calc R . . C14 C 0.8352(2) 0.60117(8) 0.6547(3) 0.0314(5) Uani 1 1 d . . . H14A H 0.7511 0.5932 0.5662 0.038 Uiso 1 1 calc R . . H14B H 0.8079 0.6035 0.7738 0.038 Uiso 1 1 calc R . . C15 C 0.9415(3) 0.56028(8) 0.6575(4) 0.0432(6) Uani 1 1 d . . . H15A H 0.9646 0.5567 0.5365 0.052 Uiso 1 1 calc R . . H15B H 1.0276 0.5692 0.7407 0.052 Uiso 1 1 calc R . . C16 C 0.8884(4) 0.51195(10) 0.7151(5) 0.0637(8) Uani 1 1 d . . . H16A H 0.9597 0.4869 0.7155 0.076 Uiso 1 1 calc R . . H16B H 0.8044 0.5026 0.6314 0.076 Uiso 1 1 calc R . . H16C H 0.8668 0.5152 0.8357 0.076 Uiso 1 1 calc R . . N1 N 0.51803(17) 0.91980(6) 0.7566(2) 0.0245(4) Uani 1 1 d . . . N2 N 0.62692(16) 0.89591(6) 0.7023(2) 0.0225(3) Uani 1 1 d . . . N3 N 0.51161(16) 0.82666(6) 0.7535(2) 0.0208(3) Uani 1 1 d . . . N4 N 0.37582(16) 0.76407(6) 0.8202(2) 0.0208(3) Uani 1 1 d . . . N5 N 0.28583(17) 0.79962(6) 0.8544(2) 0.0246(4) Uani 1 1 d . . . N6 N 0.43962(19) 0.90234(6) 1.1683(2) 0.0297(4) Uani 1 1 d . . . N7 N 0.12188(18) 0.88434(7) 0.6502(3) 0.0311(4) Uani 1 1 d . . . O1 O 0.46844(16) 0.86049(5) 1.1126(2) 0.0316(3) Uani 1 1 d . . . O2 O 0.4761(2) 0.91479(7) 1.3230(2) 0.0535(5) Uani 1 1 d . . . O3 O 0.36972(17) 0.92955(6) 1.0517(2) 0.0369(4) Uani 1 1 d . . . O4 O 0.13719(17) 0.88700(6) 0.8176(2) 0.0381(4) Uani 1 1 d . . . O5 O 0.00724(17) 0.88170(7) 0.5535(3) 0.0486(5) Uani 1 1 d . . . O6 O 0.23231(15) 0.88357(6) 0.5850(2) 0.0341(4) Uani 1 1 d . . . O7 O 0.78944(15) 0.68630(5) 0.6352(2) 0.0331(4) Uani 1 1 d . . . O8 O 0.91891(15) 0.74746(6) 0.5528(2) 0.0372(4) 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 0.02017(17) 0.01891(16) 0.02612(17) -0.00124(10) 0.00524(11) 0.00171(9) C1 0.0348(12) 0.0202(10) 0.0459(13) -0.0033(9) 0.0097(10) -0.0017(8) C2 0.0391(13) 0.0231(11) 0.0494(14) -0.0017(9) 0.0140(11) -0.0077(9) C3 0.0314(11) 0.0264(10) 0.0355(11) -0.0007(9) 0.0093(9) -0.0084(8) C4 0.0210(9) 0.0217(9) 0.0201(9) -0.0010(7) 0.0022(7) -0.0018(7) C5 0.0213(10) 0.0260(10) 0.0250(10) -0.0010(8) 0.0047(8) -0.0033(7) C6 0.0182(9) 0.0247(10) 0.0231(9) -0.0025(7) 0.0028(7) 0.0018(7) C7 0.0208(10) 0.0287(10) 0.0262(10) -0.0025(8) 0.0045(8) 0.0006(8) C8 0.0221(10) 0.0187(9) 0.0239(9) -0.0016(7) 0.0031(8) -0.0007(7) C9 0.0199(9) 0.0216(9) 0.0193(9) -0.0012(7) 0.0024(7) -0.0008(7) C10 0.0264(10) 0.0198(9) 0.0257(10) 0.0007(7) 0.0037(8) -0.0038(8) C11 0.0253(10) 0.0296(11) 0.0278(10) 0.0003(8) 0.0072(8) -0.0079(8) C12 0.0204(10) 0.0308(11) 0.0312(11) -0.0009(8) 0.0074(8) -0.0028(8) C13 0.0273(11) 0.0266(11) 0.0416(12) -0.0051(9) 0.0070(9) 0.0071(8) C14 0.0324(11) 0.0278(11) 0.0331(11) -0.0032(9) 0.0036(9) 0.0025(9) C15 0.0496(15) 0.0286(12) 0.0523(15) -0.0047(10) 0.0111(12) 0.0091(10) C16 0.088(2) 0.0311(14) 0.075(2) 0.0032(13) 0.0236(18) 0.0107(14) N1 0.0223(8) 0.0209(8) 0.0314(9) -0.0017(7) 0.0076(7) 0.0012(6) N2 0.0199(8) 0.0207(8) 0.0276(8) -0.0003(7) 0.0059(6) -0.0024(6) N3 0.0192(8) 0.0200(8) 0.0230(8) -0.0017(6) 0.0030(6) -0.0005(6) N4 0.0183(8) 0.0192(8) 0.0256(8) -0.0007(6) 0.0061(6) 0.0004(6) N5 0.0212(8) 0.0218(8) 0.0313(9) -0.0032(7) 0.0060(7) 0.0015(6) N6 0.0354(10) 0.0254(9) 0.0280(9) -0.0020(7) 0.0051(7) -0.0002(7) N7 0.0253(10) 0.0263(9) 0.0407(11) 0.0036(7) 0.0036(8) 0.0025(7) O1 0.0398(9) 0.0212(7) 0.0331(8) 0.0004(6) 0.0049(7) 0.0045(6) O2 0.0808(14) 0.0492(11) 0.0258(9) -0.0091(7) -0.0036(8) 0.0040(10) O3 0.0496(10) 0.0284(8) 0.0316(8) 0.0007(6) 0.0039(7) 0.0119(7) O4 0.0423(10) 0.0341(8) 0.0387(9) -0.0011(7) 0.0091(7) 0.0101(7) O5 0.0228(9) 0.0622(12) 0.0564(11) 0.0082(9) -0.0047(8) 0.0011(7) O6 0.0256(8) 0.0374(9) 0.0383(9) 0.0053(7) 0.0034(7) -0.0007(6) O7 0.0284(8) 0.0224(7) 0.0518(10) -0.0024(7) 0.0159(7) 0.0039(6) O8 0.0280(8) 0.0316(8) 0.0565(10) -0.0014(7) 0.0198(7) 0.0026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.1412(16) . ? Co1 O6 2.1542(16) . ? Co1 O1 2.1582(16) . ? Co1 N1 2.1587(17) . ? Co1 N5 2.1805(17) . ? Co1 O3 2.1997(16) . ? Co1 O4 2.2197(17) . ? C1 N1 1.330(3) . ? C1 C2 1.402(3) . ? C1 H1A 0.9500 . ? C2 C3 1.359(3) . ? C2 H2A 0.9500 . ? C3 N2 1.364(3) . ? C3 H3A 0.9500 . ? C4 N3 1.333(2) . ? C4 C5 1.391(3) . ? C4 N2 1.403(3) . ? C5 C6 1.397(3) . ? C5 H5A 0.9500 . ? C6 C8 1.395(3) . ? C6 C7 1.504(3) . ? C7 O8 1.205(2) . ? C7 O7 1.333(2) . ? C8 C9 1.381(3) . ? C8 H8A 0.9500 . ? C9 N3 1.333(2) . ? C9 N4 1.404(2) . ? C10 C11 1.367(3) . ? C10 N4 1.369(2) . ? C10 H10A 0.9500 . ? C11 C12 1.403(3) . ? C11 H11A 0.9500 . ? C12 N5 1.319(3) . ? C12 H12A 0.9500 . ? C13 O7 1.463(2) . ? C13 C14 1.509(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.528(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.517(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N1 N2 1.376(2) . ? N4 N5 1.370(2) . ? N6 O2 1.215(2) . ? N6 O3 1.263(2) . ? N6 O1 1.273(2) . ? N7 O5 1.229(2) . ? N7 O4 1.255(2) . ? N7 O6 1.268(2) . ? 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 N3 Co1 O6 96.76(6) . . ? N3 Co1 O1 87.82(6) . . ? O6 Co1 O1 171.85(6) . . ? N3 Co1 N1 72.94(6) . . ? O6 Co1 N1 89.49(6) . . ? O1 Co1 N1 98.31(6) . . ? N3 Co1 N5 73.16(6) . . ? O6 Co1 N5 89.94(6) . . ? O1 Co1 N5 84.93(6) . . ? N1 Co1 N5 145.78(6) . . ? N3 Co1 O3 135.58(6) . . ? O6 Co1 O3 120.34(6) . . ? O1 Co1 O3 58.81(6) . . ? N1 Co1 O3 83.17(7) . . ? N5 Co1 O3 125.66(6) . . ? N3 Co1 O4 142.63(6) . . ? O6 Co1 O4 58.61(6) . . ? O1 Co1 O4 114.01(6) . . ? N1 Co1 O4 128.55(6) . . ? N5 Co1 O4 78.79(6) . . ? O3 Co1 O4 81.17(6) . . ? N1 C1 C2 111.51(19) . . ? N1 C1 H1A 124.2 . . ? C2 C1 H1A 124.2 . . ? C3 C2 C1 105.93(19) . . ? C3 C2 H2A 127.0 . . ? C1 C2 H2A 127.0 . . ? C2 C3 N2 106.82(19) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? N3 C4 C5 123.52(18) . . ? N3 C4 N2 112.77(16) . . ? C5 C4 N2 123.70(17) . . ? C4 C5 C6 116.09(18) . . ? C4 C5 H5A 122.0 . . ? C6 C5 H5A 122.0 . . ? C8 C6 C5 121.51(18) . . ? C8 C6 C7 120.27(17) . . ? C5 C6 C7 118.22(17) . . ? O8 C7 O7 125.56(19) . . ? O8 C7 C6 123.86(19) . . ? O7 C7 C6 110.57(16) . . ? C9 C8 C6 116.51(17) . . ? C9 C8 H8A 121.7 . . ? C6 C8 H8A 121.7 . . ? N3 C9 C8 123.65(18) . . ? N3 C9 N4 113.08(16) . . ? C8 C9 N4 123.27(17) . . ? C11 C10 N4 106.77(17) . . ? C11 C10 H10A 126.6 . . ? N4 C10 H10A 126.6 . . ? C10 C11 C12 105.28(17) . . ? C10 C11 H11A 127.4 . . ? C12 C11 H11A 127.4 . . ? N5 C12 C11 111.97(18) . . ? N5 C12 H12A 124.0 . . ? C11 C12 H12A 124.0 . . ? O7 C13 C14 106.27(17) . . ? O7 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? O7 C13 H13B 110.5 . . ? C14 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? C13 C14 C15 111.76(19) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 112.2(2) . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? 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 . . ? C1 N1 N2 104.41(17) . . ? C1 N1 Co1 139.69(15) . . ? N2 N1 Co1 115.80(12) . . ? C3 N2 N1 111.33(16) . . ? C3 N2 C4 131.12(17) . . ? N1 N2 C4 117.56(15) . . ? C9 N3 C4 118.70(16) . . ? C9 N3 Co1 120.39(13) . . ? C4 N3 Co1 120.81(13) . . ? C10 N4 N5 111.10(16) . . ? C10 N4 C9 130.63(17) . . ? N5 N4 C9 118.24(15) . . ? C12 N5 N4 104.88(16) . . ? C12 N5 Co1 140.13(14) . . ? N4 N5 Co1 114.55(12) . . ? O2 N6 O3 122.81(19) . . ? O2 N6 O1 122.06(18) . . ? O3 N6 O1 115.13(17) . . ? O5 N7 O4 122.7(2) . . ? O5 N7 O6 121.1(2) . . ? O4 N7 O6 116.16(18) . . ? N6 O1 Co1 93.85(11) . . ? N6 O3 Co1 92.21(11) . . ? N7 O4 Co1 90.72(12) . . ? N7 O6 Co1 93.40(12) . . ? C7 O7 C13 117.76(16) . . ? 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 N1 C1 C2 C3 -0.2(3) . . . . ? C1 C2 C3 N2 0.2(3) . . . . ? N3 C4 C5 C6 -1.3(3) . . . . ? N2 C4 C5 C6 177.70(17) . . . . ? C4 C5 C6 C8 1.0(3) . . . . ? C4 C5 C6 C7 -178.36(17) . . . . ? C8 C6 C7 O8 177.3(2) . . . . ? C5 C6 C7 O8 -3.3(3) . . . . ? C8 C6 C7 O7 -2.2(2) . . . . ? C5 C6 C7 O7 177.12(17) . . . . ? C5 C6 C8 C9 0.0(3) . . . . ? C7 C6 C8 C9 179.35(17) . . . . ? C6 C8 C9 N3 -0.8(3) . . . . ? C6 C8 C9 N4 179.84(17) . . . . ? N4 C10 C11 C12 0.5(2) . . . . ? C10 C11 C12 N5 -0.4(2) . . . . ? O7 C13 C14 C15 -171.85(18) . . . . ? C13 C14 C15 C16 176.7(2) . . . . ? C2 C1 N1 N2 0.0(2) . . . . ? C2 C1 N1 Co1 175.84(17) . . . . ? N3 Co1 N1 C1 -178.5(2) . . . . ? O6 Co1 N1 C1 84.3(2) . . . . ? O1 Co1 N1 C1 -93.4(2) . . . . ? N5 Co1 N1 C1 173.4(2) . . . . ? O3 Co1 N1 C1 -36.4(2) . . . . ? O4 Co1 N1 C1 36.6(3) . . . . ? N3 Co1 N1 N2 -2.96(12) . . . . ? O6 Co1 N1 N2 -100.19(13) . . . . ? O1 Co1 N1 N2 82.16(13) . . . . ? N5 Co1 N1 N2 -11.0(2) . . . . ? O3 Co1 N1 N2 139.16(13) . . . . ? O4 Co1 N1 N2 -147.89(12) . . . . ? C2 C3 N2 N1 -0.2(2) . . . . ? C2 C3 N2 C4 179.80(19) . . . . ? C1 N1 N2 C3 0.1(2) . . . . ? Co1 N1 N2 C3 -176.87(13) . . . . ? C1 N1 N2 C4 -179.89(17) . . . . ? Co1 N1 N2 C4 3.1(2) . . . . ? N3 C4 N2 C3 179.17(19) . . . . ? C5 C4 N2 C3 0.0(3) . . . . ? N3 C4 N2 N1 -0.8(2) . . . . ? C5 C4 N2 N1 -179.94(17) . . . . ? C8 C9 N3 C4 0.5(3) . . . . ? N4 C9 N3 C4 179.89(16) . . . . ? C8 C9 N3 Co1 -176.01(14) . . . . ? N4 C9 N3 Co1 3.4(2) . . . . ? C5 C4 N3 C9 0.7(3) . . . . ? N2 C4 N3 C9 -178.48(16) . . . . ? C5 C4 N3 Co1 177.14(14) . . . . ? N2 C4 N3 Co1 -2.0(2) . . . . ? O6 Co1 N3 C9 -93.45(14) . . . . ? O1 Co1 N3 C9 79.80(14) . . . . ? N1 Co1 N3 C9 179.18(15) . . . . ? N5 Co1 N3 C9 -5.56(14) . . . . ? O3 Co1 N3 C9 118.59(14) . . . . ? O4 Co1 N3 C9 -48.59(19) . . . . ? O6 Co1 N3 C4 90.13(14) . . . . ? O1 Co1 N3 C4 -96.63(14) . . . . ? N1 Co1 N3 C4 2.75(14) . . . . ? N5 Co1 N3 C4 178.01(15) . . . . ? O3 Co1 N3 C4 -57.84(17) . . . . ? O4 Co1 N3 C4 134.98(14) . . . . ? C11 C10 N4 N5 -0.5(2) . . . . ? C11 C10 N4 C9 -178.42(18) . . . . ? N3 C9 N4 C10 -179.18(18) . . . . ? C8 C9 N4 C10 0.2(3) . . . . ? N3 C9 N4 N5 3.0(2) . . . . ? C8 C9 N4 N5 -177.61(17) . . . . ? C11 C12 N5 N4 0.2(2) . . . . ? C11 C12 N5 Co1 -171.27(16) . . . . ? C10 N4 N5 C12 0.2(2) . . . . ? C9 N4 N5 C12 178.42(16) . . . . ? C10 N4 N5 Co1 174.16(12) . . . . ? C9 N4 N5 Co1 -7.6(2) . . . . ? N3 Co1 N5 C12 177.6(2) . . . . ? O6 Co1 N5 C12 -85.4(2) . . . . ? O1 Co1 N5 C12 88.3(2) . . . . ? N1 Co1 N5 C12 -174.36(19) . . . . ? O3 Co1 N5 C12 43.0(2) . . . . ? O4 Co1 N5 C12 -27.4(2) . . . . ? N3 Co1 N5 N4 6.67(12) . . . . ? O6 Co1 N5 N4 103.75(13) . . . . ? O1 Co1 N5 N4 -82.58(13) . . . . ? N1 Co1 N5 N4 14.74(19) . . . . ? O3 Co1 N5 N4 -127.87(12) . . . . ? O4 Co1 N5 N4 161.69(14) . . . . ? O2 N6 O1 Co1 179.5(2) . . . . ? O3 N6 O1 Co1 0.14(18) . . . . ? N3 Co1 O1 N6 149.08(12) . . . . ? O6 Co1 O1 N6 -86.5(4) . . . . ? N1 Co1 O1 N6 76.68(12) . . . . ? N5 Co1 O1 N6 -137.64(12) . . . . ? O3 Co1 O1 N6 -0.09(11) . . . . ? O4 Co1 O1 N6 -62.30(13) . . . . ? O2 N6 O3 Co1 -179.5(2) . . . . ? O1 N6 O3 Co1 -0.14(18) . . . . ? N3 Co1 O3 N6 -46.95(16) . . . . ? O6 Co1 O3 N6 170.66(11) . . . . ? O1 Co1 O3 N6 0.09(11) . . . . ? N1 Co1 O3 N6 -103.96(13) . . . . ? N5 Co1 O3 N6 55.92(14) . . . . ? O4 Co1 O3 N6 125.21(13) . . . . ? O5 N7 O4 Co1 168.71(19) . . . . ? O6 N7 O4 Co1 -10.02(18) . . . . ? N3 Co1 O4 N7 -48.95(16) . . . . ? O6 Co1 O4 N7 6.18(11) . . . . ? O1 Co1 O4 N7 -169.92(11) . . . . ? N1 Co1 O4 N7 66.22(14) . . . . ? N5 Co1 O4 N7 -90.69(12) . . . . ? O3 Co1 O4 N7 140.09(12) . . . . ? O5 N7 O6 Co1 -168.40(18) . . . . ? O4 N7 O6 Co1 10.34(18) . . . . ? N3 Co1 O6 N7 143.78(12) . . . . ? O1 Co1 O6 N7 19.9(5) . . . . ? N1 Co1 O6 N7 -143.47(12) . . . . ? N5 Co1 O6 N7 70.74(12) . . . . ? O3 Co1 O6 N7 -61.69(13) . . . . ? O4 Co1 O6 N7 -6.13(11) . . . . ? O8 C7 O7 C13 5.4(3) . . . . ? C6 C7 O7 C13 -175.08(17) . . . . ? C14 C13 O7 C7 177.28(17) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.331 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.061 data_1heating243K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.804(4) _cell_length_b 27.417(10) _cell_length_c 7.659(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.030(5) _cell_angle_gamma 90.00 _cell_volume 2027.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 4582 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7723 _exptl_absorpt_correction_T_max 0.9147 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14242 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4582 _reflns_number_gt 3539 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4582 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.002 _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 0.36448(2) 0.373725(8) 0.84006(3) 0.02500(9) Uani 1 1 d . . . C1 C 0.5476(2) 0.46701(7) 0.7445(3) 0.0396(5) Uani 1 1 d . . . H1A H 0.4919 0.4925 0.7751 0.047 Uiso 1 1 calc R . . C2 C 0.6722(2) 0.47390(7) 0.6825(3) 0.0437(5) Uani 1 1 d . . . H2A H 0.7140 0.5038 0.6630 0.052 Uiso 1 1 calc R . . C3 C 0.7203(2) 0.42857(7) 0.6561(2) 0.0353(4) Uani 1 1 d . . . H3A H 0.8028 0.4209 0.6154 0.042 Uiso 1 1 calc R . . C4 C 0.62377(17) 0.34526(6) 0.6964(2) 0.0223(3) Uani 1 1 d . . . C5 C 0.72609(18) 0.31655(6) 0.6450(2) 0.0264(4) Uani 1 1 d . . . H5A H 0.8027 0.3303 0.6047 0.032 Uiso 1 1 calc R . . C6 C 0.70978(17) 0.26625(6) 0.6561(2) 0.0246(3) Uani 1 1 d . . . C7 C 0.82021(18) 0.23371(6) 0.6073(2) 0.0297(4) Uani 1 1 d . . . C8 C 0.59486(17) 0.24621(6) 0.7139(2) 0.0242(3) Uani 1 1 d . . . H8A H 0.5832 0.2123 0.7220 0.029 Uiso 1 1 calc R . . C9 C 0.49927(17) 0.27858(6) 0.7587(2) 0.0220(3) Uani 1 1 d . . . C10 C 0.32892(18) 0.21852(6) 0.8455(2) 0.0277(4) Uani 1 1 d . . . H10A H 0.3725 0.1887 0.8302 0.033 Uiso 1 1 calc R . . C11 C 0.20487(19) 0.22470(7) 0.8991(2) 0.0314(4) Uani 1 1 d . . . H11A H 0.1457 0.2002 0.9287 0.038 Uiso 1 1 calc R . . C12 C 0.18398(18) 0.27521(7) 0.9007(2) 0.0313(4) Uani 1 1 d . . . H12A H 0.1057 0.2902 0.9328 0.038 Uiso 1 1 calc R . . C13 C 0.89313(19) 0.15049(7) 0.6060(3) 0.0370(4) Uani 1 1 d . . . H13A H 0.9824 0.1571 0.6821 0.044 Uiso 1 1 calc R . . H13B H 0.9065 0.1505 0.4822 0.044 Uiso 1 1 calc R . . C14 C 0.8367(2) 0.10202(7) 0.6530(3) 0.0375(4) Uani 1 1 d . . . H14A H 0.7532 0.0943 0.5671 0.045 Uiso 1 1 calc R . . H14B H 0.8104 0.1043 0.7704 0.045 Uiso 1 1 calc R . . C15 C 0.9410(3) 0.06113(8) 0.6541(3) 0.0531(6) Uani 1 1 d . . . H15A H 0.9628 0.0576 0.5346 0.064 Uiso 1 1 calc R . . H15B H 1.0267 0.0699 0.7341 0.064 Uiso 1 1 calc R . . C16 C 0.8895(3) 0.01301(9) 0.7119(4) 0.0793(9) Uani 1 1 d . . . H16A H 0.9605 -0.0116 0.7119 0.095 Uiso 1 1 calc R . . H16B H 0.8066 0.0035 0.6306 0.095 Uiso 1 1 calc R . . H16C H 0.8683 0.0162 0.8304 0.095 Uiso 1 1 calc R . . N1 N 0.51803(15) 0.42016(5) 0.75477(19) 0.0290(3) Uani 1 1 d . . . N2 N 0.62617(15) 0.39629(5) 0.69994(18) 0.0260(3) Uani 1 1 d . . . N3 N 0.51258(14) 0.32692(5) 0.75131(17) 0.0223(3) Uani 1 1 d . . . N4 N 0.37802(14) 0.26392(5) 0.81827(17) 0.0230(3) Uani 1 1 d . . . N5 N 0.28773(15) 0.29925(5) 0.85164(19) 0.0281(3) Uani 1 1 d . . . N6 N 0.44038(17) 0.40153(6) 1.1656(2) 0.0364(4) Uani 1 1 d . . . N7 N 0.12249(17) 0.38473(6) 0.6513(2) 0.0387(4) Uani 1 1 d . . . O1 O 0.46965(15) 0.36004(4) 1.10786(17) 0.0365(3) Uani 1 1 d . . . O2 O 0.4764(2) 0.41341(6) 1.31916(18) 0.0665(5) Uani 1 1 d . . . O3 O 0.37203(16) 0.42935(5) 1.05091(17) 0.0455(4) Uani 1 1 d . . . O4 O 0.13815(16) 0.38703(5) 0.8175(2) 0.0478(4) Uani 1 1 d . . . O5 O 0.00813(16) 0.38293(6) 0.5551(2) 0.0646(5) Uani 1 1 d . . . O6 O 0.23231(14) 0.38410(5) 0.58670(19) 0.0418(3) Uani 1 1 d . . . O7 O 0.79166(14) 0.18714(5) 0.63334(18) 0.0395(3) Uani 1 1 d . . . O8 O 0.91936(14) 0.24819(5) 0.55116(19) 0.0446(4) 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 0.02371(14) 0.02203(13) 0.02998(14) -0.00159(9) 0.00670(9) 0.00241(9) C1 0.0428(12) 0.0215(9) 0.0562(12) -0.0030(8) 0.0135(9) -0.0022(8) C2 0.0470(13) 0.0247(10) 0.0625(14) -0.0023(8) 0.0186(10) -0.0096(8) C3 0.0336(11) 0.0317(10) 0.0433(11) -0.0018(8) 0.0142(8) -0.0103(8) C4 0.0218(8) 0.0230(8) 0.0220(8) -0.0011(6) 0.0039(6) -0.0021(6) C5 0.0231(9) 0.0286(9) 0.0292(9) -0.0008(6) 0.0092(7) -0.0025(7) C6 0.0207(8) 0.0282(9) 0.0251(8) -0.0029(6) 0.0048(6) 0.0021(7) C7 0.0249(9) 0.0326(9) 0.0317(9) -0.0042(7) 0.0054(7) 0.0013(7) C8 0.0241(9) 0.0221(8) 0.0265(8) -0.0015(6) 0.0047(7) -0.0006(6) C9 0.0221(8) 0.0235(8) 0.0204(8) -0.0012(6) 0.0034(6) -0.0016(6) C10 0.0312(10) 0.0226(8) 0.0294(9) 0.0002(6) 0.0057(7) -0.0037(7) C11 0.0299(10) 0.0334(10) 0.0319(9) 0.0007(7) 0.0087(7) -0.0093(8) C12 0.0230(9) 0.0365(10) 0.0367(10) -0.0020(7) 0.0111(7) -0.0045(7) C13 0.0286(10) 0.0340(10) 0.0496(12) -0.0074(8) 0.0097(8) 0.0088(8) C14 0.0396(11) 0.0340(10) 0.0391(11) -0.0036(8) 0.0069(8) 0.0060(9) C15 0.0628(16) 0.0367(12) 0.0624(14) -0.0053(10) 0.0179(12) 0.0149(11) C16 0.111(3) 0.0356(14) 0.096(2) 0.0025(13) 0.0323(18) 0.0162(14) N1 0.0280(8) 0.0226(7) 0.0373(8) -0.0027(6) 0.0087(6) -0.0002(6) N2 0.0244(8) 0.0229(7) 0.0314(8) -0.0006(5) 0.0071(6) -0.0029(6) N3 0.0222(7) 0.0211(7) 0.0241(7) -0.0015(5) 0.0057(5) -0.0017(5) N4 0.0208(7) 0.0209(7) 0.0282(7) -0.0005(5) 0.0067(6) 0.0002(5) N5 0.0224(7) 0.0267(8) 0.0368(8) -0.0018(6) 0.0096(6) 0.0009(6) N6 0.0452(10) 0.0308(8) 0.0331(9) -0.0022(6) 0.0064(7) -0.0018(7) N7 0.0302(9) 0.0332(9) 0.0516(11) 0.0044(7) 0.0040(8) 0.0033(7) O1 0.0467(9) 0.0243(6) 0.0384(7) -0.0004(5) 0.0069(6) 0.0054(6) O2 0.1036(15) 0.0607(11) 0.0303(8) -0.0134(7) -0.0023(8) 0.0053(10) O3 0.0649(11) 0.0341(8) 0.0367(8) 0.0006(6) 0.0065(7) 0.0168(7) O4 0.0531(10) 0.0422(8) 0.0507(10) 0.0009(6) 0.0162(7) 0.0151(7) O5 0.0266(9) 0.0832(13) 0.0783(12) 0.0132(9) -0.0067(8) 0.0012(8) O6 0.0287(8) 0.0487(8) 0.0473(8) 0.0079(6) 0.0050(6) -0.0002(6) O7 0.0313(7) 0.0269(7) 0.0646(9) -0.0039(6) 0.0202(6) 0.0051(5) O8 0.0319(8) 0.0396(8) 0.0690(10) -0.0008(7) 0.0277(7) 0.0022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.1356(14) . ? Co1 O6 2.1563(15) . ? Co1 N1 2.1578(15) . ? Co1 O1 2.1619(15) . ? Co1 N5 2.1833(16) . ? Co1 O3 2.2129(14) . ? Co1 O4 2.2255(17) . ? C1 N1 1.322(2) . ? C1 C2 1.399(3) . ? C1 H1A 0.9400 . ? C2 C3 1.357(3) . ? C2 H2A 0.9400 . ? C3 N2 1.362(2) . ? C3 H3A 0.9400 . ? C4 N3 1.333(2) . ? C4 C5 1.385(2) . ? C4 N2 1.399(2) . ? C5 C6 1.392(2) . ? C5 H5A 0.9400 . ? C6 C8 1.393(2) . ? C6 C7 1.500(2) . ? C7 O8 1.197(2) . ? C7 O7 1.330(2) . ? C8 C9 1.377(2) . ? C8 H8A 0.9400 . ? C9 N3 1.3337(19) . ? C9 N4 1.404(2) . ? C10 C11 1.360(2) . ? C10 N4 1.364(2) . ? C10 H10A 0.9400 . ? C11 C12 1.400(3) . ? C11 H11A 0.9400 . ? C12 N5 1.320(2) . ? C12 H12A 0.9400 . ? C13 O7 1.454(2) . ? C13 C14 1.507(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.516(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.506(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? N1 N2 1.373(2) . ? N4 N5 1.3659(18) . ? N6 O2 1.2124(19) . ? N6 O3 1.2635(19) . ? N6 O1 1.2711(19) . ? N7 O5 1.230(2) . ? N7 O4 1.257(2) . ? N7 O6 1.261(2) . ? 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 N3 Co1 O6 97.36(6) . . ? N3 Co1 N1 73.10(6) . . ? O6 Co1 N1 89.50(6) . . ? N3 Co1 O1 87.67(5) . . ? O6 Co1 O1 171.57(5) . . ? N1 Co1 O1 98.45(6) . . ? N3 Co1 N5 73.09(5) . . ? O6 Co1 N5 90.15(5) . . ? N1 Co1 N5 145.85(5) . . ? O1 Co1 N5 84.84(5) . . ? N3 Co1 O3 135.09(5) . . ? O6 Co1 O3 120.28(6) . . ? N1 Co1 O3 82.99(6) . . ? O1 Co1 O3 58.50(5) . . ? N5 Co1 O3 125.65(6) . . ? N3 Co1 O4 142.92(5) . . ? O6 Co1 O4 58.25(6) . . ? N1 Co1 O4 128.21(6) . . ? O1 Co1 O4 113.98(5) . . ? N5 Co1 O4 79.08(6) . . ? O3 Co1 O4 81.36(6) . . ? N1 C1 C2 111.39(17) . . ? N1 C1 H1A 124.3 . . ? C2 C1 H1A 124.3 . . ? C3 C2 C1 105.88(17) . . ? C3 C2 H2A 127.1 . . ? C1 C2 H2A 127.1 . . ? C2 C3 N2 106.89(17) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? N3 C4 C5 123.21(15) . . ? N3 C4 N2 112.50(14) . . ? C5 C4 N2 124.28(15) . . ? C4 C5 C6 116.69(15) . . ? C4 C5 H5A 121.7 . . ? C6 C5 H5A 121.7 . . ? C5 C6 C8 121.18(15) . . ? C5 C6 C7 118.59(15) . . ? C8 C6 C7 120.22(15) . . ? O8 C7 O7 125.30(16) . . ? O8 C7 C6 123.97(17) . . ? O7 C7 C6 110.73(15) . . ? C9 C8 C6 116.62(15) . . ? C9 C8 H8A 121.7 . . ? C6 C8 H8A 121.7 . . ? N3 C9 C8 123.65(15) . . ? N3 C9 N4 113.13(14) . . ? C8 C9 N4 123.22(15) . . ? C11 C10 N4 106.88(15) . . ? C11 C10 H10A 126.6 . . ? N4 C10 H10A 126.6 . . ? C10 C11 C12 105.42(15) . . ? C10 C11 H11A 127.3 . . ? C12 C11 H11A 127.3 . . ? N5 C12 C11 111.71(16) . . ? N5 C12 H12A 124.1 . . ? C11 C12 H12A 124.1 . . ? O7 C13 C14 106.64(15) . . ? O7 C13 H13A 110.4 . . ? C14 C13 H13A 110.4 . . ? O7 C13 H13B 110.4 . . ? C14 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? C13 C14 C15 112.25(17) . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 112.9(2) . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? 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 . . ? C1 N1 N2 104.85(15) . . ? C1 N1 Co1 139.71(13) . . ? N2 N1 Co1 115.35(10) . . ? C3 N2 N1 110.99(14) . . ? C3 N2 C4 130.88(15) . . ? N1 N2 C4 118.13(13) . . ? C4 N3 C9 118.65(14) . . ? C4 N3 Co1 120.82(11) . . ? C9 N3 Co1 120.44(11) . . ? C10 N4 N5 111.16(14) . . ? C10 N4 C9 130.72(14) . . ? N5 N4 C9 118.08(13) . . ? C12 N5 N4 104.82(14) . . ? C12 N5 Co1 140.03(12) . . ? N4 N5 Co1 114.60(10) . . ? O2 N6 O3 122.80(17) . . ? O2 N6 O1 122.18(16) . . ? O3 N6 O1 115.02(14) . . ? O5 N7 O4 123.09(19) . . ? O5 N7 O6 121.07(19) . . ? O4 N7 O6 115.84(17) . . ? N6 O1 Co1 94.32(10) . . ? N6 O3 Co1 92.15(10) . . ? N7 O4 Co1 90.84(11) . . ? N7 O6 Co1 93.97(11) . . ? C7 O7 C13 118.34(15) . . ? 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 N1 C1 C2 C3 -0.7(2) . . . . ? C1 C2 C3 N2 0.5(2) . . . . ? N3 C4 C5 C6 -1.2(2) . . . . ? N2 C4 C5 C6 177.55(14) . . . . ? C4 C5 C6 C8 0.8(2) . . . . ? C4 C5 C6 C7 -178.13(14) . . . . ? C5 C6 C7 O8 -3.6(3) . . . . ? C8 C6 C7 O8 177.46(17) . . . . ? C5 C6 C7 O7 177.03(14) . . . . ? C8 C6 C7 O7 -1.9(2) . . . . ? C5 C6 C8 C9 0.1(2) . . . . ? C7 C6 C8 C9 179.05(15) . . . . ? C6 C8 C9 N3 -0.8(2) . . . . ? C6 C8 C9 N4 179.68(14) . . . . ? N4 C10 C11 C12 0.32(19) . . . . ? C10 C11 C12 N5 0.0(2) . . . . ? O7 C13 C14 C15 -172.37(16) . . . . ? C13 C14 C15 C16 176.39(19) . . . . ? C2 C1 N1 N2 0.6(2) . . . . ? C2 C1 N1 Co1 176.57(14) . . . . ? N3 Co1 N1 C1 -178.5(2) . . . . ? O6 Co1 N1 C1 83.7(2) . . . . ? O1 Co1 N1 C1 -93.5(2) . . . . ? N5 Co1 N1 C1 173.19(18) . . . . ? O3 Co1 N1 C1 -36.9(2) . . . . ? O4 Co1 N1 C1 36.2(2) . . . . ? N3 Co1 N1 N2 -2.76(10) . . . . ? O6 Co1 N1 N2 -100.61(11) . . . . ? O1 Co1 N1 N2 82.19(11) . . . . ? N5 Co1 N1 N2 -11.08(17) . . . . ? O3 Co1 N1 N2 138.78(12) . . . . ? O4 Co1 N1 N2 -148.04(10) . . . . ? C2 C3 N2 N1 -0.2(2) . . . . ? C2 C3 N2 C4 179.47(16) . . . . ? C1 N1 N2 C3 -0.24(19) . . . . ? Co1 N1 N2 C3 -177.38(11) . . . . ? C1 N1 N2 C4 -179.94(14) . . . . ? Co1 N1 N2 C4 2.92(17) . . . . ? N3 C4 N2 C3 179.59(16) . . . . ? C5 C4 N2 C3 0.7(3) . . . . ? N3 C4 N2 N1 -0.79(19) . . . . ? C5 C4 N2 N1 -179.63(15) . . . . ? C5 C4 N3 C9 0.5(2) . . . . ? N2 C4 N3 C9 -178.34(13) . . . . ? C5 C4 N3 Co1 177.02(12) . . . . ? N2 C4 N3 Co1 -1.84(17) . . . . ? C8 C9 N3 C4 0.5(2) . . . . ? N4 C9 N3 C4 -179.93(13) . . . . ? C8 C9 N3 Co1 -175.97(12) . . . . ? N4 C9 N3 Co1 3.56(18) . . . . ? O6 Co1 N3 C4 89.78(12) . . . . ? N1 Co1 N3 C4 2.56(12) . . . . ? O1 Co1 N3 C4 -97.00(12) . . . . ? N5 Co1 N3 C4 177.69(13) . . . . ? O3 Co1 N3 C4 -58.40(14) . . . . ? O4 Co1 N3 C4 134.63(12) . . . . ? O6 Co1 N3 C9 -93.78(12) . . . . ? N1 Co1 N3 C9 178.99(13) . . . . ? O1 Co1 N3 C9 79.43(12) . . . . ? N5 Co1 N3 C9 -5.87(11) . . . . ? O3 Co1 N3 C9 118.03(12) . . . . ? O4 Co1 N3 C9 -48.93(16) . . . . ? C11 C10 N4 N5 -0.51(18) . . . . ? C11 C10 N4 C9 -178.31(16) . . . . ? N3 C9 N4 C10 -179.10(14) . . . . ? C8 C9 N4 C10 0.4(3) . . . . ? N3 C9 N4 N5 3.2(2) . . . . ? C8 C9 N4 N5 -177.25(14) . . . . ? C11 C12 N5 N4 -0.28(19) . . . . ? C11 C12 N5 Co1 -170.78(13) . . . . ? C10 N4 N5 C12 0.49(17) . . . . ? C9 N4 N5 C12 178.60(14) . . . . ? C10 N4 N5 Co1 173.79(10) . . . . ? C9 N4 N5 Co1 -8.10(17) . . . . ? N3 Co1 N5 C12 177.0(2) . . . . ? O6 Co1 N5 C12 -85.36(19) . . . . ? N1 Co1 N5 C12 -174.69(17) . . . . ? O1 Co1 N5 C12 87.86(19) . . . . ? O3 Co1 N5 C12 43.1(2) . . . . ? O4 Co1 N5 C12 -27.80(19) . . . . ? N3 Co1 N5 N4 7.10(10) . . . . ? O6 Co1 N5 N4 104.75(11) . . . . ? N1 Co1 N5 N4 15.42(16) . . . . ? O1 Co1 N5 N4 -82.03(11) . . . . ? O3 Co1 N5 N4 -126.76(10) . . . . ? O4 Co1 N5 N4 162.31(11) . . . . ? O2 N6 O1 Co1 179.36(17) . . . . ? O3 N6 O1 Co1 -1.02(17) . . . . ? N3 Co1 O1 N6 149.51(11) . . . . ? O6 Co1 O1 N6 -83.6(4) . . . . ? N1 Co1 O1 N6 76.98(11) . . . . ? N5 Co1 O1 N6 -137.26(11) . . . . ? O3 Co1 O1 N6 0.62(10) . . . . ? O4 Co1 O1 N6 -61.64(12) . . . . ? O2 N6 O3 Co1 -179.39(18) . . . . ? O1 N6 O3 Co1 1.00(16) . . . . ? N3 Co1 O3 N6 -47.60(14) . . . . ? O6 Co1 O3 N6 169.66(10) . . . . ? N1 Co1 O3 N6 -105.04(12) . . . . ? O1 Co1 O3 N6 -0.62(10) . . . . ? N5 Co1 O3 N6 54.66(13) . . . . ? O4 Co1 O3 N6 124.49(12) . . . . ? O5 N7 O4 Co1 169.63(17) . . . . ? O6 N7 O4 Co1 -10.01(16) . . . . ? N3 Co1 O4 N7 -49.16(14) . . . . ? O6 Co1 O4 N7 6.17(10) . . . . ? N1 Co1 O4 N7 66.17(12) . . . . ? O1 Co1 O4 N7 -170.14(10) . . . . ? N5 Co1 O4 N7 -90.86(11) . . . . ? O3 Co1 O4 N7 140.11(11) . . . . ? O5 N7 O6 Co1 -169.29(16) . . . . ? O4 N7 O6 Co1 10.35(16) . . . . ? N3 Co1 O6 N7 143.83(11) . . . . ? N1 Co1 O6 N7 -143.29(11) . . . . ? O1 Co1 O6 N7 17.5(4) . . . . ? N5 Co1 O6 N7 70.86(11) . . . . ? O3 Co1 O6 N7 -61.71(12) . . . . ? O4 Co1 O6 N7 -6.17(10) . . . . ? O8 C7 O7 C13 5.3(3) . . . . ? C6 C7 O7 C13 -175.30(14) . . . . ? C14 C13 O7 C7 177.40(15) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.311 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.052 data_1heating253K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.8515(18) _cell_length_b 25.892(5) _cell_length_c 8.1511(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.820(2) _cell_angle_gamma 90.00 _cell_volume 2042.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 4548 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7737 _exptl_absorpt_correction_T_max 0.9153 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15133 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4548 _reflns_number_gt 3559 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4548 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _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 0.44271(2) 0.375234(8) 0.80015(3) 0.02913(9) Uani 1 1 d . . . C1 C 0.5940(2) 0.47846(7) 0.6962(2) 0.0418(4) Uani 1 1 d . . . H1A H 0.5363 0.5031 0.7298 0.050 Uiso 1 1 calc R . . C2 C 0.7098(2) 0.49010(7) 0.6261(2) 0.0433(4) Uani 1 1 d . . . H2A H 0.7421 0.5227 0.6046 0.052 Uiso 1 1 calc R . . C3 C 0.76473(18) 0.44387(7) 0.5963(2) 0.0363(4) Uani 1 1 d . . . H3A H 0.8432 0.4386 0.5504 0.044 Uiso 1 1 calc R . . C4 C 0.69455(16) 0.35293(6) 0.64660(19) 0.0263(3) Uani 1 1 d . . . C5 C 0.79957(17) 0.32565(6) 0.5948(2) 0.0304(4) Uani 1 1 d . . . H5A H 0.8690 0.3423 0.5522 0.036 Uiso 1 1 calc R . . C6 C 0.79678(16) 0.27229(6) 0.60901(19) 0.0293(3) Uani 1 1 d . . . C7 C 0.91196(18) 0.24170(7) 0.5572(2) 0.0357(4) Uani 1 1 d . . . C8 C 0.69068(16) 0.24761(6) 0.66927(19) 0.0283(3) Uani 1 1 d . . . H8A H 0.6876 0.2118 0.6784 0.034 Uiso 1 1 calc R . . C9 C 0.59040(16) 0.27866(6) 0.71473(18) 0.0244(3) Uani 1 1 d . . . C10 C 0.43999(18) 0.21092(6) 0.80926(19) 0.0333(4) Uani 1 1 d . . . H10A H 0.4905 0.1811 0.7991 0.040 Uiso 1 1 calc R . . C11 C 0.31704(19) 0.21364(7) 0.8612(2) 0.0385(4) Uani 1 1 d . . . H11A H 0.2665 0.1864 0.8937 0.046 Uiso 1 1 calc R . . C12 C 0.28258(19) 0.26593(7) 0.8555(2) 0.0402(4) Uani 1 1 d . . . H12A H 0.2026 0.2792 0.8847 0.048 Uiso 1 1 calc R . . C13 C 1.0080(2) 0.15843(8) 0.5426(3) 0.0566(6) Uani 1 1 d . . . H13A H 1.0969 0.1753 0.5747 0.068 Uiso 1 1 calc R A 1 H13B H 0.9926 0.1520 0.4233 0.068 Uiso 1 1 calc R A 1 C14 C 1.0085(5) 0.10729(14) 0.6364(6) 0.0473(13) Uani 0.594(7) 1 d P B 1 H14A H 1.0909 0.0877 0.6276 0.057 Uiso 0.594(7) 1 calc PR B 1 H14B H 1.0093 0.1139 0.7537 0.057 Uiso 0.594(7) 1 calc PR B 1 C15 C 0.8816(5) 0.07675(18) 0.5625(8) 0.0634(15) Uani 0.594(7) 1 d P B 1 H15A H 0.8840 0.0685 0.4470 0.076 Uiso 0.594(7) 1 calc PR B 1 H15B H 0.7998 0.0974 0.5646 0.076 Uiso 0.594(7) 1 calc PR B 1 C14' C 0.9390(7) 0.1023(2) 0.5260(9) 0.050(2) Uani 0.406(7) 1 d P B 2 H14C H 0.8482 0.1041 0.4554 0.060 Uiso 0.406(7) 1 calc PR B 2 H14D H 0.9953 0.0789 0.4742 0.060 Uiso 0.406(7) 1 calc PR B 2 C15' C 0.9267(10) 0.0828(3) 0.6891(11) 0.080(3) Uani 0.406(7) 1 d P B 2 H15C H 0.8616 0.1035 0.7365 0.096 Uiso 0.406(7) 1 calc PR B 2 H15D H 1.0156 0.0838 0.7642 0.096 Uiso 0.406(7) 1 calc PR B 2 C16 C 0.8738(4) 0.02554(10) 0.6630(4) 0.0997(11) Uani 1 1 d . . . H16A H 0.7892 0.0078 0.6190 0.120 Uiso 1 1 calc R B 1 H16B H 0.8766 0.0336 0.7785 0.120 Uiso 1 1 calc R B 1 H16C H 0.9508 0.0038 0.6530 0.120 Uiso 1 1 calc R B 1 N1 N 0.57711(14) 0.42833(5) 0.70875(17) 0.0334(3) Uani 1 1 d . . . N2 N 0.68374(14) 0.40667(5) 0.64604(16) 0.0280(3) Uani 1 1 d . . . N3 N 0.59220(13) 0.32998(5) 0.70546(15) 0.0247(3) Uani 1 1 d . . . N4 N 0.47524(14) 0.25988(5) 0.77497(16) 0.0269(3) Uani 1 1 d . . . N5 N 0.37770(15) 0.29446(5) 0.80318(18) 0.0341(3) Uani 1 1 d . . . N6 N 0.53173(17) 0.40186(6) 1.11286(19) 0.0420(4) Uani 1 1 d . . . N7 N 0.19201(16) 0.39523(6) 0.6645(2) 0.0467(4) Uani 1 1 d . . . O1 O 0.55480(14) 0.35952(5) 1.04303(15) 0.0424(3) Uani 1 1 d . . . O2 O 0.56984(18) 0.40775(6) 1.26316(18) 0.0667(5) Uani 1 1 d . . . O3 O 0.46706(18) 0.43483(6) 1.01892(18) 0.0640(5) Uani 1 1 d . . . O4 O 0.23077(16) 0.38988(6) 0.8201(2) 0.0574(4) Uani 1 1 d . . . O5 O 0.07191(16) 0.40275(7) 0.5997(3) 0.0871(6) Uani 1 1 d . . . O6 O 0.28736(14) 0.39255(5) 0.58028(16) 0.0451(3) Uani 1 1 d . . . O7 O 0.89867(14) 0.19184(5) 0.58197(18) 0.0486(4) Uani 1 1 d . B . O8 O 1.00283(15) 0.26121(5) 0.4997(2) 0.0580(4) 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 0.02825(14) 0.02677(12) 0.03391(15) 0.00078(9) 0.00984(10) 0.00461(9) C1 0.0478(11) 0.0255(8) 0.0529(12) -0.0010(7) 0.0120(9) 0.0046(8) C2 0.0498(12) 0.0274(9) 0.0524(11) 0.0047(8) 0.0088(9) -0.0056(8) C3 0.0376(10) 0.0315(9) 0.0415(10) 0.0054(7) 0.0116(8) -0.0076(7) C4 0.0270(8) 0.0247(7) 0.0272(8) -0.0012(6) 0.0051(6) -0.0014(6) C5 0.0272(8) 0.0317(8) 0.0348(9) -0.0010(7) 0.0121(7) -0.0024(6) C6 0.0253(8) 0.0320(8) 0.0320(9) -0.0041(7) 0.0089(7) 0.0014(6) C7 0.0297(9) 0.0359(9) 0.0428(10) -0.0060(7) 0.0099(8) 0.0032(7) C8 0.0283(8) 0.0244(7) 0.0329(9) -0.0023(6) 0.0076(7) 0.0003(6) C9 0.0252(8) 0.0247(7) 0.0238(8) -0.0013(6) 0.0055(6) -0.0024(6) C10 0.0394(10) 0.0276(8) 0.0341(9) 0.0024(7) 0.0099(7) -0.0044(7) C11 0.0382(10) 0.0408(10) 0.0389(10) 0.0041(8) 0.0132(8) -0.0110(8) C12 0.0316(10) 0.0427(10) 0.0509(11) -0.0003(8) 0.0196(8) -0.0057(8) C13 0.0511(13) 0.0406(11) 0.0863(17) -0.0071(10) 0.0344(12) 0.0126(9) C14 0.051(3) 0.044(2) 0.045(3) -0.0007(17) 0.006(2) 0.0166(18) C15 0.058(3) 0.042(2) 0.088(4) 0.001(2) 0.009(3) 0.003(2) C14' 0.057(4) 0.039(3) 0.056(4) -0.005(3) 0.018(4) 0.009(3) C15' 0.137(8) 0.049(4) 0.065(5) 0.008(3) 0.046(5) 0.026(4) C16 0.140(3) 0.0434(15) 0.132(3) 0.0064(15) 0.065(2) 0.0057(16) N1 0.0334(8) 0.0271(7) 0.0421(9) -0.0014(6) 0.0132(7) 0.0037(6) N2 0.0283(7) 0.0245(6) 0.0323(7) 0.0006(5) 0.0088(6) 0.0001(5) N3 0.0238(7) 0.0243(6) 0.0268(7) -0.0010(5) 0.0067(5) 0.0006(5) N4 0.0258(7) 0.0256(7) 0.0307(7) -0.0003(5) 0.0089(5) -0.0010(5) N5 0.0284(8) 0.0316(7) 0.0456(9) -0.0008(6) 0.0155(6) 0.0013(6) N6 0.0557(10) 0.0332(8) 0.0377(9) -0.0022(7) 0.0104(8) 0.0011(7) N7 0.0312(9) 0.0351(8) 0.0723(12) 0.0016(8) 0.0063(9) 0.0021(7) O1 0.0582(9) 0.0302(6) 0.0391(7) -0.0023(5) 0.0098(6) 0.0086(6) O2 0.1003(14) 0.0621(10) 0.0342(8) -0.0104(7) 0.0038(8) -0.0073(9) O3 0.0986(13) 0.0444(8) 0.0521(9) 0.0089(6) 0.0216(8) 0.0317(8) O4 0.0564(10) 0.0583(9) 0.0645(10) 0.0080(7) 0.0295(8) 0.0190(7) O5 0.0286(9) 0.0784(13) 0.1435(17) 0.0004(12) -0.0119(10) 0.0072(8) O6 0.0436(8) 0.0434(7) 0.0482(8) 0.0069(6) 0.0081(6) 0.0021(6) O7 0.0471(8) 0.0317(7) 0.0757(10) -0.0039(6) 0.0343(7) 0.0071(6) O8 0.0422(8) 0.0444(8) 0.0985(11) 0.0028(7) 0.0412(8) 0.0039(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.1174(13) . ? Co1 N3 2.1365(12) . ? Co1 N1 2.1374(14) . ? Co1 O4 2.1581(15) . ? Co1 O6 2.1738(14) . ? Co1 N5 2.1888(15) . ? Co1 O3 2.3361(15) . ? C1 N1 1.315(2) . ? C1 C2 1.401(3) . ? C1 H1A 0.9300 . ? C2 C3 1.354(3) . ? C2 H2A 0.9300 . ? C3 N2 1.360(2) . ? C3 H3A 0.9300 . ? C4 N3 1.3348(19) . ? C4 C5 1.383(2) . ? C4 N2 1.396(2) . ? C5 C6 1.387(2) . ? C5 H5A 0.9300 . ? C6 C8 1.391(2) . ? C6 C7 1.508(2) . ? C7 O8 1.197(2) . ? C7 O7 1.317(2) . ? C8 C9 1.377(2) . ? C8 H8A 0.9300 . ? C9 N3 1.3311(19) . ? C9 N4 1.4050(18) . ? C10 N4 1.357(2) . ? C10 C11 1.358(2) . ? C10 H10A 0.9300 . ? C11 C12 1.395(3) . ? C11 H11A 0.9300 . ? C12 N5 1.325(2) . ? C12 H12A 0.9300 . ? C13 O7 1.464(2) . ? C13 C14 1.528(4) . ? C13 C14' 1.600(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.507(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.568(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C14' C15' 1.448(12) . ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' C16 1.573(8) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 N2 1.3715(18) . ? N4 N5 1.3641(18) . ? N6 O2 1.222(2) . ? N6 O3 1.240(2) . ? N6 O1 1.2753(18) . ? N7 O5 1.217(2) . ? N7 O4 1.262(2) . ? N7 O6 1.265(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N3 87.62(5) . . ? O1 Co1 N1 101.60(5) . . ? N3 Co1 N1 73.31(5) . . ? O1 Co1 O4 107.79(6) . . ? N3 Co1 O4 149.98(6) . . ? N1 Co1 O4 125.78(5) . . ? O1 Co1 O6 166.74(5) . . ? N3 Co1 O6 103.98(5) . . ? N1 Co1 O6 88.07(5) . . ? O4 Co1 O6 58.97(6) . . ? O1 Co1 N5 84.73(5) . . ? N3 Co1 N5 72.72(5) . . ? N1 Co1 N5 145.11(5) . . ? O4 Co1 N5 82.98(6) . . ? O6 Co1 N5 92.53(5) . . ? O1 Co1 O3 56.80(5) . . ? N3 Co1 O3 131.23(5) . . ? N1 Co1 O3 81.93(6) . . ? O4 Co1 O3 77.80(6) . . ? O6 Co1 O3 116.65(5) . . ? N5 Co1 O3 127.65(5) . . ? N1 C1 C2 111.64(16) . . ? N1 C1 H1A 124.2 . . ? C2 C1 H1A 124.2 . . ? C3 C2 C1 105.45(16) . . ? C3 C2 H2A 127.3 . . ? C1 C2 H2A 127.3 . . ? C2 C3 N2 107.20(16) . . ? C2 C3 H3A 126.4 . . ? N2 C3 H3A 126.4 . . ? N3 C4 C5 122.78(14) . . ? N3 C4 N2 112.51(13) . . ? C5 C4 N2 124.71(14) . . ? C4 C5 C6 117.10(14) . . ? C4 C5 H5A 121.5 . . ? C6 C5 H5A 121.5 . . ? C5 C6 C8 121.01(14) . . ? C5 C6 C7 118.17(14) . . ? C8 C6 C7 120.83(15) . . ? O8 C7 O7 125.23(16) . . ? O8 C7 C6 123.04(16) . . ? O7 C7 C6 111.73(14) . . ? C9 C8 C6 116.82(14) . . ? C9 C8 H8A 121.6 . . ? C6 C8 H8A 121.6 . . ? N3 C9 C8 123.34(14) . . ? N3 C9 N4 112.68(13) . . ? C8 C9 N4 123.99(14) . . ? N4 C10 C11 107.07(15) . . ? N4 C10 H10A 126.5 . . ? C11 C10 H10A 126.5 . . ? C10 C11 C12 105.41(15) . . ? C10 C11 H11A 127.3 . . ? C12 C11 H11A 127.3 . . ? N5 C12 C11 111.69(16) . . ? N5 C12 H12A 124.2 . . ? C11 C12 H12A 124.2 . . ? O7 C13 C14 109.6(2) . . ? O7 C13 C14' 103.7(3) . . ? C14 C13 C14' 38.4(2) . . ? O7 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? C14' C13 H13A 141.4 . . ? O7 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? C14' C13 H13B 77.0 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C13 109.3(4) . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C14 C15 C16 110.7(4) . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15' C14' C13 110.3(6) . . ? C15' C14' H14C 109.6 . . ? C13 C14' H14C 109.6 . . ? C15' C14' H14D 109.6 . . ? C13 C14' H14D 109.6 . . ? H14C C14' H14D 108.1 . . ? C14' C15' C16 106.7(7) . . ? C14' C15' H15C 110.4 . . ? C16 C15' H15C 110.4 . . ? C14' C15' H15D 110.4 . . ? C16 C15' H15D 110.4 . . ? H15C C15' H15D 108.6 . . ? C15 C16 C15' 39.3(3) . . ? C15 C16 H16A 109.5 . . ? C15' C16 H16A 138.0 . . ? C15 C16 H16B 109.5 . . ? C15' C16 H16B 73.4 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? C15' C16 H16C 108.4 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 N2 104.91(14) . . ? C1 N1 Co1 139.28(12) . . ? N2 N1 Co1 115.78(10) . . ? C3 N2 N1 110.78(13) . . ? C3 N2 C4 131.17(14) . . ? N1 N2 C4 118.02(12) . . ? C9 N3 C4 118.94(13) . . ? C9 N3 Co1 120.63(10) . . ? C4 N3 Co1 120.27(10) . . ? C10 N4 N5 111.27(13) . . ? C10 N4 C9 130.53(14) . . ? N5 N4 C9 118.19(13) . . ? C12 N5 N4 104.56(14) . . ? C12 N5 Co1 139.68(12) . . ? N4 N5 Co1 114.10(10) . . ? O2 N6 O3 123.98(16) . . ? O2 N6 O1 120.53(15) . . ? O3 N6 O1 115.47(15) . . ? O5 N7 O4 122.67(19) . . ? O5 N7 O6 122.2(2) . . ? O4 N7 O6 115.09(15) . . ? N6 O1 Co1 98.44(10) . . ? N6 O3 Co1 89.08(11) . . ? N7 O4 Co1 93.33(10) . . ? N7 O6 Co1 92.49(10) . . ? C7 O7 C13 116.57(14) . . ? 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 N1 C1 C2 C3 -0.3(2) . . . . ? C1 C2 C3 N2 0.4(2) . . . . ? N3 C4 C5 C6 -1.2(2) . . . . ? N2 C4 C5 C6 177.88(14) . . . . ? C4 C5 C6 C8 1.5(2) . . . . ? C4 C5 C6 C7 -178.58(14) . . . . ? C5 C6 C7 O8 -2.4(3) . . . . ? C8 C6 C7 O8 177.54(18) . . . . ? C5 C6 C7 O7 178.06(15) . . . . ? C8 C6 C7 O7 -2.0(2) . . . . ? C5 C6 C8 C9 -0.5(2) . . . . ? C7 C6 C8 C9 179.57(14) . . . . ? C6 C8 C9 N3 -0.9(2) . . . . ? C6 C8 C9 N4 178.82(14) . . . . ? N4 C10 C11 C12 0.0(2) . . . . ? C10 C11 C12 N5 0.0(2) . . . . ? O7 C13 C14 C15 70.1(4) . . . . ? C14' C13 C14 C15 -17.3(4) . . . . ? C13 C14 C15 C16 -176.4(3) . . . . ? O7 C13 C14' C15' -72.8(6) . . . . ? C14 C13 C14' C15' 31.6(5) . . . . ? C13 C14' C15' C16 -173.8(4) . . . . ? C14 C15 C16 C15' 31.6(5) . . . . ? C14' C15' C16 C15 -19.2(4) . . . . ? C2 C1 N1 N2 0.1(2) . . . . ? C2 C1 N1 Co1 177.77(13) . . . . ? O1 Co1 N1 C1 -95.25(19) . . . . ? N3 Co1 N1 C1 -179.2(2) . . . . ? O4 Co1 N1 C1 26.9(2) . . . . ? O6 Co1 N1 C1 75.60(19) . . . . ? N5 Co1 N1 C1 167.26(17) . . . . ? O3 Co1 N1 C1 -41.66(19) . . . . ? O1 Co1 N1 N2 82.25(11) . . . . ? N3 Co1 N1 N2 -1.68(10) . . . . ? O4 Co1 N1 N2 -155.59(10) . . . . ? O6 Co1 N1 N2 -106.90(11) . . . . ? N5 Co1 N1 N2 -15.25(16) . . . . ? O3 Co1 N1 N2 135.83(11) . . . . ? C2 C3 N2 N1 -0.3(2) . . . . ? C2 C3 N2 C4 -178.54(15) . . . . ? C1 N1 N2 C3 0.14(18) . . . . ? Co1 N1 N2 C3 -178.17(11) . . . . ? C1 N1 N2 C4 178.62(14) . . . . ? Co1 N1 N2 C4 0.31(17) . . . . ? N3 C4 N2 C3 -179.66(16) . . . . ? C5 C4 N2 C3 1.2(3) . . . . ? N3 C4 N2 N1 2.23(19) . . . . ? C5 C4 N2 N1 -176.94(15) . . . . ? C8 C9 N3 C4 1.2(2) . . . . ? N4 C9 N3 C4 -178.53(13) . . . . ? C8 C9 N3 Co1 -174.20(12) . . . . ? N4 C9 N3 Co1 6.05(17) . . . . ? C5 C4 N3 C9 -0.1(2) . . . . ? N2 C4 N3 C9 -179.30(12) . . . . ? C5 C4 N3 Co1 175.32(12) . . . . ? N2 C4 N3 Co1 -3.86(17) . . . . ? O1 Co1 N3 C9 75.61(12) . . . . ? N1 Co1 N3 C9 178.47(12) . . . . ? O4 Co1 N3 C9 -47.02(17) . . . . ? O6 Co1 N3 C9 -97.90(11) . . . . ? N5 Co1 N3 C9 -9.61(11) . . . . ? O3 Co1 N3 C9 115.70(11) . . . . ? O1 Co1 N3 C4 -99.74(12) . . . . ? N1 Co1 N3 C4 3.12(11) . . . . ? O4 Co1 N3 C4 137.62(13) . . . . ? O6 Co1 N3 C4 86.75(12) . . . . ? N5 Co1 N3 C4 175.04(12) . . . . ? O3 Co1 N3 C4 -59.65(13) . . . . ? C11 C10 N4 N5 -0.10(19) . . . . ? C11 C10 N4 C9 -178.75(15) . . . . ? N3 C9 N4 C10 -176.60(15) . . . . ? C8 C9 N4 C10 3.7(3) . . . . ? N3 C9 N4 N5 4.84(19) . . . . ? C8 C9 N4 N5 -174.91(15) . . . . ? C11 C12 N5 N4 -0.1(2) . . . . ? C11 C12 N5 Co1 -163.48(14) . . . . ? C10 N4 N5 C12 0.11(18) . . . . ? C9 N4 N5 C12 178.94(13) . . . . ? C10 N4 N5 Co1 168.43(10) . . . . ? C9 N4 N5 Co1 -12.74(17) . . . . ? O1 Co1 N5 C12 84.5(2) . . . . ? N3 Co1 N5 C12 173.7(2) . . . . ? N1 Co1 N5 C12 -172.74(17) . . . . ? O4 Co1 N5 C12 -24.2(2) . . . . ? O6 Co1 N5 C12 -82.5(2) . . . . ? O3 Co1 N5 C12 44.5(2) . . . . ? O1 Co1 N5 N4 -77.85(11) . . . . ? N3 Co1 N5 N4 11.29(10) . . . . ? N1 Co1 N5 N4 24.90(16) . . . . ? O4 Co1 N5 N4 173.46(12) . . . . ? O6 Co1 N5 N4 115.15(11) . . . . ? O3 Co1 N5 N4 -117.89(11) . . . . ? O2 N6 O1 Co1 173.91(16) . . . . ? O3 N6 O1 Co1 -4.64(18) . . . . ? N3 Co1 O1 N6 147.29(11) . . . . ? N1 Co1 O1 N6 74.86(11) . . . . ? O4 Co1 O1 N6 -58.97(12) . . . . ? O6 Co1 O1 N6 -61.3(3) . . . . ? N5 Co1 O1 N6 -139.85(11) . . . . ? O3 Co1 O1 N6 2.65(11) . . . . ? O2 N6 O3 Co1 -174.33(18) . . . . ? O1 N6 O3 Co1 4.16(17) . . . . ? O1 Co1 O3 N6 -2.70(11) . . . . ? N3 Co1 O3 N6 -52.96(14) . . . . ? N1 Co1 O3 N6 -112.30(12) . . . . ? O4 Co1 O3 N6 118.30(13) . . . . ? O6 Co1 O3 N6 163.97(11) . . . . ? N5 Co1 O3 N6 47.25(14) . . . . ? O5 N7 O4 Co1 177.09(17) . . . . ? O6 N7 O4 Co1 -3.36(16) . . . . ? O1 Co1 O4 N7 -177.32(10) . . . . ? N3 Co1 O4 N7 -59.40(16) . . . . ? N1 Co1 O4 N7 63.25(13) . . . . ? O6 Co1 O4 N7 2.07(10) . . . . ? N5 Co1 O4 N7 -95.17(11) . . . . ? O3 Co1 O4 N7 133.81(11) . . . . ? O5 N7 O6 Co1 -177.12(17) . . . . ? O4 N7 O6 Co1 3.33(16) . . . . ? O1 Co1 O6 N7 0.5(3) . . . . ? N3 Co1 O6 N7 151.01(10) . . . . ? N1 Co1 O6 N7 -136.72(10) . . . . ? O4 Co1 O6 N7 -2.06(10) . . . . ? N5 Co1 O6 N7 78.19(10) . . . . ? O3 Co1 O6 N7 -56.75(11) . . . . ? O8 C7 O7 C13 2.9(3) . . . . ? C6 C7 O7 C13 -177.53(16) . . . . ? C14 C13 O7 C7 158.6(2) . . . . ? C14' C13 O7 C7 -161.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.299 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.046 data_1heating273K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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 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 9.865(2) _cell_length_b 25.934(6) _cell_length_c 8.172(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.762(3) _cell_angle_gamma 90.00 _cell_volume 2053.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4578 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7748 _exptl_absorpt_correction_T_max 0.9157 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15006 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4578 _reflns_number_gt 3515 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4578 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.44142(2) 0.375150(9) 0.79983(3) 0.03200(9) Uani 1 1 d . . . C1 C 0.5933(2) 0.47824(7) 0.6966(2) 0.0451(5) Uani 1 1 d . . . H1A H 0.5359 0.5029 0.7304 0.054 Uiso 1 1 calc R . . C2 C 0.7087(2) 0.48970(7) 0.6262(2) 0.0471(5) Uani 1 1 d . . . H2A H 0.7408 0.5222 0.6043 0.057 Uiso 1 1 calc R . . C3 C 0.7637(2) 0.44360(7) 0.5964(2) 0.0402(4) Uani 1 1 d . . . H3A H 0.8421 0.4383 0.5507 0.048 Uiso 1 1 calc R . . C4 C 0.69316(17) 0.35278(6) 0.6467(2) 0.0287(3) Uani 1 1 d . . . C5 C 0.79808(17) 0.32550(7) 0.5946(2) 0.0334(4) Uani 1 1 d . . . H5A H 0.8675 0.3422 0.5521 0.040 Uiso 1 1 calc R . . C6 C 0.79504(17) 0.27227(7) 0.6086(2) 0.0320(4) Uani 1 1 d . . . C7 C 0.91010(19) 0.24165(7) 0.5569(2) 0.0390(4) Uani 1 1 d . . . C8 C 0.68889(17) 0.24768(6) 0.6686(2) 0.0307(4) Uani 1 1 d . . . H8A H 0.6857 0.2120 0.6774 0.037 Uiso 1 1 calc R . . C9 C 0.58866(16) 0.27863(6) 0.71435(19) 0.0270(3) Uani 1 1 d . . . C10 C 0.43848(19) 0.21099(7) 0.8087(2) 0.0365(4) Uani 1 1 d . . . H10A H 0.4889 0.1812 0.7985 0.044 Uiso 1 1 calc R . . C11 C 0.3155(2) 0.21380(7) 0.8607(2) 0.0417(4) Uani 1 1 d . . . H11A H 0.2649 0.1866 0.8929 0.050 Uiso 1 1 calc R . . C12 C 0.28115(19) 0.26594(8) 0.8557(2) 0.0435(5) Uani 1 1 d . . . H12A H 0.2015 0.2791 0.8854 0.052 Uiso 1 1 calc R . . C13 C 1.0061(3) 0.15851(9) 0.5422(3) 0.0620(6) Uani 1 1 d . . . H13A H 1.0947 0.1755 0.5735 0.074 Uiso 1 1 calc R A 1 H13B H 0.9905 0.1518 0.4234 0.074 Uiso 1 1 calc R A 1 C14 C 1.0072(5) 0.10764(17) 0.6373(7) 0.0520(15) Uani 0.575(8) 1 d P B 1 H14A H 1.0900 0.0883 0.6296 0.062 Uiso 0.575(8) 1 calc PR B 1 H14B H 1.0072 0.1145 0.7540 0.062 Uiso 0.575(8) 1 calc PR B 1 C15 C 0.8815(6) 0.0768(2) 0.5637(9) 0.0693(17) Uani 0.575(8) 1 d P B 1 H15A H 0.8846 0.0685 0.4487 0.083 Uiso 0.575(8) 1 calc PR B 1 H15B H 0.7994 0.0972 0.5651 0.083 Uiso 0.575(8) 1 calc PR B 1 C14' C 0.9383(8) 0.1023(2) 0.5272(10) 0.056(2) Uani 0.425(8) 1 d P B 2 H14C H 0.8479 0.1039 0.4561 0.067 Uiso 0.425(8) 1 calc PR B 2 H14D H 0.9953 0.0790 0.4762 0.067 Uiso 0.425(8) 1 calc PR B 2 C15' C 0.9253(11) 0.0829(3) 0.6890(11) 0.086(3) Uani 0.425(8) 1 d P B 2 H15C H 0.8598 0.1035 0.7356 0.104 Uiso 0.425(8) 1 calc PR B 2 H15D H 1.0137 0.0841 0.7644 0.104 Uiso 0.425(8) 1 calc PR B 2 C16 C 0.8732(4) 0.02565(11) 0.6635(4) 0.1100(12) Uani 1 1 d . . . H16A H 0.7917 0.0069 0.6148 0.132 Uiso 1 1 calc R B 1 H16B H 0.8696 0.0338 0.7772 0.132 Uiso 1 1 calc R B 1 H16C H 0.9532 0.0049 0.6597 0.132 Uiso 1 1 calc R B 1 N1 N 0.57613(15) 0.42808(5) 0.70889(18) 0.0368(3) Uani 1 1 d . . . N2 N 0.68270(14) 0.40653(5) 0.64613(17) 0.0312(3) Uani 1 1 d . . . N3 N 0.59070(13) 0.32987(5) 0.70514(15) 0.0270(3) Uani 1 1 d . . . N4 N 0.47366(14) 0.25993(5) 0.77451(17) 0.0293(3) Uani 1 1 d . . . N5 N 0.37650(15) 0.29452(6) 0.80314(19) 0.0376(3) Uani 1 1 d . . . N6 N 0.53010(18) 0.40181(6) 1.1125(2) 0.0455(4) Uani 1 1 d . . . N7 N 0.19100(17) 0.39510(7) 0.6634(3) 0.0510(4) Uani 1 1 d . . . O1 O 0.55317(15) 0.35957(5) 1.04240(16) 0.0464(3) Uani 1 1 d . . . O2 O 0.5676(2) 0.40763(7) 1.26219(19) 0.0733(5) Uani 1 1 d . . . O3 O 0.46516(19) 0.43456(6) 1.01871(19) 0.0706(5) Uani 1 1 d . . . O4 O 0.22915(18) 0.38979(6) 0.8188(2) 0.0633(4) Uani 1 1 d . . . O5 O 0.07105(17) 0.40281(8) 0.5985(3) 0.0960(7) Uani 1 1 d . . . O6 O 0.28669(15) 0.39256(6) 0.57994(17) 0.0494(3) Uani 1 1 d . . . O7 O 0.89670(15) 0.19188(5) 0.58119(19) 0.0530(4) Uani 1 1 d . B . O8 O 1.00127(16) 0.26104(6) 0.4995(2) 0.0630(4) 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 0.03057(14) 0.02964(13) 0.03745(16) 0.00084(9) 0.01069(10) 0.00504(9) C1 0.0515(12) 0.0277(9) 0.0571(12) -0.0011(8) 0.0130(10) 0.0051(8) C2 0.0537(12) 0.0293(9) 0.0578(12) 0.0043(8) 0.0091(10) -0.0058(8) C3 0.0409(10) 0.0345(9) 0.0469(11) 0.0057(8) 0.0130(8) -0.0082(8) C4 0.0298(8) 0.0274(8) 0.0286(8) -0.0012(6) 0.0052(7) -0.0018(6) C5 0.0297(9) 0.0340(9) 0.0391(10) -0.0009(7) 0.0132(7) -0.0035(7) C6 0.0267(8) 0.0343(9) 0.0366(9) -0.0041(7) 0.0097(7) 0.0017(7) C7 0.0314(9) 0.0387(10) 0.0485(11) -0.0057(8) 0.0114(8) 0.0036(7) C8 0.0304(9) 0.0268(8) 0.0355(9) -0.0028(6) 0.0075(7) 0.0004(6) C9 0.0262(8) 0.0279(8) 0.0273(8) -0.0011(6) 0.0063(7) -0.0025(6) C10 0.0421(10) 0.0303(9) 0.0385(10) 0.0018(7) 0.0111(8) -0.0042(7) C11 0.0422(11) 0.0440(10) 0.0414(10) 0.0035(8) 0.0140(8) -0.0120(8) C12 0.0333(10) 0.0479(11) 0.0539(12) -0.0006(9) 0.0202(9) -0.0054(8) C13 0.0571(14) 0.0435(12) 0.0941(18) -0.0067(11) 0.0364(13) 0.0142(10) C14 0.054(3) 0.052(2) 0.048(3) -0.002(2) 0.004(2) 0.019(2) C15 0.066(3) 0.046(3) 0.094(5) 0.001(3) 0.012(3) 0.003(2) C14' 0.068(4) 0.040(3) 0.065(5) -0.004(3) 0.022(4) 0.013(3) C15' 0.146(8) 0.055(4) 0.069(6) 0.005(4) 0.049(6) 0.027(5) C16 0.152(3) 0.0483(17) 0.147(3) 0.0079(17) 0.072(3) 0.0061(18) N1 0.0368(8) 0.0292(7) 0.0468(9) -0.0023(6) 0.0144(7) 0.0047(6) N2 0.0311(7) 0.0264(7) 0.0371(8) 0.0007(6) 0.0092(6) -0.0001(6) N3 0.0253(7) 0.0270(7) 0.0295(7) -0.0013(5) 0.0073(6) 0.0003(5) N4 0.0284(7) 0.0281(7) 0.0328(7) -0.0003(5) 0.0092(6) -0.0017(6) N5 0.0310(8) 0.0351(8) 0.0503(10) -0.0006(6) 0.0170(7) 0.0010(6) N6 0.0591(11) 0.0367(9) 0.0412(9) -0.0020(7) 0.0105(8) 0.0005(8) N7 0.0339(9) 0.0400(9) 0.0779(14) 0.0020(9) 0.0075(9) 0.0015(7) O1 0.0632(9) 0.0335(7) 0.0428(8) -0.0022(6) 0.0111(7) 0.0098(6) O2 0.1097(15) 0.0678(11) 0.0386(8) -0.0120(8) 0.0042(9) -0.0074(10) O3 0.1091(15) 0.0486(9) 0.0573(10) 0.0098(7) 0.0238(9) 0.0346(9) O4 0.0629(11) 0.0640(10) 0.0716(11) 0.0100(8) 0.0346(9) 0.0221(8) O5 0.0321(9) 0.0873(14) 0.157(2) 0.0016(14) -0.0129(11) 0.0085(9) O6 0.0463(8) 0.0484(8) 0.0534(9) 0.0076(6) 0.0090(7) 0.0038(6) O7 0.0505(9) 0.0345(7) 0.0830(11) -0.0039(7) 0.0360(8) 0.0079(6) O8 0.0463(9) 0.0490(9) 0.1054(12) 0.0029(8) 0.0446(9) 0.0049(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 O1 2.1193(14) . ? Co1 N1 2.1382(15) . ? Co1 N3 2.1383(13) . ? Co1 O4 2.1620(16) . ? Co1 O6 2.1768(15) . ? Co1 N5 2.1886(16) . ? Co1 O3 2.3391(17) . ? C1 N1 1.318(2) . ? C1 C2 1.400(3) . ? C1 H1A 0.9300 . ? C2 C3 1.354(3) . ? C2 H2A 0.9300 . ? C3 N2 1.360(2) . ? C3 H3A 0.9300 . ? C4 N3 1.335(2) . ? C4 C5 1.385(2) . ? C4 N2 1.398(2) . ? C5 C6 1.386(2) . ? C5 H5A 0.9300 . ? C6 C8 1.391(2) . ? C6 C7 1.509(2) . ? C7 O8 1.200(2) . ? C7 O7 1.316(2) . ? C8 C9 1.378(2) . ? C8 H8A 0.9300 . ? C9 N3 1.331(2) . ? C9 N4 1.4044(19) . ? C10 N4 1.359(2) . ? C10 C11 1.360(3) . ? C10 H10A 0.9300 . ? C11 C12 1.393(3) . ? C11 H11A 0.9300 . ? C12 N5 1.330(2) . ? C12 H12A 0.9300 . ? C13 O7 1.464(2) . ? C13 C14 1.530(5) . ? C13 C14' 1.598(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.504(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.566(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C14' C15' 1.443(13) . ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' C16 1.573(9) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 N2 1.3718(19) . ? N4 N5 1.3645(19) . ? N6 O2 1.219(2) . ? N6 O3 1.239(2) . ? N6 O1 1.276(2) . ? N7 O5 1.220(2) . ? N7 O4 1.263(2) . ? N7 O6 1.265(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N1 101.48(6) . . ? O1 Co1 N3 87.74(5) . . ? N1 Co1 N3 73.26(5) . . ? O1 Co1 O4 107.93(6) . . ? N1 Co1 O4 125.83(6) . . ? N3 Co1 O4 149.79(6) . . ? O1 Co1 O6 166.84(5) . . ? N1 Co1 O6 88.02(6) . . ? N3 Co1 O6 103.85(5) . . ? O4 Co1 O6 58.91(6) . . ? O1 Co1 N5 84.75(6) . . ? N1 Co1 N5 145.08(5) . . ? N3 Co1 N5 72.70(5) . . ? O4 Co1 N5 82.95(6) . . ? O6 Co1 N5 92.67(6) . . ? O1 Co1 O3 56.64(5) . . ? N1 Co1 O3 82.12(6) . . ? N3 Co1 O3 131.38(6) . . ? O4 Co1 O3 77.85(7) . . ? O6 Co1 O3 116.69(6) . . ? N5 Co1 O3 127.42(6) . . ? N1 C1 C2 111.51(17) . . ? N1 C1 H1A 124.2 . . ? C2 C1 H1A 124.2 . . ? C3 C2 C1 105.69(17) . . ? C3 C2 H2A 127.2 . . ? C1 C2 H2A 127.2 . . ? C2 C3 N2 107.05(17) . . ? C2 C3 H3A 126.5 . . ? N2 C3 H3A 126.5 . . ? N3 C4 C5 122.80(15) . . ? N3 C4 N2 112.61(14) . . ? C5 C4 N2 124.58(15) . . ? C4 C5 C6 117.04(15) . . ? C4 C5 H5A 121.5 . . ? C6 C5 H5A 121.5 . . ? C5 C6 C8 120.99(15) . . ? C5 C6 C7 118.16(15) . . ? C8 C6 C7 120.85(16) . . ? O8 C7 O7 125.00(17) . . ? O8 C7 C6 123.17(17) . . ? O7 C7 C6 111.82(15) . . ? C9 C8 C6 117.00(15) . . ? C9 C8 H8A 121.5 . . ? C6 C8 H8A 121.5 . . ? N3 C9 C8 123.14(14) . . ? N3 C9 N4 112.72(13) . . ? C8 C9 N4 124.13(15) . . ? N4 C10 C11 106.93(16) . . ? N4 C10 H10A 126.5 . . ? C11 C10 H10A 126.5 . . ? C10 C11 C12 105.61(16) . . ? C10 C11 H11A 127.2 . . ? C12 C11 H11A 127.2 . . ? N5 C12 C11 111.58(17) . . ? N5 C12 H12A 124.2 . . ? C11 C12 H12A 124.2 . . ? O7 C13 C14 109.6(2) . . ? O7 C13 C14' 103.9(3) . . ? C14 C13 C14' 38.4(2) . . ? O7 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? C14' C13 H13A 141.2 . . ? O7 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? C14' C13 H13B 76.9 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C13 109.2(5) . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C14 C15 C16 111.2(5) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15' C14' C13 110.8(7) . . ? C15' C14' H14C 109.5 . . ? C13 C14' H14C 109.5 . . ? C15' C14' H14D 109.5 . . ? C13 C14' H14D 109.5 . . ? H14C C14' H14D 108.1 . . ? C14' C15' C16 106.9(7) . . ? C14' C15' H15C 110.3 . . ? C16 C15' H15C 110.3 . . ? C14' C15' H15D 110.3 . . ? C16 C15' H15D 110.3 . . ? H15C C15' H15D 108.6 . . ? C15 C16 C15' 38.9(3) . . ? C15 C16 H16A 109.5 . . ? C15' C16 H16A 139.5 . . ? C15 C16 H16B 109.5 . . ? C15' C16 H16B 74.6 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? C15' C16 H16C 106.4 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 N2 104.79(15) . . ? C1 N1 Co1 139.21(13) . . ? N2 N1 Co1 115.97(10) . . ? C3 N2 N1 110.96(14) . . ? C3 N2 C4 131.22(15) . . ? N1 N2 C4 117.80(13) . . ? C9 N3 C4 119.00(13) . . ? C9 N3 Co1 120.60(10) . . ? C4 N3 Co1 120.24(11) . . ? C10 N4 N5 111.37(14) . . ? C10 N4 C9 130.45(14) . . ? N5 N4 C9 118.18(13) . . ? C12 N5 N4 104.52(15) . . ? C12 N5 Co1 139.69(13) . . ? N4 N5 Co1 114.17(10) . . ? O2 N6 O3 124.08(18) . . ? O2 N6 O1 120.69(17) . . ? O3 N6 O1 115.20(16) . . ? O5 N7 O4 122.6(2) . . ? O5 N7 O6 122.3(2) . . ? O4 N7 O6 115.10(16) . . ? N6 O1 Co1 98.68(11) . . ? N6 O3 Co1 89.29(11) . . ? N7 O4 Co1 93.31(11) . . ? N7 O6 Co1 92.55(11) . . ? C7 O7 C13 116.61(16) . . ? 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 N1 C1 C2 C3 -0.6(2) . . . . ? C1 C2 C3 N2 0.6(2) . . . . ? N3 C4 C5 C6 -1.3(3) . . . . ? N2 C4 C5 C6 177.94(15) . . . . ? C4 C5 C6 C8 1.6(2) . . . . ? C4 C5 C6 C7 -178.46(15) . . . . ? C5 C6 C7 O8 -2.5(3) . . . . ? C8 C6 C7 O8 177.52(19) . . . . ? C5 C6 C7 O7 178.12(16) . . . . ? C8 C6 C7 O7 -1.9(2) . . . . ? C5 C6 C8 C9 -0.6(3) . . . . ? C7 C6 C8 C9 179.45(15) . . . . ? C6 C8 C9 N3 -0.8(2) . . . . ? C6 C8 C9 N4 178.90(15) . . . . ? N4 C10 C11 C12 -0.1(2) . . . . ? C10 C11 C12 N5 0.2(2) . . . . ? O7 C13 C14 C15 70.7(5) . . . . ? C14' C13 C14 C15 -17.2(4) . . . . ? C13 C14 C15 C16 -176.7(3) . . . . ? O7 C13 C14' C15' -72.4(7) . . . . ? C14 C13 C14' C15' 31.6(5) . . . . ? C13 C14' C15' C16 -174.0(4) . . . . ? C14 C15 C16 C15' 31.6(5) . . . . ? C14' C15' C16 C15 -19.1(5) . . . . ? C2 C1 N1 N2 0.3(2) . . . . ? C2 C1 N1 Co1 178.02(14) . . . . ? O1 Co1 N1 C1 -95.1(2) . . . . ? N3 Co1 N1 C1 -179.2(2) . . . . ? O4 Co1 N1 C1 27.2(2) . . . . ? O6 Co1 N1 C1 75.7(2) . . . . ? N5 Co1 N1 C1 167.52(17) . . . . ? O3 Co1 N1 C1 -41.6(2) . . . . ? O1 Co1 N1 N2 82.42(12) . . . . ? N3 Co1 N1 N2 -1.67(11) . . . . ? O4 Co1 N1 N2 -155.29(11) . . . . ? O6 Co1 N1 N2 -106.76(12) . . . . ? N5 Co1 N1 N2 -14.93(17) . . . . ? O3 Co1 N1 N2 135.94(12) . . . . ? C2 C3 N2 N1 -0.4(2) . . . . ? C2 C3 N2 C4 -178.66(17) . . . . ? C1 N1 N2 C3 0.07(19) . . . . ? Co1 N1 N2 C3 -178.28(11) . . . . ? C1 N1 N2 C4 178.58(14) . . . . ? Co1 N1 N2 C4 0.24(18) . . . . ? N3 C4 N2 C3 -179.51(17) . . . . ? C5 C4 N2 C3 1.2(3) . . . . ? N3 C4 N2 N1 2.3(2) . . . . ? C5 C4 N2 N1 -177.01(15) . . . . ? C8 C9 N3 C4 1.0(2) . . . . ? N4 C9 N3 C4 -178.68(13) . . . . ? C8 C9 N3 Co1 -174.27(12) . . . . ? N4 C9 N3 Co1 6.03(17) . . . . ? C5 C4 N3 C9 0.1(2) . . . . ? N2 C4 N3 C9 -179.28(13) . . . . ? C5 C4 N3 Co1 175.39(12) . . . . ? N2 C4 N3 Co1 -3.96(18) . . . . ? O1 Co1 N3 C9 75.70(12) . . . . ? N1 Co1 N3 C9 178.40(13) . . . . ? O4 Co1 N3 C9 -47.30(18) . . . . ? O6 Co1 N3 C9 -97.99(12) . . . . ? N5 Co1 N3 C9 -9.51(11) . . . . ? O3 Co1 N3 C9 115.51(12) . . . . ? O1 Co1 N3 C4 -99.54(12) . . . . ? N1 Co1 N3 C4 3.16(12) . . . . ? O4 Co1 N3 C4 137.46(13) . . . . ? O6 Co1 N3 C4 86.77(12) . . . . ? N5 Co1 N3 C4 175.26(13) . . . . ? O3 Co1 N3 C4 -59.72(14) . . . . ? C11 C10 N4 N5 0.0(2) . . . . ? C11 C10 N4 C9 -178.75(16) . . . . ? N3 C9 N4 C10 -176.57(16) . . . . ? C8 C9 N4 C10 3.7(3) . . . . ? N3 C9 N4 N5 4.7(2) . . . . ? C8 C9 N4 N5 -174.99(15) . . . . ? C11 C12 N5 N4 -0.1(2) . . . . ? C11 C12 N5 Co1 -163.72(15) . . . . ? C10 N4 N5 C12 0.06(19) . . . . ? C9 N4 N5 C12 179.02(14) . . . . ? C10 N4 N5 Co1 168.50(11) . . . . ? C9 N4 N5 Co1 -12.54(18) . . . . ? O1 Co1 N5 C12 84.4(2) . . . . ? N1 Co1 N5 C12 -173.02(18) . . . . ? N3 Co1 N5 C12 173.7(2) . . . . ? O4 Co1 N5 C12 -24.4(2) . . . . ? O6 Co1 N5 C12 -82.6(2) . . . . ? O3 Co1 N5 C12 44.4(2) . . . . ? O1 Co1 N5 N4 -78.13(12) . . . . ? N1 Co1 N5 N4 24.44(17) . . . . ? N3 Co1 N5 N4 11.14(11) . . . . ? O4 Co1 N5 N4 173.03(12) . . . . ? O6 Co1 N5 N4 114.81(12) . . . . ? O3 Co1 N5 N4 -118.17(11) . . . . ? O2 N6 O1 Co1 173.73(17) . . . . ? O3 N6 O1 Co1 -4.4(2) . . . . ? N1 Co1 O1 N6 75.01(12) . . . . ? N3 Co1 O1 N6 147.42(12) . . . . ? O4 Co1 O1 N6 -58.91(13) . . . . ? O6 Co1 O1 N6 -60.5(3) . . . . ? N5 Co1 O1 N6 -139.75(12) . . . . ? O3 Co1 O1 N6 2.53(11) . . . . ? O2 N6 O3 Co1 -174.12(19) . . . . ? O1 N6 O3 Co1 3.96(18) . . . . ? O1 Co1 O3 N6 -2.58(12) . . . . ? N1 Co1 O3 N6 -111.95(13) . . . . ? N3 Co1 O3 N6 -52.57(15) . . . . ? O4 Co1 O3 N6 118.68(14) . . . . ? O6 Co1 O3 N6 164.29(12) . . . . ? N5 Co1 O3 N6 47.51(15) . . . . ? O5 N7 O4 Co1 177.39(19) . . . . ? O6 N7 O4 Co1 -3.54(17) . . . . ? O1 Co1 O4 N7 -177.39(11) . . . . ? N1 Co1 O4 N7 63.15(14) . . . . ? N3 Co1 O4 N7 -59.13(17) . . . . ? O6 Co1 O4 N7 2.18(10) . . . . ? N5 Co1 O4 N7 -95.26(12) . . . . ? O3 Co1 O4 N7 133.97(12) . . . . ? O5 N7 O6 Co1 -177.42(19) . . . . ? O4 N7 O6 Co1 3.52(17) . . . . ? O1 Co1 O6 N7 -0.4(3) . . . . ? N1 Co1 O6 N7 -136.99(11) . . . . ? N3 Co1 O6 N7 150.79(11) . . . . ? O4 Co1 O6 N7 -2.17(10) . . . . ? N5 Co1 O6 N7 77.95(11) . . . . ? O3 Co1 O6 N7 -56.83(12) . . . . ? O8 C7 O7 C13 3.2(3) . . . . ? C6 C7 O7 C13 -177.38(17) . . . . ? C14 C13 O7 C7 157.9(3) . . . . ? C14' C13 O7 C7 -162.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.256 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.047 data_1heating303K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Co N7 O8' _chemical_formula_sum 'C16 H17 Co N7 O8' _chemical_formula_weight 494.30 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' '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 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 9.8591(12) _cell_length_b 26.027(3) _cell_length_c 8.1886(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.676(3) _cell_angle_gamma 90.00 _cell_volume 2064.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 303(2) _cell_measurement_reflns_used 3818 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7758 _exptl_absorpt_correction_T_max 0.9161 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 303(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17707 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3818 _reflns_number_gt 3123 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+1.9662P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3818 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.06167(6) 0.12502(2) 0.20078(7) 0.0443(2) Uani 1 1 d . . . C1 C 1.2221(5) 0.23387(18) 0.1455(6) 0.0578(12) Uani 1 1 d . . . H1A H 1.3022 0.2207 0.1168 0.069 Uiso 1 1 calc R . . C2 C 1.1883(5) 0.28576(18) 0.1397(5) 0.0547(11) Uani 1 1 d . . . H2A H 1.2389 0.3128 0.1068 0.066 Uiso 1 1 calc R . . C3 C 1.0658(4) 0.28874(16) 0.1922(5) 0.0481(10) Uani 1 1 d . . . H3A H 1.0159 0.3185 0.2032 0.058 Uiso 1 1 calc R . . C4 C 0.9149(4) 0.22134(15) 0.2866(4) 0.0384(9) Uani 1 1 d . . . C5 C 0.8143(4) 0.25216(16) 0.3323(5) 0.0420(9) Uani 1 1 d . . . H11A H 0.8174 0.2877 0.3235 0.050 Uiso 1 1 calc R . . C6 C 0.7091(4) 0.22779(16) 0.3917(5) 0.0431(9) Uani 1 1 d . . . C7 C 0.5936(4) 0.25814(17) 0.4433(5) 0.0511(11) Uani 1 1 d . . . C8 C 0.7052(4) 0.17478(16) 0.4049(5) 0.0458(10) Uani 1 1 d . . . H8 H 0.6349 0.1583 0.4459 0.055 Uiso 1 1 calc R . . C9 C 0.8101(4) 0.14745(15) 0.3545(5) 0.0402(9) Uani 1 1 d . . . C10 C 0.7397(5) 0.05692(17) 0.4034(5) 0.0535(11) Uani 1 1 d . . . H10A H 0.6617 0.0622 0.4499 0.064 Uiso 1 1 calc R . . C11 C 0.7936(5) 0.01127(17) 0.3730(6) 0.0591(12) Uani 1 1 d . . . H11B H 0.7609 -0.0211 0.3945 0.071 Uiso 1 1 calc R . . C12 C 0.9081(5) 0.02231(16) 0.3028(6) 0.0585(12) Uani 1 1 d . . . H12A H 0.9650 -0.0024 0.2689 0.070 Uiso 1 1 calc R . . C13 C 0.4983(5) 0.34147(19) 0.4585(7) 0.0762(16) Uani 1 1 d . . . H13A H 0.5139 0.3480 0.5771 0.091 Uiso 1 1 calc R A 1 H13B H 0.4093 0.3248 0.4268 0.091 Uiso 1 1 calc R A 1 C16 C 0.6290(9) 0.4741(3) 0.3358(10) 0.135(3) Uani 1 1 d . . . H16A H 0.7028 0.4721 0.2743 0.162 Uiso 1 1 calc R B 1 H16B H 0.6460 0.5019 0.4138 0.162 Uiso 1 1 calc R B 1 H16C H 0.5434 0.4798 0.2606 0.162 Uiso 1 1 calc R B 1 N1 N 0.9260(3) 0.07230(13) 0.2902(4) 0.0490(9) Uani 1 1 d . . . N2 N 0.8203(3) 0.09406(13) 0.3535(4) 0.0424(8) Uani 1 1 d . . . N3 N 0.9124(3) 0.17008(12) 0.2949(4) 0.0386(8) Uani 1 1 d . . . N4 N 1.0299(3) 0.23979(12) 0.2257(4) 0.0393(8) Uani 1 1 d . . . N5 N 1.1274(3) 0.20558(13) 0.1966(4) 0.0480(9) Uani 1 1 d . . . N7 N 1.3119(4) 0.10526(15) 0.3389(7) 0.0673(12) Uani 1 1 d . . . N6 N 0.9735(4) 0.09863(16) -0.1118(5) 0.0624(10) Uani 1 1 d . . . O6 O 1.2150(3) 0.10769(12) 0.4199(4) 0.0640(9) Uani 1 1 d . . . O5 O 1.4304(4) 0.09751(18) 0.4053(7) 0.1196(17) Uani 1 1 d . . . O4 O 1.2746(4) 0.11042(14) 0.1831(5) 0.0817(11) Uani 1 1 d . . . O3 O 1.0388(5) 0.06608(14) -0.0187(4) 0.0892(12) Uani 1 1 d . . . O2 O 0.9367(5) 0.09317(15) -0.2617(4) 0.0928(13) Uani 1 1 d . . . O1 O 0.9503(3) 0.14028(11) -0.0416(4) 0.0593(8) Uani 1 1 d . . . O7 O 0.6077(3) 0.30795(12) 0.4186(4) 0.0661(9) Uani 1 1 d . C . O8 O 0.5024(3) 0.23929(13) 0.5002(5) 0.0799(11) Uani 1 1 d . . . C14 C 0.4992(15) 0.3922(4) 0.364(2) 0.085(5) Uani 0.63(2) 1 d P C 1 H14A H 0.4985 0.3853 0.2475 0.102 Uiso 0.63(2) 1 calc PR C 1 H14B H 0.4169 0.4118 0.3721 0.102 Uiso 0.63(2) 1 calc PR C 1 C15 C 0.6206(15) 0.4220(5) 0.432(3) 0.105(5) Uani 0.63(2) 1 d P C 1 H15A H 0.7023 0.4017 0.4280 0.126 Uiso 0.63(2) 1 calc PR C 1 H15B H 0.6194 0.4296 0.5481 0.126 Uiso 0.63(2) 1 calc PR C 1 C14' C 0.565(2) 0.3971(6) 0.478(3) 0.054(6) Uani 0.37(2) 1 d P C 2 H14C H 0.5080 0.4201 0.5292 0.065 Uiso 0.37(2) 1 calc PR C 2 H14D H 0.6558 0.3955 0.5491 0.065 Uiso 0.37(2) 1 calc PR C 2 C15' C 0.578(3) 0.4172(8) 0.307(3) 0.094(8) Uani 0.37(2) 1 d P C 2 H15C H 0.4901 0.4158 0.2314 0.113 Uiso 0.37(2) 1 calc PR C 2 H15D H 0.6447 0.3969 0.2601 0.113 Uiso 0.37(2) 1 calc PR C 2 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 0.0434(3) 0.0401(3) 0.0516(4) 0.0005(3) 0.0148(3) 0.0064(3) C1 0.048(3) 0.061(3) 0.072(3) -0.003(2) 0.029(2) -0.011(2) C2 0.055(3) 0.054(3) 0.057(3) 0.005(2) 0.016(2) -0.015(2) C3 0.056(3) 0.037(2) 0.052(2) 0.0009(19) 0.013(2) -0.006(2) C4 0.039(2) 0.039(2) 0.036(2) -0.0018(17) 0.0061(18) -0.0025(17) C5 0.043(2) 0.036(2) 0.047(2) -0.0027(18) 0.0087(18) 0.0009(18) C6 0.040(2) 0.040(2) 0.050(2) -0.0051(18) 0.0125(19) 0.0010(18) C7 0.045(3) 0.046(3) 0.064(3) -0.006(2) 0.015(2) 0.005(2) C8 0.040(2) 0.048(3) 0.053(2) -0.002(2) 0.017(2) -0.0050(19) C9 0.041(2) 0.037(2) 0.042(2) 0.0011(18) 0.0068(18) 0.0004(18) C10 0.055(3) 0.051(3) 0.057(3) 0.005(2) 0.017(2) -0.008(2) C11 0.070(3) 0.037(3) 0.071(3) 0.006(2) 0.013(3) -0.009(2) C12 0.065(3) 0.033(2) 0.078(3) -0.001(2) 0.016(3) 0.007(2) C13 0.069(3) 0.051(3) 0.116(5) -0.006(3) 0.038(3) 0.020(3) C16 0.189(9) 0.068(5) 0.170(8) 0.011(5) 0.090(7) 0.002(5) N1 0.049(2) 0.040(2) 0.060(2) -0.0024(16) 0.0148(17) 0.0065(16) N2 0.0398(19) 0.040(2) 0.0489(19) 0.0027(15) 0.0118(16) 0.0007(15) N3 0.0394(19) 0.0362(19) 0.0418(18) -0.0014(14) 0.0115(15) -0.0017(14) N4 0.0384(18) 0.0376(19) 0.0433(18) -0.0016(14) 0.0117(15) -0.0021(15) N5 0.0408(19) 0.038(2) 0.069(2) -0.0025(17) 0.0186(17) 0.0015(16) N7 0.046(3) 0.046(2) 0.109(4) 0.004(2) 0.011(3) 0.0036(18) N6 0.080(3) 0.049(2) 0.060(3) 0.001(2) 0.016(2) 0.004(2) O6 0.055(2) 0.064(2) 0.074(2) 0.0069(16) 0.0137(17) 0.0049(16) O5 0.043(2) 0.112(4) 0.190(5) 0.004(3) -0.015(3) 0.010(2) O4 0.078(3) 0.084(3) 0.092(3) 0.012(2) 0.039(2) 0.026(2) O3 0.133(3) 0.065(2) 0.074(2) 0.0088(19) 0.029(2) 0.042(2) O2 0.140(4) 0.085(3) 0.050(2) -0.0162(19) 0.012(2) -0.008(3) O1 0.079(2) 0.0422(18) 0.0584(18) -0.0001(14) 0.0176(17) 0.0119(15) O7 0.061(2) 0.0453(19) 0.102(3) -0.0072(17) 0.0390(19) 0.0080(15) O8 0.060(2) 0.063(2) 0.130(3) 0.005(2) 0.052(2) 0.0043(18) C14 0.095(9) 0.077(8) 0.082(9) -0.016(7) 0.016(8) 0.023(6) C15 0.091(9) 0.078(9) 0.145(16) 0.011(10) 0.018(9) 0.001(7) C14' 0.068(11) 0.035(8) 0.062(13) -0.009(7) 0.021(9) 0.011(7) C15' 0.15(2) 0.087(14) 0.046(11) 0.017(10) 0.027(12) 0.007(14) _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 O1 2.120(3) . ? Co1 N3 2.134(3) . ? Co1 N1 2.138(3) . ? Co1 O4 2.164(4) . ? Co1 O6 2.169(3) . ? Co1 N5 2.197(3) . ? Co1 O3 2.342(4) . ? C1 N5 1.317(5) . ? C1 C2 1.390(6) . ? C1 H1A 0.9300 . ? C2 C3 1.357(6) . ? C2 H2A 0.9300 . ? C3 N4 1.364(5) . ? C3 H3A 0.9300 . ? C4 N3 1.336(5) . ? C4 C5 1.380(5) . ? C4 N4 1.405(4) . ? C5 C6 1.380(5) . ? C5 H11A 0.9300 . ? C6 C8 1.385(5) . ? C6 C7 1.509(5) . ? C7 O8 1.192(5) . ? C7 O7 1.323(5) . ? C8 C9 1.379(5) . ? C8 H8 0.9300 . ? C9 N3 1.336(5) . ? C9 N2 1.393(5) . ? C10 C11 1.343(6) . ? C10 N2 1.361(5) . ? C10 H10A 0.9300 . ? C11 C12 1.388(6) . ? C11 H11B 0.9300 . ? C12 N1 1.320(5) . ? C12 H12A 0.9300 . ? C13 O7 1.470(5) . ? C13 C14 1.532(14) . ? C13 C14' 1.588(19) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C16 C15' 1.57(3) . ? C16 C15 1.578(18) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 N2 1.369(4) . ? N4 N5 1.363(4) . ? N7 O5 1.210(5) . ? N7 O6 1.261(5) . ? N7 O4 1.268(5) . ? N6 O2 1.222(5) . ? N6 O3 1.238(5) . ? N6 O1 1.267(4) . ? C14 C15 1.45(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C14' C15' 1.53(3) . ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' H15C 0.9700 . ? C15' H15D 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 O1 Co1 N3 87.88(12) . . ? O1 Co1 N1 101.10(13) . . ? N3 Co1 N1 73.25(12) . . ? O1 Co1 O4 108.10(14) . . ? N3 Co1 O4 149.64(14) . . ? N1 Co1 O4 125.90(13) . . ? O1 Co1 O6 166.95(12) . . ? N3 Co1 O6 103.72(12) . . ? N1 Co1 O6 88.15(13) . . ? O4 Co1 O6 58.85(14) . . ? O1 Co1 N5 84.83(12) . . ? N3 Co1 N5 72.92(12) . . ? N1 Co1 N5 145.37(12) . . ? O4 Co1 N5 82.77(13) . . ? O6 Co1 N5 92.80(13) . . ? O1 Co1 O3 56.27(12) . . ? N3 Co1 O3 131.48(13) . . ? N1 Co1 O3 82.25(14) . . ? O4 Co1 O3 77.89(16) . . ? O6 Co1 O3 116.86(13) . . ? N5 Co1 O3 126.88(13) . . ? N5 C1 C2 112.0(4) . . ? N5 C1 H1A 124.0 . . ? C2 C1 H1A 124.0 . . ? C3 C2 C1 105.5(4) . . ? C3 C2 H2A 127.3 . . ? C1 C2 H2A 127.3 . . ? C2 C3 N4 106.8(4) . . ? C2 C3 H3A 126.6 . . ? N4 C3 H3A 126.6 . . ? N3 C4 C5 123.1(3) . . ? N3 C4 N4 112.5(3) . . ? C5 C4 N4 124.4(4) . . ? C6 C5 C4 117.0(4) . . ? C6 C5 H11A 121.5 . . ? C4 C5 H11A 121.5 . . ? C5 C6 C8 121.2(4) . . ? C5 C6 C7 120.9(4) . . ? C8 C6 C7 117.9(4) . . ? O8 C7 O7 124.9(4) . . ? O8 C7 C6 123.8(4) . . ? O7 C7 C6 111.3(4) . . ? C9 C8 C6 117.3(4) . . ? C9 C8 H8 121.4 . . ? C6 C8 H8 121.4 . . ? N3 C9 C8 122.7(4) . . ? N3 C9 N2 112.1(3) . . ? C8 C9 N2 125.1(4) . . ? C11 C10 N2 107.5(4) . . ? C11 C10 H10A 126.3 . . ? N2 C10 H10A 126.3 . . ? C10 C11 C12 105.8(4) . . ? C10 C11 H11B 127.1 . . ? C12 C11 H11B 127.1 . . ? N1 C12 C11 111.6(4) . . ? N1 C12 H12A 124.2 . . ? C11 C12 H12A 124.2 . . ? O7 C13 C14 109.1(6) . . ? O7 C13 C14' 104.8(6) . . ? C14 C13 C14' 39.1(6) . . ? O7 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? C14' C13 H13A 75.7 . . ? O7 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? C14' C13 H13B 140.7 . . ? H13A C13 H13B 108.3 . . ? C15' C16 C15 38.8(6) . . ? C15' C16 H16A 96.9 . . ? C15 C16 H16A 109.5 . . ? C15' C16 H16B 145.7 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15' C16 H16C 80.3 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 N1 N2 104.8(3) . . ? C12 N1 Co1 139.5(3) . . ? N2 N1 Co1 115.6(2) . . ? C10 N2 N1 110.3(3) . . ? C10 N2 C9 131.3(3) . . ? N1 N2 C9 118.4(3) . . ? C9 N3 C4 118.8(3) . . ? C9 N3 Co1 120.5(3) . . ? C4 N3 Co1 120.6(2) . . ? N5 N4 C3 110.9(3) . . ? N5 N4 C4 118.7(3) . . ? C3 N4 C4 130.3(3) . . ? C1 N5 N4 104.8(3) . . ? C1 N5 Co1 140.1(3) . . ? N4 N5 Co1 113.7(2) . . ? O5 N7 O6 122.3(5) . . ? O5 N7 O4 123.1(5) . . ? O6 N7 O4 114.6(4) . . ? O2 N6 O3 124.3(4) . . ? O2 N6 O1 120.6(4) . . ? O3 N6 O1 115.1(4) . . ? N7 O6 Co1 93.2(3) . . ? N7 O4 Co1 93.2(3) . . ? N6 O3 Co1 89.4(3) . . ? N6 O1 Co1 99.1(3) . . ? C7 O7 C13 116.4(3) . . ? C15 C14 C13 110.4(15) . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 112.5(15) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15' C14' C13 108.8(18) . . ? C15' C14' H14C 109.9 . . ? C13 C14' H14C 109.9 . . ? C15' C14' H14D 109.9 . . ? C13 C14' H14D 109.9 . . ? H14C C14' H14D 108.3 . . ? C14' C15' C16 105.1(17) . . ? C14' C15' H15C 110.7 . . ? C16 C15' H15C 110.7 . . ? C14' C15' H15D 110.7 . . ? C16 C15' H15D 110.7 . . ? H15C C15' H15D 108.8 . . ? 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 N5 C1 C2 C3 0.6(5) . . . . ? C1 C2 C3 N4 -0.5(5) . . . . ? N3 C4 C5 C6 1.3(6) . . . . ? N4 C4 C5 C6 -179.2(3) . . . . ? C4 C5 C6 C8 0.1(6) . . . . ? C4 C5 C6 C7 -179.4(4) . . . . ? C5 C6 C7 O8 -177.6(4) . . . . ? C8 C6 C7 O8 2.9(7) . . . . ? C5 C6 C7 O7 1.8(6) . . . . ? C8 C6 C7 O7 -177.7(4) . . . . ? C5 C6 C8 C9 -0.6(6) . . . . ? C7 C6 C8 C9 178.9(4) . . . . ? C6 C8 C9 N3 -0.1(6) . . . . ? C6 C8 C9 N2 -177.7(4) . . . . ? N2 C10 C11 C12 -0.3(5) . . . . ? C10 C11 C12 N1 0.3(5) . . . . ? C11 C12 N1 N2 -0.1(5) . . . . ? C11 C12 N1 Co1 -178.6(3) . . . . ? O1 Co1 N1 C12 95.2(5) . . . . ? N3 Co1 N1 C12 179.5(5) . . . . ? O4 Co1 N1 C12 -27.0(5) . . . . ? O6 Co1 N1 C12 -75.5(5) . . . . ? N5 Co1 N1 C12 -167.8(4) . . . . ? O3 Co1 N1 C12 41.9(5) . . . . ? O1 Co1 N1 N2 -83.2(3) . . . . ? N3 Co1 N1 N2 1.2(2) . . . . ? O4 Co1 N1 N2 154.6(3) . . . . ? O6 Co1 N1 N2 106.1(3) . . . . ? N5 Co1 N1 N2 13.9(4) . . . . ? O3 Co1 N1 N2 -136.5(3) . . . . ? C11 C10 N2 N1 0.2(5) . . . . ? C11 C10 N2 C9 179.0(4) . . . . ? C12 N1 N2 C10 -0.1(4) . . . . ? Co1 N1 N2 C10 178.9(3) . . . . ? C12 N1 N2 C9 -179.0(4) . . . . ? Co1 N1 N2 C9 -0.1(4) . . . . ? N3 C9 N2 C10 179.5(4) . . . . ? C8 C9 N2 C10 -2.7(7) . . . . ? N3 C9 N2 N1 -1.8(5) . . . . ? C8 C9 N2 N1 176.0(4) . . . . ? C8 C9 N3 C4 1.4(6) . . . . ? N2 C9 N3 C4 179.2(3) . . . . ? C8 C9 N3 Co1 -174.9(3) . . . . ? N2 C9 N3 Co1 3.0(4) . . . . ? C5 C4 N3 C9 -2.0(6) . . . . ? N4 C4 N3 C9 178.5(3) . . . . ? C5 C4 N3 Co1 174.3(3) . . . . ? N4 C4 N3 Co1 -5.3(4) . . . . ? O1 Co1 N3 C9 99.9(3) . . . . ? N1 Co1 N3 C9 -2.3(3) . . . . ? O4 Co1 N3 C9 -136.6(3) . . . . ? O6 Co1 N3 C9 -86.1(3) . . . . ? N5 Co1 N3 C9 -174.8(3) . . . . ? O3 Co1 N3 C9 60.7(3) . . . . ? O1 Co1 N3 C4 -76.3(3) . . . . ? N1 Co1 N3 C4 -178.5(3) . . . . ? O4 Co1 N3 C4 47.2(4) . . . . ? O6 Co1 N3 C4 97.7(3) . . . . ? N5 Co1 N3 C4 9.0(3) . . . . ? O3 Co1 N3 C4 -115.5(3) . . . . ? C2 C3 N4 N5 0.4(4) . . . . ? C2 C3 N4 C4 178.5(4) . . . . ? N3 C4 N4 N5 -5.3(5) . . . . ? C5 C4 N4 N5 175.1(4) . . . . ? N3 C4 N4 C3 176.7(4) . . . . ? C5 C4 N4 C3 -2.9(6) . . . . ? C2 C1 N5 N4 -0.3(5) . . . . ? C2 C1 N5 Co1 163.8(3) . . . . ? C3 N4 N5 C1 0.0(4) . . . . ? C4 N4 N5 C1 -178.4(3) . . . . ? C3 N4 N5 Co1 -169.0(3) . . . . ? C4 N4 N5 Co1 12.6(4) . . . . ? O1 Co1 N5 C1 -84.8(5) . . . . ? N3 Co1 N5 C1 -174.1(5) . . . . ? N1 Co1 N5 C1 173.2(4) . . . . ? O4 Co1 N5 C1 24.2(5) . . . . ? O6 Co1 N5 C1 82.4(5) . . . . ? O3 Co1 N5 C1 -44.7(5) . . . . ? O1 Co1 N5 N4 78.5(3) . . . . ? N3 Co1 N5 N4 -10.9(2) . . . . ? N1 Co1 N5 N4 -23.6(4) . . . . ? O4 Co1 N5 N4 -172.5(3) . . . . ? O6 Co1 N5 N4 -114.4(3) . . . . ? O3 Co1 N5 N4 118.6(3) . . . . ? O5 N7 O6 Co1 177.7(4) . . . . ? O4 N7 O6 Co1 -3.8(4) . . . . ? O1 Co1 O6 N7 1.7(7) . . . . ? N3 Co1 O6 N7 -150.5(2) . . . . ? N1 Co1 O6 N7 137.2(3) . . . . ? O4 Co1 O6 N7 2.4(2) . . . . ? N5 Co1 O6 N7 -77.4(3) . . . . ? O3 Co1 O6 N7 56.9(3) . . . . ? O5 N7 O4 Co1 -177.7(4) . . . . ? O6 N7 O4 Co1 3.9(4) . . . . ? O1 Co1 O4 N7 177.5(3) . . . . ? N3 Co1 O4 N7 58.7(4) . . . . ? N1 Co1 O4 N7 -63.4(3) . . . . ? O6 Co1 O4 N7 -2.4(2) . . . . ? N5 Co1 O4 N7 95.3(3) . . . . ? O3 Co1 O4 N7 -134.4(3) . . . . ? O2 N6 O3 Co1 173.7(5) . . . . ? O1 N6 O3 Co1 -3.8(4) . . . . ? O1 Co1 O3 N6 2.5(3) . . . . ? N3 Co1 O3 N6 52.0(3) . . . . ? N1 Co1 O3 N6 111.4(3) . . . . ? O4 Co1 O3 N6 -119.2(3) . . . . ? O6 Co1 O3 N6 -164.6(3) . . . . ? N5 Co1 O3 N6 -48.0(3) . . . . ? O2 N6 O1 Co1 -173.3(4) . . . . ? O3 N6 O1 Co1 4.3(4) . . . . ? N3 Co1 O1 N6 -147.7(3) . . . . ? N1 Co1 O1 N6 -75.2(3) . . . . ? O4 Co1 O1 N6 58.6(3) . . . . ? O6 Co1 O1 N6 59.2(6) . . . . ? N5 Co1 O1 N6 139.3(3) . . . . ? O3 Co1 O1 N6 -2.5(3) . . . . ? O8 C7 O7 C13 -2.8(7) . . . . ? C6 C7 O7 C13 177.8(4) . . . . ? C14 C13 O7 C7 -158.5(7) . . . . ? C14' C13 O7 C7 160.9(8) . . . . ? O7 C13 C14 C15 -70.3(13) . . . . ? C14' C13 C14 C15 19.8(12) . . . . ? C13 C14 C15 C16 178.2(8) . . . . ? C15' C16 C15 C14 -33.3(16) . . . . ? O7 C13 C14' C15' 72.6(17) . . . . ? C14 C13 C14' C15' -29.7(14) . . . . ? C13 C14' C15' C16 173.7(11) . . . . ? C15 C16 C15' C14' 18.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.281 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.063