Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Adriano Bigotto' 'Alessandro Felluga' 'Renata Dreos' 'Giorgio Nardin' 'Lucio Randaccio' 'Giovanni Tauzher' 'Claudio Tavagnacco' _publ_contact_author_name 'Prof Lucio Randaccio' _publ_contact_author_address ; Prof Lucio Randaccio Dipartimento di Scienze Chimiche Universita di Trieste Via L Giorgieri 1 Trieste 34127 ITALY ; data_2c _database_code_CSD 157412 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H33 Cl Co2 F6 N6 O7' _chemical_formula_weight 808.89 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 21.026(3) _cell_length_b 11.6760(10) _cell_length_c 27.547(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.490(15) _cell_angle_gamma 90.00 _cell_volume 6576.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.6 mm _exptl_crystal_size_mid 0.38 mm _exptl_crystal_size_min 0.15 mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method ? _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8086 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.98 _reflns_number_total 7921 _reflns_number_observed 4775 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2= ^ or flagged by the user for potential systematic errors. Weighted R-factor= s wR and all goodnesses 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 observed criteri= on of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.0677P)^2^+2.3530P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7921 _refine_ls_number_parameters 437 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_obs 0.0456 _refine_ls_wR_factor_all 0.1216 _refine_ls_wR_factor_obs 0.1061 _refine_ls_goodness_of_fit_all 0.906 _refine_ls_goodness_of_fit_obs 1.036 _refine_ls_restrained_S_all 0.906 _refine_ls_restrained_S_obs 1.036 _refine_ls_shift/esd_max -1.573 _refine_ls_shift/esd_mean 0.029 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.86212(2) 0.11728(4) 0.62893(2) 0.03561(12) Uani 1 d . . O2H O 0.83290(10) -0.0356(2) 0.63784(8) 0.0377(5) Uani 1 d D . H2OH H 0.7915 -0.0507 0.6139 0.045 Uiso 1 d D . O1 O 0.89435(11) -0.0449(2) 0.56252(8) 0.0402(5) Uani 1 d . . N1 N 0.89326(12) 0.0658(2) 0.57410(10) 0.0365(6) Uani 1 d . . N2 N 0.89857(13) 0.2576(2) 0.61264(11) 0.0446(7) Uani 1 d . . N3 N 0.83455(15) 0.1768(2) 0.68740(10) 0.0464(7) Uani 1 d . . C1 C 0.9427(2) 0.1149(4) 0.5049(2) 0.0612(11) Uani 1 d . . H1A H 0.9344(13) 0.1773(11) 0.4816(5) 0.092 Uiso 1 calc R . H1B H 0.9221(10) 0.0468(14) 0.4891(6) 0.092 Uiso 1 calc R . H1C H 0.9890(3) 0.1026(24) 0.5157(2) 0.092 Uiso 1 calc R . C2 C 0.9159(2) 0.1426(3) 0.54849(13) 0.0415(8) Uani 1 d . . C3 C 0.9171(2) 0.2561(3) 0.57098(14) 0.0459(9) Uani 1 d . . C4 C 0.9385(2) 0.3585(3) 0.5461(2) 0.0657(12) Uani 1 d . . H4A H 0.9350(14) 0.4259(5) 0.5653(6) 0.099 Uiso 1 calc R . H4B H 0.9112(10) 0.3666(16) 0.5132(5) 0.099 Uiso 1 calc R . H4C H 0.9831(5) 0.3487(12) 0.5441(10) 0.099 Uiso 1 calc R . C5 C 0.9062(2) 0.3582(3) 0.6441(2) 0.0579(10) Uani 1 d . . H5A H 0.8664(2) 0.4035(3) 0.6362(2) 0.070 Uiso 1 calc R . H5B H 0.9418(2) 0.4050(3) 0.6382(2) 0.070 Uiso 1 calc R . C6 C 0.9206(2) 0.3217(3) 0.6985(2) 0.0650(12) Uani 1 d . . H6A H 0.9570(2) 0.2683(3) 0.7046(2) 0.078 Uiso 1 calc R . H6B H 0.9342(2) 0.3885(3) 0.7193(2) 0.078 Uiso 1 calc R . C7 C 0.8649(2) 0.2672(3) 0.71413(14) 0.0588(11) Uani 1 d . . C8 C 0.8438(3) 0.3054(4) 0.7552(2) 0.084(2) Uani 1 d . . H8 H 0.8638(3) 0.3684(4) 0.7731(2) 0.100 Uiso 1 calc R . C9 C 0.7939(3) 0.2516(5) 0.7696(2) 0.096(2) Uani 1 d . . H9 H 0.7810(3) 0.2761(5) 0.7980(2) 0.116 Uiso 1 calc R . C10 C 0.7629(3) 0.1619(5) 0.7427(2) 0.0814(15) Uani 1 d . . H10 H 0.7279(3) 0.1258(5) 0.7517(2) 0.098 Uiso 1 calc R . C11 C 0.7842(2) 0.1261(4) 0.70197(14) 0.0563(10) Uani 1 d . . H11 H 0.7632(2) 0.0645(4) 0.68355(14) 0.068 Uiso 1 calc R . C12 C 0.7748(2) 0.1496(3) 0.58396(13) 0.0426(8) Uani 1 d . . H12A H 0.7753(2) 0.1173(3) 0.55162(13) 0.051 Uiso 1 calc R . H12B H 0.7428(2) 0.1062(3) 0.59673(13) 0.051 Uiso 1 calc R . C13 C 0.7490(2) 0.2675(4) 0.57497(14) 0.0530(10) Uani 1 d . . F1 F 0.74736(13) 0.3260(2) 0.61643(10) 0.0803(8) Uani 1 d . . F2 F 0.78055(12) 0.3350(2) 0.54857(10) 0.0755(7) Uani 1 d . . F3 F 0.68598(11) 0.2672(2) 0.54807(9) 0.0763(7) Uani 1 d . . Co1A Co 0.89962(2) -0.13629(3) 0.62566(2) 0.03422(12) Uani 1 d . . O1A O 0.94611(11) 0.0691(2) 0.67440(9) 0.0444(6) Uani 1 d . . N1A N 0.96225(12) -0.0322(2) 0.65950(10) 0.0373(6) Uani 1 d . . N2A N 0.97612(14) -0.2150(2) 0.61918(10) 0.0409(6) Uani 1 d . . N3A N 0.83730(13) -0.2482(2) 0.58687(10) 0.0390(6) Uani 1 d . . C1A C 1.0775(2) 0.0158(4) 0.6933(2) 0.0699(13) Uani 1 d . . H1A1 H 1.0803(10) 0.0812(14) 0.6728(5) 0.105 Uiso 1 calc R . H1A2 H 1.1182(3) -0.0251(9) 0.6999(11) 0.105 Uiso 1 calc R . H1A3 H 1.0686(8) 0.0407(22) 0.7243(6) 0.105 Uiso 1 calc R . C2A C 1.0235(2) -0.0614(3) 0.66673(14) 0.0458(8) Uani 1 d . . C3A C 1.0303(2) -0.1704(3) 0.64299(13) 0.0432(8) Uani 1 d . . C4A C 1.0965(2) -0.2202(4) 0.6454(2) 0.0667(12) Uani 1 d . . H4A1 H 1.1185(6) -0.1754(16) 0.6251(10) 0.100 Uiso 1 calc R . H4A2 H 1.0920(2) -0.2976(10) 0.6333(11) 0.100 Uiso 1 calc R . H4A3 H 1.1216(6) -0.2194(25) 0.6793(2) 0.100 Uiso 1 calc R . C5A C 0.9736(2) -0.3162(3) 0.58752(14) 0.0488(9) Uani 1 d . . H5A1 H 0.9657(2) -0.3839(3) 0.60563(14) 0.059 Uiso 1 calc R . H5A2 H 1.0150(2) -0.3258(3) 0.57830(14) 0.059 Uiso 1 calc R . C6A C 0.9186(2) -0.3018(3) 0.54053(13) 0.0475(8) Uani 1 d . . H6A1 H 0.9228(2) -0.2272(3) 0.52611(13) 0.057 Uiso 1 calc R . H6A2 H 0.9238(2) -0.3592(3) 0.51629(13) 0.057 Uiso 1 calc R . C7A C 0.8518(2) -0.3123(3) 0.54995(12) 0.0412(8) Uani 1 d . . C8A C 0.8063(2) -0.3856(3) 0.52209(14) 0.0527(9) Uani 1 d . . H8A H 0.8175(2) -0.4298(3) 0.49725(14) 0.063 Uiso 1 calc R . C9A C 0.7444(2) -0.3942(3) 0.5305(2) 0.0601(11) Uani 1 d . . H9A H 0.7134(2) -0.4428(3) 0.5113(2) 0.072 Uiso 1 calc R . C10A C 0.7298(2) -0.3294(3) 0.56786(15) 0.0534(10) Uani 1 d . . H10A H 0.6885(2) -0.3331(3) 0.57447(15) 0.064 Uiso 1 calc R . C11A C 0.7769(2) -0.2590(3) 0.59549(13) 0.0450(8) Uani 1 d . . H11A H 0.7668(2) -0.2167(3) 0.62129(13) 0.054 Uiso 1 calc R . C12A C 0.9007(2) -0.2104(3) 0.69150(13) 0.0486(9) Uani 1 d . . H12C H 0.9374(2) -0.1771(3) 0.71529(13) 0.058 Uiso 1 calc R . H12D H 0.8616(2) -0.1840(3) 0.70107(13) 0.058 Uiso 1 calc R . C13A C 0.9042(2) -0.3323(4) 0.7006(2) 0.0587(10) Uani 1 d . . F1A F 0.90372(15) -0.3615(2) 0.74754(9) 0.0808(8) Uani 1 d . . F2A F 0.9579(2) -0.3826(3) 0.69282(12) 0.1091(12) Uani 1 d . . F3A F 0.8557(2) -0.3938(3) 0.67261(12) 0.1189(13) Uani 1 d . . Cl Cl 0.61517(5) -0.07099(9) 0.60883(4) 0.0561(2) Uani 1 d . . O3 O 0.6828(2) -0.0649(3) 0.6313(2) 0.1009(12) Uani 1 d . . O4 O 0.6000(2) -0.1871(3) 0.5961(2) 0.1140(14) Uani 1 d . . O5 O 0.5779(2) -0.0350(4) 0.64197(13) 0.1041(13) Uani 1 d . . O6 O 0.5972(2) -0.0037(3) 0.56513(12) 0.0964(12) Uani 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 0.0377(2) 0.0268(2) 0.0386(2) -0.0038(2) 0.0014(2) 0.0037(2) O2H 0.0363(11) 0.0314(11) 0.0429(13) -0.0029(9) 0.0041(10) 0.0018(9) O1 0.0492(13) 0.0285(11) 0.0407(12) -0.0029(10) 0.0063(10) 0.0041(10) N1 0.0344(14) 0.0305(13) 0.0401(15) -0.0012(11) -0.0003(12) 0.0036(11) N2 0.044(2) 0.0280(14) 0.056(2) -0.0004(13) -0.0003(14) 0.0023(12) N3 0.054(2) 0.041(2) 0.039(2) -0.0054(13) 0.0005(14) 0.0128(14) C1 0.058(2) 0.056(2) 0.077(3) 0.014(2) 0.032(2) 0.019(2) C2 0.035(2) 0.037(2) 0.050(2) 0.008(2) 0.0055(15) 0.0039(14) C3 0.038(2) 0.034(2) 0.061(2) 0.007(2) 0.001(2) -0.0023(15) C4 0.060(3) 0.046(2) 0.089(3) 0.021(2) 0.012(2) -0.005(2) C5 0.062(2) 0.030(2) 0.074(3) -0.008(2) 0.002(2) -0.002(2) C6 0.076(3) 0.042(2) 0.063(3) -0.018(2) -0.010(2) 0.002(2) C7 0.077(3) 0.045(2) 0.047(2) -0.010(2) -0.002(2) 0.014(2) C8 0.118(4) 0.070(3) 0.055(3) -0.031(2) 0.004(3) 0.014(3) C9 0.130(5) 0.102(4) 0.066(3) -0.033(3) 0.040(3) 0.014(4) C10 0.083(3) 0.102(4) 0.066(3) -0.015(3) 0.031(3) 0.017(3) C11 0.055(2) 0.064(3) 0.047(2) -0.009(2) 0.006(2) 0.013(2) C12 0.037(2) 0.044(2) 0.042(2) -0.0036(15) 0.0002(14) 0.0032(15) C13 0.046(2) 0.056(2) 0.053(2) -0.001(2) 0.004(2) 0.016(2) F1 0.089(2) 0.070(2) 0.077(2) -0.0152(13) 0.0084(14) 0.0386(14) F2 0.071(2) 0.0596(15) 0.091(2) 0.0303(14) 0.0080(14) 0.0121(13) F3 0.0472(12) 0.088(2) 0.084(2) 0.0089(15) -0.0053(12) 0.0249(13) Co1A 0.0365(2) 0.0262(2) 0.0379(2) -0.0028(2) 0.0045(2) 0.0027(2) O1A 0.0432(13) 0.0333(12) 0.0486(14) -0.0081(10) -0.0057(11) 0.0030(10) N1A 0.0386(14) 0.0293(13) 0.0392(15) -0.0032(11) -0.0010(12) 0.0035(11) N2A 0.045(2) 0.0309(13) 0.045(2) 0.0005(12) 0.0076(13) 0.0084(12) N3A 0.044(2) 0.0330(14) 0.0380(15) -0.0009(12) 0.0056(12) 0.0010(12) C1A 0.044(2) 0.068(3) 0.088(3) -0.011(2) -0.006(2) -0.006(2) C2A 0.038(2) 0.045(2) 0.050(2) 0.002(2) 0.001(2) 0.001(2) C3A 0.037(2) 0.044(2) 0.047(2) 0.006(2) 0.007(2) 0.0101(15) C4A 0.047(2) 0.074(3) 0.076(3) -0.006(2) 0.009(2) 0.020(2) C5A 0.053(2) 0.038(2) 0.057(2) -0.004(2) 0.017(2) 0.012(2) C6A 0.058(2) 0.041(2) 0.044(2) -0.008(2) 0.013(2) 0.004(2) C7A 0.052(2) 0.029(2) 0.039(2) -0.0009(14) 0.003(2) 0.0041(15) C8A 0.068(3) 0.037(2) 0.048(2) -0.010(2) 0.002(2) 0.004(2) C9A 0.062(3) 0.040(2) 0.066(3) -0.011(2) -0.008(2) -0.004(2) C10A 0.046(2) 0.044(2) 0.064(2) -0.005(2) 0.001(2) -0.004(2) C11A 0.044(2) 0.039(2) 0.051(2) -0.003(2) 0.009(2) -0.001(2) C12A 0.061(2) 0.035(2) 0.047(2) 0.001(2) 0.007(2) 0.002(2) C13A 0.061(3) 0.056(2) 0.055(2) 0.011(2) 0.006(2) 0.003(2) F1A 0.109(2) 0.074(2) 0.063(2) 0.0247(14) 0.0276(15) 0.010(2) F2A 0.144(3) 0.087(2) 0.115(2) 0.043(2) 0.067(2) 0.061(2) F3A 0.160(3) 0.064(2) 0.101(2) 0.021(2) -0.033(2) -0.040(2) Cl 0.0523(5) 0.0593(6) 0.0553(6) 0.0024(5) 0.0099(4) 0.0110(5) O3 0.054(2) 0.105(3) 0.132(3) 0.018(2) -0.001(2) -0.002(2) O4 0.100(3) 0.067(2) 0.162(4) -0.014(3) 0.004(3) 0.006(2) O5 0.122(3) 0.127(3) 0.074(2) 0.010(2) 0.046(2) 0.046(3) O6 0.128(3) 0.104(3) 0.059(2) 0.026(2) 0.025(2) 0.031(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic= ) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.880(3) . ? Co1 N2 1.906(3) . ? Co1 O2H 1.922(2) . ? Co1 N3 1.962(3) . ? Co1 O1A 1.993(2) . ? Co1 C12 1.997(3) . ? Co1 Co1A 3.0706(6) . ? O2H Co1A 1.919(2) . ? O1 N1 1.332(3) . ? O1 Co1A 2.022(2) . ? N1 C2 1.299(4) . ? N2 C3 1.296(5) . ? N2 C5 1.446(4) . ? N3 C11 1.353(5) . ? N3 C7 1.358(5) . ? C1 C2 1.476(5) . ? C2 C3 1.460(5) . ? C3 C4 1.498(5) . ? C5 C6 1.518(6) . ? C6 C7 1.482(6) . ? C7 C8 1.382(6) . ? C8 C9 1.358(8) . ? C9 C10 1.359(7) . ? C10 C11 1.366(6) . ? C12 C13 1.478(5) . ? C13 F1 1.338(4) . ? C13 F2 1.347(5) . ? C13 F3 1.360(4) . ? Co1A N1A 1.873(3) . ? Co1A N2A 1.897(3) . ? Co1A N3A 1.978(3) . ? Co1A C12A 2.005(4) . ? O1A N1A 1.322(3) . ? N1A C2A 1.303(4) . ? N2A C3A 1.284(4) . ? N2A C5A 1.462(4) . ? N3A C11A 1.351(4) . ? N3A C7A 1.354(4) . ? C1A C2A 1.500(5) . ? C2A C3A 1.453(5) . ? C3A C4A 1.497(5) . ? C5A C6A 1.530(5) . ? C6A C7A 1.492(5) . ? C7A C8A 1.376(5) . ? C8A C9A 1.379(6) . ? C9A C10A 1.368(6) . ? C10A C11A 1.373(5) . ? C12A C13A 1.444(5) . ? C13A F3A 1.335(5) . ? C13A F2A 1.335(5) . ? C13A F1A 1.340(5) . ? Cl O5 1.399(3) . ? Cl O3 1.415(3) . ? Cl O6 1.414(3) . ? Cl O4 1.417(4) . ? 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 N1 Co1 N2 81.46(12) . . ? N1 Co1 O2H 89.26(11) . . ? N2 Co1 O2H 170.52(11) . . ? N1 Co1 N3 176.44(12) . . ? N2 Co1 N3 95.77(13) . . ? O2H Co1 N3 93.43(11) . . ? N1 Co1 O1A 89.48(10) . . ? N2 Co1 O1A 92.57(11) . . ? O2H Co1 O1A 85.43(9) . . ? N3 Co1 O1A 88.41(11) . . ? N1 Co1 C12 90.26(13) . . ? N2 Co1 C12 93.07(13) . . ? O2H Co1 C12 88.83(12) . . ? N3 Co1 C12 92.12(13) . . ? O1A Co1 C12 174.26(12) . . ? N1 Co1 Co1A 61.83(8) . . ? N2 Co1 Co1A 134.57(9) . . ? O2H Co1 Co1A 36.89(7) . . ? N3 Co1 Co1A 119.53(9) . . ? O1A Co1 Co1A 63.27(6) . . ? C12 Co1 Co1A 111.68(10) . . ? Co1A O2H Co1 106.16(11) . . ? N1 O1 Co1A 107.8(2) . . ? C2 N1 O1 120.7(3) . . ? C2 N1 Co1 117.1(2) . . ? O1 N1 Co1 122.1(2) . . ? C3 N2 C5 121.9(3) . . ? C3 N2 Co1 114.7(2) . . ? C5 N2 Co1 123.4(3) . . ? C11 N3 C7 118.7(3) . . ? C11 N3 Co1 119.3(2) . . ? C7 N3 Co1 122.0(3) . . ? N1 C2 C3 111.6(3) . . ? N1 C2 C1 123.3(3) . . ? C3 C2 C1 124.9(3) . . ? N2 C3 C2 114.2(3) . . ? N2 C3 C4 125.3(4) . . ? C2 C3 C4 120.5(4) . . ? N2 C5 C6 109.4(3) . . ? C7 C6 C5 114.7(3) . . ? N3 C7 C8 119.6(5) . . ? N3 C7 C6 118.6(4) . . ? C8 C7 C6 121.7(4) . . ? C9 C8 C7 120.5(5) . . ? C8 C9 C10 120.1(5) . . ? C9 C10 C11 118.4(5) . . ? N3 C11 C10 122.6(4) . . ? C13 C12 Co1 121.8(2) . . ? F1 C13 F2 106.1(3) . . ? F1 C13 F3 104.5(3) . . ? F2 C13 F3 104.3(3) . . ? F1 C13 C12 114.4(3) . . ? F2 C13 C12 115.4(3) . . ? F3 C13 C12 111.1(3) . . ? N1A Co1A N2A 81.27(12) . . ? N1A Co1A O2H 88.46(10) . . ? N2A Co1A O2H 169.71(11) . . ? N1A Co1A N3A 176.20(12) . . ? N2A Co1A N3A 95.64(12) . . ? O2H Co1A N3A 94.60(10) . . ? N1A Co1A C12A 88.36(14) . . ? N2A Co1A C12A 92.59(14) . . ? O2H Co1A C12A 87.74(13) . . ? N3A Co1A C12A 94.01(13) . . ? N1A Co1A O1 88.66(10) . . ? N2A Co1A O1 93.00(11) . . ? O2H Co1A O1 86.06(9) . . ? N3A Co1A O1 89.30(10) . . ? C12A Co1A O1 173.19(12) . . ? N1A Co1A Co1 61.00(8) . . ? N2A Co1A Co1 134.37(9) . . ? O2H Co1A Co1 36.95(7) . . ? N3A Co1A Co1 120.70(8) . . ? C12A Co1A Co1 109.76(10) . . ? O1 Co1A Co1 63.47(6) . . ? N1A O1A Co1 108.1(2) . . ? C2A N1A O1A 120.2(3) . . ? C2A N1A Co1A 117.5(2) . . ? O1A N1A Co1A 122.2(2) . . ? C3A N2A C5A 122.5(3) . . ? C3A N2A Co1A 115.2(2) . . ? C5A N2A Co1A 122.3(2) . . ? C11A N3A C7A 117.8(3) . . ? C11A N3A Co1A 119.9(2) . . ? C7A N3A Co1A 122.3(2) . . ? N1A C2A C3A 110.9(3) . . ? N1A C2A C1A 121.7(3) . . ? C3A C2A C1A 127.2(3) . . ? N2A C3A C2A 114.7(3) . . ? N2A C3A C4A 124.8(3) . . ? C2A C3A C4A 120.5(3) . . ? N2A C5A C6A 109.3(3) . . ? C7A C6A C5A 113.6(3) . . ? N3A C7A C8A 120.9(3) . . ? N3A C7A C6A 118.1(3) . . ? C8A C7A C6A 121.0(3) . . ? C7A C8A C9A 120.9(4) . . ? C10A C9A C8A 118.1(4) . . ? C9A C10A C11A 119.3(4) . . ? N3A C11A C10A 123.0(3) . . ? C13A C12A Co1A 124.8(3) . . ? F3A C13A F2A 103.3(4) . . ? F3A C13A F1A 104.1(4) . . ? F2A C13A F1A 103.8(3) . . ? F3A C13A C12A 115.5(4) . . ? F2A C13A C12A 114.6(4) . . ? F1A C13A C12A 114.0(4) . . ? O5 Cl O3 111.1(3) . . ? O5 Cl O6 108.0(2) . . ? O3 Cl O6 112.7(2) . . ? O5 Cl O4 108.7(3) . . ? O3 Cl O4 107.5(2) . . ? O6 Cl O4 108.7(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 Co1 O2H Co1A 39.71(11) . . . . ? N2 Co1 O2H Co1A 28.3(7) . . . . ? N3 Co1 O2H Co1A -137.95(12) . . . . ? O1A Co1 O2H Co1A -49.83(11) . . . . ? C12 Co1 O2H Co1A 129.99(13) . . . . ? Co1A Co1 O2H Co1A 0.0 . . . . ? Co1A O1 N1 C2 151.9(2) . . . . ? Co1A O1 N1 Co1 -25.8(3) . . . . ? N2 Co1 N1 C2 -7.5(2) . . . . ? O2H Co1 N1 C2 174.4(2) . . . . ? N3 Co1 N1 C2 -46.5(19) . . . . ? O1A Co1 N1 C2 -100.2(2) . . . . ? C12 Co1 N1 C2 85.6(2) . . . . ? Co1A Co1 N1 C2 -159.8(3) . . . . ? N2 Co1 N1 O1 170.4(2) . . . . ? O2H Co1 N1 O1 -7.8(2) . . . . ? N3 Co1 N1 O1 131.3(17) . . . . ? O1A Co1 N1 O1 77.7(2) . . . . ? C12 Co1 N1 O1 -96.6(2) . . . . ? Co1A Co1 N1 O1 18.0(2) . . . . ? N1 Co1 N2 C3 9.0(2) . . . . ? O2H Co1 N2 C3 20.6(8) . . . . ? N3 Co1 N2 C3 -173.2(2) . . . . ? O1A Co1 N2 C3 98.1(2) . . . . ? C12 Co1 N2 C3 -80.8(3) . . . . ? Co1A Co1 N2 C3 44.1(3) . . . . ? N1 Co1 N2 C5 -170.1(3) . . . . ? O2H Co1 N2 C5 -158.5(5) . . . . ? N3 Co1 N2 C5 7.6(3) . . . . ? O1A Co1 N2 C5 -81.0(3) . . . . ? C12 Co1 N2 C5 100.1(3) . . . . ? Co1A Co1 N2 C5 -135.0(2) . . . . ? N1 Co1 N3 C11 -166.9(17) . . . . ? N2 Co1 N3 C11 154.3(3) . . . . ? O2H Co1 N3 C11 -27.9(3) . . . . ? O1A Co1 N3 C11 -113.2(3) . . . . ? C12 Co1 N3 C11 61.0(3) . . . . ? Co1A Co1 N3 C11 -55.4(3) . . . . ? N1 Co1 N3 C7 12.5(19) . . . . ? N2 Co1 N3 C7 -26.2(3) . . . . ? O2H Co1 N3 C7 151.5(3) . . . . ? O1A Co1 N3 C7 66.2(3) . . . . ? C12 Co1 N3 C7 -119.5(3) . . . . ? Co1A Co1 N3 C7 124.0(3) . . . . ? O1 N1 C2 C3 -173.2(3) . . . . ? Co1 N1 C2 C3 4.6(4) . . . . ? O1 N1 C2 C1 1.4(5) . . . . ? Co1 N1 C2 C1 179.3(3) . . . . ? C5 N2 C3 C2 170.2(3) . . . . ? Co1 N2 C3 C2 -9.0(4) . . . . ? C5 N2 C3 C4 -9.8(5) . . . . ? Co1 N2 C3 C4 171.0(3) . . . . ? N1 C2 C3 N2 3.0(4) . . . . ? C1 C2 C3 N2 -171.6(3) . . . . ? N1 C2 C3 C4 -177.0(3) . . . . ? C1 C2 C3 C4 8.4(5) . . . . ? C3 N2 C5 C6 -145.8(4) . . . . ? Co1 N2 C5 C6 33.3(4) . . . . ? N2 C5 C6 C7 -69.7(4) . . . . ? C11 N3 C7 C8 -0.2(5) . . . . ? Co1 N3 C7 C8 -179.6(3) . . . . ? C11 N3 C7 C6 179.2(3) . . . . ? Co1 N3 C7 C6 -0.3(5) . . . . ? C5 C6 C7 N3 53.3(5) . . . . ? C5 C6 C7 C8 -127.4(4) . . . . ? N3 C7 C8 C9 1.5(7) . . . . ? C6 C7 C8 C9 -177.9(5) . . . . ? C7 C8 C9 C10 -2.3(9) . . . . ? C8 C9 C10 C11 1.7(8) . . . . ? C7 N3 C11 C10 -0.4(6) . . . . ? Co1 N3 C11 C10 179.1(3) . . . . ? C9 C10 C11 N3 -0.4(7) . . . . ? N1 Co1 C12 C13 -113.8(3) . . . . ? N2 Co1 C12 C13 -32.4(3) . . . . ? O2H Co1 C12 C13 156.9(3) . . . . ? N3 Co1 C12 C13 63.5(3) . . . . ? O1A Co1 C12 C13 158.7(11) . . . . ? Co1A Co1 C12 C13 -173.4(3) . . . . ? Co1 C12 C13 F1 -54.7(5) . . . . ? Co1 C12 C13 F2 68.8(4) . . . . ? Co1 C12 C13 F3 -172.7(2) . . . . ? Co1 O2H Co1A N1A 39.55(12) . . . . ? Co1 O2H Co1A N2A 35.9(6) . . . . ? Co1 O2H Co1A N3A -138.18(11) . . . . ? Co1 O2H Co1A C12A 127.98(14) . . . . ? Co1 O2H Co1A O1 -49.21(10) . . . . ? Co1 O2H Co1A Co1 0.0 . . . . ? N1 O1 Co1A N1A -43.3(2) . . . . ? N1 O1 Co1A N2A -124.5(2) . . . . ? N1 O1 Co1A O2H 45.2(2) . . . . ? N1 O1 Co1A N3A 139.9(2) . . . . ? N1 O1 Co1A C12A 20.7(12) . . . . ? N1 O1 Co1A Co1 14.6(2) . . . . ? N1 Co1 Co1A N1A 93.15(13) . . . . ? N2 Co1 Co1A N1A 53.0(2) . . . . ? O2H Co1 Co1A N1A -133.29(15) . . . . ? N3 Co1 Co1A N1A -83.09(14) . . . . ? O1A Co1 Co1A N1A -11.81(13) . . . . ? C12 Co1 Co1A N1A 171.2(2) . . . . ? N1 Co1 Co1A N2A 54.87(15) . . . . ? N2 Co1 Co1A N2A 14.7(2) . . . . ? O2H Co1 Co1A N2A -171.6(2) . . . . ? N3 Co1 Co1A N2A -121.4(2) . . . . ? O1A Co1 Co1A N2A -50.09(15) . . . . ? C12 Co1 Co1A N2A 132.9(2) . . . . ? N1 Co1 Co1A O2H -133.55(14) . . . . ? N2 Co1 Co1A O2H -173.7(2) . . . . ? O2H Co1 Co1A O2H 0.0 . . . . ? N3 Co1 Co1A O2H 50.20(15) . . . . ? O1A Co1 Co1A O2H 121.48(13) . . . . ? C12 Co1 Co1A O2H -55.5(2) . . . . ? N1 Co1 Co1A N3A -82.93(13) . . . . ? N2 Co1 Co1A N3A -123.1(2) . . . . ? O2H Co1 Co1A N3A 50.63(14) . . . . ? N3 Co1 Co1A N3A 100.83(14) . . . . ? O1A Co1 Co1A N3A 172.11(12) . . . . ? C12 Co1 Co1A N3A -4.89(15) . . . . ? N1 Co1 Co1A C12A 169.63(15) . . . . ? N2 Co1 Co1A C12A 129.5(2) . . . . ? O2H Co1 Co1A C12A -56.8(2) . . . . ? N3 Co1 Co1A C12A -6.6(2) . . . . ? O1A Co1 Co1A C12A 64.66(15) . . . . ? C12 Co1 Co1A C12A -112.3(2) . . . . ? N1 Co1 Co1A O1 -11.14(12) . . . . ? N2 Co1 Co1A O1 -51.30(14) . . . . ? O2H Co1 Co1A O1 122.42(13) . . . . ? N3 Co1 Co1A O1 172.62(13) . . . . ? O1A Co1 Co1A O1 -116.10(11) . . . . ? C12 Co1 Co1A O1 66.90(14) . . . . ? N1 Co1 O1A N1A -42.9(2) . . . . ? N2 Co1 O1A N1A -124.3(2) . . . . ? O2H Co1 O1A N1A 46.4(2) . . . . ? N3 Co1 O1A N1A 140.0(2) . . . . ? C12 Co1 O1A N1A 44.6(13) . . . . ? Co1A Co1 O1A N1A 15.5(2) . . . . ? Co1 O1A N1A C2A 150.3(3) . . . . ? Co1 O1A N1A Co1A -27.5(3) . . . . ? N2A Co1A N1A C2A -5.5(3) . . . . ? O2H Co1A N1A C2A 175.2(3) . . . . ? N3A Co1A N1A C2A -41.3(18) . . . . ? C12A Co1A N1A C2A 87.4(3) . . . . ? O1 Co1A N1A C2A -98.7(3) . . . . ? Co1 Co1A N1A C2A -158.9(3) . . . . ? N2A Co1A N1A O1A 172.4(3) . . . . ? O2H Co1A N1A O1A -6.9(2) . . . . ? N3A Co1A N1A O1A 136.6(16) . . . . ? C12A Co1A N1A O1A -94.7(3) . . . . ? O1 Co1A N1A O1A 79.2(2) . . . . ? Co1 Co1A N1A O1A 19.0(2) . . . . ? N1A Co1A N2A C3A 6.1(3) . . . . ? O2H Co1A N2A C3A 9.8(8) . . . . ? N3A Co1A N2A C3A -176.2(3) . . . . ? C12A Co1A N2A C3A -81.9(3) . . . . ? O1 Co1A N2A C3A 94.3(3) . . . . ? Co1 Co1A N2A C3A 39.3(3) . . . . ? N1A Co1A N2A C5A -171.3(3) . . . . ? O2H Co1A N2A C5A -167.6(5) . . . . ? N3A Co1A N2A C5A 6.5(3) . . . . ? C12A Co1A N2A C5A 100.8(3) . . . . ? O1 Co1A N2A C5A -83.1(3) . . . . ? Co1 Co1A N2A C5A -138.0(2) . . . . ? N1A Co1A N3A C11A -170.6(16) . . . . ? N2A Co1A N3A C11A 153.9(3) . . . . ? O2H Co1A N3A C11A -27.2(3) . . . . ? C12A Co1A N3A C11A 60.9(3) . . . . ? O1 Co1A N3A C11A -113.2(3) . . . . ? Co1 Co1A N3A C11A -55.0(3) . . . . ? N1A Co1A N3A C7A 6.5(18) . . . . ? N2A Co1A N3A C7A -29.0(3) . . . . ? O2H Co1A N3A C7A 149.9(2) . . . . ? C12A Co1A N3A C7A -122.0(3) . . . . ? O1 Co1A N3A C7A 64.0(2) . . . . ? Co1 Co1A N3A C7A 122.2(2) . . . . ? O1A N1A C2A C3A -174.1(3) . . . . ? Co1A N1A C2A C3A 3.8(4) . . . . ? O1A N1A C2A C1A 2.0(5) . . . . ? Co1A N1A C2A C1A 179.9(3) . . . . ? C5A N2A C3A C2A 171.6(3) . . . . ? Co1A N2A C3A C2A -5.7(4) . . . . ? C5A N2A C3A C4A -5.7(6) . . . . ? Co1A N2A C3A C4A 177.0(3) . . . . ? N1A C2A C3A N2A 1.3(5) . . . . ? C1A C2A C3A N2A -174.5(4) . . . . ? N1A C2A C3A C4A 178.7(3) . . . . ? C1A C2A C3A C4A 2.9(6) . . . . ? C3A N2A C5A C6A -140.5(3) . . . . ? Co1A N2A C5A C6A 36.7(4) . . . . ? N2A C5A C6A C7A -72.2(4) . . . . ? C11A N3A C7A C8A 0.3(5) . . . . ? Co1A N3A C7A C8A -176.9(3) . . . . ? C11A N3A C7A C6A -179.4(3) . . . . ? Co1A N3A C7A C6A 3.4(4) . . . . ? C5A C6A C7A N3A 51.3(4) . . . . ? C5A C6A C7A C8A -128.3(3) . . . . ? N3A C7A C8A C9A 1.0(5) . . . . ? C6A C7A C8A C9A -179.3(3) . . . . ? C7A C8A C9A C10A -1.0(6) . . . . ? C8A C9A C10A C11A -0.2(6) . . . . ? C7A N3A C11A C10A -1.5(5) . . . . ? Co1A N3A C11A C10A 175.7(3) . . . . ? C9A C10A C11A N3A 1.5(6) . . . . ? N1A Co1A C12A C13A -133.9(4) . . . . ? N2A Co1A C12A C13A -52.7(4) . . . . ? O2H Co1A C12A C13A 137.6(4) . . . . ? N3A Co1A C12A C13A 43.1(4) . . . . ? O1 Co1A C12A C13A 162.0(9) . . . . ? Co1 Co1A C12A C13A 167.8(3) . . . . ? Co1A C12A C13A F3A -59.0(5) . . . . ? Co1A C12A C13A F2A 61.0(5) . . . . ? Co1A C12A C13A F1A -179.5(3) . . . . ? _refine_diff_density_max 0.453 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.069 # == == == END data_2e _database_code_CSD 157413 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34.33 H52.33 Cl Co2 N6 O7.34' _chemical_formula_weight 819.85 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'H' 'H' 0.0000 0.0000 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 9.765(2) _cell_length_b 20.296(3) _cell_length_c 19.717(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.14(2) _cell_angle_gamma 90.00 _cell_volume 3877.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.6 mm _exptl_crystal_size_mid 0.4 mm _exptl_crystal_size_min 0.2 mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method ? _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7021 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.1546 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6817 _reflns_number_observed 3198 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criteri= on of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.0747P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6817 _refine_ls_number_parameters 462 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2007 _refine_ls_R_factor_obs 0.0693 _refine_ls_wR_factor_all 0.1648 _refine_ls_wR_factor_obs 0.1410 _refine_ls_goodness_of_fit_all 0.910 _refine_ls_goodness_of_fit_obs 1.181 _refine_ls_restrained_S_all 0.910 _refine_ls_restrained_S_obs 1.181 _refine_ls_shift/esd_max 0.082 _refine_ls_shift/esd_mean 0.007 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.33000(8) 0.16289(4) 0.34041(4) 0.0413(3) Uani 1 d . . N1 N 0.1590(5) 0.1251(3) 0.3506(3) 0.0453(13) Uani 1 d . . N2 N 0.3764(6) 0.1261(3) 0.4284(3) 0.0491(14) Uani 1 d . . N3 N 0.5144(5) 0.1976(3) 0.3307(3) 0.0439(13) Uani 1 d . . O1 O 0.0546(4) 0.1264(2) 0.3014(2) 0.0494(11) Uani 1 d . . O2H O 0.2649(4) 0.18643(19) 0.2473(2) 0.0416(11) Uani 1 d D . H H 0.2164 0.2290 0.2465 0.050 Uiso 1 d D . C1 C 0.0245(7) 0.0539(4) 0.4186(4) 0.069(2) Uani 1 d . . H1A H 0.0496 0.0092 0.4302 0.104 Uiso 1 calc R . H1B H -0.0406 0.0545 0.3778 0.104 Uiso 1 calc R . H1C H -0.0166 0.0738 0.4554 0.104 Uiso 1 calc R . C2 C 0.1504(7) 0.0918(3) 0.4066(3) 0.0504(18) Uani 1 d . . C3 C 0.2785(7) 0.0937(3) 0.4520(3) 0.0496(18) Uani 1 d . . C4 C 0.2880(8) 0.0562(4) 0.5179(4) 0.077(2) Uani 1 d . . H4A H 0.3758 0.0646 0.5442 0.115 Uiso 1 calc R . H4B H 0.2790 0.0099 0.5084 0.115 Uiso 1 calc R . H4C H 0.2154 0.0702 0.5433 0.115 Uiso 1 calc R . C5 C 0.5191(7) 0.1282(4) 0.4624(3) 0.061(2) Uani 1 d . . H5A H 0.5316 0.0949 0.4979 0.074 Uiso 1 calc R . H5B H 0.5371 0.1709 0.4838 0.074 Uiso 1 calc R . C6 C 0.6200(7) 0.1162(4) 0.4110(3) 0.0570(19) Uani 1 d . . H6A H 0.7102 0.1068 0.4356 0.068 Uiso 1 calc R . H6B H 0.5906 0.0777 0.3841 0.068 Uiso 1 calc R . C7 C 0.6327(7) 0.1724(3) 0.3642(3) 0.0472(17) Uani 1 d . . C8 C 0.7595(7) 0.1983(4) 0.3542(4) 0.070(2) Uani 1 d . . H8 H 0.8394 0.1810 0.3782 0.084 Uiso 1 calc R . C9 C 0.7692(8) 0.2485(4) 0.3101(4) 0.075(2) Uani 1 d . . H9 H 0.8550 0.2653 0.3033 0.090 Uiso 1 calc R . C10 C 0.6513(7) 0.2743(4) 0.2754(4) 0.061(2) Uani 1 d . . H10 H 0.6551 0.3087 0.2445 0.074 Uiso 1 calc R . C11 C 0.5282(7) 0.2481(3) 0.2874(3) 0.0516(18) Uani 1 d . . H11 H 0.4482 0.2662 0.2642 0.062 Uiso 1 calc R . C12 C 0.2684(7) 0.2482(4) 0.3790(4) 0.060(2) Uani 1 d . . H12 H 0.2191 0.2270 0.4134 0.072 Uiso 1 calc R . C13 C 0.1499(9) 0.2773(5) 0.3439(6) 0.127(5) Uani 1 d . . H13A H 0.0785 0.2438 0.3376 0.152 Uiso 1 calc R . H13B H 0.1709 0.2896 0.2987 0.152 Uiso 1 calc R . C14 C 0.0900(8) 0.3370(4) 0.3751(5) 0.086(3) Uani 1 d . . H14A H 0.0535 0.3663 0.3384 0.103 Uiso 1 calc R . H14B H 0.0129 0.3226 0.3980 0.103 Uiso 1 calc R . C15 C 0.1815(11) 0.3741(6) 0.4228(8) 0.186(8) Uani 1 d . . H15A H 0.2101 0.4123 0.3986 0.224 Uiso 1 calc R . H15B H 0.1277 0.3903 0.4575 0.224 Uiso 1 calc R . C16 C 0.2975(10) 0.3463(4) 0.4559(5) 0.103(3) Uani 1 d . . H16A H 0.2785 0.3359 0.5018 0.124 Uiso 1 calc R . H16B H 0.3685 0.3800 0.4602 0.124 Uiso 1 calc R . C17 C 0.3589(8) 0.2858(4) 0.4281(4) 0.083(3) Uani 1 d . . H17A H 0.4390 0.2990 0.4068 0.100 Uiso 1 calc R . H17B H 0.3911 0.2572 0.4662 0.100 Uiso 1 calc R . Cl Cl 0.9167(2) 0.16596(15) 0.58366(13) 0.0876(7) Uani 1 d . . O3 O 0.9728(11) 0.1935(5) 0.5312(4) 0.197(4) Uani 1 d . . O4 O 0.8115(8) 0.1240(6) 0.5624(4) 0.205(5) Uani 1 d . . O5 O 0.8975(10) 0.2057(5) 0.6372(4) 0.201(5) Uani 1 d . . O6 O 1.0225(9) 0.1228(4) 0.6156(5) 0.179(4) Uani 1 d . . Co1A Co 0.14118(9) 0.11856(5) 0.21172(4) 0.0457(3) Uani 1 d . . N1A N 0.2631(6) 0.0566(3) 0.2556(3) 0.0505(14) Uani 1 d . . N2A N 0.0330(6) 0.0427(3) 0.1899(3) 0.0575(16) Uani 1 d . . N3A N 0.0040(5) 0.1827(3) 0.1703(3) 0.0484(15) Uani 1 d . . O1A O 0.3784(4) 0.0738(2) 0.2941(2) 0.0567(13) Uani 1 d . . C1A C 0.3016(10) -0.0578(4) 0.2906(4) 0.093(3) Uani 1 d . . H1A1 H 0.3784 -0.0395 0.3197 0.139 Uiso 1 calc R . H1A2 H 0.3348 -0.0877 0.2586 0.139 Uiso 1 calc R . H1A3 H 0.2428 -0.0811 0.3180 0.139 Uiso 1 calc R . C2A C 0.2229(8) -0.0044(4) 0.2533(4) 0.058(2) Uani 1 d . . C3A C 0.0865(9) -0.0111(4) 0.2155(4) 0.061(2) Uani 1 d . . C4A C 0.0167(9) -0.0772(4) 0.2116(4) 0.088(3) Uani 1 d . . H4A1 H -0.0393 -0.0812 0.2481 0.132 Uiso 1 calc R . H4A2 H 0.0853 -0.1114 0.2156 0.132 Uiso 1 calc R . H4A3 H -0.0404 -0.0813 0.1685 0.132 Uiso 1 calc R . C5A C -0.1096(8) 0.0464(4) 0.1565(4) 0.079(3) Uani 1 d . . H5A1 H -0.1584 0.0064 0.1656 0.095 Uiso 1 calc R . H5A2 H -0.1097 0.0503 0.1075 0.095 Uiso 1 calc R . C6A C -0.1831(7) 0.1057(4) 0.1829(4) 0.074(2) Uani 1 d . . H6A1 H -0.2809 0.1019 0.1671 0.089 Uiso 1 calc R . H6A2 H -0.1723 0.1038 0.2324 0.089 Uiso 1 calc R . C7A C -0.1344(7) 0.1712(4) 0.1620(3) 0.058(2) Uani 1 d . . C8A C -0.2245(8) 0.2190(5) 0.1343(4) 0.076(3) Uani 1 d . . H8A H -0.3184 0.2096 0.1270 0.091 Uiso 1 calc R . C9A C -0.1802(10) 0.2793(5) 0.1174(4) 0.086(3) Uani 1 d . . H9A H -0.2429 0.3113 0.0997 0.103 Uiso 1 calc R . C10A C -0.0417(9) 0.2924(4) 0.1268(3) 0.070(2) Uani 1 d . . H10A H -0.0075 0.3333 0.1158 0.083 Uiso 1 calc R . C11A C 0.0459(7) 0.2425(4) 0.1534(3) 0.0567(19) Uani 1 d . . H11A H 0.1401 0.2512 0.1599 0.068 Uiso 1 calc R . C12A C 0.2322(7) 0.1168(4) 0.1245(3) 0.0586(19) Uani 1 d . . H12A H 0.2531 0.1633 0.1169 0.070 Uiso 1 calc R . C13A C 0.3685(8) 0.0842(5) 0.1271(4) 0.087(3) Uani 1 d . . H13C H 0.3577 0.0376 0.1359 0.104 Uiso 1 calc R . H13D H 0.4301 0.1024 0.1649 0.104 Uiso 1 calc R . C14A C 0.4347(9) 0.0923(6) 0.0613(4) 0.102(3) Uani 1 d . . H14C H 0.4626 0.1378 0.0574 0.122 Uiso 1 calc R . H14D H 0.5171 0.0652 0.0642 0.122 Uiso 1 calc R . C15A C 0.3400(9) 0.0735(5) -0.0021(4) 0.095(3) Uani 1 d . . H15C H 0.3822 0.0861 -0.0422 0.114 Uiso 1 calc R . H15D H 0.3276 0.0260 -0.0031 0.114 Uiso 1 calc R . C16A C 0.2047(10) 0.1056(6) -0.0043(4) 0.112(4) Uani 1 d . . H16C H 0.1431 0.0871 -0.0419 0.134 Uiso 1 calc R . H16D H 0.2153 0.1521 -0.0135 0.134 Uiso 1 calc R . C17A C 0.1381(8) 0.0982(5) 0.0612(4) 0.092(3) Uani 1 d . . H17C H 0.0562 0.1257 0.0581 0.110 Uiso 1 calc R . H17D H 0.1091 0.0528 0.0654 0.110 Uiso 1 calc R . C181 C 0.6103(33) 0.0085(16) 0.2515(16) 0.163(9) Uiso 0.17 d PD . O71 O 0.6103(33) 0.0085(16) 0.2515(16) 0.163(9) Uiso 0.17 d P . O72 O 0.6754(32) -0.0421(15) 0.2884(16) 0.163(9) Uiso 0.17 d PD . C182 C 0.6754(32) -0.0421(15) 0.2884(16) 0.163(9) Uiso 0.17 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0359(5) 0.0472(5) 0.0392(5) 0.0027(5) -0.0013(4) 0.0037(5) N1 0.042(3) 0.042(3) 0.051(3) -0.002(3) 0.003(3) 0.008(3) N2 0.050(3) 0.049(4) 0.046(3) 0.005(3) -0.004(3) 0.003(3) N3 0.032(3) 0.049(3) 0.048(3) 0.003(3) -0.007(2) 0.003(3) O1 0.040(2) 0.061(3) 0.045(3) 0.000(2) -0.002(2) 0.000(2) O2H 0.036(2) 0.040(3) 0.047(2) -0.001(2) -0.004(2) 0.0018(19) C1 0.067(5) 0.065(5) 0.078(5) 0.013(4) 0.014(4) -0.006(4) C2 0.055(4) 0.051(4) 0.044(4) 0.008(3) 0.004(3) 0.004(4) C3 0.057(4) 0.054(5) 0.038(4) 0.005(3) 0.009(3) 0.013(4) C4 0.089(6) 0.082(6) 0.060(5) 0.023(5) 0.015(4) 0.003(5) C5 0.055(4) 0.082(6) 0.043(4) 0.012(4) -0.013(3) 0.016(4) C6 0.045(4) 0.072(5) 0.051(4) 0.008(4) -0.007(3) 0.019(4) C7 0.043(4) 0.055(5) 0.041(4) 0.001(3) -0.006(3) 0.003(4) C8 0.026(4) 0.092(6) 0.086(6) 0.005(5) -0.011(4) 0.012(4) C9 0.039(4) 0.081(6) 0.102(6) 0.006(5) 0.000(4) 0.002(4) C10 0.043(4) 0.068(5) 0.073(5) 0.010(4) 0.007(4) -0.006(4) C11 0.044(4) 0.062(5) 0.047(4) 0.007(4) 0.000(3) 0.002(4) C12 0.052(4) 0.058(5) 0.064(5) -0.014(4) -0.016(4) 0.013(4) C13 0.081(6) 0.097(7) 0.181(10) -0.075(7) -0.067(7) 0.052(6) C14 0.054(5) 0.075(6) 0.126(8) -0.030(6) 0.001(5) 0.020(5) C15 0.084(7) 0.151(11) 0.303(18) -0.157(12) -0.064(10) 0.049(8) C16 0.112(8) 0.074(7) 0.113(8) -0.048(6) -0.023(6) 0.013(6) C17 0.069(5) 0.096(7) 0.080(6) -0.033(5) -0.006(5) 0.013(5) Cl 0.0759(15) 0.113(2) 0.0724(15) -0.0199(16) 0.0022(12) -0.0075(16) O3 0.235(10) 0.244(11) 0.115(7) 0.027(7) 0.031(7) -0.054(9) O4 0.130(7) 0.357(14) 0.116(6) -0.020(7) -0.026(5) -0.130(8) O5 0.216(10) 0.239(10) 0.140(7) -0.102(7) -0.010(7) 0.082(8) O6 0.124(6) 0.156(8) 0.251(11) 0.015(8) 0.003(7) 0.028(6) Co1A 0.0423(5) 0.0491(6) 0.0439(5) -0.0032(5) -0.0014(4) -0.0008(5) N1A 0.059(4) 0.044(4) 0.048(3) -0.001(3) 0.007(3) 0.005(3) N2A 0.058(4) 0.059(4) 0.056(4) -0.012(3) 0.006(3) -0.007(3) N3A 0.039(3) 0.067(4) 0.037(3) -0.007(3) -0.004(2) -0.002(3) O1A 0.051(3) 0.057(3) 0.059(3) -0.002(2) -0.005(2) 0.006(2) C1A 0.122(8) 0.059(6) 0.095(7) 0.007(5) 0.007(6) 0.013(6) C2A 0.074(5) 0.046(5) 0.055(5) 0.000(4) 0.009(4) 0.010(4) C3A 0.079(6) 0.051(5) 0.057(5) -0.012(4) 0.023(4) -0.008(4) C4A 0.107(7) 0.057(5) 0.102(7) -0.015(5) 0.019(6) -0.028(5) C5A 0.068(5) 0.075(6) 0.087(6) -0.013(5) -0.016(5) -0.026(5) C6A 0.044(4) 0.089(7) 0.086(6) -0.015(5) -0.006(4) -0.008(5) C7A 0.048(4) 0.076(6) 0.048(4) -0.013(4) -0.002(3) -0.005(4) C8A 0.043(4) 0.120(8) 0.060(5) -0.017(6) -0.014(4) 0.022(5) C9A 0.077(7) 0.101(8) 0.073(6) 0.000(6) -0.018(5) 0.038(6) C10A 0.076(6) 0.078(6) 0.053(5) 0.020(4) -0.001(4) 0.017(5) C11A 0.052(4) 0.064(5) 0.053(4) 0.003(4) -0.001(4) 0.002(4) C12A 0.052(4) 0.069(5) 0.053(4) -0.007(4) -0.002(3) 0.006(4) C13A 0.065(5) 0.143(8) 0.052(5) 0.006(5) 0.006(4) 0.015(6) C14A 0.074(6) 0.176(10) 0.058(5) -0.007(6) 0.019(5) 0.015(6) C15A 0.086(7) 0.146(9) 0.059(5) -0.015(6) 0.033(5) 0.004(7) C16A 0.094(7) 0.196(12) 0.044(5) -0.020(6) 0.003(5) 0.010(8) C17A 0.053(5) 0.165(10) 0.056(5) -0.034(6) 0.006(4) -0.015(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 N1 1.8707(52) . ? Co1 N2 1.8910(51) . ? Co1 O2H 1.9267(40) . ? Co1 N3 1.9654(50) . ? Co1 C12 2.0133(67) . ? Co1 O1A 2.1061(47) . ? Co1 Co1A 3.0797(13) . ? N1 C2 1.3055(76) . ? N1 O1 1.3165(56) . ? N2 C3 1.2940(80) . ? N2 C5 1.4711(74) . ? N3 C11 1.3516(76) . ? N3 C7 1.3576(71) . ? O1 Co1A 2.0596(42) . ? O2H Co1A 1.9074(39) . ? C1 C2 1.4940(90) . ? C2 C3 1.4458(86) . ? C3 C4 1.4975(86) . ? C5 C6 1.5188(88) . ? C6 C7 1.4816(87) . ? C7 C8 1.3818(90) . ? C8 C9 1.3496(101) . ? C9 C10 1.3683(90) . ? C10 C11 1.3619(86) . ? C12 C13 1.4026(88) . ? C12 C17 1.4457(89) . ? C13 C14 1.5106(100) . ? C14 C15 1.4272(107) . ? C15 C16 1.3579(117) . ? C16 C17 1.4987(102) . ? Cl O3 1.3510(88) . ? Cl O5 1.3610(75) . ? Cl O4 1.3605(74) . ? Cl O6 1.4381(84) . ? Co1A N1A 1.8684(54) . ? Co1A N2A 1.8873(57) . ? Co1A N3A 1.9706(54) . ? Co1A C12A 2.0321(69) . ? N1A C2A 1.2984(81) . ? N1A O1A 1.3235(60) . ? N2A C3A 1.2849(86) . ? N2A C5A 1.4660(85) . ? N3A C11A 1.3360(80) . ? N3A C7A 1.3612(79) . ? C1A C2A 1.4725(96) . ? C2A C3A 1.4492(99) . ? C3A C4A 1.5035(97) . ? C5A C6A 1.5243(99) . ? C6A C7A 1.4891(100) . ? C7A C8A 1.3750(99) . ? C8A C9A 1.3543(112) . ? C9A C10A 1.3687(106) . ? C10A C11A 1.3856(91) . ? C12A C13A 1.4820(94) . ? C12A C17A 1.5027(87) . ? C13A C14A 1.5280(99) . ? C14A C15A 1.5088(104) . ? C15A C16A 1.4690(110) . ? C16A C17A 1.5247(102) . ? C181 C182 1.3695(181) . ? C181 O72 1.3695(181) . ? O71 C182 1.3695(181) . ? O71 O72 1.3695(181) . ? 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 N1 Co1 N2 81.6(2) . . ? N1 Co1 O2H 90.6(2) . . ? N2 Co1 O2H 170.0(2) . . ? N1 Co1 N3 176.7(2) . . ? N2 Co1 N3 96.5(2) . . ? O2H Co1 N3 90.93(19) . . ? N1 Co1 C12 90.0(3) . . ? N2 Co1 C12 92.4(3) . . ? O2H Co1 C12 93.9(2) . . ? N3 Co1 C12 92.8(3) . . ? N1 Co1 O1A 86.9(2) . . ? N2 Co1 O1A 91.0(2) . . ? O2H Co1 O1A 82.23(17) . . ? N3 Co1 O1A 90.5(2) . . ? C12 Co1 O1A 175.0(2) . . ? N1 Co1 Co1A 61.14(16) . . ? N2 Co1 Co1A 133.67(17) . . ? O2H Co1 Co1A 36.35(12) . . ? N3 Co1 Co1A 119.12(15) . . ? C12 Co1 Co1A 112.72(18) . . ? O1A Co1 Co1A 62.31(11) . . ? C2 N1 O1 120.5(5) . . ? C2 N1 Co1 117.1(4) . . ? O1 N1 Co1 122.2(4) . . ? C3 N2 C5 123.5(5) . . ? C3 N2 Co1 115.3(4) . . ? C5 N2 Co1 120.8(4) . . ? C11 N3 C7 116.6(6) . . ? C11 N3 Co1 119.9(4) . . ? C7 N3 Co1 123.5(4) . . ? N1 O1 Co1A 105.5(3) . . ? Co1A O2H Co1 106.88(19) . . ? N1 C2 C3 111.7(6) . . ? N1 C2 C1 122.8(6) . . ? C3 C2 C1 125.5(6) . . ? N2 C3 C2 114.2(6) . . ? N2 C3 C4 126.9(6) . . ? C2 C3 C4 118.7(7) . . ? N2 C5 C6 110.3(5) . . ? C7 C6 C5 113.8(6) . . ? N3 C7 C8 120.7(6) . . ? N3 C7 C6 117.5(6) . . ? C8 C7 C6 121.9(6) . . ? C9 C8 C7 121.0(7) . . ? C8 C9 C10 119.3(7) . . ? C11 C10 C9 118.0(7) . . ? N3 C11 C10 124.4(6) . . ? C13 C12 C17 120.5(7) . . ? C13 C12 Co1 116.2(5) . . ? C17 C12 Co1 121.4(5) . . ? C12 C13 C14 118.3(7) . . ? C15 C14 C13 116.7(7) . . ? C16 C15 C14 121.0(9) . . ? C15 C16 C17 120.8(8) . . ? C12 C17 C16 116.0(7) . . ? O3 Cl O5 117.2(7) . . ? O3 Cl O4 112.7(6) . . ? O5 Cl O4 116.1(7) . . ? O3 Cl O6 104.5(6) . . ? O5 Cl O6 100.5(6) . . ? O4 Cl O6 103.1(6) . . ? N1A Co1A N2A 82.1(3) . . ? N1A Co1A O2H 88.7(2) . . ? N2A Co1A O2H 169.9(2) . . ? N1A Co1A N3A 176.0(2) . . ? N2A Co1A N3A 96.5(3) . . ? O2H Co1A N3A 92.4(2) . . ? N1A Co1A C12A 93.4(3) . . ? N2A Co1A C12A 94.8(3) . . ? O2H Co1A C12A 90.0(2) . . ? N3A Co1A C12A 90.4(3) . . ? N1A Co1A O1 87.7(2) . . ? N2A Co1A O1 88.9(2) . . ? O2H Co1A O1 86.37(17) . . ? N3A Co1A O1 88.50(19) . . ? C12A Co1A O1 176.2(3) . . ? N1A Co1A Co1 62.16(18) . . ? N2A Co1A Co1 133.41(19) . . ? O2H Co1A Co1 36.77(12) . . ? N3A Co1A Co1 117.04(15) . . ? C12A Co1A Co1 114.97(19) . . ? O1 Co1A Co1 62.44(11) . . ? C2A N1A O1A 120.2(6) . . ? C2A N1A Co1A 116.9(5) . . ? O1A N1A Co1A 122.4(4) . . ? C3A N2A C5A 122.6(7) . . ? C3A N2A Co1A 114.4(5) . . ? C5A N2A Co1A 122.2(5) . . ? C11A N3A C7A 117.1(6) . . ? C11A N3A Co1A 119.4(4) . . ? C7A N3A Co1A 123.4(5) . . ? N1A O1A Co1 104.7(3) . . ? N1A C2A C3A 111.2(7) . . ? N1A C2A C1A 123.2(7) . . ? C3A C2A C1A 125.3(8) . . ? N2A C3A C2A 115.2(7) . . ? N2A C3A C4A 125.3(8) . . ? C2A C3A C4A 119.4(8) . . ? N2A C5A C6A 110.4(6) . . ? C7A C6A C5A 115.5(7) . . ? N3A C7A C8A 120.3(8) . . ? N3A C7A C6A 117.7(7) . . ? C8A C7A C6A 122.0(7) . . ? C9A C8A C7A 121.8(8) . . ? C8A C9A C10A 118.8(8) . . ? C9A C10A C11A 117.5(8) . . ? N3A C11A C10A 124.4(7) . . ? C13A C12A C17A 111.8(6) . . ? C13A C12A Co1A 117.6(5) . . ? C17A C12A Co1A 114.8(5) . . ? C12A C13A C14A 113.2(7) . . ? C15A C14A C13A 113.4(7) . . ? C16A C15A C14A 111.6(7) . . ? C15A C16A C17A 114.1(8) . . ? C12A C17A C16A 113.4(6) . . ? C182 C181 O72 0.0(38) . . ? C182 O71 O72 0.0(38) . . ? O71 O72 C181 0.0(39) . . ? O71 C182 C181 0.0(39) . . ? 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 N2 Co1 N1 C2 -2.1(5) . . . . ? O2H Co1 N1 C2 171.5(5) . . . . ? N3 Co1 N1 C2 53.6(40) . . . . ? C12 Co1 N1 C2 -94.6(5) . . . . ? O1A Co1 N1 C2 89.3(5) . . . . ? Co1A Co1 N1 C2 149.2(5) . . . . ? N2 Co1 N1 O1 -176.2(5) . . . . ? O2H Co1 N1 O1 -2.6(4) . . . . ? N3 Co1 N1 O1 -120.5(37) . . . . ? C12 Co1 N1 O1 91.3(5) . . . . ? O1A Co1 N1 O1 -84.8(4) . . . . ? Co1A Co1 N1 O1 -24.9(4) . . . . ? N1 Co1 N2 C3 1.2(5) . . . . ? O2H Co1 N2 C3 -38.3(15) . . . . ? N3 Co1 N2 C3 -176.0(5) . . . . ? C12 Co1 N2 C3 90.9(5) . . . . ? O1A Co1 N2 C3 -85.5(5) . . . . ? Co1A Co1 N2 C3 -34.2(6) . . . . ? N1 Co1 N2 C5 174.3(5) . . . . ? O2H Co1 N2 C5 134.8(11) . . . . ? N3 Co1 N2 C5 -3.0(5) . . . . ? C12 Co1 N2 C5 -96.0(5) . . . . ? O1A Co1 N2 C5 87.6(5) . . . . ? Co1A Co1 N2 C5 138.8(4) . . . . ? N1 Co1 N3 C11 147.8(37) . . . . ? N2 Co1 N3 C11 -156.8(5) . . . . ? O2H Co1 N3 C11 29.9(5) . . . . ? C12 Co1 N3 C11 -64.0(5) . . . . ? O1A Co1 N3 C11 112.2(5) . . . . ? Co1A Co1 N3 C11 54.0(5) . . . . ? N1 Co1 N3 C7 -30.3(41) . . . . ? N2 Co1 N3 C7 25.2(5) . . . . ? O2H Co1 N3 C7 -148.1(5) . . . . ? C12 Co1 N3 C7 117.9(5) . . . . ? O1A Co1 N3 C7 -65.9(5) . . . . ? Co1A Co1 N3 C7 -124.1(5) . . . . ? C2 N1 O1 Co1A -139.1(5) . . . . ? Co1 N1 O1 Co1A 34.8(5) . . . . ? N1 Co1 O2H Co1A -34.1(2) . . . . ? N2 Co1 O2H Co1A 5.0(13) . . . . ? N3 Co1 O2H Co1A 143.1(2) . . . . ? C12 Co1 O2H Co1A -124.1(3) . . . . ? O1A Co1 O2H Co1A 52.71(19) . . . . ? Co1A Co1 O2H Co1A 0.0 . . . . ? O1 N1 C2 C3 176.7(5) . . . . ? Co1 N1 C2 C3 2.5(7) . . . . ? O1 N1 C2 C1 0.0(10) . . . . ? Co1 N1 C2 C1 -174.2(5) . . . . ? C5 N2 C3 C2 -173.1(6) . . . . ? Co1 N2 C3 C2 -0.3(8) . . . . ? C5 N2 C3 C4 3.3(11) . . . . ? Co1 N2 C3 C4 176.2(6) . . . . ? N1 C2 C3 N2 -1.4(9) . . . . ? C1 C2 C3 N2 175.2(7) . . . . ? N1 C2 C3 C4 -178.2(6) . . . . ? C1 C2 C3 C4 -1.6(10) . . . . ? C3 N2 C5 C6 133.4(7) . . . . ? Co1 N2 C5 C6 -39.1(8) . . . . ? N2 C5 C6 C7 72.8(8) . . . . ? C11 N3 C7 C8 0.6(9) . . . . ? Co1 N3 C7 C8 178.8(5) . . . . ? C11 N3 C7 C6 -178.9(6) . . . . ? Co1 N3 C7 C6 -0.8(8) . . . . ? C5 C6 C7 N3 -51.5(8) . . . . ? C5 C6 C7 C8 129.0(7) . . . . ? N3 C7 C8 C9 -1.2(12) . . . . ? C6 C7 C8 C9 178.4(7) . . . . ? C7 C8 C9 C10 0.6(13) . . . . ? C8 C9 C10 C11 0.3(12) . . . . ? C7 N3 C11 C10 0.4(10) . . . . ? Co1 N3 C11 C10 -177.8(6) . . . . ? C9 C10 C11 N3 -0.9(11) . . . . ? N1 Co1 C12 C13 -58.6(8) . . . . ? N2 Co1 C12 C13 -140.2(8) . . . . ? O2H Co1 C12 C13 32.0(8) . . . . ? N3 Co1 C12 C13 123.2(8) . . . . ? O1A Co1 C12 C13 -6.8(36) . . . . ? Co1A Co1 C12 C13 -0.1(8) . . . . ? N1 Co1 C12 C17 137.0(7) . . . . ? N2 Co1 C12 C17 55.3(7) . . . . ? O2H Co1 C12 C17 -132.4(7) . . . . ? N3 Co1 C12 C17 -41.3(7) . . . . ? O1A Co1 C12 C17 -171.3(27) . . . . ? Co1A Co1 C12 C17 -164.6(6) . . . . ? C17 C12 C13 C14 -22.3(15) . . . . ? Co1 C12 C13 C14 173.0(7) . . . . ? C12 C13 C14 C15 22.6(16) . . . . ? C13 C14 C15 C16 -22.1(20) . . . . ? C14 C15 C16 C17 20.8(21) . . . . ? C13 C12 C17 C16 19.8(13) . . . . ? Co1 C12 C17 C16 -176.4(7) . . . . ? C15 C16 C17 C12 -18.7(16) . . . . ? Co1 O2H Co1A N1A -41.4(2) . . . . ? Co1 O2H Co1A N2A -16.1(14) . . . . ? Co1 O2H Co1A N3A 134.7(2) . . . . ? Co1 O2H Co1A C12A -134.8(3) . . . . ? Co1 O2H Co1A O1 46.40(19) . . . . ? Co1 O2H Co1A Co1 0.0 . . . . ? N1 O1 Co1A N1A 40.2(4) . . . . ? N1 O1 Co1A N2A 122.4(4) . . . . ? N1 O1 Co1A O2H -48.6(4) . . . . ? N1 O1 Co1A N3A -141.1(4) . . . . ? N1 O1 Co1A C12A -67.4(34) . . . . ? N1 O1 Co1A Co1 -19.3(3) . . . . ? N1 Co1 Co1A N1A -88.1(3) . . . . ? N2 Co1 Co1A N1A -47.2(3) . . . . ? O2H Co1 Co1A N1A 131.6(3) . . . . ? N3 Co1 Co1A N1A 88.1(3) . . . . ? C12 Co1 Co1A N1A -164.8(3) . . . . ? O1A Co1 Co1A N1A 14.5(2) . . . . ? N1 Co1 Co1A N2A -43.6(3) . . . . ? N2 Co1 Co1A N2A -2.7(4) . . . . ? O2H Co1 Co1A N2A 176.1(3) . . . . ? N3 Co1 Co1A N2A 132.7(3) . . . . ? C12 Co1 Co1A N2A -120.3(4) . . . . ? O1A Co1 Co1A N2A 59.0(3) . . . . ? N1 Co1 Co1A O2H 140.3(3) . . . . ? N2 Co1 Co1A O2H -178.8(3) . . . . ? O2H Co1 Co1A O2H 0.0 . . . . ? N3 Co1 Co1A O2H -43.5(3) . . . . ? C12 Co1 Co1A O2H 63.6(3) . . . . ? O1A Co1 Co1A O2H -117.1(2) . . . . ? N1 Co1 Co1A N3A 87.4(3) . . . . ? N2 Co1 Co1A N3A 128.4(3) . . . . ? O2H Co1 Co1A N3A -52.8(3) . . . . ? N3 Co1 Co1A N3A -96.3(3) . . . . ? C12 Co1 Co1A N3A 10.7(3) . . . . ? O1A Co1 Co1A N3A -169.9(2) . . . . ? N1 Co1 Co1A C12A -168.3(3) . . . . ? N2 Co1 Co1A C12A -127.3(3) . . . . ? O2H Co1 Co1A C12A 51.5(3) . . . . ? N3 Co1 Co1A C12A 8.0(3) . . . . ? C12 Co1 Co1A C12A 115.0(3) . . . . ? O1A Co1 Co1A C12A -65.6(3) . . . . ? N1 Co1 Co1A O1 14.9(2) . . . . ? N2 Co1 Co1A O1 55.8(3) . . . . ? O2H Co1 Co1A O1 -125.4(2) . . . . ? N3 Co1 Co1A O1 -168.9(2) . . . . ? C12 Co1 Co1A O1 -61.8(3) . . . . ? O1A Co1 Co1A O1 117.5(2) . . . . ? N2A Co1A N1A C2A -1.3(5) . . . . ? O2H Co1A N1A C2A 174.4(6) . . . . ? N3A Co1A N1A C2A 68.3(35) . . . . ? C12A Co1A N1A C2A -95.7(6) . . . . ? O1 Co1A N1A C2A 88.0(5) . . . . ? Co1 Co1A N1A C2A 147.8(6) . . . . ? N2A Co1A N1A O1A -173.8(5) . . . . ? O2H Co1A N1A O1A 1.9(5) . . . . ? N3A Co1A N1A O1A -104.2(33) . . . . ? C12A Co1A N1A O1A 91.8(5) . . . . ? O1 Co1A N1A O1A -84.5(5) . . . . ? Co1 Co1A N1A O1A -24.7(4) . . . . ? N1A Co1A N2A C3A 2.5(5) . . . . ? O2H Co1A N2A C3A -23.0(16) . . . . ? N3A Co1A N2A C3A -173.8(5) . . . . ? C12A Co1A N2A C3A 95.3(6) . . . . ? O1 Co1A N2A C3A -85.4(5) . . . . ? Co1 Co1A N2A C3A -36.3(6) . . . . ? N1A Co1A N2A C5A 172.6(6) . . . . ? O2H Co1A N2A C5A 147.1(11) . . . . ? N3A Co1A N2A C5A -3.6(6) . . . . ? C12A Co1A N2A C5A -94.6(6) . . . . ? O1 Co1A N2A C5A 84.8(6) . . . . ? Co1 Co1A N2A C5A 133.9(5) . . . . ? N1A Co1A N3A C11A 131.8(33) . . . . ? N2A Co1A N3A C11A -159.1(5) . . . . ? O2H Co1A N3A C11A 25.8(5) . . . . ? C12A Co1A N3A C11A -64.2(5) . . . . ? O1 Co1A N3A C11A 112.1(5) . . . . ? Co1 Co1A N3A C11A 54.3(5) . . . . ? N1A Co1A N3A C7A -43.5(36) . . . . ? N2A Co1A N3A C7A 25.5(5) . . . . ? O2H Co1A N3A C7A -149.5(5) . . . . ? C12A Co1A N3A C7A 120.4(5) . . . . ? O1 Co1A N3A C7A -63.2(5) . . . . ? Co1 Co1A N3A C7A -121.0(5) . . . . ? C2A N1A O1A Co1 -138.3(6) . . . . ? Co1A N1A O1A Co1 34.0(5) . . . . ? N1 Co1 O1A N1A 40.0(4) . . . . ? N2 Co1 O1A N1A 121.6(4) . . . . ? O2H Co1 O1A N1A -51.0(4) . . . . ? N3 Co1 O1A N1A -141.9(4) . . . . ? C12 Co1 O1A N1A -11.9(32) . . . . ? Co1A Co1 O1A N1A -18.9(3) . . . . ? O1A N1A C2A C3A 172.6(5) . . . . ? Co1A N1A C2A C3A 0.0(8) . . . . ? O1A N1A C2A C1A -1.5(11) . . . . ? Co1A N1A C2A C1A -174.1(6) . . . . ? C5A N2A C3A C2A -173.3(6) . . . . ? Co1A N2A C3A C2A -3.2(8) . . . . ? C5A N2A C3A C4A 3.9(11) . . . . ? Co1A N2A C3A C4A 174.0(6) . . . . ? N1A C2A C3A N2A 2.1(9) . . . . ? C1A C2A C3A N2A 176.1(7) . . . . ? N1A C2A C3A C4A -175.2(7) . . . . ? C1A C2A C3A C4A -1.3(11) . . . . ? C3A N2A C5A C6A 132.4(8) . . . . ? Co1A N2A C5A C6A -36.9(9) . . . . ? N2A C5A C6A C7A 69.4(9) . . . . ? C11A N3A C7A C8A 2.9(10) . . . . ? Co1A N3A C7A C8A 178.3(5) . . . . ? C11A N3A C7A C6A -177.9(6) . . . . ? Co1A N3A C7A C6A -2.5(8) . . . . ? C5A C6A C7A N3A -48.7(9) . . . . ? C5A C6A C7A C8A 130.5(7) . . . . ? N3A C7A C8A C9A -3.0(12) . . . . ? C6A C7A C8A C9A 177.8(8) . . . . ? C7A C8A C9A C10A 1.5(13) . . . . ? C8A C9A C10A C11A 0.0(12) . . . . ? C7A N3A C11A C10A -1.5(10) . . . . ? Co1A N3A C11A C10A -177.1(5) . . . . ? C9A C10A C11A N3A 0.0(11) . . . . ? N1A Co1A C12A C13A -12.7(7) . . . . ? N2A Co1A C12A C13A -95.1(6) . . . . ? O2H Co1A C12A C13A 76.0(6) . . . . ? N3A Co1A C12A C13A 168.4(6) . . . . ? O1 Co1A C12A C13A 94.7(34) . . . . ? Co1 Co1A C12A C13A 48.0(7) . . . . ? N1A Co1A C12A C17A 121.9(6) . . . . ? N2A Co1A C12A C17A 39.6(7) . . . . ? O2H Co1A C12A C17A -149.4(6) . . . . ? N3A Co1A C12A C17A -57.0(6) . . . . ? O1 Co1A C12A C17A -130.6(31) . . . . ? Co1 Co1A C12A C17A -177.3(5) . . . . ? C17A C12A C13A C14A 50.4(11) . . . . ? Co1A C12A C13A C14A -173.7(6) . . . . ? C12A C13A C14A C15A -51.3(12) . . . . ? C13A C14A C15A C16A 50.2(12) . . . . ? C14A C15A C16A C17A -49.9(12) . . . . ? C13A C12A C17A C16A -49.8(11) . . . . ? Co1A C12A C17A C16A 172.9(7) . . . . ? C15A C16A C17A C12A 50.7(12) . . . . ? C182 O71 O72 C181 0.0(1000) . . . . ? C182 C181 O72 O71 0.0(1000) . . . . ? O72 O71 C182 C181 0.0(1000) . . . . ? O72 C181 C182 O71 0.0(1000) . . . . ? _refine_diff_density_max 0.574 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.079