# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? _journal_year ? loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Jack M. Harrowfield' ; Institut de Science et d'Ing\'enierie Supramol\'eculaires, Universit\'e Louis Pasteur, 8, all\'ee Gaspard Monge, 67083 Strasbourg, France ; ; Chemistry Section, M313, School of Biomedical, Biomolecular and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; 'Alexandre N. Sobolev' ; Chemistry Section, M313, School of Biomedical, Biomolecular and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; . _publ_contact_author_address ; Institut de Science et d'Ing\'enierie Supramol\'eculaires, Universit\'e Louis Pasteur, 8, all\'ee Gaspard Monge, 67083 Strasbourg, France ; _publ_contact_author_email harrowfield@isis.u-strasbg.fr _publ_contact_author_fax '+33 03 90 245140' _publ_contact_author_phone '+33 03 90 245165' #TrackingRef '13505_web_deposit_cif_file_0_JackHarrowfield_1345797825.as840.cif' _publ_contact_author_name 'Prof. Jack M. Harrowfield' _publ_contact_letter ; Please consider this submission for publication as a New paper in Chemical Communication. The figures, chemical structure diagram (scheme), Transfer of Copyright Agreement form and structure factor listing will be sent on receipt of your acknowledgement email or letter. ; _publ_requested_coeditor_name ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? #<< paper title text ; data_artur15 _database_code_depnum_ccdc_archive 'CCDC 826148' #TrackingRef '- artur15.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 N10, H2 O' _chemical_formula_sum 'C22 H26 N10 O' _chemical_formula_weight 446.53 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.0604(3) _cell_length_b 20.2397(11) _cell_length_c 10.3186(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.884(3) _cell_angle_gamma 90.00 _cell_volume 2260.40(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11577 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16336 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5178 _reflns_number_gt 2971 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1138P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5178 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1196 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1966 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 C1 C -0.16252(19) -0.06865(13) -0.5396(2) 0.0420(6) Uani 1 1 d . . . H1 H -0.1018 -0.0675 -0.5927 0.050 Uiso 1 1 calc R . . C2 C -0.1805(2) -0.12565(13) -0.4727(2) 0.0414(6) Uani 1 1 d . . . H2 H -0.1322 -0.1638 -0.4800 0.050 Uiso 1 1 calc R . . C3 C -0.26866(18) -0.12755(12) -0.3946(2) 0.0351(5) Uani 1 1 d . . . H3 H -0.2814 -0.1671 -0.3498 0.042 Uiso 1 1 calc R . . C4 C -0.33850(18) -0.07159(11) -0.3817(2) 0.0300(5) Uani 1 1 d . . . C5 C -0.32025(19) -0.01450(12) -0.4504(2) 0.0360(5) Uani 1 1 d . . . H5 H -0.3679 0.0239 -0.4430 0.043 Uiso 1 1 calc R . . C6 C -0.2327(2) -0.01332(13) -0.5295(2) 0.0415(6) Uani 1 1 d . . . H6 H -0.2212 0.0257 -0.5768 0.050 Uiso 1 1 calc R . . C7 C -0.43035(17) -0.07212(11) -0.29320(19) 0.0286(5) Uani 1 1 d . . . C8 C -0.54236(17) -0.12897(10) -0.16915(19) 0.0278(5) Uani 1 1 d . . . C9 C -0.59552(17) -0.07098(10) -0.13505(19) 0.0279(5) Uani 1 1 d . . . H9 H -0.6551 -0.0709 -0.0805 0.033 Uiso 1 1 calc R . . C10 C -0.55600(17) -0.01318(10) -0.18578(19) 0.0270(5) Uani 1 1 d . . . C11 C -0.5101(2) -0.25079(11) -0.1508(2) 0.0395(6) Uani 1 1 d . . . H11A H -0.4681 -0.2722 -0.0686 0.059 Uiso 1 1 calc R . . H11B H -0.4499 -0.2408 -0.2057 0.059 Uiso 1 1 calc R . . H11C H -0.5737 -0.2805 -0.1992 0.059 Uiso 1 1 calc R . . C12 C -0.6867(2) -0.24542(11) 0.0019(2) 0.0343(5) Uani 1 1 d . . . H12 H -0.6542 -0.2858 -0.0230 0.041 Uiso 1 1 calc R . . C13 C -0.77505(19) -0.24540(11) 0.0872(2) 0.0333(5) Uani 1 1 d . . . C14 C -0.8324(2) -0.29585(12) 0.1384(2) 0.0414(6) Uani 1 1 d . . . H14 H -0.8209 -0.3414 0.1223 0.050 Uiso 1 1 calc R . . C15 C -0.89769(19) -0.20632(12) 0.2123(2) 0.0351(5) Uani 1 1 d . . . C16 C -0.9616(2) -0.15777(13) 0.2825(2) 0.0453(6) Uani 1 1 d . . . H16A H -0.9369 -0.1129 0.2631 0.068 Uiso 1 1 calc R . . H16B H -0.9388 -0.1657 0.3781 0.068 Uiso 1 1 calc R . . H16C H -1.0512 -0.1626 0.2527 0.068 Uiso 1 1 calc R . . C17 C -0.55927(19) 0.10820(10) -0.2186(2) 0.0336(5) Uani 1 1 d . . . H17A H -0.6317 0.1339 -0.2612 0.050 Uiso 1 1 calc R . . H17B H -0.5106 0.0963 -0.2844 0.050 Uiso 1 1 calc R . . H17C H -0.5084 0.1347 -0.1484 0.050 Uiso 1 1 calc R . . C18 C -0.72585(18) 0.10742(11) -0.0547(2) 0.0318(5) Uani 1 1 d . . . H18 H -0.6915 0.1464 -0.0836 0.038 Uiso 1 1 calc R . . C19 C -0.82086(18) 0.11281(10) 0.0231(2) 0.0304(5) Uani 1 1 d . . . C20 C -0.86995(19) 0.17022(12) 0.0598(2) 0.0383(6) Uani 1 1 d . . . H20 H -0.8477 0.2140 0.0414 0.046 Uiso 1 1 calc R . . C21 C -0.95886(17) 0.08481(12) 0.1325(2) 0.0334(5) Uani 1 1 d . . . C22 C -1.0402(2) 0.04624(13) 0.2016(2) 0.0462(7) Uani 1 1 d . . . H22A H -1.0922 0.0765 0.2403 0.069 Uiso 1 1 calc R . . H22B H -0.9895 0.0198 0.2719 0.069 Uiso 1 1 calc R . . H22C H -1.0927 0.0169 0.1382 0.069 Uiso 1 1 calc R . . N1 N -0.46251(15) -0.13076(9) -0.25240(17) 0.0310(4) Uani 1 1 d . . . N2 N -0.46972(14) -0.01297(9) -0.26227(17) 0.0293(4) Uani 1 1 d . . . N3 N -0.56749(15) -0.18999(9) -0.11947(17) 0.0325(4) Uani 1 1 d . . . N4 N -0.65264(14) -0.19028(9) -0.03975(17) 0.0308(4) Uani 1 1 d . . . N5 N -0.81785(14) -0.18857(9) 0.13615(17) 0.0328(4) Uani 1 1 d . . . H5N H -0.7967 -0.1479 0.1204 0.039 Uiso 1 1 calc R . . N6 N -0.90924(17) -0.27154(10) 0.21657(18) 0.0410(5) Uani 1 1 d . . . N7 N -0.59923(15) 0.04866(9) -0.16174(17) 0.0297(4) Uani 1 1 d . . . N8 N -0.68762(14) 0.05050(9) -0.08483(16) 0.0287(4) Uani 1 1 d . . . N9 N -0.87732(14) 0.05958(9) 0.06880(17) 0.0323(4) Uani 1 1 d . . . N10 N -0.95766(15) 0.15145(9) 0.12859(17) 0.0376(5) Uani 1 1 d . . . H10N H -1.0048 0.1781 0.1640 0.045 Uiso 1 1 calc R . . O1 O -0.75978(13) -0.05929(7) -0.86384(16) 0.0437(4) Uani 1 1 d . . . H1W H -0.8069 -0.0200 -0.8957 0.050 Uiso 1 1 d . . . H2W H -0.6844 -0.0379 -0.8106 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0381(12) 0.0529(17) 0.0404(13) -0.0051(12) 0.0207(10) -0.0035(11) C2 0.0396(12) 0.0444(16) 0.0451(14) -0.0067(12) 0.0204(10) 0.0039(11) C3 0.0374(12) 0.0355(14) 0.0355(13) -0.0036(10) 0.0145(9) 0.0006(10) C4 0.0293(10) 0.0351(13) 0.0278(11) -0.0046(10) 0.0110(8) -0.0008(9) C5 0.0384(12) 0.0358(14) 0.0375(13) 0.0011(11) 0.0163(10) 0.0021(10) C6 0.0440(13) 0.0470(16) 0.0379(13) 0.0033(11) 0.0184(10) -0.0045(11) C7 0.0295(10) 0.0294(13) 0.0281(11) 0.0000(9) 0.0088(8) -0.0013(9) C8 0.0288(10) 0.0267(12) 0.0289(11) 0.0000(9) 0.0082(8) -0.0028(9) C9 0.0266(10) 0.0271(12) 0.0323(11) 0.0001(9) 0.0115(8) -0.0007(8) C10 0.0274(10) 0.0258(12) 0.0289(11) 0.0002(9) 0.0084(8) 0.0007(9) C11 0.0475(13) 0.0268(13) 0.0500(15) 0.0005(11) 0.0237(11) 0.0056(10) C12 0.0392(12) 0.0265(13) 0.0403(13) 0.0004(10) 0.0155(10) -0.0035(9) C13 0.0374(12) 0.0276(13) 0.0359(13) 0.0002(10) 0.0099(9) -0.0058(9) C14 0.0503(13) 0.0307(14) 0.0475(15) 0.0020(11) 0.0201(11) -0.0074(11) C15 0.0348(11) 0.0382(15) 0.0343(12) 0.0056(10) 0.0120(9) -0.0027(10) C16 0.0468(13) 0.0486(16) 0.0465(15) 0.0034(12) 0.0233(11) 0.0022(12) C17 0.0402(12) 0.0250(12) 0.0400(13) 0.0022(10) 0.0184(10) -0.0025(9) C18 0.0358(11) 0.0244(12) 0.0375(13) -0.0007(10) 0.0132(9) 0.0017(9) C19 0.0326(11) 0.0282(13) 0.0309(12) -0.0023(9) 0.0076(9) 0.0033(9) C20 0.0442(13) 0.0297(13) 0.0445(14) 0.0009(11) 0.0175(10) 0.0080(10) C21 0.0296(11) 0.0384(14) 0.0327(12) -0.0071(10) 0.0075(9) 0.0014(9) C22 0.0431(13) 0.0516(17) 0.0497(15) -0.0124(12) 0.0230(11) -0.0081(11) N1 0.0335(9) 0.0294(11) 0.0339(10) -0.0006(8) 0.0155(8) -0.0006(8) N2 0.0284(9) 0.0295(11) 0.0331(10) -0.0008(8) 0.0135(7) 0.0009(7) N3 0.0386(10) 0.0239(10) 0.0401(11) -0.0005(8) 0.0201(8) 0.0010(8) N4 0.0337(9) 0.0280(11) 0.0341(10) -0.0017(8) 0.0148(8) -0.0029(8) N5 0.0350(9) 0.0280(11) 0.0379(11) 0.0047(8) 0.0135(8) -0.0033(8) N6 0.0482(11) 0.0335(12) 0.0453(12) 0.0027(10) 0.0193(9) -0.0080(9) N7 0.0324(9) 0.0254(10) 0.0359(10) 0.0016(8) 0.0180(7) 0.0002(7) N8 0.0284(9) 0.0286(10) 0.0319(10) -0.0021(8) 0.0127(7) 0.0003(7) N9 0.0316(9) 0.0307(11) 0.0368(10) -0.0050(8) 0.0120(7) 0.0013(8) N10 0.0400(10) 0.0347(12) 0.0406(11) -0.0042(9) 0.0143(8) 0.0127(8) O1 0.0442(9) 0.0249(9) 0.0624(11) -0.0017(8) 0.0117(8) -0.0027(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 C1 C6 1.379(3) . ? C1 C2 1.380(3) . ? C1 H1 0.9500 . ? C2 C3 1.388(3) . ? C2 H2 0.9500 . ? C3 C4 1.393(3) . ? C3 H3 0.9500 . ? C4 C5 1.391(3) . ? C4 C7 1.500(3) . ? C5 C6 1.390(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.332(3) . ? C7 N2 1.335(3) . ? C8 N1 1.353(2) . ? C8 N3 1.387(3) . ? C8 C9 1.390(3) . ? C9 C10 1.389(3) . ? C9 H9 0.9500 . ? C10 N2 1.358(2) . ? C10 N7 1.380(3) . ? C11 N3 1.451(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N4 1.280(3) . ? C12 C13 1.444(3) . ? C12 H12 0.9500 . ? C13 C14 1.364(3) . ? C13 N5 1.379(3) . ? C14 N6 1.378(3) . ? C14 H14 0.9500 . ? C15 N6 1.328(3) . ? C15 N5 1.346(2) . ? C15 C16 1.483(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N7 1.448(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N8 1.287(3) . ? C18 C19 1.452(3) . ? C18 H18 0.9500 . ? C19 C20 1.369(3) . ? C19 N9 1.376(3) . ? C20 N10 1.369(3) . ? C20 H20 0.9500 . ? C21 N9 1.323(2) . ? C21 N10 1.350(3) . ? C21 C22 1.480(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N3 N4 1.372(2) . ? N5 H5N 0.8800 . ? N7 N8 1.381(2) . ? N10 H10N 0.8800 . ? O1 H1W 0.9703 . ? O1 H2W 0.9978 . ? 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 C6 C1 C2 120.0(2) . . ? C6 C1 H1 120.0 . . ? C2 C1 H1 120.0 . . ? C1 C2 C3 120.3(2) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C4 120.2(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.06(18) . . ? C5 C4 C7 120.23(19) . . ? C3 C4 C7 120.70(19) . . ? C6 C5 C4 120.3(2) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C1 C6 C5 120.1(2) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? N1 C7 N2 127.02(18) . . ? N1 C7 C4 117.22(18) . . ? N2 C7 C4 115.75(18) . . ? N1 C8 N3 114.67(18) . . ? N1 C8 C9 123.27(19) . . ? N3 C8 C9 122.06(17) . . ? C10 C9 C8 115.69(18) . . ? C10 C9 H9 122.2 . . ? C8 C9 H9 122.2 . . ? N2 C10 N7 114.37(17) . . ? N2 C10 C9 122.36(18) . . ? N7 C10 C9 123.27(17) . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C13 119.2(2) . . ? N4 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 N5 105.11(19) . . ? C14 C13 C12 131.5(2) . . ? N5 C13 C12 123.38(19) . . ? C13 C14 N6 110.6(2) . . ? C13 C14 H14 124.7 . . ? N6 C14 H14 124.7 . . ? N6 C15 N5 111.31(19) . . ? N6 C15 C16 125.7(2) . . ? N5 C15 C16 123.0(2) . . ? 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 . . ? N7 C17 H17A 109.5 . . ? N7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N8 C18 C19 120.80(19) . . ? N8 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 N9 109.61(18) . . ? C20 C19 C18 126.2(2) . . ? N9 C19 C18 124.19(19) . . ? N10 C20 C19 105.8(2) . . ? N10 C20 H20 127.1 . . ? C19 C20 H20 127.1 . . ? N9 C21 N10 111.06(19) . . ? N9 C21 C22 125.4(2) . . ? N10 C21 C22 123.49(19) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C7 N1 C8 115.37(17) . . ? C7 N2 C10 116.05(17) . . ? N4 N3 C8 116.09(16) . . ? N4 N3 C11 121.03(16) . . ? C8 N3 C11 122.86(16) . . ? C12 N4 N3 119.39(18) . . ? C15 N5 C13 107.89(18) . . ? C15 N5 H5N 126.1 . . ? C13 N5 H5N 126.1 . . ? C15 N6 C14 105.12(18) . . ? C10 N7 N8 116.12(16) . . ? C10 N7 C17 122.40(16) . . ? N8 N7 C17 121.42(16) . . ? C18 N8 N7 118.02(17) . . ? C21 N9 C19 105.78(18) . . ? C21 N10 C20 107.76(17) . . ? C21 N10 H10N 126.1 . . ? C20 N10 H10N 126.1 . . ? H1W O1 H2W 99.2 . . ? 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 C6 C1 C2 C3 -0.2(4) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? C2 C3 C4 C5 1.3(3) . . . . ? C2 C3 C4 C7 -177.42(18) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C7 C4 C5 C6 178.18(18) . . . . ? C2 C1 C6 C5 1.0(4) . . . . ? C4 C5 C6 C1 -0.6(3) . . . . ? C5 C4 C7 N1 166.37(19) . . . . ? C3 C4 C7 N1 -14.9(3) . . . . ? C5 C4 C7 N2 -14.6(3) . . . . ? C3 C4 C7 N2 164.16(19) . . . . ? N1 C8 C9 C10 -3.7(3) . . . . ? N3 C8 C9 C10 176.15(18) . . . . ? C8 C9 C10 N2 -0.9(3) . . . . ? C8 C9 C10 N7 180.00(18) . . . . ? N4 C12 C13 C14 175.3(2) . . . . ? N4 C12 C13 N5 -5.7(3) . . . . ? N5 C13 C14 N6 0.2(3) . . . . ? C12 C13 C14 N6 179.4(2) . . . . ? N8 C18 C19 C20 -179.1(2) . . . . ? N8 C18 C19 N9 -0.6(3) . . . . ? N9 C19 C20 N10 -0.1(2) . . . . ? C18 C19 C20 N10 178.58(19) . . . . ? N2 C7 N1 C8 -1.1(3) . . . . ? C4 C7 N1 C8 177.87(16) . . . . ? N3 C8 N1 C7 -175.23(17) . . . . ? C9 C8 N1 C7 4.7(3) . . . . ? N1 C7 N2 C10 -3.2(3) . . . . ? C4 C7 N2 C10 177.86(15) . . . . ? N7 C10 N2 C7 -176.72(17) . . . . ? C9 C10 N2 C7 4.1(3) . . . . ? N1 C8 N3 N4 -177.01(16) . . . . ? C9 C8 N3 N4 3.1(3) . . . . ? N1 C8 N3 C11 1.8(3) . . . . ? C9 C8 N3 C11 -178.12(19) . . . . ? C13 C12 N4 N3 179.18(17) . . . . ? C8 N3 N4 C12 175.12(18) . . . . ? C11 N3 N4 C12 -3.7(3) . . . . ? N6 C15 N5 C13 0.3(2) . . . . ? C16 C15 N5 C13 179.51(19) . . . . ? C14 C13 N5 C15 -0.3(2) . . . . ? C12 C13 N5 C15 -179.54(19) . . . . ? N5 C15 N6 C14 -0.1(2) . . . . ? C16 C15 N6 C14 -179.3(2) . . . . ? C13 C14 N6 C15 -0.1(3) . . . . ? N2 C10 N7 N8 179.68(15) . . . . ? C9 C10 N7 N8 -1.2(3) . . . . ? N2 C10 N7 C17 2.5(3) . . . . ? C9 C10 N7 C17 -178.29(18) . . . . ? C19 C18 N8 N7 178.44(17) . . . . ? C10 N7 N8 C18 176.63(18) . . . . ? C17 N7 N8 C18 -6.2(3) . . . . ? N10 C21 N9 C19 0.5(2) . . . . ? C22 C21 N9 C19 -178.55(19) . . . . ? C20 C19 N9 C21 -0.2(2) . . . . ? C18 C19 N9 C21 -178.93(19) . . . . ? N9 C21 N10 C20 -0.5(2) . . . . ? C22 C21 N10 C20 178.49(19) . . . . ? C19 C20 N10 C21 0.4(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10N N6 0.88 1.99 2.849(2) 166.5 2_355 N5 H5N O1 0.88 1.84 2.694(2) 163.4 1_556 O1 H1W N9 0.97 1.79 2.755(2) 170.2 1_554 O1 H2W N2 1.00 2.00 2.986(2) 168.7 3_454 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.342 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.071 # Attachment '- as23.cif' data_as23 _database_code_depnum_ccdc_archive 'CCDC 826149' #TrackingRef '- as23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H24 N10 O' _chemical_formula_weight 432.50 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.0437(7) _cell_length_b 15.1679(10) _cell_length_c 16.2868(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.566(4) _cell_angle_gamma 90.00 _cell_volume 2231.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13798 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _diffrn_measurement_method 'phi&omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15094 _diffrn_reflns_av_R_equivalents 0.1440 _diffrn_reflns_av_sigmaI/netI 0.1742 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.63 _reflns_number_total 5127 _reflns_number_gt 2046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker 8.6' _computing_publication_material 'CrystalMaker 8.6' _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^)+(0.0566P)^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 5127 _refine_ls_number_parameters 296 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2600 _refine_ls_R_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 C1 C 0.7435(5) 0.3751(3) 0.0868(2) 0.0642(11) Uani 1 1 d . . . H1 H 0.7187 0.4081 0.0401 0.077 Uiso 1 1 calc R . . C2 C 0.8549(4) 0.2905(2) 0.1716(3) 0.0663(11) Uani 1 1 d . . . H2 H 0.9248 0.2519 0.1949 0.080 Uiso 1 1 calc R . . C3 C 0.7315(4) 0.3175(2) 0.2093(2) 0.0480(9) Uani 1 1 d . . . C4 C 0.6797(4) 0.3036(2) 0.2907(2) 0.0513(9) Uani 1 1 d . . . H4 H 0.7250 0.2629 0.3264 0.062 Uiso 1 1 calc R . . C5 C 0.5777(4) 0.2803(2) 0.4493(2) 0.0641(11) Uani 1 1 d . . . H5A H 0.5673 0.2213 0.4285 0.096 Uiso 1 1 calc R . . H5B H 0.5264 0.2855 0.4994 0.096 Uiso 1 1 calc R . . H5C H 0.6807 0.2933 0.4598 0.096 Uiso 1 1 calc R . . C6 C 0.4194(3) 0.4091(2) 0.4100(2) 0.0395(8) Uani 1 1 d . . . C7 C 0.3821(3) 0.4762(2) 0.3550(2) 0.0454(9) Uani 1 1 d . . . H7 H 0.4165 0.4772 0.3021 0.054 Uiso 1 1 calc R . . C8 C 0.2915(3) 0.5413(2) 0.3833(2) 0.0421(8) Uani 1 1 d . . . C9 C 0.2799(3) 0.4726(2) 0.5062(2) 0.0406(8) Uani 1 1 d . . . C10 C 0.2223(3) 0.4731(2) 0.5900(2) 0.0409(9) Uani 1 1 d . . . C11 C 0.2945(4) 0.4271(2) 0.6537(2) 0.0477(9) Uani 1 1 d . . . H11 H 0.3765 0.3925 0.6431 0.057 Uiso 1 1 calc R . . C12 C 0.2454(4) 0.4323(2) 0.7331(2) 0.0575(10) Uani 1 1 d . . . H12 H 0.2958 0.4025 0.7757 0.069 Uiso 1 1 calc R . . C13 C 0.1226(4) 0.4814(2) 0.7486(2) 0.0595(10) Uani 1 1 d . . . H13 H 0.0885 0.4837 0.8016 0.071 Uiso 1 1 calc R . . C14 C 0.0499(4) 0.5270(2) 0.6863(2) 0.0561(10) Uani 1 1 d . . . H14 H -0.0336 0.5602 0.6970 0.067 Uiso 1 1 calc R . . C15 C 0.1005(4) 0.5239(2) 0.6077(2) 0.0489(9) Uani 1 1 d . . . H15 H 0.0522 0.5563 0.5661 0.059 Uiso 1 1 calc R . . C16 C 0.1481(4) 0.6799(2) 0.3609(2) 0.0661(11) Uani 1 1 d . . . H16A H 0.1996 0.7334 0.3755 0.099 Uiso 1 1 calc R . . H16B H 0.0981 0.6582 0.4076 0.099 Uiso 1 1 calc R . . H16C H 0.0770 0.6915 0.3167 0.099 Uiso 1 1 calc R . . C17 C 0.3124(4) 0.6925(2) 0.2207(2) 0.0553(10) Uani 1 1 d . . . H17 H 0.2502 0.7375 0.2370 0.066 Uiso 1 1 calc R . . C18 C 0.3925(4) 0.7019(2) 0.1466(2) 0.0504(9) Uani 1 1 d . . . C19 C 0.4137(4) 0.7759(2) 0.1013(2) 0.0634(11) Uani 1 1 d . . . H19 H 0.3764 0.8318 0.1113 0.076 Uiso 1 1 calc R . . C20 C 0.5275(4) 0.6668(3) 0.0481(2) 0.0643(11) Uani 1 1 d . . . H20 H 0.5846 0.6345 0.0128 0.077 Uiso 1 1 calc R . . C21 C 0.2372(5) 0.4470(3) 0.1305(3) 0.0959(15) Uani 1 1 d . . . H21A H 0.2122 0.4677 0.1838 0.144 Uiso 1 1 calc R . . H21B H 0.2122 0.3857 0.1253 0.144 Uiso 1 1 calc R . . H21C H 0.1829 0.4801 0.0889 0.144 Uiso 1 1 calc R . . N1 N 0.8631(4) 0.3271(2) 0.0954(2) 0.0727(10) Uani 1 1 d . . . N2 N 0.6604(3) 0.37144(18) 0.15301(18) 0.0535(8) Uani 1 1 d . . . H2A H 0.5777 0.3981 0.1589 0.064 Uiso 1 1 calc R . . N3 N 0.5688(3) 0.34955(16) 0.31210(17) 0.0465(7) Uani 1 1 d . . . N4 N 0.5154(3) 0.34201(17) 0.38900(17) 0.0483(8) Uani 1 1 d . . . N5 N 0.3688(3) 0.40606(16) 0.48642(16) 0.0427(7) Uani 1 1 d . . . N6 N 0.2383(3) 0.54094(16) 0.45875(17) 0.0429(7) Uani 1 1 d . . . N7 N 0.2529(3) 0.61468(17) 0.33515(17) 0.0500(8) Uani 1 1 d . . . N8 N 0.3269(3) 0.62250(18) 0.26405(17) 0.0486(8) Uani 1 1 d . . . N9 N 0.4658(3) 0.63280(19) 0.11218(19) 0.0586(8) Uani 1 1 d . . . N10 N 0.4996(3) 0.7525(2) 0.03894(19) 0.0665(9) Uani 1 1 d . . . H10 H 0.5302 0.7863 0.0009 0.080 Uiso 1 1 calc R . . O1 O 0.3888(3) 0.4579(2) 0.12104(19) 0.0768(8) Uani 1 1 d D . . H1O H 0.420(5) 0.5089(12) 0.123(3) 0.14(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.062(3) 0.084(3) 0.047(3) -0.009(2) 0.012(2) -0.001(2) C2 0.059(3) 0.086(3) 0.054(3) -0.017(3) 0.006(2) 0.026(2) C3 0.050(2) 0.053(2) 0.042(2) -0.009(2) 0.005(2) 0.0101(19) C4 0.055(2) 0.049(2) 0.050(3) -0.0063(19) 0.0034(19) 0.0060(19) C5 0.087(3) 0.055(2) 0.051(3) 0.008(2) 0.012(2) 0.017(2) C6 0.038(2) 0.040(2) 0.041(2) -0.0049(18) 0.0085(17) -0.0023(17) C7 0.046(2) 0.053(2) 0.038(2) -0.0010(19) 0.0105(16) 0.0066(18) C8 0.044(2) 0.044(2) 0.039(2) 0.0047(18) 0.0046(17) -0.0027(17) C9 0.037(2) 0.047(2) 0.039(2) -0.0038(19) 0.0093(16) -0.0096(17) C10 0.038(2) 0.044(2) 0.041(2) -0.0014(18) 0.0083(17) -0.0074(17) C11 0.055(2) 0.045(2) 0.043(2) 0.0007(19) 0.0095(19) -0.0042(18) C12 0.068(3) 0.063(3) 0.041(3) 0.004(2) 0.005(2) -0.004(2) C13 0.075(3) 0.070(3) 0.035(2) 0.002(2) 0.015(2) -0.016(2) C14 0.051(2) 0.066(3) 0.053(3) -0.004(2) 0.018(2) -0.007(2) C15 0.048(2) 0.062(2) 0.037(2) 0.0010(19) 0.0077(17) -0.0033(19) C16 0.081(3) 0.062(2) 0.057(3) 0.011(2) 0.026(2) 0.022(2) C17 0.064(3) 0.057(2) 0.046(3) 0.006(2) 0.019(2) 0.0101(19) C18 0.055(2) 0.059(2) 0.039(2) 0.008(2) 0.0115(18) 0.005(2) C19 0.075(3) 0.071(3) 0.046(3) 0.012(2) 0.020(2) 0.002(2) C20 0.059(3) 0.085(3) 0.050(3) -0.001(2) 0.014(2) 0.008(2) C21 0.066(3) 0.118(4) 0.105(4) -0.006(3) 0.018(3) -0.002(3) N1 0.059(2) 0.106(3) 0.054(2) -0.022(2) 0.0133(18) 0.017(2) N2 0.0467(19) 0.070(2) 0.044(2) -0.0069(16) 0.0111(16) 0.0103(15) N3 0.0529(19) 0.0462(17) 0.041(2) -0.0049(14) 0.0099(15) 0.0051(15) N4 0.057(2) 0.0486(17) 0.040(2) 0.0032(15) 0.0106(15) 0.0103(15) N5 0.0473(18) 0.0437(17) 0.0379(19) -0.0013(14) 0.0126(14) 0.0010(14) N6 0.0466(18) 0.0503(18) 0.0329(18) 0.0045(15) 0.0121(14) -0.0011(14) N7 0.0595(19) 0.0520(18) 0.040(2) 0.0085(16) 0.0231(15) 0.0141(15) N8 0.0545(19) 0.0551(19) 0.037(2) 0.0083(15) 0.0164(14) 0.0039(14) N9 0.067(2) 0.071(2) 0.039(2) 0.0107(17) 0.0161(16) 0.0113(17) N10 0.071(2) 0.087(3) 0.043(2) 0.0168(19) 0.0137(18) -0.0089(19) O1 0.063(2) 0.075(2) 0.094(2) -0.0036(18) 0.0222(15) 0.0096(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.306(4) . ? C1 N2 1.342(4) . ? C1 H1 0.9300 . ? C2 C3 1.360(4) . ? C2 N1 1.365(4) . ? C2 H2 0.9300 . ? C3 N2 1.368(4) . ? C3 C4 1.442(4) . ? C4 N3 1.283(4) . ? C4 H4 0.9300 . ? C5 N4 1.452(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N5 1.346(4) . ? C6 C7 1.388(4) . ? C6 N4 1.390(4) . ? C7 C8 1.375(4) . ? C7 H7 0.9300 . ? C8 N6 1.339(4) . ? C8 N7 1.397(4) . ? C9 N6 1.337(4) . ? C9 N5 1.338(4) . ? C9 C10 1.483(4) . ? C10 C15 1.385(4) . ? C10 C11 1.389(4) . ? C11 C12 1.388(4) . ? C11 H11 0.9300 . ? C12 C13 1.370(4) . ? C12 H12 0.9300 . ? C13 C14 1.373(5) . ? C13 H13 0.9300 . ? C14 C15 1.379(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N7 1.445(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N8 1.279(4) . ? C17 C18 1.442(4) . ? C17 H17 0.9300 . ? C18 C19 1.361(4) . ? C18 N9 1.373(4) . ? C19 N10 1.354(4) . ? C19 H19 0.9300 . ? C20 N9 1.310(4) . ? C20 N10 1.330(4) . ? C20 H20 0.9300 . ? C21 O1 1.396(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? N2 H2A 0.8600 . ? N3 N4 1.367(3) . ? N7 N8 1.369(3) . ? N10 H10 0.8600 . ? O1 H1O 0.823(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 N1 C1 N2 112.5(4) . . ? N1 C1 H1 123.8 . . ? N2 C1 H1 123.8 . . ? C3 C2 N1 111.5(3) . . ? C3 C2 H2 124.2 . . ? N1 C2 H2 124.2 . . ? C2 C3 N2 104.4(3) . . ? C2 C3 C4 132.7(4) . . ? N2 C3 C4 122.8(3) . . ? N3 C4 C3 117.4(3) . . ? N3 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N5 C6 C7 122.6(3) . . ? N5 C6 N4 116.4(3) . . ? C7 C6 N4 121.0(3) . . ? C8 C7 C6 116.2(3) . . ? C8 C7 H7 121.9 . . ? C6 C7 H7 121.9 . . ? N6 C8 C7 123.2(3) . . ? N6 C8 N7 115.3(3) . . ? C7 C8 N7 121.5(3) . . ? N6 C9 N5 127.0(3) . . ? N6 C9 C10 115.3(3) . . ? N5 C9 C10 117.7(3) . . ? C15 C10 C11 118.4(3) . . ? C15 C10 C9 120.7(3) . . ? C11 C10 C9 120.8(3) . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.9(3) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? N7 C16 H16A 109.5 . . ? N7 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N7 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N8 C17 C18 120.0(3) . . ? N8 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 N9 109.0(3) . . ? C19 C18 C17 128.5(4) . . ? N9 C18 C17 122.5(3) . . ? N10 C19 C18 106.9(3) . . ? N10 C19 H19 126.6 . . ? C18 C19 H19 126.6 . . ? N9 C20 N10 112.9(3) . . ? N9 C20 H20 123.6 . . ? N10 C20 H20 123.6 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C1 N1 C2 104.2(3) . . ? C1 N2 C3 107.4(3) . . ? C1 N2 H2A 126.3 . . ? C3 N2 H2A 126.3 . . ? C4 N3 N4 121.0(3) . . ? N3 N4 C6 114.5(3) . . ? N3 N4 C5 122.1(3) . . ? C6 N4 C5 122.2(3) . . ? C9 N5 C6 115.5(3) . . ? C9 N6 C8 115.5(3) . . ? N8 N7 C8 115.1(3) . . ? N8 N7 C16 122.6(3) . . ? C8 N7 C16 122.2(3) . . ? C17 N8 N7 119.8(3) . . ? C20 N9 C18 104.8(3) . . ? C20 N10 C19 106.5(3) . . ? C20 N10 H10 126.8 . . ? C19 N10 H10 126.8 . . ? C21 O1 H1O 116(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.164 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.047 # Attachment '- artur5.cif' data_artur5 _database_code_depnum_ccdc_archive 'CCDC 826150' _publ_section_title_footnote ; ? #<< paper footnote text ; # 4. TEXT _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; #Barbour, L. J. (2001). J. Supramol. Chem., 1, 189-191. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # 5. CHEMICAL DATA _publ_section_figure_captions ; ? #<< figure captions ; #============================================================================== # 6. CRYSTALLOGRAPHY _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 N10, C2 H6 O' _chemical_formula_sum 'C22 H26 N10 O' _chemical_formula_weight 446.53 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8886(3) _cell_length_b 11.4824(7) _cell_length_c 25.5965(16) _cell_angle_alpha 92.693(2) _cell_angle_beta 92.650(3) _cell_angle_gamma 94.577(4) _cell_volume 2305.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 54208 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9746 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24324 _diffrn_reflns_av_R_equivalents 0.1346 _diffrn_reflns_av_sigmaI/netI 0.2673 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.52 _reflns_number_total 10438 _reflns_number_gt 3588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0500P)^2^+13.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10438 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3179 _refine_ls_R_factor_gt 0.1393 _refine_ls_wR_factor_ref 0.3405 _refine_ls_wR_factor_gt 0.2728 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 C1 C 0.3383(9) 0.7063(7) 0.3283(3) 0.0419(19) Uani 1 1 d . . . C2 C 0.4695(8) 0.8176(6) 0.2672(3) 0.0330(17) Uani 1 1 d . . . C3 C 0.5144(8) 0.7162(6) 0.2442(3) 0.0289(16) Uani 1 1 d . . . H3 H 0.5786 0.7187 0.2137 0.035 Uiso 1 1 calc R . . C4 C 0.4681(7) 0.6100(6) 0.2645(3) 0.0264(15) Uani 1 1 d . . . C5 C 0.4789(9) 1.0360(6) 0.2779(3) 0.0407(18) Uani 1 1 d . . . H5A H 0.5198 1.1020 0.2577 0.061 Uiso 1 1 calc R . . H5B H 0.5391 1.0413 0.3124 0.061 Uiso 1 1 calc R . . H5C H 0.3564 1.0383 0.2823 0.061 Uiso 1 1 calc R . . C6 C 0.6492(8) 1.0229(6) 0.1857(3) 0.0372(18) Uani 1 1 d . . . H6 H 0.6346 1.0965 0.2028 0.045 Uiso 1 1 calc R . . C7 C 0.7341(9) 1.0144(6) 0.1369(3) 0.0360(18) Uani 1 1 d . . . C8 C 0.8355(9) 0.9394(7) 0.0658(3) 0.0414(19) Uani 1 1 d . . . H8 H 0.8606 0.8863 0.0382 0.050 Uiso 1 1 calc R . . C9 C 0.8885(10) 1.0544(7) 0.0719(3) 0.046(2) Uani 1 1 d . . . H9 H 0.9600 1.0954 0.0489 0.055 Uiso 1 1 calc R . . C10 C 0.4838(9) 0.3948(6) 0.2699(3) 0.0388(18) Uani 1 1 d . . . H10A H 0.5222 0.3315 0.2476 0.058 Uiso 1 1 calc R . . H10B H 0.3628 0.3783 0.2761 0.058 Uiso 1 1 calc R . . H10C H 0.5500 0.4006 0.3034 0.058 Uiso 1 1 calc R . . C11 C 0.6406(8) 0.4168(7) 0.1756(3) 0.0380(18) Uani 1 1 d . . . H11 H 0.6238 0.3427 0.1905 0.046 Uiso 1 1 calc R . . C12 C 0.7260(9) 0.4302(6) 0.1264(3) 0.0395(19) Uani 1 1 d . . . C13 C 0.8297(9) 0.4936(7) 0.0565(3) 0.048(2) Uani 1 1 d . . . H13 H 0.8604 0.5434 0.0293 0.057 Uiso 1 1 calc R . . C14 C 0.8680(10) 0.3819(8) 0.0594(3) 0.050(2) Uani 1 1 d . . . H14 H 0.9293 0.3395 0.0349 0.060 Uiso 1 1 calc R . . C15 C 0.2412(8) 0.7039(7) 0.3782(3) 0.0374(18) Uani 1 1 d . . . C16 C 0.2094(9) 0.6006(8) 0.4020(3) 0.051(2) Uani 1 1 d . . . H16 H 0.2430 0.5301 0.3861 0.061 Uiso 1 1 calc R . . C17 C 0.1282(10) 0.5975(9) 0.4493(3) 0.059(3) Uani 1 1 d . . . H17 H 0.1091 0.5259 0.4661 0.071 Uiso 1 1 calc R . . C18 C 0.0760(11) 0.6997(10) 0.4713(4) 0.067(3) Uani 1 1 d . . . H18 H 0.0189 0.6981 0.5031 0.081 Uiso 1 1 calc R . . C19 C 0.1058(10) 0.8035(9) 0.4476(3) 0.056(2) Uani 1 1 d . . . H19 H 0.0692 0.8735 0.4630 0.067 Uiso 1 1 calc R . . C20 C 0.1906(9) 0.8060(8) 0.4005(3) 0.050(2) Uani 1 1 d . . . H20A H 0.2128 0.8779 0.3842 0.060 Uiso 1 1 calc R . . N1 N 0.3752(7) 0.8143(5) 0.3113(2) 0.0382(15) Uani 1 1 d . . . N2 N 0.3748(7) 0.6045(5) 0.3080(2) 0.0339(14) Uani 1 1 d . . . N3 N 0.5100(7) 0.9282(5) 0.2507(2) 0.0340(14) Uani 1 1 d . . . N4 N 0.5943(7) 0.9261(5) 0.2049(2) 0.0402(15) Uani 1 1 d . . . N5 N 0.7389(7) 0.9149(5) 0.1074(2) 0.0415(15) Uani 1 1 d . . . H5 H 0.6886 0.8462 0.1137 0.050 Uiso 1 1 calc R . . N6 N 0.8238(7) 1.1040(5) 0.1166(2) 0.0435(16) Uani 1 1 d . . . N7 N 0.5081(7) 0.5041(5) 0.2443(2) 0.0321(14) Uani 1 1 d . . . N8 N 0.5894(7) 0.5089(5) 0.1979(2) 0.0377(15) Uani 1 1 d . . . N9 N 0.7394(8) 0.5248(5) 0.0990(2) 0.0445(16) Uani 1 1 d . . . N10 N 0.8021(7) 0.3401(5) 0.1044(2) 0.0386(15) Uani 1 1 d . . . H10 H 0.8082 0.2698 0.1163 0.046 Uiso 1 1 calc R . . C21 C 0.1944(9) 0.2327(6) 0.1632(3) 0.0379(18) Uani 1 1 d . . . C22 C 0.0584(8) 0.3446(6) 0.2227(3) 0.0294(16) Uani 1 1 d . . . C23 C 0.0140(8) 0.2441(6) 0.2475(3) 0.0308(16) Uani 1 1 d . . . H23 H -0.0511 0.2475 0.2777 0.037 Uiso 1 1 calc R . . C24 C 0.0628(7) 0.1391(5) 0.2289(2) 0.0244(15) Uani 1 1 d . . . C25 C 0.0483(9) 0.5590(6) 0.2111(3) 0.044(2) Uani 1 1 d . . . H25A H 0.1074 0.5414 0.1792 0.066 Uiso 1 1 calc R . . H25B H 0.1181 0.6182 0.2333 0.066 Uiso 1 1 calc R . . H25C H -0.0614 0.5890 0.2017 0.066 Uiso 1 1 calc R . . C26 C -0.1102(8) 0.5484(7) 0.3049(3) 0.0354(17) Uani 1 1 d . . . H26 H -0.0920 0.6196 0.2877 0.042 Uiso 1 1 calc R . . C27 C -0.1948(8) 0.5440(6) 0.3548(3) 0.0340(17) Uani 1 1 d . . . C28 C -0.3001(9) 0.4710(7) 0.4246(3) 0.0426(19) Uani 1 1 d . . . H28 H -0.3296 0.4199 0.4514 0.051 Uiso 1 1 calc R . . C29 C -0.3427(9) 0.5811(7) 0.4207(3) 0.0445(19) Uani 1 1 d . . . H29 H -0.4078 0.6210 0.4450 0.053 Uiso 1 1 calc R . . C30 C 0.0522(8) -0.0788(5) 0.2259(3) 0.0335(17) Uani 1 1 d . . . H30A H 0.1145 -0.0672 0.1941 0.050 Uiso 1 1 calc R . . H30B H -0.0579 -0.1225 0.2168 0.050 Uiso 1 1 calc R . . H30C H 0.1186 -0.1230 0.2502 0.050 Uiso 1 1 calc R . . C31 C -0.1121(9) -0.0513(7) 0.3188(3) 0.0425(19) Uani 1 1 d . . . H31 H -0.0929 -0.1266 0.3044 0.051 Uiso 1 1 calc R . . C32 C -0.2011(9) -0.0372(6) 0.3676(3) 0.0362(17) Uani 1 1 d . . . C33 C -0.3083(9) 0.0313(7) 0.4364(3) 0.0433(19) Uani 1 1 d . . . H33 H -0.3406 0.0840 0.4631 0.052 Uiso 1 1 calc R . . C34 C -0.3475(10) -0.0856(7) 0.4332(3) 0.050(2) Uani 1 1 d . . . H34 H -0.4108 -0.1291 0.4574 0.060 Uiso 1 1 calc R . . C35 C 0.2895(8) 0.2239(7) 0.1148(3) 0.0375(18) Uani 1 1 d . . . C36 C 0.3524(8) 0.1210(7) 0.0987(3) 0.0425(19) Uani 1 1 d . . . H36 H 0.3337 0.0543 0.1189 0.051 Uiso 1 1 calc R . . C37 C 0.4439(10) 0.1116(7) 0.0530(3) 0.049(2) Uani 1 1 d . . . H37 H 0.4873 0.0398 0.0423 0.059 Uiso 1 1 calc R . . C38 C 0.4691(9) 0.2094(7) 0.0240(3) 0.048(2) Uani 1 1 d . . . H38 H 0.5305 0.2047 -0.0070 0.058 Uiso 1 1 calc R . . C39 C 0.4074(9) 0.3124(7) 0.0391(3) 0.047(2) Uani 1 1 d . . . H39 H 0.4244 0.3784 0.0184 0.056 Uiso 1 1 calc R . . C40 C 0.3185(9) 0.3217(7) 0.0853(3) 0.047(2) Uani 1 1 d . . . H40 H 0.2785 0.3943 0.0963 0.056 Uiso 1 1 calc R . . N11 N 0.1493(7) 0.3376(6) 0.1787(2) 0.0378(15) Uani 1 1 d . . . N12 N 0.1613(7) 0.1325(5) 0.1866(2) 0.0368(15) Uani 1 1 d . . . N13 N 0.0200(7) 0.4542(5) 0.2393(2) 0.0356(14) Uani 1 1 d . . . N14 N -0.0627(7) 0.4540(5) 0.2859(2) 0.0354(14) Uani 1 1 d . . . N15 N -0.2053(7) 0.4460(5) 0.3821(2) 0.0399(15) Uani 1 1 d . . . H15 H -0.1608 0.3798 0.3744 0.048 Uiso 1 1 calc R . . N16 N -0.2778(7) 0.6286(5) 0.3758(2) 0.0395(15) Uani 1 1 d . . . N17 N 0.0249(7) 0.0326(4) 0.2502(2) 0.0345(14) Uani 1 1 d . . . N18 N -0.0615(7) 0.0415(5) 0.2964(2) 0.0366(14) Uani 1 1 d . . . N19 N -0.2130(8) 0.0615(5) 0.3940(3) 0.0459(16) Uani 1 1 d . . . N20 N -0.2794(7) -0.1307(5) 0.3887(2) 0.0420(16) Uani 1 1 d . . . H20B H -0.2859 -0.2041 0.3768 0.050 Uiso 1 1 calc R . . C42 C 0.2638(12) 0.7633(8) 0.1126(4) 0.078(3) Uani 1 1 d . . . H42A H 0.1433 0.7352 0.1130 0.117 Uiso 1 1 calc R . . H42B H 0.2797 0.8172 0.0843 0.117 Uiso 1 1 calc R . . H42C H 0.3001 0.8042 0.1462 0.117 Uiso 1 1 calc R . . O1 O 0.5383(6) 0.7065(4) 0.1032(2) 0.0487(14) Uani 1 1 d . . . H1A H 0.6006 0.6505 0.1028 0.073 Uiso 1 1 calc R . . C41 C 0.3669(10) 0.6628(7) 0.1039(3) 0.055(2) Uani 1 1 d . . . H41A H 0.3519 0.6079 0.1323 0.066 Uiso 1 1 calc R . . H41B H 0.3306 0.6205 0.0701 0.066 Uiso 1 1 calc R . . O2 O -0.0028(7) 0.2621(4) 0.3914(2) 0.0543(15) Uani 1 1 d . B . H2A H -0.0589 0.1975 0.3939 0.081 Uiso 1 1 calc R . . C43 C 0.1693(11) 0.2427(9) 0.3802(4) 0.071(3) Uani 1 1 d . . . H43A H 0.2121 0.3025 0.3563 0.086 Uiso 0.50 1 calc PR A 1 H43B H 0.1708 0.1651 0.3617 0.086 Uiso 0.50 1 calc PR A 1 H43C H 0.2343 0.3171 0.3803 0.086 Uiso 0.50 1 d PR A 2 H43D H 0.1718 0.2056 0.3459 0.086 Uiso 0.50 1 d PR A 2 C44 C 0.283(3) 0.247(2) 0.4265(10) 0.074(7) Uani 0.50 1 d P B 1 H44A H 0.3987 0.2348 0.4162 0.111 Uiso 0.50 1 calc PR B 1 H44B H 0.2444 0.1865 0.4498 0.111 Uiso 0.50 1 calc PR B 1 H44C H 0.2835 0.3244 0.4449 0.111 Uiso 0.50 1 calc PR B 1 C44' C 0.252(4) 0.171(2) 0.4204(11) 0.092(9) Uani 0.50 1 d P B 2 H44D H 0.3692 0.1608 0.4116 0.137 Uiso 0.50 1 calc PR B 2 H44E H 0.1879 0.0944 0.4210 0.137 Uiso 0.50 1 calc PR B 2 H44F H 0.2514 0.2114 0.4550 0.137 Uiso 0.50 1 calc PR B 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 C1 0.030(4) 0.049(5) 0.045(5) 0.002(4) -0.004(3) 0.000(4) C2 0.030(4) 0.037(5) 0.030(4) -0.005(3) -0.015(3) 0.003(3) C3 0.027(3) 0.027(4) 0.032(4) 0.005(3) -0.004(3) -0.001(3) C4 0.024(3) 0.022(4) 0.032(4) 0.005(3) -0.015(3) 0.000(3) C5 0.036(4) 0.042(5) 0.044(5) -0.006(4) 0.006(3) 0.006(3) C6 0.039(4) 0.028(4) 0.044(5) -0.001(4) 0.002(3) -0.003(3) C7 0.040(4) 0.017(4) 0.052(5) 0.008(4) -0.001(4) 0.005(3) C8 0.050(4) 0.047(5) 0.028(4) 0.000(4) 0.014(4) 0.003(4) C9 0.053(5) 0.043(5) 0.042(5) 0.002(4) 0.016(4) -0.002(4) C10 0.038(4) 0.024(4) 0.054(5) 0.010(4) -0.003(3) -0.004(3) C11 0.035(4) 0.039(5) 0.039(5) -0.001(4) 0.002(3) 0.001(4) C12 0.036(4) 0.031(4) 0.051(5) 0.008(4) -0.010(4) 0.000(3) C13 0.045(5) 0.057(6) 0.044(5) 0.018(4) 0.013(4) 0.008(4) C14 0.050(5) 0.060(6) 0.042(5) 0.005(4) 0.015(4) 0.005(4) C15 0.030(4) 0.055(5) 0.026(4) 0.002(4) 0.004(3) -0.003(4) C16 0.042(4) 0.063(6) 0.049(5) 0.011(4) 0.007(4) 0.001(4) C17 0.047(5) 0.101(8) 0.031(5) 0.013(5) 0.012(4) 0.000(5) C18 0.048(5) 0.114(9) 0.040(5) 0.015(6) 0.000(4) 0.008(6) C19 0.050(5) 0.087(7) 0.033(5) -0.002(5) 0.014(4) 0.012(5) C20 0.040(4) 0.079(7) 0.033(5) 0.005(4) 0.004(4) 0.003(4) N1 0.031(3) 0.058(4) 0.026(3) 0.000(3) 0.011(3) 0.002(3) N2 0.035(3) 0.047(4) 0.021(3) 0.004(3) 0.011(3) 0.004(3) N3 0.037(3) 0.034(4) 0.030(3) 0.002(3) 0.001(3) -0.002(3) N4 0.035(3) 0.044(4) 0.041(4) 0.008(3) 0.003(3) -0.006(3) N5 0.047(4) 0.030(4) 0.047(4) 0.001(3) 0.006(3) -0.001(3) N6 0.044(4) 0.047(4) 0.039(4) 0.005(3) 0.006(3) -0.001(3) N7 0.036(3) 0.023(3) 0.037(4) 0.005(3) -0.001(3) 0.000(3) N8 0.037(3) 0.044(4) 0.031(4) 0.007(3) 0.001(3) 0.001(3) N9 0.048(4) 0.043(4) 0.044(4) 0.010(3) 0.014(3) 0.003(3) N10 0.047(4) 0.033(4) 0.038(4) 0.013(3) 0.011(3) 0.008(3) C21 0.042(4) 0.031(4) 0.041(5) 0.002(4) -0.003(4) 0.010(4) C22 0.022(3) 0.034(4) 0.031(4) 0.010(3) -0.004(3) -0.003(3) C23 0.030(4) 0.026(4) 0.035(4) -0.003(3) -0.011(3) 0.001(3) C24 0.024(3) 0.019(4) 0.028(4) -0.001(3) -0.003(3) -0.005(3) C25 0.040(4) 0.043(5) 0.050(5) 0.016(4) 0.015(4) 0.001(4) C26 0.033(4) 0.036(5) 0.037(4) 0.005(4) 0.001(3) 0.003(3) C27 0.032(4) 0.024(4) 0.046(5) -0.003(4) -0.005(3) 0.006(3) C28 0.045(4) 0.051(5) 0.032(4) 0.005(4) 0.004(4) -0.001(4) C29 0.048(5) 0.045(5) 0.042(5) 0.001(4) 0.007(4) 0.013(4) C30 0.037(4) 0.021(4) 0.044(4) -0.006(3) 0.009(3) 0.006(3) C31 0.038(4) 0.040(5) 0.050(5) 0.006(4) 0.003(4) 0.002(4) C32 0.041(4) 0.028(4) 0.038(4) 0.005(4) -0.006(3) -0.001(3) C33 0.053(5) 0.040(5) 0.038(5) 0.000(4) 0.017(4) 0.008(4) C34 0.060(5) 0.058(6) 0.034(5) 0.008(4) 0.015(4) 0.009(4) C35 0.032(4) 0.055(5) 0.025(4) 0.000(4) -0.002(3) 0.006(4) C36 0.035(4) 0.063(6) 0.030(4) -0.003(4) 0.001(3) 0.007(4) C37 0.053(5) 0.056(6) 0.041(5) -0.002(4) 0.005(4) 0.019(4) C38 0.044(5) 0.060(6) 0.041(5) 0.004(4) -0.003(4) 0.005(4) C39 0.050(5) 0.046(5) 0.045(5) 0.012(4) 0.006(4) 0.006(4) C40 0.041(4) 0.056(5) 0.044(5) 0.002(4) 0.016(4) 0.004(4) N11 0.026(3) 0.057(4) 0.031(4) 0.010(3) 0.001(3) 0.001(3) N12 0.032(3) 0.048(4) 0.031(3) 0.005(3) 0.003(3) 0.005(3) N13 0.037(3) 0.031(4) 0.040(4) 0.000(3) 0.000(3) 0.011(3) N14 0.035(3) 0.038(4) 0.033(4) -0.004(3) 0.004(3) 0.007(3) N15 0.039(3) 0.039(4) 0.043(4) 0.005(3) 0.000(3) 0.010(3) N16 0.048(4) 0.043(4) 0.029(3) 0.001(3) 0.003(3) 0.015(3) N17 0.039(3) 0.018(3) 0.047(4) -0.002(3) 0.005(3) 0.002(3) N18 0.040(3) 0.040(4) 0.031(3) 0.003(3) 0.009(3) 0.006(3) N19 0.047(4) 0.041(4) 0.050(4) -0.003(3) 0.005(3) -0.002(3) N20 0.055(4) 0.033(4) 0.038(4) 0.007(3) 0.004(3) 0.002(3) C42 0.080(7) 0.071(7) 0.087(8) 0.007(6) 0.026(6) 0.026(6) O1 0.050(3) 0.042(3) 0.056(4) 0.007(3) 0.012(3) 0.004(3) C41 0.047(5) 0.064(6) 0.053(5) 0.009(4) -0.006(4) -0.001(4) O2 0.061(4) 0.042(3) 0.062(4) 0.011(3) 0.011(3) 0.008(3) C43 0.061(6) 0.086(8) 0.067(7) 0.005(6) 0.003(5) 0.008(5) C44 0.060(13) 0.093(19) 0.065(14) -0.021(16) -0.021(10) 0.003(15) C44' 0.10(2) 0.079(19) 0.10(2) -0.017(18) -0.027(15) 0.031(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.315(9) . ? C1 N1 1.348(9) . ? C1 C15 1.519(10) . ? C2 C3 1.360(9) . ? C2 N3 1.376(8) . ? C2 N1 1.380(8) . ? C3 C4 1.377(8) . ? C3 H3 0.9500 . ? C4 N2 1.365(8) . ? C4 N7 1.364(8) . ? C5 N3 1.436(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N4 1.288(8) . ? C6 C7 1.446(10) . ? C6 H6 0.9500 . ? C7 N6 1.341(8) . ? C7 N5 1.345(8) . ? C8 C9 1.352(10) . ? C8 N5 1.363(8) . ? C8 H8 0.9500 . ? C9 N6 1.390(9) . ? C9 H9 0.9500 . ? C10 N7 1.446(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N8 1.280(8) . ? C11 C12 1.465(10) . ? C11 H11 0.9500 . ? C12 N9 1.320(8) . ? C12 N10 1.349(9) . ? C13 C14 1.345(10) . ? C13 N9 1.376(9) . ? C13 H13 0.9500 . ? C14 N10 1.377(9) . ? C14 H14 0.9500 . ? C15 C16 1.370(10) . ? C15 C20 1.376(10) . ? C16 C17 1.396(10) . ? C16 H16 0.9500 . ? C17 C18 1.378(12) . ? C17 H17 0.9500 . ? C18 C19 1.371(12) . ? C18 H18 0.9500 . ? C19 C20 1.406(10) . ? C19 H19 0.9500 . ? C20 H20A 0.9500 . ? N3 N4 1.374(8) . ? N5 H5 0.8800 . ? N7 N8 1.377(8) . ? N10 H10 0.8800 . ? C21 N11 1.331(9) . ? C21 N12 1.334(8) . ? C21 C35 1.481(10) . ? C22 N11 1.366(8) . ? C22 C23 1.371(9) . ? C22 N13 1.371(8) . ? C23 C24 1.365(8) . ? C23 H23 0.9500 . ? C24 N12 1.364(8) . ? C24 N17 1.379(8) . ? C25 N13 1.439(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N14 1.259(8) . ? C26 C27 1.469(10) . ? C26 H26 0.9500 . ? C27 N16 1.322(8) . ? C27 N15 1.352(8) . ? C28 C29 1.340(10) . ? C28 N15 1.379(9) . ? C28 H28 0.9500 . ? C29 N16 1.394(9) . ? C29 H29 0.9500 . ? C30 N17 1.433(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N18 1.278(8) . ? C31 C32 1.470(10) . ? C31 H31 0.9500 . ? C32 N19 1.305(9) . ? C32 N20 1.343(8) . ? C33 C34 1.350(10) . ? C33 N19 1.389(9) . ? C33 H33 0.9500 . ? C34 N20 1.379(9) . ? C34 H34 0.9500 . ? C35 C36 1.371(10) . ? C35 C40 1.392(10) . ? C36 C37 1.408(10) . ? C36 H36 0.9500 . ? C37 C38 1.381(10) . ? C37 H37 0.9500 . ? C38 C39 1.362(10) . ? C38 H38 0.9500 . ? C39 C40 1.405(10) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? N13 N14 1.385(7) . ? N15 H15 0.8800 . ? N17 N18 1.395(7) . ? N20 H20B 0.8800 . ? C42 C41 1.478(11) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O1 C41 1.405(8) . ? O1 H1A 0.8400 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O2 C43 1.433(9) . ? O2 H2A 0.8400 . ? C43 C44 1.45(2) . ? C43 C44' 1.50(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 H43C 0.9600 . ? C43 H43D 0.9599 . ? C44 H43C 1.5100 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 129.2(7) . . ? N2 C1 C15 116.4(7) . . ? N1 C1 C15 114.4(7) . . ? C3 C2 N3 125.8(7) . . ? C3 C2 N1 119.7(7) . . ? N3 C2 N1 114.5(6) . . ? C2 C3 C4 120.9(7) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? N2 C4 N7 114.5(6) . . ? N2 C4 C3 120.4(6) . . ? N7 C4 C3 125.1(6) . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 C7 116.9(7) . . ? N4 C6 H6 121.5 . . ? C7 C6 H6 121.5 . . ? N6 C7 N5 111.4(7) . . ? N6 C7 C6 124.2(7) . . ? N5 C7 C6 124.3(6) . . ? C9 C8 N5 106.2(6) . . ? C9 C8 H8 126.9 . . ? N5 C8 H8 126.9 . . ? C8 C9 N6 110.4(6) . . ? C8 C9 H9 124.8 . . ? N6 C9 H9 124.8 . . ? N7 C10 H10A 109.5 . . ? N7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N8 C11 C12 117.4(7) . . ? N8 C11 H11 121.3 . . ? C12 C11 H11 121.3 . . ? N9 C12 N10 112.9(7) . . ? N9 C12 C11 126.8(7) . . ? N10 C12 C11 120.3(6) . . ? C14 C13 N9 109.7(7) . . ? C14 C13 H13 125.2 . . ? N9 C13 H13 125.2 . . ? C13 C14 N10 107.6(7) . . ? C13 C14 H14 126.2 . . ? N10 C14 H14 126.2 . . ? C16 C15 C20 119.9(7) . . ? C16 C15 C1 119.9(7) . . ? C20 C15 C1 120.1(7) . . ? C15 C16 C17 120.8(9) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 119.1(9) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 120.7(9) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.8(9) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C15 C20 C19 119.7(8) . . ? C15 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C1 N1 C2 114.7(6) . . ? C1 N2 C4 115.0(6) . . ? N4 N3 C2 112.1(6) . . ? N4 N3 C5 121.9(6) . . ? C2 N3 C5 126.0(6) . . ? C6 N4 N3 119.8(6) . . ? C7 N5 C8 107.9(6) . . ? C7 N5 H5 126.1 . . ? C8 N5 H5 126.1 . . ? C7 N6 C9 104.1(6) . . ? C4 N7 N8 114.4(5) . . ? C4 N7 C10 125.0(6) . . ? N8 N7 C10 120.4(6) . . ? C11 N8 N7 121.2(6) . . ? C12 N9 C13 104.7(6) . . ? C12 N10 C14 105.2(6) . . ? C12 N10 H10 127.4 . . ? C14 N10 H10 127.4 . . ? N11 C21 N12 126.6(7) . . ? N11 C21 C35 117.7(7) . . ? N12 C21 C35 115.7(7) . . ? N11 C22 C23 118.9(7) . . ? N11 C22 N13 116.4(6) . . ? C23 C22 N13 124.7(6) . . ? C24 C23 C22 120.5(7) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? N12 C24 C23 120.8(6) . . ? N12 C24 N17 113.5(6) . . ? C23 C24 N17 125.6(6) . . ? N13 C25 H25A 109.5 . . ? N13 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N13 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N14 C26 C27 117.3(6) . . ? N14 C26 H26 121.4 . . ? C27 C26 H26 121.4 . . ? N16 C27 N15 112.9(6) . . ? N16 C27 C26 125.4(6) . . ? N15 C27 C26 121.6(6) . . ? C29 C28 N15 107.0(7) . . ? C29 C28 H28 126.5 . . ? N15 C28 H28 126.5 . . ? C28 C29 N16 110.4(7) . . ? C28 C29 H29 124.8 . . ? N16 C29 H29 124.8 . . ? N17 C30 H30A 109.5 . . ? N17 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N17 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N18 C31 C32 117.5(7) . . ? N18 C31 H31 121.2 . . ? C32 C31 H31 121.2 . . ? N19 C32 N20 114.2(7) . . ? N19 C32 C31 125.6(7) . . ? N20 C32 C31 120.3(7) . . ? C34 C33 N19 108.7(7) . . ? C34 C33 H33 125.7 . . ? N19 C33 H33 125.7 . . ? C33 C34 N20 108.1(7) . . ? C33 C34 H34 126.0 . . ? N20 C34 H34 126.0 . . ? C36 C35 C40 118.9(7) . . ? C36 C35 C21 121.1(7) . . ? C40 C35 C21 120.0(7) . . ? C35 C36 C37 121.7(8) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C38 C37 C36 118.3(8) . . ? C38 C37 H37 120.8 . . ? C36 C37 H37 120.8 . . ? C39 C38 C37 121.0(8) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 120.4(8) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C35 C40 C39 119.7(7) . . ? C35 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C21 N11 C22 117.4(6) . . ? C21 N12 C24 115.6(6) . . ? C22 N13 N14 112.4(6) . . ? C22 N13 C25 125.8(6) . . ? N14 N13 C25 121.6(6) . . ? C26 N14 N13 119.3(6) . . ? C27 N15 C28 105.8(6) . . ? C27 N15 H15 127.1 . . ? C28 N15 H15 127.1 . . ? C27 N16 C29 103.9(6) . . ? C24 N17 N18 113.2(5) . . ? C24 N17 C30 125.0(6) . . ? N18 N17 C30 121.4(5) . . ? C31 N18 N17 119.6(6) . . ? C32 N19 C33 104.6(6) . . ? C32 N20 C34 104.4(6) . . ? C32 N20 H20B 127.8 . . ? C34 N20 H20B 127.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 O1 H1A 109.5 . . ? O1 C41 C42 107.8(7) . . ? O1 C41 H41A 110.1 . . ? C42 C41 H41A 110.1 . . ? O1 C41 H41B 110.1 . . ? C42 C41 H41B 110.1 . . ? H41A C41 H41B 108.5 . . ? C43 O2 H2A 109.5 . . ? O2 C43 C44 113.5(13) . . ? O2 C43 C44' 112.2(14) . . ? C44 C43 C44' 35.3(10) . . ? O2 C43 H43A 108.9 . . ? C44 C43 H43A 108.9 . . ? C44' C43 H43A 134.5 . . ? O2 C43 H43B 108.9 . . ? C44 C43 H43B 108.9 . . ? C44' C43 H43B 76.8 . . ? H43A C43 H43B 107.7 . . ? O2 C43 H43C 108.6 . . ? C44 C43 H43C 74.5 . . ? C44' C43 H43C 107.8 . . ? H43A C43 H43C 38.4 . . ? H43B C43 H43C 136.6 . . ? O2 C43 H43D 109.6 . . ? C44 C43 H43D 133.3 . . ? C44' C43 H43D 110.5 . . ? H43A C43 H43D 72.1 . . ? H43B C43 H43D 37.8 . . ? H43C C43 H43D 108.0 . . ? C43 C44 H43C 37.8 . . ? C43 C44 H44A 109.5 . . ? H43C C44 H44A 96.7 . . ? C43 C44 H44B 109.5 . . ? H43C C44 H44B 145.2 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H43C C44 H44C 81.6 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C44' H44D 109.5 . . ? C43 C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C43 C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? 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 N3 C2 C3 C4 179.4(6) . . . . ? N1 C2 C3 C4 -0.5(9) . . . . ? C2 C3 C4 N2 0.5(9) . . . . ? C2 C3 C4 N7 -179.6(6) . . . . ? N4 C6 C7 N6 -167.9(6) . . . . ? N4 C6 C7 N5 9.3(11) . . . . ? N5 C8 C9 N6 -1.1(9) . . . . ? N8 C11 C12 N9 -8.3(11) . . . . ? N8 C11 C12 N10 171.5(6) . . . . ? N9 C13 C14 N10 -0.2(9) . . . . ? N2 C1 C15 C16 5.7(10) . . . . ? N1 C1 C15 C16 -174.2(6) . . . . ? N2 C1 C15 C20 -176.7(6) . . . . ? N1 C1 C15 C20 3.4(9) . . . . ? C20 C15 C16 C17 -1.0(11) . . . . ? C1 C15 C16 C17 176.6(7) . . . . ? C15 C16 C17 C18 1.6(12) . . . . ? C16 C17 C18 C19 -1.1(13) . . . . ? C17 C18 C19 C20 -0.1(13) . . . . ? C16 C15 C20 C19 -0.2(11) . . . . ? C1 C15 C20 C19 -177.9(7) . . . . ? C18 C19 C20 C15 0.8(12) . . . . ? N2 C1 N1 C2 -2.4(10) . . . . ? C15 C1 N1 C2 177.4(6) . . . . ? C3 C2 N1 C1 1.3(9) . . . . ? N3 C2 N1 C1 -178.6(6) . . . . ? N1 C1 N2 C4 2.5(10) . . . . ? C15 C1 N2 C4 -177.4(6) . . . . ? N7 C4 N2 C1 178.7(6) . . . . ? C3 C4 N2 C1 -1.4(8) . . . . ? C3 C2 N3 N4 4.0(9) . . . . ? N1 C2 N3 N4 -176.1(5) . . . . ? C3 C2 N3 C5 -172.9(6) . . . . ? N1 C2 N3 C5 7.0(9) . . . . ? C7 C6 N4 N3 -178.9(6) . . . . ? C2 N3 N4 C6 -176.3(6) . . . . ? C5 N3 N4 C6 0.7(9) . . . . ? N6 C7 N5 C8 0.0(8) . . . . ? C6 C7 N5 C8 -177.5(7) . . . . ? C9 C8 N5 C7 0.6(8) . . . . ? N5 C7 N6 C9 -0.7(8) . . . . ? C6 C7 N6 C9 176.9(7) . . . . ? C8 C9 N6 C7 1.1(8) . . . . ? N2 C4 N7 N8 174.6(5) . . . . ? C3 C4 N7 N8 -5.3(9) . . . . ? N2 C4 N7 C10 -10.6(8) . . . . ? C3 C4 N7 C10 169.5(6) . . . . ? C12 C11 N8 N7 -179.9(6) . . . . ? C4 N7 N8 C11 177.2(6) . . . . ? C10 N7 N8 C11 2.1(9) . . . . ? N10 C12 N9 C13 0.2(8) . . . . ? C11 C12 N9 C13 -180.0(7) . . . . ? C14 C13 N9 C12 0.0(9) . . . . ? N9 C12 N10 C14 -0.3(8) . . . . ? C11 C12 N10 C14 179.9(6) . . . . ? C13 C14 N10 C12 0.3(8) . . . . ? N11 C22 C23 C24 1.2(9) . . . . ? N13 C22 C23 C24 -177.9(6) . . . . ? C22 C23 C24 N12 2.3(9) . . . . ? C22 C23 C24 N17 -179.6(6) . . . . ? N14 C26 C27 N16 -167.9(6) . . . . ? N14 C26 C27 N15 7.0(10) . . . . ? N15 C28 C29 N16 0.4(8) . . . . ? N18 C31 C32 N19 -9.9(11) . . . . ? N18 C31 C32 N20 170.0(6) . . . . ? N19 C33 C34 N20 -0.7(9) . . . . ? N11 C21 C35 C36 174.6(6) . . . . ? N12 C21 C35 C36 -6.1(10) . . . . ? N11 C21 C35 C40 -4.4(10) . . . . ? N12 C21 C35 C40 174.9(6) . . . . ? C40 C35 C36 C37 -0.6(11) . . . . ? C21 C35 C36 C37 -179.6(7) . . . . ? C35 C36 C37 C38 -0.3(11) . . . . ? C36 C37 C38 C39 0.1(11) . . . . ? C37 C38 C39 C40 1.0(12) . . . . ? C36 C35 C40 C39 1.6(11) . . . . ? C21 C35 C40 C39 -179.4(7) . . . . ? C38 C39 C40 C35 -1.8(11) . . . . ? N12 C21 N11 C22 -0.7(10) . . . . ? C35 C21 N11 C22 178.6(6) . . . . ? C23 C22 N11 C21 -2.0(9) . . . . ? N13 C22 N11 C21 177.2(6) . . . . ? N11 C21 N12 C24 4.0(10) . . . . ? C35 C21 N12 C24 -175.3(6) . . . . ? C23 C24 N12 C21 -4.7(9) . . . . ? N17 C24 N12 C21 177.0(6) . . . . ? N11 C22 N13 N14 -176.2(5) . . . . ? C23 C22 N13 N14 3.0(9) . . . . ? N11 C22 N13 C25 8.1(9) . . . . ? C23 C22 N13 C25 -172.7(6) . . . . ? C27 C26 N14 N13 -179.0(6) . . . . ? C22 N13 N14 C26 -177.9(6) . . . . ? C25 N13 N14 C26 -2.0(9) . . . . ? N16 C27 N15 C28 -1.1(8) . . . . ? C26 C27 N15 C28 -176.6(6) . . . . ? C29 C28 N15 C27 0.4(8) . . . . ? N15 C27 N16 C29 1.3(8) . . . . ? C26 C27 N16 C29 176.6(7) . . . . ? C28 C29 N16 C27 -1.0(8) . . . . ? N12 C24 N17 N18 174.1(5) . . . . ? C23 C24 N17 N18 -4.2(9) . . . . ? N12 C24 N17 C30 -12.5(9) . . . . ? C23 C24 N17 C30 169.2(6) . . . . ? C32 C31 N18 N17 179.5(6) . . . . ? C24 N17 N18 C31 176.4(6) . . . . ? C30 N17 N18 C31 2.7(9) . . . . ? N20 C32 N19 C33 -0.3(8) . . . . ? C31 C32 N19 C33 179.7(7) . . . . ? C34 C33 N19 C32 0.6(8) . . . . ? N19 C32 N20 C34 -0.1(8) . . . . ? C31 C32 N20 C34 179.9(6) . . . . ? C33 C34 N20 C32 0.5(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5 O1 0.88 1.92 2.757(7) 158.8 . N10 H10 N6 0.88 1.92 2.762(8) 159.9 1_545 N15 H15 O2 0.88 1.96 2.760(8) 150.4 . N20 H20B N16 0.88 1.93 2.770(8) 160.0 1_545 O1 H1A N9 0.84 1.88 2.721(8) 177.7 . O2 H2A N19 0.84 1.90 2.734(8) 171.3 . _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.539 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.095 # Attachment '- as22.cif' data_as22 _database_code_depnum_ccdc_archive 'CCDC 826151' #TrackingRef '- as22.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H98 B8 F32 Fe4 N52 O3.50' _chemical_formula_weight 3050.22 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' B B 0.0013 0.0007 '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' Fe Fe 0.3463 0.8444 '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 Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 18.5204(3) _cell_length_b 27.2996(5) _cell_length_c 29.4421(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14885.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 65732 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6184 _exptl_absorpt_coefficient_mu 0.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8052 _exptl_absorpt_correction_T_max 0.8380 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi&omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86112 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.1136 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.49 _reflns_number_total 33805 _reflns_number_gt 19378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker 8.6' _computing_publication_material 'CrystalMaker 8.6' _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. geometrical restraints were used for the refinement of the disordered solvent molecules ; _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^)+(0.1369P)^2^+5.5254P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.054(17) _refine_ls_number_reflns 33805 _refine_ls_number_parameters 1911 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.1674 _refine_ls_R_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.2546 _refine_ls_wR_factor_gt 0.2181 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.037 _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 C1 C 0.7977(5) 0.0987(3) 0.5396(3) 0.059(2) Uani 1 1 d . . . H1 H 0.8134 0.0656 0.5392 0.071 Uiso 1 1 calc R . . C2 C 0.7610(5) 0.1722(3) 0.5163(3) 0.066(2) Uani 1 1 d . . . H2 H 0.7467 0.1988 0.4976 0.079 Uiso 1 1 calc R . . C3 C 0.7657(4) 0.1717(3) 0.5631(2) 0.0480(17) Uani 1 1 d . . . C4 C 0.7536(4) 0.2082(3) 0.5968(2) 0.0444(16) Uani 1 1 d . . . H4 H 0.7392 0.2407 0.5896 0.053 Uiso 1 1 calc R . . C5 C 0.7289(4) 0.2753(2) 0.6680(2) 0.0485(17) Uani 1 1 d . . . H5A H 0.7283 0.2830 0.6355 0.073 Uiso 1 1 calc R . . H5B H 0.7627 0.2972 0.6835 0.073 Uiso 1 1 calc R . . H5C H 0.6804 0.2798 0.6806 0.073 Uiso 1 1 calc R . . C6 C 0.7578(3) 0.2023(2) 0.7160(2) 0.0370(14) Uani 1 1 d . . . C7 C 0.7431(3) 0.2269(2) 0.7567(2) 0.0420(15) Uani 1 1 d . . . H7 H 0.7272 0.2600 0.7568 0.050 Uiso 1 1 calc R . . C8 C 0.7526(3) 0.2014(2) 0.7963(2) 0.0352(14) Uani 1 1 d . . . C9 C 0.7837(3) 0.1326(2) 0.7567(2) 0.0351(13) Uani 1 1 d . . . C10 C 0.8011(4) 0.0789(2) 0.7558(2) 0.0449(15) Uani 1 1 d . . . C11 C 0.7431(4) 0.0454(2) 0.7572(3) 0.0477(16) Uani 1 1 d . . . H11 H 0.6948 0.0570 0.7580 0.057 Uiso 1 1 calc R . . C12 C 0.7566(5) -0.0038(3) 0.7575(3) 0.068(2) Uani 1 1 d . . . H12 H 0.7177 -0.0264 0.7589 0.082 Uiso 1 1 calc R . . C13 C 0.8271(6) -0.0208(3) 0.7557(3) 0.074(3) Uani 1 1 d . . . H13 H 0.8362 -0.0551 0.7557 0.089 Uiso 1 1 calc R . . C14 C 0.8853(5) 0.0122(3) 0.7537(3) 0.069(2) Uani 1 1 d . . . H14 H 0.9335 0.0006 0.7514 0.082 Uiso 1 1 calc R . . C15 C 0.8710(4) 0.0621(2) 0.7552(3) 0.0519(17) Uani 1 1 d . . . H15 H 0.9098 0.0848 0.7559 0.062 Uiso 1 1 calc R . . C16 C 0.7146(4) 0.2716(3) 0.8442(3) 0.057(2) Uani 1 1 d . . . H16A H 0.7078 0.2779 0.8767 0.086 Uiso 1 1 calc R . . H16B H 0.6687 0.2763 0.8283 0.086 Uiso 1 1 calc R . . H16C H 0.7508 0.2943 0.8321 0.086 Uiso 1 1 calc R . . C17 C 0.7357(4) 0.2053(3) 0.9147(2) 0.0452(16) Uani 1 1 d . . . H17 H 0.7188 0.2373 0.9217 0.054 Uiso 1 1 calc R . . C18 C 0.7497(4) 0.1689(3) 0.9497(2) 0.0456(17) Uani 1 1 d . . . C19 C 0.7443(5) 0.1691(3) 0.9942(3) 0.058(2) Uani 1 1 d . . . H19 H 0.7300 0.1959 1.0128 0.070 Uiso 1 1 calc R . . C20 C 0.7807(4) 0.0983(3) 0.9730(3) 0.0542(19) Uani 1 1 d . . . H20 H 0.7976 0.0654 0.9746 0.065 Uiso 1 1 calc R . . C21 C 0.6189(4) 0.0995(3) 0.6588(3) 0.059(2) Uani 1 1 d . . . H21 H 0.6017 0.1317 0.6642 0.070 Uiso 1 1 calc R . . C22 C 0.6205(4) 0.0196(3) 0.6486(3) 0.066(2) Uani 1 1 d . . . H22 H 0.6060 -0.0136 0.6455 0.079 Uiso 1 1 calc R . . C23 C 0.6892(4) 0.0375(2) 0.6472(2) 0.0446(16) Uani 1 1 d . . . C24 C 0.7579(4) 0.0127(3) 0.6428(3) 0.0501(17) Uani 1 1 d . . . H24 H 0.7618 -0.0217 0.6389 0.060 Uiso 1 1 calc R . . C25 C 0.8948(4) -0.0299(2) 0.6389(4) 0.070(2) Uani 1 1 d . . . H25A H 0.8483 -0.0470 0.6398 0.105 Uiso 1 1 calc R . . H25B H 0.9246 -0.0405 0.6646 0.105 Uiso 1 1 calc R . . H25C H 0.9197 -0.0375 0.6104 0.105 Uiso 1 1 calc R . . C26 C 0.9364(4) 0.0563(2) 0.6414(2) 0.0447(16) Uani 1 1 d . . . C27 C 1.0077(3) 0.0435(2) 0.6371(2) 0.0438(16) Uani 1 1 d . . . H27 H 1.0222 0.0103 0.6344 0.053 Uiso 1 1 calc R . . C28 C 1.0574(3) 0.0811(2) 0.6368(2) 0.0438(16) Uani 1 1 d . . . C29 C 0.9665(3) 0.1383(2) 0.6415(2) 0.0384(14) Uani 1 1 d . . . C30 C 0.9466(3) 0.1906(2) 0.6397(2) 0.0383(14) Uani 1 1 d . . . C31 C 0.9396(4) 0.2117(3) 0.5976(3) 0.0516(18) Uani 1 1 d . . . H31 H 0.9470 0.1929 0.5708 0.062 Uiso 1 1 calc R . . C32 C 0.9206(4) 0.2631(3) 0.5946(3) 0.066(2) Uani 1 1 d . . . H32 H 0.9152 0.2784 0.5658 0.079 Uiso 1 1 calc R . . C33 C 0.9107(4) 0.2888(3) 0.6326(4) 0.075(3) Uani 1 1 d . . . H33 H 0.8988 0.3226 0.6307 0.090 Uiso 1 1 calc R . . C34 C 0.9177(5) 0.2664(3) 0.6758(3) 0.070(2) Uani 1 1 d . . . H34 H 0.9111 0.2851 0.7027 0.084 Uiso 1 1 calc R . . C35 C 0.9341(4) 0.2175(2) 0.6784(3) 0.0469(17) Uani 1 1 d . . . H35 H 0.9369 0.2021 0.7072 0.056 Uiso 1 1 calc R . . C36 C 1.1605(4) 0.0222(3) 0.6305(3) 0.065(2) Uani 1 1 d . . . H36A H 1.2133 0.0242 0.6285 0.097 Uiso 1 1 calc R . . H36B H 1.1416 0.0053 0.6037 0.097 Uiso 1 1 calc R . . H36C H 1.1469 0.0040 0.6579 0.097 Uiso 1 1 calc R . . C37 C 1.2427(4) 0.1087(3) 0.6316(3) 0.057(2) Uani 1 1 d . . . H37 H 1.2670 0.0783 0.6279 0.068 Uiso 1 1 calc R . . C38 C 1.2807(4) 0.1547(2) 0.6342(3) 0.0485(17) Uani 1 1 d . . . C39 C 1.3529(5) 0.1653(3) 0.6345(3) 0.069(2) Uani 1 1 d . . . H39 H 1.3921 0.1429 0.6334 0.082 Uiso 1 1 calc R . . C40 C 1.2884(4) 0.2329(3) 0.6393(2) 0.0504(17) Uani 1 1 d . . . H40 H 1.2769 0.2667 0.6421 0.060 Uiso 1 1 calc R . . C41 C 1.1334(5) 0.1666(3) 0.5258(3) 0.060(2) Uani 1 1 d . . . H41 H 1.1445 0.1327 0.5246 0.072 Uiso 1 1 calc R . . C42 C 1.1085(5) 0.2425(4) 0.5029(3) 0.072(3) Uani 1 1 d . . . H42 H 1.0991 0.2703 0.4844 0.087 Uiso 1 1 calc R . . C43 C 1.1092(4) 0.2391(3) 0.5491(3) 0.0565(19) Uani 1 1 d . . . C44 C 1.0986(4) 0.2756(3) 0.5837(3) 0.0527(19) Uani 1 1 d . . . H44 H 1.0894 0.3090 0.5765 0.063 Uiso 1 1 calc R . . C45 C 1.0852(5) 0.3430(2) 0.6534(3) 0.0554(19) Uani 1 1 d . . . H45A H 1.0837 0.3495 0.6207 0.083 Uiso 1 1 calc R . . H45B H 1.1265 0.3601 0.6669 0.083 Uiso 1 1 calc R . . H45C H 1.0405 0.3546 0.6675 0.083 Uiso 1 1 calc R . . C46 C 1.0973(3) 0.2693(2) 0.7026(2) 0.0415(16) Uani 1 1 d . . . C47 C 1.0851(3) 0.2944(2) 0.7429(2) 0.0416(15) Uani 1 1 d . . . H47 H 1.0738 0.3283 0.7424 0.050 Uiso 1 1 calc R . . C48 C 1.0896(3) 0.2699(2) 0.7831(2) 0.0347(14) Uani 1 1 d . . . C49 C 1.1174(3) 0.19973(19) 0.7443(2) 0.0335(13) Uani 1 1 d . . . C50 C 1.1421(4) 0.1473(2) 0.7454(2) 0.0456(16) Uani 1 1 d . . . C51 C 1.2161(5) 0.1389(3) 0.7446(3) 0.065(2) Uani 1 1 d . . . H51 H 1.2486 0.1658 0.7438 0.078 Uiso 1 1 calc R . . C52 C 1.2427(7) 0.0911(4) 0.7447(4) 0.100(4) Uani 1 1 d . . . H52 H 1.2930 0.0844 0.7431 0.119 Uiso 1 1 calc R . . C53 C 1.1895(8) 0.0519(3) 0.7475(4) 0.108(4) Uani 1 1 d . . . H53 H 1.2058 0.0189 0.7487 0.129 Uiso 1 1 calc R . . C54 C 1.1176(8) 0.0610(3) 0.7484(3) 0.093(4) Uani 1 1 d . . . H54 H 1.0841 0.0347 0.7498 0.111 Uiso 1 1 calc R . . C55 C 1.0930(5) 0.1093(2) 0.7472(3) 0.060(2) Uani 1 1 d . . . H55 H 1.0427 0.1160 0.7476 0.072 Uiso 1 1 calc R . . C56 C 1.0701(5) 0.3460(2) 0.8288(3) 0.0532(19) Uani 1 1 d . . . H56A H 1.0635 0.3540 0.8609 0.080 Uiso 1 1 calc R . . H56B H 1.0272 0.3560 0.8116 0.080 Uiso 1 1 calc R . . H56C H 1.1125 0.3634 0.8170 0.080 Uiso 1 1 calc R . . C57 C 1.0782(4) 0.2803(3) 0.9016(3) 0.0504(18) Uani 1 1 d . . . H57 H 1.0667 0.3137 0.9070 0.060 Uiso 1 1 calc R . . C58 C 1.0873(4) 0.2454(3) 0.9377(2) 0.0430(16) Uani 1 1 d . . . C59 C 1.0827(5) 0.2487(3) 0.9829(3) 0.060(2) Uani 1 1 d . . . H59 H 1.0707 0.2771 0.9999 0.072 Uiso 1 1 calc R . . C60 C 1.1101(5) 0.1738(3) 0.9643(3) 0.056(2) Uani 1 1 d . . . H60 H 1.1216 0.1401 0.9674 0.067 Uiso 1 1 calc R . . C61 C 0.6086(4) 0.0952(3) 0.8540(3) 0.0546(18) Uani 1 1 d . . . H61 H 0.5903 0.1271 0.8485 0.066 Uiso 1 1 calc R . . C62 C 0.6118(4) 0.0162(3) 0.8653(3) 0.061(2) Uani 1 1 d . . . H62 H 0.5974 -0.0169 0.8693 0.073 Uiso 1 1 calc R . . C63 C 0.6793(4) 0.0340(2) 0.8665(2) 0.0450(16) Uani 1 1 d . . . C64 C 0.7479(4) 0.0122(3) 0.8705(2) 0.0472(17) Uani 1 1 d . . . H64 H 0.7530 -0.0220 0.8755 0.057 Uiso 1 1 calc R . . C65 C 0.8864(4) -0.0305(2) 0.8740(3) 0.062(2) Uani 1 1 d . . . H65A H 0.8406 -0.0479 0.8777 0.093 Uiso 1 1 calc R . . H65B H 0.9175 -0.0369 0.9002 0.093 Uiso 1 1 calc R . . H65C H 0.9104 -0.0418 0.8463 0.093 Uiso 1 1 calc R . . C66 C 0.9249(4) 0.0569(2) 0.8645(2) 0.0394(15) Uani 1 1 d . . . C67 C 0.9963(3) 0.0453(2) 0.8627(3) 0.0474(17) Uani 1 1 d . . . H67 H 1.0108 0.0120 0.8646 0.057 Uiso 1 1 calc R . . C68 C 1.0488(4) 0.0822(3) 0.8581(2) 0.0449(16) Uani 1 1 d . . . C69 C 0.9545(3) 0.1392(2) 0.8570(2) 0.0385(14) Uani 1 1 d . . . C70 C 0.9326(3) 0.1911(2) 0.8548(2) 0.0363(14) Uani 1 1 d . . . C71 C 0.9148(4) 0.2159(3) 0.8943(3) 0.0528(18) Uani 1 1 d . . . H71 H 0.9130 0.1989 0.9224 0.063 Uiso 1 1 calc R . . C72 C 0.8996(4) 0.2656(3) 0.8928(4) 0.068(2) Uani 1 1 d . . . H72 H 0.8903 0.2830 0.9201 0.082 Uiso 1 1 calc R . . C73 C 0.8980(4) 0.2901(3) 0.8511(4) 0.068(2) Uani 1 1 d . . . H73 H 0.8862 0.3239 0.8500 0.081 Uiso 1 1 calc R . . C74 C 0.9134(4) 0.2654(3) 0.8120(3) 0.067(2) Uani 1 1 d . . . H74 H 0.9110 0.2821 0.7837 0.081 Uiso 1 1 calc R . . C75 C 0.9328(4) 0.2156(3) 0.8130(3) 0.0535(19) Uani 1 1 d . . . H75 H 0.9457 0.1989 0.7859 0.064 Uiso 1 1 calc R . . C76 C 1.1509(4) 0.0248(3) 0.8600(4) 0.068(2) Uani 1 1 d . . . H76A H 1.2036 0.0280 0.8601 0.102 Uiso 1 1 calc R . . H76B H 1.1358 0.0056 0.8335 0.102 Uiso 1 1 calc R . . H76C H 1.1353 0.0081 0.8878 0.102 Uiso 1 1 calc R . . C77 C 1.2319(4) 0.1122(3) 0.8576(3) 0.0507(17) Uani 1 1 d . . . H77 H 1.2565 0.0818 0.8598 0.061 Uiso 1 1 calc R . . C78 C 1.2687(3) 0.1573(2) 0.8559(3) 0.0472(16) Uani 1 1 d . . . C79 C 1.3389(4) 0.1708(3) 0.8579(3) 0.0542(18) Uani 1 1 d . . . H79 H 1.3794 0.1495 0.8595 0.065 Uiso 1 1 calc R . . C80 C 1.2720(4) 0.2367(3) 0.8563(2) 0.0501(17) Uani 1 1 d . . . H80 H 1.2587 0.2703 0.8569 0.060 Uiso 1 1 calc R . . C101 C 0.9942(8) 0.0787(6) 0.5095(5) 0.126(5) Uani 1 1 d . . . C102 C 1.0241(10) 0.0396(6) 0.4832(5) 0.166(7) Uani 1 1 d . . . H10A H 1.0152 0.0083 0.4986 0.248 Uiso 1 1 calc R . . H10B H 1.0762 0.0445 0.4798 0.248 Uiso 1 1 calc R . . H10C H 1.0014 0.0391 0.4532 0.248 Uiso 1 1 calc R . . C105 C 1.3183(8) 0.1824(5) 0.9846(4) 0.107(4) Uani 1 1 d . . . C106 C 1.3684(8) 0.1442(6) 0.9715(4) 0.137(6) Uani 1 1 d . . . H10D H 1.4163 0.1515 0.9838 0.205 Uiso 1 1 calc R . . H10E H 1.3711 0.1425 0.9383 0.205 Uiso 1 1 calc R . . H10F H 1.3516 0.1127 0.9834 0.205 Uiso 1 1 calc R . . C107 C 0.4929(15) -0.0192(17) 0.7530(9) 0.55(6) Uani 1 1 d D . . C108 C 0.414(2) -0.0035(19) 0.7507(9) 0.62(6) Uani 1 1 d D . . C109 C 1.3026(6) 0.3009(5) 0.7468(3) 0.096(3) Uani 1 1 d . . . C110 C 1.3395(9) 0.3475(5) 0.7450(4) 0.133(5) Uani 1 1 d . . . H11A H 1.3723 0.3504 0.7709 0.200 Uiso 1 1 calc R . . H11B H 1.3040 0.3741 0.7460 0.200 Uiso 1 1 calc R . . H11C H 1.3673 0.3497 0.7167 0.200 Uiso 1 1 calc R . . C111 C 0.8836(7) -0.0456(4) 0.5011(4) 0.097(3) Uani 1 1 d . . . C112 C 0.9222(7) -0.0871(5) 0.4778(4) 0.108(4) Uani 1 1 d . . . H11D H 0.8917 -0.1002 0.4535 0.163 Uiso 1 1 calc R . . H11E H 0.9323 -0.1131 0.4999 0.163 Uiso 1 1 calc R . . H11F H 0.9677 -0.0752 0.4649 0.163 Uiso 1 1 calc R . . C115 C 0.9338(9) 0.1545(7) 1.0082(5) 0.139(5) Uani 1 1 d DU . . C116 C 0.9164(10) 0.1927(8) 1.0445(6) 0.196(7) Uani 1 1 d DU . . C117 C 1.4836(9) 0.1744(8) 0.7514(7) 0.33(3) Uani 1 1 d D . . C118 C 1.5400(17) 0.1335(9) 0.7539(6) 0.32(2) Uani 1 1 d D . . C119 C 1.219(3) 0.0444(16) 0.985(2) 0.274(12) Uani 0.50 1 d PDU A 1 C120 C 1.281(2) 0.0148(19) 1.0057(16) 0.275(15) Uani 0.50 1 d PDU A 1 C220 C 1.2328(17) 0.0546(14) 1.0458(14) 0.181(18) Uani 0.50 1 d P A 2 C219 C 1.200(3) 0.056(2) 1.0050(16) 0.29(4) Uani 0.50 1 d P A 2 O4W O 1.2939(16) -0.0550(7) 1.0174(7) 0.177(11) Uani 0.50 1 d P B 2 B1 B 0.7776(6) 0.1252(3) 1.1295(3) 0.060(2) Uani 1 1 d . . . B2 B 0.3862(8) 0.0218(6) 0.8760(6) 0.104(5) Uani 1 1 d . . . B3 B 0.3971(8) 0.0192(5) 0.6299(8) 0.119(6) Uani 1 1 d . . . B4 B 0.7914(6) 0.1287(3) 0.3827(3) 0.062(3) Uani 1 1 d . . . B5 B 1.5505(8) 0.2275(5) 0.6274(6) 0.096(4) Uani 1 1 d . . . B6 B 1.5332(6) 0.2234(4) 0.8840(5) 0.080(3) Uani 1 1 d . . . B7 B 1.0617(5) -0.0898(3) 0.5824(3) 0.059(2) Uani 1 1 d . . . B8 B 0.9493(8) 0.4149(5) 0.7248(5) 0.088(3) Uani 1 1 d . . . F1 F 0.8020(3) 0.08966(17) 1.09944(15) 0.0779(15) Uani 1 1 d . . . F2 F 0.7276(3) 0.1538(2) 1.10506(17) 0.0857(15) Uani 1 1 d . . . F3 F 0.8348(3) 0.15626(17) 1.14272(19) 0.0762(13) Uani 1 1 d . . . F4 F 0.7458(3) 0.10478(19) 1.16623(16) 0.0854(16) Uani 1 1 d . . . F5 F 0.4367(3) -0.0126(2) 0.8715(2) 0.0957(18) Uani 1 1 d . . . F6 F 0.4122(3) 0.0642(2) 0.8616(4) 0.151(4) Uani 1 1 d . . . F7 F 0.3294(4) 0.0107(3) 0.8464(6) 0.211(6) Uani 1 1 d . . . F8 F 0.3541(9) 0.0276(5) 0.9118(5) 0.280(9) Uani 1 1 d . . . F9 F 0.4535(4) -0.0159(2) 0.6325(3) 0.125(2) Uani 1 1 d . . . F10 F 0.4262(3) 0.0609(2) 0.6481(4) 0.161(4) Uani 1 1 d . . . F11 F 0.3729(11) 0.0271(6) 0.5899(4) 0.305(10) Uani 1 1 d . . . F12 F 0.3414(4) 0.0059(4) 0.6508(5) 0.209(6) Uani 1 1 d . . . F13 F 0.8178(3) 0.09257(17) 0.41138(16) 0.0840(16) Uani 1 1 d . . . F14 F 0.7445(3) 0.1589(2) 0.40763(18) 0.0869(16) Uani 1 1 d . . . F15 F 0.8457(3) 0.15692(19) 0.36592(18) 0.0833(15) Uani 1 1 d . . . F16 F 0.7526(3) 0.1073(2) 0.34712(18) 0.0908(16) Uani 1 1 d . . . F17 F 1.5181(4) 0.1857(3) 0.6123(5) 0.218(6) Uani 1 1 d . . . F18 F 1.4929(2) 0.25956(17) 0.6404(2) 0.0817(15) Uani 1 1 d . . . F19 F 1.5897(3) 0.2130(2) 0.6641(2) 0.102(2) Uani 1 1 d . . . F20 F 1.5922(3) 0.2505(3) 0.59898(19) 0.122(3) Uani 1 1 d . . . F21 F 1.4969(4) 0.1839(3) 0.8983(4) 0.163(4) Uani 1 1 d . . . F22 F 1.4812(3) 0.2563(2) 0.8659(2) 0.0981(18) Uani 1 1 d . . . F23 F 1.5753(3) 0.2102(2) 0.8462(2) 0.0984(18) Uani 1 1 d . . . F24 F 1.5759(3) 0.2470(3) 0.91409(19) 0.113(2) Uani 1 1 d . . . F25 F 1.0535(3) -0.07731(17) 0.62651(17) 0.0746(13) Uani 1 1 d . . . F26 F 1.0590(4) -0.05028(19) 0.5547(2) 0.104(2) Uani 1 1 d . . . F27 F 1.0079(4) -0.1226(2) 0.56920(19) 0.1023(19) Uani 1 1 d . . . F28 F 1.1271(4) -0.1141(3) 0.5778(2) 0.117(2) Uani 1 1 d . . . F29 F 0.9239(4) 0.3701(2) 0.7322(3) 0.144(3) Uani 1 1 d . . . F30 F 0.9489(7) 0.4277(4) 0.6797(4) 0.209(5) Uani 1 1 d . . . F31 F 0.9142(5) 0.4493(2) 0.7468(4) 0.202(5) Uani 1 1 d . . . F32 F 1.0240(4) 0.4126(2) 0.7355(3) 0.118(2) Uani 1 1 d . . . Fe1 Fe 0.79620(5) 0.11878(3) 0.64951(3) 0.0382(2) Uani 1 1 d . . . Fe2 Fe 1.11197(5) 0.18651(3) 0.85272(3) 0.0375(2) Uani 1 1 d . . . Fe3 Fe 0.78325(5) 0.11720(3) 0.86233(3) 0.0389(2) Uani 1 1 d . . . Fe4 Fe 1.12649(5) 0.18391(3) 0.63657(3) 0.0399(2) Uani 1 1 d . . . N1 N 0.7815(4) 0.1256(3) 0.5024(2) 0.072(2) Uani 1 1 d . . . H1A H 0.7835 0.1154 0.4741 0.086 Uiso 1 1 calc R . . N2 N 0.7885(3) 0.1255(2) 0.57694(18) 0.0448(13) Uani 1 1 d . . . N3 N 0.7634(3) 0.19391(18) 0.63732(18) 0.0364(12) Uani 1 1 d . . . N4 N 0.7519(3) 0.22421(19) 0.67449(17) 0.0394(13) Uani 1 1 d . . . N5 N 0.7801(3) 0.1547(2) 0.71529(18) 0.0431(13) Uani 1 1 d . . . N6 N 0.7726(3) 0.15301(18) 0.79630(18) 0.0363(12) Uani 1 1 d . . . N7 N 0.7388(3) 0.2223(2) 0.83791(19) 0.0431(13) Uani 1 1 d . . . N8 N 0.7475(3) 0.19146(19) 0.87410(18) 0.0387(12) Uani 1 1 d . . . N9 N 0.7729(3) 0.1225(2) 0.93443(19) 0.0456(14) Uani 1 1 d . . . N10 N 0.7629(4) 0.1238(3) 1.0083(2) 0.0633(17) Uani 1 1 d . . . H10 H 0.7630 0.1134 1.0366 0.076 Uiso 1 1 calc R . . N11 N 0.5772(4) 0.0589(3) 0.6553(3) 0.079(2) Uani 1 1 d . . . H111 H 0.5297 0.0581 0.6570 0.095 Uiso 1 1 calc R . . N12 N 0.6880(3) 0.0870(2) 0.6535(2) 0.0449(13) Uani 1 1 d . . . N13 N 0.8130(3) 0.04106(19) 0.6446(2) 0.0420(13) Uani 1 1 d . . . N14 N 0.8827(3) 0.02265(18) 0.6419(2) 0.0462(14) Uani 1 1 d . . . N15 N 0.9152(3) 0.10523(17) 0.64506(17) 0.0353(11) Uani 1 1 d . . . N16 N 1.0380(3) 0.12904(18) 0.63892(17) 0.0379(12) Uani 1 1 d . . . N17 N 1.1301(3) 0.07198(19) 0.6327(2) 0.0497(15) Uani 1 1 d . . . N18 N 1.1739(3) 0.1117(2) 0.6345(2) 0.0441(13) Uani 1 1 d . . . N19 N 1.2400(3) 0.1967(2) 0.6371(2) 0.0444(13) Uani 1 1 d . . . N20 N 1.3561(3) 0.2148(2) 0.6368(2) 0.0580(16) Uani 1 1 d . . . H20A H 1.3960 0.2323 0.6367 0.070 Uiso 1 1 calc R . . N21 N 1.1250(4) 0.1948(3) 0.4895(2) 0.0691(19) Uani 1 1 d . . . H21A H 1.1293 0.1848 0.4612 0.083 Uiso 1 1 calc R . . N22 N 1.1248(3) 0.1909(2) 0.5631(2) 0.0492(14) Uani 1 1 d . . . N23 N 1.1021(3) 0.2606(2) 0.62464(19) 0.0437(13) Uani 1 1 d . . . N24 N 1.0926(3) 0.29122(18) 0.66098(19) 0.0423(13) Uani 1 1 d . . . N25 N 1.1134(3) 0.22025(18) 0.70284(18) 0.0383(12) Uani 1 1 d . . . N26 N 1.1052(3) 0.22067(18) 0.78459(18) 0.0367(12) Uani 1 1 d . . . N27 N 1.0810(3) 0.2929(2) 0.82379(18) 0.0422(13) Uani 1 1 d . . . N28 N 1.0868(3) 0.26291(17) 0.86084(18) 0.0349(11) Uani 1 1 d . . . N29 N 1.1037(3) 0.1966(2) 0.92512(18) 0.0442(13) Uani 1 1 d . . . N30 N 1.0984(4) 0.2041(3) 0.9997(2) 0.0630(18) Uani 1 1 d . . . H30 H 1.1006 0.1962 1.0287 0.076 Uiso 1 1 calc R . . N31 N 0.5680(3) 0.0553(3) 0.8572(3) 0.075(2) Uani 1 1 d . . . H31A H 0.5207 0.0543 0.8545 0.090 Uiso 1 1 calc R . . N32 N 0.6751(3) 0.0852(2) 0.8594(2) 0.0515(14) Uani 1 1 d . . . N33 N 0.8020(3) 0.03971(18) 0.86721(19) 0.0407(12) Uani 1 1 d . . . N34 N 0.8723(3) 0.02304(19) 0.8705(2) 0.0468(14) Uani 1 1 d . . . N35 N 0.9020(3) 0.10517(18) 0.86157(18) 0.0398(12) Uani 1 1 d . . . N36 N 1.0249(3) 0.13064(17) 0.85442(17) 0.0388(12) Uani 1 1 d . . . N37 N 1.1180(3) 0.07362(18) 0.8580(2) 0.0430(13) Uani 1 1 d . . . N38 N 1.1626(3) 0.11505(18) 0.8559(2) 0.0418(12) Uani 1 1 d . . . N39 N 1.2264(3) 0.2009(2) 0.8548(2) 0.0463(13) Uani 1 1 d . . . N40 N 1.3408(3) 0.2208(2) 0.8571(2) 0.0577(16) Uani 1 1 d . . . H40A H 1.3799 0.2392 0.8570 0.069 Uiso 1 1 calc R . . N51 N 0.9720(6) 0.1060(5) 0.5317(4) 0.131(4) Uani 1 1 d . . . N53 N 1.2804(8) 0.2092(4) 0.9973(6) 0.155(6) Uani 1 1 d . . . N54 N 0.5494(14) -0.0347(11) 0.7593(8) 0.276(14) Uani 1 1 d D . . N55 N 1.2740(7) 0.2640(5) 0.7477(4) 0.137(4) Uani 1 1 d . . . N56 N 0.8547(6) -0.0162(5) 0.5202(6) 0.166(6) Uani 1 1 d . . . N58 N 0.9483(8) 0.1305(6) 0.9766(5) 0.149(4) Uani 1 1 d U . . N59 N 1.4574(16) 0.2126(8) 0.7518(12) 0.38(2) Uani 1 1 d D . . N60 N 1.1696(16) 0.0594(7) 0.9667(6) 0.268(11) Uani 1 1 d DU . . C103 C 1.0635(10) 0.1360(6) 1.1186(5) 0.082(6) Uani 0.50 1 d PD C 1 C104 C 1.0191(13) 0.1300(8) 1.1617(7) 0.111(9) Uani 0.50 1 d PD C 1 H10J H 1.0380 0.1518 1.1853 0.166 Uiso 0.50 1 calc PR C 1 H10K H 1.0221 0.0959 1.1721 0.166 Uiso 0.50 1 calc PR C 1 H10L H 0.9686 0.1383 1.1554 0.166 Uiso 0.50 1 calc PR C 1 N52 N 1.0981(13) 0.1440(7) 1.0874(6) 0.111(8) Uani 0.50 1 d PD C 1 C121 C 0.4508(11) -0.1310(8) 0.8684(6) 0.119(6) Uani 0.50 1 d PDU D 1 C122 C 0.3939(13) -0.1410(8) 0.9048(7) 0.115(7) Uani 0.50 1 d PDU D 1 H12J H 0.3462 -0.1316 0.8934 0.172 Uiso 0.50 1 calc PR D 1 H12K H 0.4052 -0.1219 0.9321 0.172 Uiso 0.50 1 calc PR D 1 H12L H 0.3939 -0.1760 0.9123 0.172 Uiso 0.50 1 calc PR D 1 N61 N 0.4800(10) -0.1271(6) 0.8341(6) 0.110(6) Uani 0.50 1 d PDU D 1 O5W O 1.2857(17) 0.0900(12) 1.1905(10) 0.211(11) Uiso 0.50 1 d P E 1 C203 C 1.1787(10) 0.1199(7) 1.0971(7) 0.108(9) Uani 0.50 1 d PD F 2 C204 C 1.2315(12) 0.0946(7) 1.1292(9) 0.105(8) Uani 0.50 1 d PD F 2 H20B H 1.2673 0.0764 1.1114 0.157 Uiso 0.50 1 calc PR F 2 H20C H 1.2051 0.0719 1.1489 0.157 Uiso 0.50 1 calc PR F 2 H20D H 1.2560 0.1192 1.1479 0.157 Uiso 0.50 1 calc PR F 2 N52A N 1.1480(14) 0.1440(10) 1.0719(6) 0.129(10) Uani 0.50 1 d PD F 2 C221 C 0.2780(13) -0.1153(7) 0.8861(7) 0.104(6) Uani 0.50 1 d PDU G 2 C222 C 0.2332(13) -0.0887(5) 0.8507(8) 0.109(7) Uani 0.50 1 d PDU G 2 H22A H 0.1900 -0.0749 0.8650 0.164 Uiso 0.50 1 calc PR G 2 H22B H 0.2188 -0.1118 0.8268 0.164 Uiso 0.50 1 calc PR G 2 H22C H 0.2619 -0.0623 0.8373 0.164 Uiso 0.50 1 calc PR G 2 N61A N 0.3133(13) -0.1346(7) 0.9122(6) 0.117(6) Uani 0.50 1 d PDU G 2 O3W O 1.0653(18) 0.1673(12) 1.2707(10) 0.224(12) Uiso 0.50 1 d P H 2 C128 C 0.8940(17) -0.0906(7) 1.0355(8) 0.252(10) Uani 1 1 d DU . . C127 C 0.8729(15) -0.0455(6) 1.0075(8) 0.261(9) Uani 1 1 d DU . . N64 N 0.8709(13) -0.0068(6) 0.9918(6) 0.271(9) Uani 1 1 d DU . . O1W O 0.7405(14) 0.3548(4) 0.7604(4) 0.306(12) Uani 1 1 d . . . C126 C 0.9255(10) 0.2166(11) 0.4640(6) 0.41(2) Uani 1 1 d DU . . C125 C 0.8692(13) 0.2556(10) 0.4754(9) 0.44(2) Uani 1 1 d DU . . N63 N 0.8192(11) 0.2772(10) 0.4867(9) 0.46(2) Uani 1 1 d DU . . O2W O 1.3751(19) 0.1037(12) 0.4962(11) 0.425(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.060(5) 0.061(5) 0.057(5) 0.000(4) -0.003(4) 0.020(4) C2 0.081(6) 0.057(5) 0.059(5) -0.006(4) 0.002(4) 0.013(4) C3 0.048(4) 0.043(4) 0.054(4) 0.004(3) 0.002(3) -0.001(3) C4 0.039(4) 0.037(4) 0.056(4) 0.005(3) -0.006(3) 0.004(3) C5 0.059(5) 0.021(3) 0.066(4) 0.004(3) -0.004(4) 0.004(3) C6 0.027(3) 0.031(3) 0.053(4) -0.004(3) -0.003(3) -0.002(3) C7 0.032(3) 0.029(3) 0.065(4) 0.000(3) 0.004(3) 0.009(3) C8 0.017(3) 0.031(3) 0.057(4) -0.002(3) 0.002(3) 0.002(2) C9 0.030(3) 0.029(3) 0.046(4) 0.000(3) -0.007(3) -0.001(2) C10 0.055(4) 0.030(3) 0.050(4) -0.005(3) -0.006(3) 0.003(3) C11 0.048(4) 0.029(3) 0.066(4) 0.004(3) 0.003(3) -0.004(3) C12 0.099(7) 0.033(4) 0.073(5) -0.002(4) -0.020(5) -0.010(4) C13 0.104(8) 0.042(4) 0.077(5) 0.003(4) -0.011(5) 0.022(5) C14 0.070(6) 0.046(4) 0.089(6) -0.005(4) -0.007(5) 0.019(4) C15 0.051(5) 0.038(3) 0.066(4) -0.005(3) -0.011(4) 0.010(3) C16 0.067(5) 0.033(4) 0.072(5) -0.002(3) 0.014(4) 0.016(4) C17 0.038(4) 0.039(4) 0.059(4) -0.010(3) -0.008(3) 0.007(3) C18 0.047(4) 0.042(4) 0.048(4) 0.000(3) 0.002(3) 0.004(3) C19 0.066(5) 0.052(5) 0.056(5) 0.004(4) 0.004(4) -0.004(4) C20 0.062(5) 0.040(4) 0.060(5) 0.013(4) -0.004(4) -0.010(4) C21 0.036(4) 0.048(4) 0.092(6) 0.009(4) 0.010(4) 0.004(3) C22 0.054(5) 0.046(4) 0.098(6) 0.002(4) 0.004(5) -0.014(4) C23 0.036(4) 0.042(4) 0.056(4) 0.001(3) 0.003(3) -0.003(3) C24 0.041(4) 0.033(4) 0.076(5) -0.004(3) -0.002(4) 0.000(3) C25 0.044(4) 0.031(4) 0.135(8) -0.023(4) 0.018(5) -0.007(3) C26 0.037(4) 0.038(4) 0.058(4) -0.005(3) -0.001(3) -0.002(3) C27 0.034(4) 0.021(3) 0.076(5) -0.003(3) 0.011(3) 0.006(3) C28 0.030(3) 0.033(4) 0.068(4) -0.013(3) -0.003(3) 0.003(3) C29 0.035(3) 0.026(3) 0.055(4) -0.002(3) -0.010(3) 0.008(3) C30 0.026(3) 0.034(3) 0.055(4) -0.001(3) -0.003(3) -0.005(2) C31 0.040(4) 0.040(4) 0.074(5) 0.011(3) -0.003(3) -0.001(3) C32 0.051(5) 0.044(5) 0.102(7) 0.034(5) -0.003(4) -0.003(4) C33 0.040(4) 0.034(4) 0.150(9) -0.005(6) -0.009(5) -0.003(3) C34 0.065(6) 0.047(5) 0.099(7) -0.024(5) -0.015(5) 0.003(4) C35 0.040(4) 0.036(4) 0.064(4) -0.008(3) -0.015(3) 0.007(3) C36 0.043(4) 0.032(4) 0.120(7) -0.017(4) 0.007(4) -0.002(3) C37 0.040(4) 0.038(4) 0.093(6) -0.010(4) 0.006(4) -0.004(3) C38 0.037(4) 0.039(4) 0.069(5) -0.008(3) 0.000(3) -0.007(3) C39 0.050(5) 0.057(5) 0.099(6) -0.007(5) 0.011(5) -0.005(4) C40 0.046(4) 0.043(4) 0.062(4) 0.008(3) -0.002(4) -0.010(3) C41 0.062(5) 0.055(5) 0.062(5) -0.005(4) 0.003(4) -0.018(4) C42 0.075(6) 0.092(7) 0.049(5) 0.007(4) -0.001(4) -0.034(5) C43 0.049(5) 0.053(5) 0.068(5) 0.001(4) 0.007(4) -0.015(4) C44 0.046(5) 0.039(4) 0.073(5) 0.006(4) 0.002(4) -0.006(3) C45 0.076(5) 0.026(3) 0.064(5) 0.002(3) -0.001(4) 0.005(3) C46 0.024(3) 0.033(3) 0.068(4) 0.005(3) 0.001(3) -0.006(3) C47 0.037(4) 0.023(3) 0.065(4) -0.006(3) -0.004(3) 0.002(2) C48 0.029(3) 0.021(3) 0.054(4) 0.001(3) 0.005(3) -0.004(2) C49 0.027(3) 0.026(3) 0.048(4) -0.002(3) -0.007(3) -0.003(2) C50 0.066(5) 0.027(3) 0.044(4) -0.002(3) -0.010(3) 0.004(3) C51 0.060(5) 0.050(4) 0.086(5) -0.004(4) 0.001(5) 0.021(4) C52 0.118(9) 0.070(6) 0.111(8) -0.025(6) -0.024(7) 0.059(6) C53 0.177(13) 0.033(4) 0.114(8) -0.022(5) -0.038(9) 0.043(6) C54 0.170(12) 0.026(4) 0.082(6) 0.009(4) -0.037(8) -0.004(5) C55 0.089(6) 0.036(3) 0.056(4) -0.008(3) -0.017(4) 0.002(4) C56 0.068(5) 0.027(3) 0.065(5) -0.008(3) -0.002(4) 0.004(3) C57 0.035(4) 0.048(4) 0.068(5) -0.006(4) -0.007(3) -0.002(3) C58 0.037(4) 0.046(4) 0.047(4) -0.006(3) 0.003(3) -0.002(3) C59 0.066(5) 0.045(4) 0.069(5) -0.009(4) -0.007(4) -0.014(4) C60 0.065(5) 0.044(4) 0.058(5) -0.002(4) -0.001(4) -0.012(4) C61 0.031(4) 0.054(4) 0.079(5) 0.003(4) -0.007(4) 0.002(3) C62 0.048(5) 0.042(4) 0.093(6) 0.001(4) 0.000(4) -0.005(3) C63 0.042(4) 0.025(3) 0.068(4) -0.004(3) 0.001(3) -0.007(3) C64 0.043(4) 0.037(4) 0.062(4) -0.002(3) -0.002(3) -0.010(3) C65 0.053(5) 0.026(4) 0.107(6) 0.007(4) -0.008(4) -0.005(3) C66 0.043(4) 0.022(3) 0.053(4) 0.003(3) -0.013(3) -0.004(3) C67 0.026(3) 0.026(3) 0.090(5) 0.013(3) -0.011(3) -0.003(2) C68 0.036(4) 0.042(4) 0.056(4) 0.002(3) -0.011(3) 0.008(3) C69 0.035(4) 0.033(3) 0.047(4) 0.001(3) -0.017(3) 0.000(3) C70 0.019(3) 0.029(3) 0.061(4) -0.005(3) 0.007(3) -0.005(2) C71 0.038(4) 0.041(4) 0.080(5) -0.006(4) 0.004(4) -0.001(3) C72 0.042(5) 0.046(5) 0.116(7) -0.035(5) 0.005(5) -0.001(4) C73 0.037(4) 0.033(4) 0.133(8) -0.002(5) -0.005(5) 0.004(3) C74 0.046(5) 0.043(5) 0.113(7) 0.030(5) -0.010(5) -0.002(4) C75 0.039(4) 0.044(4) 0.077(5) 0.014(4) -0.001(4) -0.001(3) C76 0.041(4) 0.032(4) 0.131(7) 0.009(4) -0.013(5) 0.011(3) C77 0.035(4) 0.040(4) 0.077(5) 0.010(4) -0.005(3) 0.006(3) C78 0.028(3) 0.042(4) 0.072(5) -0.001(3) -0.003(3) -0.003(3) C79 0.041(4) 0.052(5) 0.070(5) -0.001(4) -0.006(4) 0.001(3) C80 0.052(4) 0.043(4) 0.056(4) 0.004(3) 0.001(3) -0.007(3) C101 0.121(12) 0.145(13) 0.111(10) -0.055(9) 0.034(8) -0.045(10) C102 0.207(18) 0.125(12) 0.164(13) -0.055(10) 0.096(13) -0.009(12) C105 0.115(11) 0.080(8) 0.125(9) 0.000(7) 0.000(8) 0.007(8) C106 0.138(12) 0.179(14) 0.093(8) 0.040(8) 0.010(8) 0.077(11) C107 1.00(12) 0.58(8) 0.064(14) 0.13(3) -0.13(4) -0.55(9) C108 0.87(10) 0.87(10) 0.115(19) -0.06(4) -0.02(4) 0.73(9) C109 0.101(8) 0.140(10) 0.047(5) 0.008(6) -0.002(5) -0.020(7) C110 0.200(15) 0.140(11) 0.059(6) -0.004(7) 0.014(8) -0.058(10) C111 0.082(8) 0.077(8) 0.133(10) -0.002(7) -0.027(7) -0.012(6) C112 0.106(9) 0.115(10) 0.105(8) 0.004(7) 0.002(7) 0.022(8) C115 0.100(9) 0.203(15) 0.115(10) 0.007(9) 0.006(8) -0.043(10) C116 0.130(12) 0.292(19) 0.164(13) -0.028(13) 0.010(11) -0.045(14) C117 0.107(14) 0.78(9) 0.096(12) 0.09(3) 0.003(11) 0.00(3) C118 0.62(6) 0.29(3) 0.048(9) -0.030(13) 0.06(2) 0.02(4) C119 0.45(4) 0.210(19) 0.160(17) -0.021(14) -0.076(17) 0.13(2) C120 0.44(4) 0.23(3) 0.16(2) -0.03(2) -0.07(2) 0.09(3) C220 0.10(2) 0.20(3) 0.24(4) 0.13(3) -0.10(2) -0.03(2) C219 0.32(6) 0.30(6) 0.24(5) 0.22(5) -0.17(5) -0.25(5) O4W 0.27(3) 0.104(14) 0.155(16) -0.013(12) -0.041(18) 0.100(17) B1 0.081(7) 0.040(5) 0.060(5) 0.001(4) 0.007(5) 0.005(5) B2 0.074(9) 0.091(10) 0.146(13) 0.018(9) 0.047(9) 0.009(8) B3 0.074(9) 0.054(7) 0.23(2) 0.005(9) -0.068(11) 0.014(7) B4 0.082(7) 0.043(5) 0.060(5) -0.005(4) 0.003(5) -0.014(5) B5 0.079(9) 0.070(8) 0.140(12) -0.035(8) -0.013(9) -0.001(7) B6 0.046(6) 0.051(6) 0.143(11) 0.002(6) -0.002(7) -0.003(5) B7 0.053(6) 0.046(5) 0.079(7) 0.007(5) 0.006(5) -0.017(4) B8 0.082(9) 0.066(8) 0.117(10) 0.006(6) 0.006(7) 0.013(6) F1 0.116(4) 0.048(3) 0.070(3) -0.004(2) 0.016(3) 0.010(3) F2 0.089(4) 0.079(4) 0.089(3) 0.005(3) -0.016(3) 0.008(3) F3 0.063(3) 0.056(3) 0.110(4) -0.004(3) -0.004(3) -0.007(2) F4 0.116(4) 0.073(3) 0.068(3) -0.005(2) 0.016(3) -0.026(3) F5 0.059(3) 0.071(3) 0.157(5) 0.010(3) 0.007(3) 0.026(3) F6 0.061(4) 0.056(4) 0.338(12) 0.035(5) -0.011(6) 0.005(3) F7 0.049(4) 0.099(6) 0.49(2) -0.015(9) -0.017(8) 0.001(4) F8 0.345(19) 0.264(15) 0.231(12) 0.062(11) 0.175(14) 0.164(14) F9 0.088(4) 0.072(4) 0.216(7) -0.007(4) -0.018(5) 0.030(3) F10 0.058(4) 0.075(4) 0.352(13) -0.008(6) -0.041(6) 0.000(3) F11 0.49(3) 0.274(16) 0.152(9) -0.017(9) -0.070(12) 0.238(18) F12 0.060(5) 0.143(8) 0.425(19) 0.039(10) 0.007(8) -0.036(5) F13 0.131(5) 0.046(3) 0.075(3) 0.005(2) -0.015(3) 0.018(3) F14 0.095(4) 0.074(4) 0.092(3) 0.002(3) 0.015(3) 0.023(3) F15 0.078(3) 0.076(3) 0.096(4) 0.004(3) 0.003(3) -0.018(3) F16 0.110(4) 0.075(4) 0.088(3) 0.002(3) -0.012(3) -0.026(3) F17 0.079(5) 0.107(6) 0.469(18) -0.103(9) -0.084(8) 0.024(4) F18 0.045(3) 0.054(3) 0.147(5) 0.005(3) 0.005(3) -0.003(2) F19 0.061(4) 0.109(5) 0.136(5) 0.056(4) -0.002(3) 0.006(3) F20 0.066(4) 0.225(9) 0.077(4) 0.024(4) 0.011(3) -0.022(5) F21 0.092(5) 0.136(7) 0.262(10) 0.088(7) 0.033(6) -0.001(5) F22 0.049(3) 0.097(4) 0.148(5) -0.018(4) -0.004(3) -0.004(3) F23 0.087(4) 0.093(4) 0.115(4) -0.035(3) -0.007(3) 0.012(3) F24 0.077(4) 0.181(7) 0.080(3) -0.047(4) -0.011(3) 0.017(4) F25 0.076(3) 0.060(3) 0.088(4) -0.017(2) 0.015(3) -0.007(2) F26 0.147(6) 0.061(3) 0.103(4) 0.021(3) 0.005(4) -0.031(4) F27 0.138(5) 0.073(4) 0.096(4) 0.011(3) -0.005(3) -0.052(4) F28 0.105(5) 0.108(5) 0.138(5) -0.004(4) 0.043(4) 0.035(4) F29 0.124(6) 0.054(3) 0.253(9) -0.009(4) 0.038(6) -0.008(3) F30 0.206(11) 0.239(12) 0.181(9) 0.050(8) -0.005(8) 0.126(10) F31 0.219(10) 0.049(3) 0.339(13) -0.011(6) 0.122(10) 0.037(5) F32 0.109(5) 0.074(4) 0.170(6) -0.007(4) -0.019(4) 0.009(3) Fe1 0.0332(5) 0.0265(4) 0.0550(5) -0.0028(4) -0.0021(4) 0.0013(4) Fe2 0.0347(5) 0.0228(4) 0.0550(5) 0.0015(4) -0.0040(4) -0.0009(4) Fe3 0.0337(5) 0.0290(5) 0.0538(5) 0.0021(4) -0.0008(4) -0.0002(4) Fe4 0.0353(5) 0.0311(5) 0.0532(5) -0.0025(4) 0.0014(4) -0.0037(4) N1 0.102(6) 0.054(4) 0.061(4) -0.010(3) 0.013(4) 0.007(4) N2 0.046(3) 0.035(3) 0.053(3) -0.005(3) 0.003(3) -0.001(3) N3 0.026(3) 0.032(3) 0.052(3) -0.002(2) -0.004(2) 0.002(2) N4 0.041(3) 0.031(3) 0.047(3) 0.002(2) -0.006(2) 0.004(2) N5 0.041(3) 0.033(3) 0.056(3) -0.001(2) -0.011(3) 0.005(2) N6 0.024(3) 0.029(3) 0.057(3) -0.003(2) -0.001(2) -0.001(2) N7 0.038(3) 0.035(3) 0.056(3) -0.004(3) 0.000(3) 0.004(2) N8 0.034(3) 0.033(3) 0.050(3) 0.002(3) 0.002(2) 0.000(2) N9 0.037(3) 0.037(3) 0.062(4) -0.003(3) 0.000(3) -0.001(3) N10 0.066(5) 0.067(5) 0.057(4) 0.007(4) -0.002(3) 0.001(4) N11 0.033(4) 0.061(5) 0.144(7) 0.004(5) -0.004(4) -0.002(3) N12 0.036(3) 0.034(3) 0.065(4) 0.002(3) -0.006(3) 0.001(2) N13 0.033(3) 0.030(3) 0.063(3) 0.000(3) -0.001(3) -0.008(2) N14 0.036(3) 0.020(3) 0.083(4) -0.003(3) 0.012(3) -0.002(2) N15 0.036(3) 0.022(3) 0.048(3) -0.002(2) 0.005(2) -0.005(2) N16 0.036(3) 0.028(3) 0.050(3) -0.011(2) 0.001(2) 0.000(2) N17 0.033(3) 0.031(3) 0.086(4) -0.012(3) 0.005(3) -0.002(2) N18 0.029(3) 0.034(3) 0.069(4) -0.007(3) 0.003(3) 0.000(2) N19 0.030(3) 0.039(3) 0.065(3) -0.004(3) -0.006(3) -0.004(2) N20 0.031(3) 0.060(4) 0.082(4) 0.005(3) 0.005(3) -0.013(3) N21 0.080(5) 0.078(5) 0.049(4) -0.007(4) 0.005(3) -0.020(4) N22 0.036(3) 0.051(4) 0.060(4) -0.009(3) 0.000(3) -0.006(3) N23 0.037(3) 0.045(3) 0.049(3) 0.001(3) -0.001(2) -0.007(3) N24 0.048(3) 0.022(3) 0.057(3) 0.006(2) -0.005(3) 0.001(2) N25 0.030(3) 0.028(3) 0.057(3) 0.005(2) -0.005(2) -0.003(2) N26 0.027(3) 0.027(3) 0.056(3) 0.002(2) 0.000(2) 0.001(2) N27 0.041(3) 0.035(3) 0.050(3) 0.006(3) -0.004(2) 0.001(2) N28 0.033(3) 0.021(2) 0.051(3) 0.000(2) -0.003(2) -0.002(2) N29 0.045(3) 0.039(3) 0.048(3) 0.013(2) -0.005(2) -0.001(3) N30 0.056(4) 0.079(5) 0.054(4) 0.016(3) -0.005(3) -0.012(4) N31 0.026(3) 0.061(4) 0.137(7) -0.008(4) 0.003(4) -0.008(3) N32 0.041(3) 0.046(3) 0.068(4) 0.002(3) -0.010(3) -0.006(3) N33 0.040(3) 0.023(3) 0.060(3) 0.007(2) 0.001(3) -0.002(2) N34 0.033(3) 0.026(3) 0.082(4) 0.008(3) -0.001(3) 0.001(2) N35 0.037(3) 0.024(3) 0.058(3) 0.008(2) -0.006(3) 0.000(2) N36 0.047(3) 0.021(3) 0.048(3) 0.011(2) -0.006(3) -0.002(2) N37 0.029(3) 0.030(3) 0.071(4) 0.007(3) 0.000(3) -0.001(2) N38 0.031(3) 0.024(3) 0.071(4) 0.002(3) 0.001(3) -0.001(2) N39 0.035(3) 0.038(3) 0.066(4) 0.000(3) -0.008(3) 0.003(2) N40 0.036(3) 0.052(4) 0.086(4) 0.013(3) -0.011(3) -0.014(3) N51 0.100(8) 0.163(12) 0.131(9) -0.048(8) 0.006(7) -0.029(8) N53 0.135(11) 0.074(7) 0.256(16) -0.047(9) -0.023(10) 0.021(7) N54 0.41(3) 0.27(2) 0.15(2) -0.018(17) 0.09(2) -0.17(2) N55 0.158(11) 0.156(10) 0.096(7) 0.002(7) -0.010(7) -0.083(9) N56 0.091(9) 0.094(8) 0.311(19) -0.089(10) -0.015(10) 0.009(7) N58 0.118(9) 0.172(13) 0.156(11) 0.018(9) -0.014(9) 0.001(9) N59 0.50(5) 0.158(17) 0.48(4) 0.06(2) -0.24(4) 0.06(2) N60 0.45(4) 0.196(16) 0.161(14) -0.020(11) -0.078(15) 0.153(18) C103 0.117(17) 0.041(9) 0.087(13) 0.018(9) -0.011(12) -0.026(10) C104 0.13(2) 0.072(15) 0.128(18) 0.036(13) 0.053(16) 0.029(14) N52 0.17(2) 0.075(12) 0.090(14) 0.060(10) 0.043(14) 0.021(13) C121 0.134(16) 0.055(10) 0.167(16) 0.024(11) -0.003(13) 0.016(11) C122 0.148(19) 0.067(12) 0.129(17) 0.029(11) -0.004(14) -0.011(13) N61 0.113(13) 0.070(10) 0.149(14) 0.059(10) 0.074(11) 0.016(9) C203 0.14(2) 0.088(17) 0.098(17) -0.024(14) 0.066(16) -0.045(17) C204 0.095(17) 0.064(13) 0.15(2) 0.011(13) -0.032(15) 0.006(11) N52A 0.15(2) 0.18(3) 0.052(12) 0.009(13) -0.022(13) -0.02(2) C221 0.141(15) 0.043(9) 0.129(14) -0.011(9) -0.042(11) 0.005(10) C222 0.142(16) 0.011(6) 0.176(17) -0.003(9) -0.031(14) -0.003(9) N61A 0.177(18) 0.084(12) 0.089(12) 0.011(9) -0.016(12) 0.004(12) C128 0.33(2) 0.186(18) 0.241(19) 0.037(15) 0.068(18) 0.011(19) C127 0.39(2) 0.183(17) 0.212(16) 0.016(13) 0.037(16) 0.090(18) N64 0.45(2) 0.169(14) 0.193(13) 0.063(11) 0.023(14) 0.188(15) O1W 0.67(4) 0.116(8) 0.131(9) 0.032(7) -0.001(15) 0.008(15) C126 0.117(15) 0.92(5) 0.188(15) 0.30(2) -0.095(15) -0.23(3) C125 0.154(18) 0.91(5) 0.259(17) 0.31(2) -0.12(2) -0.28(3) N63 0.18(2) 0.89(5) 0.30(2) 0.33(3) -0.14(2) -0.24(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.331(9) . ? C1 N1 1.352(10) . ? C1 H1 0.9500 . ? C2 C3 1.378(11) . ? C2 N1 1.388(10) . ? C2 H2 0.9500 . ? C3 N2 1.392(9) . ? C3 C4 1.426(10) . ? C4 N3 1.267(8) . ? C4 H4 0.9500 . ? C5 N4 1.471(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N5 1.362(8) . ? C6 N4 1.364(8) . ? C6 C7 1.401(9) . ? C7 C8 1.369(9) . ? C7 H7 0.9500 . ? C8 N6 1.372(8) . ? C8 N7 1.377(8) . ? C9 N6 1.308(8) . ? C9 N5 1.364(8) . ? C9 C10 1.499(8) . ? C10 C15 1.374(10) . ? C10 C11 1.411(9) . ? C11 C12 1.367(9) . ? C11 H11 0.9500 . ? C12 C13 1.387(12) . ? C12 H12 0.9500 . ? C13 C14 1.406(12) . ? C13 H13 0.9500 . ? C14 C15 1.388(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N7 1.431(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N8 1.273(8) . ? C17 C18 1.454(10) . ? C17 H17 0.9500 . ? C18 C19 1.315(10) . ? C18 N9 1.410(9) . ? C19 N10 1.351(10) . ? C19 H19 0.9500 . ? C20 N10 1.295(10) . ? C20 N9 1.322(9) . ? C20 H20 0.9500 . ? C21 N12 1.333(9) . ? C21 N11 1.356(10) . ? C21 H21 0.9500 . ? C22 N11 1.353(11) . ? C22 C23 1.363(10) . ? C22 H22 0.9500 . ? C23 N12 1.365(9) . ? C23 C24 1.446(9) . ? C24 N13 1.282(8) . ? C24 H24 0.9500 . ? C25 N14 1.454(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N14 1.354(8) . ? C26 C27 1.372(9) . ? C26 N15 1.397(8) . ? C27 C28 1.379(9) . ? C27 H27 0.9500 . ? C28 N16 1.358(8) . ? C28 N17 1.374(8) . ? C29 N15 1.315(8) . ? C29 N16 1.351(8) . ? C29 C30 1.475(9) . ? C30 C31 1.375(10) . ? C30 C35 1.374(10) . ? C31 C32 1.449(11) . ? C31 H31 0.9500 . ? C32 C33 1.333(13) . ? C32 H32 0.9500 . ? C33 C34 1.416(14) . ? C33 H33 0.9500 . ? C34 C35 1.372(11) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 N17 1.472(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N18 1.278(9) . ? C37 C38 1.442(10) . ? C37 H37 0.9500 . ? C38 C39 1.369(11) . ? C38 N19 1.373(9) . ? C39 N20 1.353(10) . ? C39 H39 0.9500 . ? C40 N19 1.338(8) . ? C40 N20 1.350(9) . ? C40 H40 0.9500 . ? C41 N22 1.292(10) . ? C41 N21 1.326(10) . ? C41 H41 0.9500 . ? C42 C43 1.365(11) . ? C42 N21 1.395(12) . ? C42 H42 0.9500 . ? C43 N22 1.411(10) . ? C43 C44 1.439(11) . ? C44 N23 1.274(9) . ? C44 H44 0.9500 . ? C45 N24 1.437(8) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N24 1.366(9) . ? C46 N25 1.373(8) . ? C46 C47 1.388(10) . ? C47 C48 1.363(9) . ? C47 H47 0.9500 . ? C48 N27 1.361(8) . ? C48 N26 1.375(8) . ? C49 N26 1.336(8) . ? C49 N25 1.345(8) . ? C49 C50 1.505(8) . ? C50 C55 1.379(10) . ? C50 C51 1.389(10) . ? C51 C52 1.395(11) . ? C51 H51 0.9500 . ? C52 C53 1.456(17) . ? C52 H52 0.9500 . ? C53 C54 1.356(16) . ? C53 H53 0.9500 . ? C54 C55 1.395(11) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 N27 1.472(8) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 N28 1.299(9) . ? C57 C58 1.439(10) . ? C57 H57 0.9500 . ? C58 C59 1.335(10) . ? C58 N29 1.418(9) . ? C59 N30 1.346(10) . ? C59 H59 0.9500 . ? C60 N29 1.316(9) . ? C60 N30 1.348(10) . ? C60 H60 0.9500 . ? C61 N32 1.272(9) . ? C61 N31 1.326(10) . ? C61 H61 0.9500 . ? C62 C63 1.343(10) . ? C62 N31 1.362(10) . ? C62 H62 0.9500 . ? C63 C64 1.407(10) . ? C63 N32 1.415(9) . ? C64 N33 1.257(8) . ? C64 H64 0.9500 . ? C65 N34 1.487(8) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 N34 1.353(8) . ? C66 C67 1.361(9) . ? C66 N35 1.388(8) . ? C67 C68 1.408(9) . ? C67 H67 0.9500 . ? C68 N37 1.304(8) . ? C68 N36 1.398(8) . ? C69 N36 1.328(8) . ? C69 N35 1.351(8) . ? C69 C70 1.476(8) . ? C70 C71 1.385(10) . ? C70 C75 1.401(10) . ? C71 C72 1.386(11) . ? C71 H71 0.9500 . ? C72 C73 1.399(13) . ? C72 H72 0.9500 . ? C73 C74 1.365(13) . ? C73 H73 0.9500 . ? C74 C75 1.407(11) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 N37 1.467(8) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 N38 1.287(8) . ? C77 C78 1.408(10) . ? C77 H77 0.9500 . ? C78 C79 1.353(10) . ? C78 N39 1.427(8) . ? C79 N40 1.364(10) . ? C79 H79 0.9500 . ? C80 N39 1.292(9) . ? C80 N40 1.347(9) . ? C80 H80 0.9500 . ? C101 N51 1.073(15) . ? C101 C102 1.432(19) . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C105 N53 1.081(15) . ? C105 C106 1.448(17) . ? C106 H10D 0.9800 . ? C106 H10E 0.9800 . ? C106 H10F 0.9800 . ? C107 N54 1.143(5) . ? C107 C108 1.521(5) . ? C109 N55 1.137(14) . ? C109 C110 1.446(16) . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C111 N56 1.117(15) . ? C111 C112 1.506(17) . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C115 N58 1.169(18) . ? C115 C116 1.526(5) . ? C117 N59 1.151(5) . ? C117 C118 1.531(5) . ? C119 N60 1.144(5) . ? C119 C120 1.525(5) . ? C220 C219 1.35(5) . ? C219 N60 1.26(4) . ? B1 F4 1.352(10) . ? B1 F1 1.389(10) . ? B1 F3 1.411(11) . ? B1 F2 1.409(11) . ? B2 F8 1.221(16) . ? B2 F6 1.322(15) . ? B2 F5 1.333(14) . ? B2 F7 1.40(2) . ? B3 F12 1.26(2) . ? B3 F11 1.28(2) . ? B3 F10 1.369(16) . ? B3 F9 1.419(13) . ? B4 F15 1.360(11) . ? B4 F13 1.387(11) . ? B4 F16 1.399(11) . ? B4 F14 1.404(11) . ? B5 F20 1.300(16) . ? B5 F17 1.364(14) . ? B5 F19 1.360(16) . ? B5 F18 1.433(14) . ? B6 F21 1.340(13) . ? B6 F24 1.348(13) . ? B6 F23 1.407(14) . ? B6 F22 1.420(13) . ? B7 F25 1.351(11) . ? B7 F26 1.352(10) . ? B7 F28 1.388(11) . ? B7 F27 1.396(10) . ? B8 F31 1.313(14) . ? B8 F29 1.329(14) . ? B8 F30 1.374(16) . ? B8 F32 1.421(15) . ? Fe1 N13 2.149(5) . ? Fe1 N2 2.149(5) . ? Fe1 N3 2.169(5) . ? Fe1 N12 2.186(6) . ? Fe1 N5 2.192(5) . ? Fe1 N15 2.238(5) . ? Fe2 N28 2.151(5) . ? Fe2 N29 2.155(5) . ? Fe2 N39 2.156(5) . ? Fe2 N38 2.166(5) . ? Fe2 N26 2.216(5) . ? Fe2 N36 2.220(5) . ? Fe3 N9 2.137(6) . ? Fe3 N33 2.149(5) . ? Fe3 N8 2.160(5) . ? Fe3 N32 2.186(6) . ? Fe3 N6 2.185(5) . ? Fe3 N35 2.224(5) . ? Fe4 N19 2.130(5) . ? Fe4 N18 2.159(5) . ? Fe4 N23 2.169(6) . ? Fe4 N22 2.170(6) . ? Fe4 N25 2.202(5) . ? Fe4 N16 2.222(5) . ? N1 H1A 0.8800 . ? N3 N4 1.388(7) . ? N7 N8 1.368(7) . ? N10 H10 0.8800 . ? N11 H111 0.8800 . ? N13 N14 1.387(7) . ? N17 N18 1.356(7) . ? N20 H20A 0.8800 . ? N21 H21A 0.8800 . ? N23 N24 1.370(8) . ? N27 N28 1.368(7) . ? N30 H30 0.8800 . ? N31 H31A 0.8800 . ? N33 N34 1.382(7) . ? N37 N38 1.401(7) . ? N40 H40A 0.8800 . ? C103 N52 1.142(4) . ? C103 C104 1.521(4) . ? C104 H10J 0.9800 . ? C104 H10K 0.9800 . ? C104 H10L 0.9800 . ? C121 N61 1.149(5) . ? C121 C122 1.527(5) . ? C122 H12J 0.9800 . ? C122 H12K 0.9800 . ? C122 H12L 0.9800 . ? C203 N52A 1.144(4) . ? C203 C204 1.524(5) . ? C204 H20B 0.9800 . ? C204 H20C 0.9800 . ? C204 H20D 0.9800 . ? C221 N61A 1.138(4) . ? C221 C222 1.518(4) . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C128 C127 1.533(5) . ? C127 N64 1.152(5) . ? C126 C125 1.527(5) . ? C125 N63 1.148(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 N2 C1 N1 109.9(7) . . ? N2 C1 H1 125.0 . . ? N1 C1 H1 125.0 . . ? C3 C2 N1 105.6(7) . . ? C3 C2 H2 127.2 . . ? N1 C2 H2 127.2 . . ? C2 C3 N2 108.7(6) . . ? C2 C3 C4 132.8(7) . . ? N2 C3 C4 118.5(6) . . ? N3 C4 C3 114.7(6) . . ? N3 C4 H4 122.7 . . ? C3 C4 H4 122.7 . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N5 C6 N4 115.4(6) . . ? N5 C6 C7 121.9(6) . . ? N4 C6 C7 122.6(6) . . ? C8 C7 C6 117.3(5) . . ? C8 C7 H7 121.3 . . ? C6 C7 H7 121.3 . . ? C7 C8 N6 121.7(6) . . ? C7 C8 N7 121.6(6) . . ? N6 C8 N7 116.6(6) . . ? N6 C9 N5 126.8(5) . . ? N6 C9 C10 117.8(5) . . ? N5 C9 C10 115.3(5) . . ? C15 C10 C11 120.0(6) . . ? C15 C10 C9 122.0(6) . . ? C11 C10 C9 118.0(6) . . ? C12 C11 C10 119.9(7) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.1(8) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 120.6(7) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 118.7(8) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C10 C15 C14 120.6(7) . . ? C10 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? N7 C16 H16A 109.5 . . ? N7 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N7 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N8 C17 C18 115.6(6) . . ? N8 C17 H17 122.2 . . ? C18 C17 H17 122.2 . . ? C19 C18 N9 110.2(6) . . ? C19 C18 C17 133.5(7) . . ? N9 C18 C17 116.3(6) . . ? C18 C19 N10 106.4(7) . . ? C18 C19 H19 126.8 . . ? N10 C19 H19 126.8 . . ? N10 C20 N9 113.1(7) . . ? N10 C20 H20 123.5 . . ? N9 C20 H20 123.5 . . ? N12 C21 N11 109.2(7) . . ? N12 C21 H21 125.4 . . ? N11 C21 H21 125.4 . . ? N11 C22 C23 106.0(7) . . ? N11 C22 H22 127.0 . . ? C23 C22 H22 127.0 . . ? C22 C23 N12 109.5(6) . . ? C22 C23 C24 131.1(7) . . ? N12 C23 C24 119.3(6) . . ? N13 C24 C23 114.5(6) . . ? N13 C24 H24 122.7 . . ? C23 C24 H24 122.7 . . ? N14 C25 H25A 109.5 . . ? N14 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N14 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N14 C26 C27 122.4(6) . . ? N14 C26 N15 116.2(6) . . ? C27 C26 N15 121.4(6) . . ? C26 C27 C28 117.0(6) . . ? C26 C27 H27 121.5 . . ? C28 C27 H27 121.5 . . ? N16 C28 N17 116.0(6) . . ? N16 C28 C27 122.7(6) . . ? N17 C28 C27 121.3(6) . . ? N15 C29 N16 125.8(5) . . ? N15 C29 C30 119.2(5) . . ? N16 C29 C30 115.1(5) . . ? C31 C30 C35 120.5(6) . . ? C31 C30 C29 117.6(6) . . ? C35 C30 C29 121.9(6) . . ? C30 C31 C32 119.0(7) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? C33 C32 C31 119.4(8) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 121.0(8) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C35 C34 C33 119.3(8) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C30 120.8(8) . . ? C34 C35 H35 119.6 . . ? C30 C35 H35 119.6 . . ? N17 C36 H36A 109.5 . . ? N17 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N17 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N18 C37 C38 115.3(7) . . ? N18 C37 H37 122.3 . . ? C38 C37 H37 122.3 . . ? C39 C38 N19 111.1(6) . . ? C39 C38 C37 131.4(7) . . ? N19 C38 C37 117.5(6) . . ? N20 C39 C38 104.7(7) . . ? N20 C39 H39 127.7 . . ? C38 C39 H39 127.7 . . ? N19 C40 N20 110.4(6) . . ? N19 C40 H40 124.8 . . ? N20 C40 H40 124.8 . . ? N22 C41 N21 111.9(8) . . ? N22 C41 H41 124.0 . . ? N21 C41 H41 124.0 . . ? C43 C42 N21 102.4(8) . . ? C43 C42 H42 128.8 . . ? N21 C42 H42 128.8 . . ? C42 C43 N22 111.0(7) . . ? C42 C43 C44 131.2(8) . . ? N22 C43 C44 117.8(7) . . ? N23 C44 C43 116.1(7) . . ? N23 C44 H44 122.0 . . ? C43 C44 H44 122.0 . . ? N24 C45 H45A 109.5 . . ? N24 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N24 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N24 C46 N25 116.5(6) . . ? N24 C46 C47 122.7(6) . . ? N25 C46 C47 120.8(6) . . ? C48 C47 C46 119.4(5) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? N27 C48 C47 122.1(5) . . ? N27 C48 N26 116.5(5) . . ? C47 C48 N26 121.3(6) . . ? N26 C49 N25 128.2(5) . . ? N26 C49 C50 116.1(5) . . ? N25 C49 C50 115.7(5) . . ? C55 C50 C51 121.8(6) . . ? C55 C50 C49 121.0(6) . . ? C51 C50 C49 117.2(6) . . ? C50 C51 C52 120.1(9) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C51 C52 C53 116.6(10) . . ? C51 C52 H52 121.7 . . ? C53 C52 H52 121.7 . . ? C54 C53 C52 122.1(8) . . ? C54 C53 H53 119.0 . . ? C52 C53 H53 119.0 . . ? C53 C54 C55 119.5(9) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C50 C55 C54 119.8(9) . . ? C50 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? N27 C56 H56A 109.5 . . ? N27 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N27 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N28 C57 C58 115.3(6) . . ? N28 C57 H57 122.4 . . ? C58 C57 H57 122.4 . . ? C59 C58 N29 109.7(6) . . ? C59 C58 C57 133.3(7) . . ? N29 C58 C57 117.0(6) . . ? C58 C59 N30 107.0(7) . . ? C58 C59 H59 126.5 . . ? N30 C59 H59 126.5 . . ? N29 C60 N30 112.0(7) . . ? N29 C60 H60 124.0 . . ? N30 C60 H60 124.0 . . ? N32 C61 N31 111.5(7) . . ? N32 C61 H61 124.3 . . ? N31 C61 H61 124.3 . . ? C63 C62 N31 106.0(7) . . ? C63 C62 H62 127.0 . . ? N31 C62 H62 127.0 . . ? C62 C63 C64 133.6(6) . . ? C62 C63 N32 107.6(6) . . ? C64 C63 N32 118.7(6) . . ? N33 C64 C63 117.4(6) . . ? N33 C64 H64 121.3 . . ? C63 C64 H64 121.3 . . ? N34 C65 H65A 109.5 . . ? N34 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N34 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N34 C66 C67 123.1(6) . . ? N34 C66 N35 115.9(6) . . ? C67 C66 N35 121.0(6) . . ? C66 C67 C68 120.6(6) . . ? C66 C67 H67 119.7 . . ? C68 C67 H67 119.7 . . ? N37 C68 N36 118.8(6) . . ? N37 C68 C67 123.4(6) . . ? N36 C68 C67 117.8(6) . . ? N36 C69 N35 126.2(6) . . ? N36 C69 C70 115.9(5) . . ? N35 C69 C70 117.9(5) . . ? C71 C70 C75 120.4(6) . . ? C71 C70 C69 119.9(6) . . ? C75 C70 C69 119.7(6) . . ? C70 C71 C72 120.0(8) . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C71 C72 C73 120.0(8) . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C74 C73 C72 120.1(7) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C73 C74 C75 120.8(8) . . ? C73 C74 H74 119.6 . . ? C75 C74 H74 119.6 . . ? C70 C75 C74 118.6(8) . . ? C70 C75 H75 120.7 . . ? C74 C75 H75 120.7 . . ? N37 C76 H76A 109.5 . . ? N37 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N37 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N38 C77 C78 115.4(6) . . ? N38 C77 H77 122.3 . . ? C78 C77 H77 122.3 . . ? C79 C78 C77 134.6(7) . . ? C79 C78 N39 107.5(6) . . ? C77 C78 N39 117.7(6) . . ? C78 C79 N40 107.3(6) . . ? C78 C79 H79 126.4 . . ? N40 C79 H79 126.4 . . ? N39 C80 N40 112.1(6) . . ? N39 C80 H80 124.0 . . ? N40 C80 H80 124.0 . . ? N51 C101 C102 175(2) . . ? C101 C102 H10A 109.5 . . ? C101 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? C101 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? N53 C105 C106 174.8(16) . . ? C105 C106 H10D 109.5 . . ? C105 C106 H10E 109.5 . . ? H10D C106 H10E 109.5 . . ? C105 C106 H10F 109.5 . . ? H10D C106 H10F 109.5 . . ? H10E C106 H10F 109.5 . . ? N54 C107 C108 171(3) . . ? N55 C109 C110 179.0(14) . . ? C109 C110 H11A 109.5 . . ? C109 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C109 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? N56 C111 C112 176.5(16) . . ? C111 C112 H11D 109.5 . . ? C111 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C111 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? N58 C115 C116 171(2) . . ? N59 C117 C118 162(2) . . ? N60 C119 C120 169(4) . . ? N60 C219 C220 177(5) . . ? F4 B1 F1 111.2(7) . . ? F4 B1 F3 110.7(7) . . ? F1 B1 F3 110.6(8) . . ? F4 B1 F2 110.5(8) . . ? F1 B1 F2 106.0(7) . . ? F3 B1 F2 107.6(7) . . ? F8 B2 F6 110.0(15) . . ? F8 B2 F5 121.2(15) . . ? F6 B2 F5 109.2(10) . . ? F8 B2 F7 101.6(14) . . ? F6 B2 F7 105.3(13) . . ? F5 B2 F7 108.2(13) . . ? F12 B3 F11 102.3(15) . . ? F12 B3 F10 111.8(17) . . ? F11 B3 F10 111.0(15) . . ? F12 B3 F9 112.5(13) . . ? F11 B3 F9 115.0(17) . . ? F10 B3 F9 104.5(10) . . ? F15 B4 F13 111.3(9) . . ? F15 B4 F16 110.1(7) . . ? F13 B4 F16 109.9(7) . . ? F15 B4 F14 108.3(7) . . ? F13 B4 F14 108.6(7) . . ? F16 B4 F14 108.6(8) . . ? F20 B5 F17 117.0(13) . . ? F20 B5 F19 109.7(11) . . ? F17 B5 F19 104.5(12) . . ? F20 B5 F18 108.6(11) . . ? F17 B5 F18 105.6(10) . . ? F19 B5 F18 111.3(11) . . ? F21 B6 F24 118.2(12) . . ? F21 B6 F23 108.6(10) . . ? F24 B6 F23 108.5(8) . . ? F21 B6 F22 106.6(8) . . ? F24 B6 F22 110.1(9) . . ? F23 B6 F22 103.9(10) . . ? F25 B7 F26 112.0(8) . . ? F25 B7 F28 108.2(8) . . ? F26 B7 F28 110.8(8) . . ? F25 B7 F27 110.4(7) . . ? F26 B7 F27 108.5(8) . . ? F28 B7 F27 106.8(8) . . ? F31 B8 F29 113.7(11) . . ? F31 B8 F30 107.1(11) . . ? F29 B8 F30 113.0(13) . . ? F31 B8 F32 113.7(12) . . ? F29 B8 F32 105.5(10) . . ? F30 B8 F32 103.4(11) . . ? N13 Fe1 N2 91.5(2) . . ? N13 Fe1 N3 164.3(2) . . ? N2 Fe1 N3 74.7(2) . . ? N13 Fe1 N12 75.2(2) . . ? N2 Fe1 N12 91.5(2) . . ? N3 Fe1 N12 97.30(19) . . ? N13 Fe1 N5 121.4(2) . . ? N2 Fe1 N5 146.2(2) . . ? N3 Fe1 N5 71.6(2) . . ? N12 Fe1 N5 90.3(2) . . ? N13 Fe1 N15 71.96(18) . . ? N2 Fe1 N15 91.2(2) . . ? N3 Fe1 N15 115.00(18) . . ? N12 Fe1 N15 147.11(19) . . ? N5 Fe1 N15 105.0(2) . . ? N28 Fe2 N29 75.6(2) . . ? N28 Fe2 N39 91.9(2) . . ? N29 Fe2 N39 91.0(2) . . ? N28 Fe2 N38 164.2(2) . . ? N29 Fe2 N38 95.9(2) . . ? N39 Fe2 N38 74.8(2) . . ? N28 Fe2 N26 71.35(19) . . ? N29 Fe2 N26 146.9(2) . . ? N39 Fe2 N26 90.3(2) . . ? N38 Fe2 N26 116.3(2) . . ? N28 Fe2 N36 120.42(19) . . ? N29 Fe2 N36 90.8(2) . . ? N39 Fe2 N36 147.0(2) . . ? N38 Fe2 N36 72.22(19) . . ? N26 Fe2 N36 105.59(19) . . ? N9 Fe3 N33 90.9(2) . . ? N9 Fe3 N8 75.5(2) . . ? N33 Fe3 N8 164.3(2) . . ? N9 Fe3 N32 89.1(2) . . ? N33 Fe3 N32 76.0(2) . . ? N8 Fe3 N32 95.8(2) . . ? N9 Fe3 N6 147.7(2) . . ? N33 Fe3 N6 121.0(2) . . ? N8 Fe3 N6 72.25(19) . . ? N32 Fe3 N6 93.5(2) . . ? N9 Fe3 N35 96.3(2) . . ? N33 Fe3 N35 72.25(19) . . ? N8 Fe3 N35 116.29(19) . . ? N32 Fe3 N35 147.8(2) . . ? N6 Fe3 N35 98.44(19) . . ? N19 Fe4 N18 75.4(2) . . ? N19 Fe4 N23 92.8(2) . . ? N18 Fe4 N23 163.9(2) . . ? N19 Fe4 N22 90.4(2) . . ? N18 Fe4 N22 93.3(2) . . ? N23 Fe4 N22 75.6(2) . . ? N19 Fe4 N25 91.6(2) . . ? N18 Fe4 N25 118.8(2) . . ? N23 Fe4 N25 71.7(2) . . ? N22 Fe4 N25 147.3(2) . . ? N19 Fe4 N16 146.9(2) . . ? N18 Fe4 N16 71.68(19) . . ? N23 Fe4 N16 120.1(2) . . ? N22 Fe4 N16 94.6(2) . . ? N25 Fe4 N16 101.22(19) . . ? C1 N1 C2 108.7(7) . . ? C1 N1 H1A 125.7 . . ? C2 N1 H1A 125.7 . . ? C1 N2 C3 107.1(6) . . ? C1 N2 Fe1 140.0(5) . . ? C3 N2 Fe1 112.9(4) . . ? C4 N3 N4 122.4(5) . . ? C4 N3 Fe1 119.2(4) . . ? N4 N3 Fe1 118.4(4) . . ? C6 N4 N3 115.6(5) . . ? C6 N4 C5 123.8(5) . . ? N3 N4 C5 120.4(5) . . ? C9 N5 C6 115.1(5) . . ? C9 N5 Fe1 125.8(4) . . ? C6 N5 Fe1 118.7(4) . . ? C9 N6 C8 116.9(5) . . ? C9 N6 Fe3 125.9(4) . . ? C8 N6 Fe3 117.1(4) . . ? N8 N7 C8 114.6(5) . . ? N8 N7 C16 121.0(5) . . ? C8 N7 C16 124.3(6) . . ? C17 N8 N7 121.9(6) . . ? C17 N8 Fe3 118.8(4) . . ? N7 N8 Fe3 119.3(4) . . ? C20 N9 C18 102.1(6) . . ? C20 N9 Fe3 144.0(5) . . ? C18 N9 Fe3 113.9(4) . . ? C20 N10 C19 108.2(6) . . ? C20 N10 H10 125.9 . . ? C19 N10 H10 125.9 . . ? C22 N11 C21 108.6(7) . . ? C22 N11 H111 125.7 . . ? C21 N11 H111 125.7 . . ? C21 N12 C23 106.5(6) . . ? C21 N12 Fe1 141.6(5) . . ? C23 N12 Fe1 111.8(4) . . ? C24 N13 N14 121.3(5) . . ? C24 N13 Fe1 118.9(5) . . ? N14 N13 Fe1 119.8(4) . . ? C26 N14 N13 116.0(5) . . ? C26 N14 C25 123.7(6) . . ? N13 N14 C25 120.3(5) . . ? C29 N15 C26 116.6(5) . . ? C29 N15 Fe1 127.0(4) . . ? C26 N15 Fe1 116.1(4) . . ? C29 N16 C28 116.3(5) . . ? C29 N16 Fe4 126.8(4) . . ? C28 N16 Fe4 116.9(4) . . ? N18 N17 C28 116.0(5) . . ? N18 N17 C36 120.7(5) . . ? C28 N17 C36 123.1(6) . . ? C37 N18 N17 122.9(6) . . ? C37 N18 Fe4 117.7(5) . . ? N17 N18 Fe4 119.2(4) . . ? C40 N19 C38 104.6(5) . . ? C40 N19 Fe4 141.6(5) . . ? C38 N19 Fe4 113.9(4) . . ? C40 N20 C39 109.2(6) . . ? C40 N20 H20A 125.4 . . ? C39 N20 H20A 125.4 . . ? C41 N21 C42 109.9(7) . . ? C41 N21 H21A 125.0 . . ? C42 N21 H21A 125.0 . . ? C41 N22 C43 104.8(6) . . ? C41 N22 Fe4 143.1(6) . . ? C43 N22 Fe4 112.1(5) . . ? C44 N23 N24 122.3(6) . . ? C44 N23 Fe4 118.4(5) . . ? N24 N23 Fe4 119.3(4) . . ? C46 N24 N23 115.1(5) . . ? C46 N24 C45 125.1(6) . . ? N23 N24 C45 119.5(5) . . ? C49 N25 C46 115.1(5) . . ? C49 N25 Fe4 127.6(4) . . ? C46 N25 Fe4 117.3(4) . . ? C49 N26 C48 115.2(5) . . ? C49 N26 Fe2 127.9(4) . . ? C48 N26 Fe2 116.9(4) . . ? C48 N27 N28 114.7(5) . . ? C48 N27 C56 123.9(6) . . ? N28 N27 C56 121.4(5) . . ? C57 N28 N27 120.5(5) . . ? C57 N28 Fe2 118.9(5) . . ? N27 N28 Fe2 120.5(4) . . ? C60 N29 C58 103.5(6) . . ? C60 N29 Fe2 143.3(5) . . ? C58 N29 Fe2 113.2(4) . . ? C59 N30 C60 107.8(6) . . ? C59 N30 H30 126.1 . . ? C60 N30 H30 126.1 . . ? C61 N31 C62 108.5(6) . . ? C61 N31 H31A 125.7 . . ? C62 N31 H31A 125.7 . . ? C61 N32 C63 106.4(6) . . ? C61 N32 Fe3 143.8(5) . . ? C63 N32 Fe3 109.8(4) . . ? C64 N33 N34 123.3(6) . . ? C64 N33 Fe3 117.7(5) . . ? N34 N33 Fe3 118.8(4) . . ? C66 N34 N33 116.3(5) . . ? C66 N34 C65 123.5(6) . . ? N33 N34 C65 119.6(5) . . ? C69 N35 C66 116.2(5) . . ? C69 N35 Fe3 127.6(4) . . ? C66 N35 Fe3 116.2(4) . . ? C69 N36 C68 118.2(5) . . ? C69 N36 Fe2 126.4(4) . . ? C68 N36 Fe2 114.9(4) . . ? C68 N37 N38 115.7(5) . . ? C68 N37 C76 124.9(6) . . ? N38 N37 C76 119.4(5) . . ? C77 N38 N37 122.5(5) . . ? C77 N38 Fe2 119.2(4) . . ? N37 N38 Fe2 118.3(4) . . ? C80 N39 C78 105.7(6) . . ? C80 N39 Fe2 141.4(5) . . ? C78 N39 Fe2 112.8(4) . . ? C80 N40 C79 107.4(6) . . ? C80 N40 H40A 126.3 . . ? C79 N40 H40A 126.3 . . ? C119 N60 C219 36(5) . . ? N52 C103 C104 175(2) . . ? N61 C121 C122 163(2) . . ? N52A C203 C204 169(2) . . ? C203 C204 H20B 109.5 . . ? C203 C204 H20C 109.5 . . ? H20B C204 H20C 109.5 . . ? C203 C204 H20D 109.5 . . ? H20B C204 H20D 109.5 . . ? H20C C204 H20D 109.5 . . ? N61A C221 C222 178(3) . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? N64 C127 C128 164(2) . . ? N63 C125 C126 167(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.830 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.100 # Attachment '- as825.cif' data_as825 _database_code_depnum_ccdc_archive 'CCDC 826152' _publ_section_title_footnote ; ? #<< paper footnote text ; # 4. TEXT _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; #Barbour, L. J. (2001). J. Supramol. Chem., 1, 189-191. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # 5. CHEMICAL DATA _publ_section_figure_captions ; ? #<< figure captions ; #============================================================================== # 6. CRYSTALLOGRAPHY _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H80 N40 Co4, 8(C F3 S O3), 6(C2 H3 N), 6(H2 O)' _chemical_formula_sum 'C100 H110 Co4 F24 N46 O30 S8' _chemical_formula_weight 3384.54 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.0408(4) _cell_length_b 29.0227(6) _cell_length_c 31.0259(5) _cell_angle_alpha 95.280(1) _cell_angle_beta 98.156(1) _cell_angle_gamma 97.466(1) _cell_volume 14964.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 267120 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method ? _exptl_crystal_F_000 6896 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8023 _exptl_absorpt_correction_T_max 0.9077 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 116734 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.1610 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 27.49 _reflns_number_total 62293 _reflns_number_gt 26784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker 8.6' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. For the reason to keep chemical integrity of the disordered parts of the structure, some geometrical/thermal parameters were constrained/restrained using DFIX/SADI/EADP instructions during structure refinement. ; _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^)+(0.1500P)^2^+45.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00018(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 62293 _refine_ls_number_parameters 3754 _refine_ls_number_restraints 945 _refine_ls_R_factor_all 0.2382 _refine_ls_R_factor_gt 0.1172 _refine_ls_wR_factor_ref 0.3503 _refine_ls_wR_factor_gt 0.2921 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.056 _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 -0.36804(6) 0.22024(4) 0.46597(3) 0.0316(3) Uani 1 1 d . . . Co2 Co -0.10661(7) 0.33417(4) 0.62212(3) 0.0315(3) Uani 1 1 d . . . Co3 Co 0.16995(7) 0.26590(4) 0.52060(3) 0.0297(3) Uani 1 1 d . . . Co4 Co -0.09426(6) 0.14834(4) 0.37036(3) 0.0295(3) Uani 1 1 d . . . N101 N -0.4545(4) 0.1883(3) 0.4111(2) 0.0444(19) Uani 1 1 d . . . C102 C -0.5046(6) 0.1472(4) 0.3939(3) 0.055(3) Uani 1 1 d . . . H102 H -0.5112 0.1195 0.4079 0.066 Uiso 1 1 calc R . . C103 C -0.5427(6) 0.1531(4) 0.3538(3) 0.064(3) Uani 1 1 d . . . H103 H -0.5790 0.1303 0.3344 0.077 Uiso 1 1 calc R . . N104 N -0.5186(5) 0.1989(3) 0.3466(2) 0.057(2) Uani 1 1 d . . . H104 H -0.5355 0.2122 0.3234 0.069 Uiso 1 1 calc R . . C105 C -0.4645(5) 0.2196(4) 0.3816(3) 0.046(2) Uani 1 1 d . . . C106 C -0.4243(5) 0.2668(3) 0.3903(3) 0.043(2) Uani 1 1 d . . . H106 H -0.4338 0.2901 0.3713 0.052 Uiso 1 1 calc R . . N107 N -0.3743(4) 0.2745(2) 0.4260(2) 0.0350(16) Uani 1 1 d . . . N108 N -0.3326(4) 0.3174(2) 0.43967(19) 0.0342(16) Uani 1 1 d . . . C109 C -0.2807(5) 0.3210(3) 0.4789(2) 0.0289(18) Uani 1 1 d . . . C110 C -0.2352(5) 0.3630(3) 0.4965(2) 0.0341(19) Uani 1 1 d . . . H110 H -0.2366 0.3903 0.4819 0.041 Uiso 1 1 calc R . . C111 C -0.1876(5) 0.3634(3) 0.5366(3) 0.0351(19) Uani 1 1 d . . . N112 N -0.1409(4) 0.4039(2) 0.5578(2) 0.0391(17) Uani 1 1 d . . . N113 N -0.0982(4) 0.3991(2) 0.5974(2) 0.0363(16) Uani 1 1 d . . . C114 C -0.0575(6) 0.4348(3) 0.6224(3) 0.043(2) Uani 1 1 d . . . H114 H -0.0536 0.4660 0.6149 0.051 Uiso 1 1 calc R . . C115 C -0.0189(5) 0.4220(3) 0.6627(3) 0.042(2) Uani 1 1 d . . . N116 N 0.0263(5) 0.4505(3) 0.6959(2) 0.054(2) Uani 1 1 d . . . H116 H 0.0386 0.4810 0.6968 0.065 Uiso 1 1 calc R . . C117 C 0.0502(6) 0.4238(3) 0.7284(3) 0.048(2) Uani 1 1 d . . . H117 H 0.0829 0.4346 0.7558 0.057 Uiso 1 1 calc R . . C118 C 0.0178(6) 0.3788(3) 0.7135(3) 0.048(2) Uani 1 1 d . . . H118 H 0.0238 0.3525 0.7291 0.057 Uiso 1 1 calc R . . N119 N -0.0254(4) 0.3777(2) 0.6720(2) 0.0360(16) Uani 1 1 d . . . N120 N -0.1838(4) 0.3241(2) 0.55724(19) 0.0333(16) Uani 1 1 d . . . C121 C -0.2307(5) 0.2862(3) 0.5377(2) 0.0277(17) Uani 1 1 d . . . N122 N -0.2790(4) 0.2813(2) 0.49890(18) 0.0284(14) Uani 1 1 d . . . C123 C -0.2327(5) 0.2436(3) 0.5620(2) 0.0297(17) Uani 1 1 d . . . C124 C -0.1817(6) 0.2117(3) 0.5561(3) 0.045(2) Uani 1 1 d . . . H124 H -0.1450 0.2160 0.5360 0.054 Uiso 1 1 calc R . . C125 C -0.1831(6) 0.1728(3) 0.5793(3) 0.052(3) Uani 1 1 d . . . H125 H -0.1461 0.1515 0.5754 0.062 Uiso 1 1 calc R . . C126 C -0.2362(7) 0.1650(4) 0.6072(4) 0.065(3) Uani 1 1 d . . . H126 H -0.2375 0.1381 0.6225 0.078 Uiso 1 1 calc R . . C127 C -0.2890(6) 0.1968(3) 0.6132(3) 0.051(2) Uani 1 1 d . . . H127 H -0.3265 0.1918 0.6327 0.061 Uiso 1 1 calc R . . C128 C -0.2870(5) 0.2363(3) 0.5905(3) 0.037(2) Uani 1 1 d . . . H128 H -0.3232 0.2580 0.5947 0.045 Uiso 1 1 calc R . . C129 C -0.3460(6) 0.3563(3) 0.4145(3) 0.056(3) Uani 1 1 d . . . H12A H -0.3420 0.3474 0.3837 0.084 Uiso 1 1 calc R . . H12B H -0.3056 0.3834 0.4262 0.084 Uiso 1 1 calc R . . H12C H -0.3996 0.3644 0.4165 0.084 Uiso 1 1 calc R . . C130 C -0.1416(6) 0.4496(3) 0.5421(3) 0.052(3) Uani 1 1 d . . . H13A H -0.0871 0.4669 0.5479 0.078 Uiso 1 1 calc R . . H13B H -0.1771 0.4670 0.5573 0.078 Uiso 1 1 calc R . . H13C H -0.1610 0.4457 0.5105 0.078 Uiso 1 1 calc R . . N201 N -0.2085(4) 0.3454(3) 0.6529(2) 0.0424(18) Uani 1 1 d . . . C202 C -0.2649(6) 0.3742(4) 0.6558(3) 0.062(3) Uani 1 1 d . . . H202 H -0.2703 0.4004 0.6399 0.075 Uiso 1 1 calc R . . C203 C -0.3120(7) 0.3595(5) 0.6848(4) 0.077(4) Uani 1 1 d . . . H203 H -0.3558 0.3735 0.6932 0.092 Uiso 1 1 calc R . . N204 N -0.2846(5) 0.3205(3) 0.6998(3) 0.059(2) Uani 1 1 d . . . H204 H -0.3044 0.3038 0.7191 0.071 Uiso 1 1 calc R . . C205 C -0.2218(5) 0.3126(3) 0.6797(3) 0.043(2) Uani 1 1 d . . . C206 C -0.1730(5) 0.2771(3) 0.6852(2) 0.039(2) Uani 1 1 d . . . H206 H -0.1799 0.2542 0.7049 0.047 Uiso 1 1 calc R . . N207 N -0.1179(4) 0.2793(2) 0.66059(19) 0.0345(16) Uani 1 1 d . . . N208 N -0.0650(4) 0.2469(2) 0.6613(2) 0.0377(17) Uani 1 1 d . . . C209 C -0.0143(5) 0.2515(3) 0.6303(2) 0.0329(19) Uani 1 1 d . . . C210 C 0.0398(5) 0.2206(3) 0.6256(2) 0.0350(19) Uani 1 1 d . . . H210 H 0.0436 0.1957 0.6433 0.042 Uiso 1 1 calc R . . C211 C 0.0882(5) 0.2274(3) 0.5937(2) 0.0293(17) Uani 1 1 d . . . N212 N 0.1467(4) 0.2001(2) 0.58846(19) 0.0341(16) Uani 1 1 d . . . N213 N 0.1853(4) 0.2072(2) 0.5534(2) 0.0355(16) Uani 1 1 d . . . C214 C 0.2381(5) 0.1814(3) 0.5428(3) 0.039(2) Uani 1 1 d . . . H214 H 0.2532 0.1562 0.5579 0.047 Uiso 1 1 calc R . . C215 C 0.2707(5) 0.1961(3) 0.5049(2) 0.037(2) Uani 1 1 d . . . N216 N 0.3139(4) 0.1717(3) 0.4807(2) 0.0433(18) Uani 1 1 d . . . H216 H 0.3309 0.1450 0.4858 0.052 Uiso 1 1 calc R . . C217 C 0.3263(6) 0.1971(3) 0.4457(3) 0.051(3) Uani 1 1 d . . . H217 H 0.3567 0.1897 0.4233 0.061 Uiso 1 1 calc R . . C218 C 0.2865(6) 0.2349(3) 0.4497(3) 0.049(2) Uani 1 1 d . . . H218 H 0.2841 0.2583 0.4301 0.058 Uiso 1 1 calc R . . N219 N 0.2508(4) 0.2337(2) 0.48642(19) 0.0356(16) Uani 1 1 d . . . N220 N 0.0819(4) 0.2620(2) 0.56723(19) 0.0296(15) Uani 1 1 d . . . C221 C 0.0281(5) 0.2906(3) 0.5748(2) 0.0308(18) Uani 1 1 d . . . N222 N -0.0210(4) 0.2872(2) 0.60512(19) 0.0292(14) Uani 1 1 d . . . C223 C 0.0263(5) 0.3316(3) 0.5502(3) 0.038(2) Uani 1 1 d . . . C224 C -0.0190(6) 0.3285(4) 0.5094(3) 0.050(2) Uani 1 1 d . . . H224 H -0.0501 0.2997 0.4964 0.060 Uiso 1 1 calc R . . C225 C -0.0190(8) 0.3685(5) 0.4871(3) 0.080(4) Uani 1 1 d . . . H225 H -0.0523 0.3669 0.4596 0.096 Uiso 1 1 calc R . . C226 C 0.0292(10) 0.4108(5) 0.5047(5) 0.094(5) Uani 1 1 d . . . H226 H 0.0323 0.4373 0.4888 0.112 Uiso 1 1 calc R . . C227 C 0.0713(8) 0.4122(4) 0.5454(5) 0.083(4) Uani 1 1 d . . . H227 H 0.1013 0.4412 0.5586 0.099 Uiso 1 1 calc R . . C228 C 0.0734(7) 0.3737(3) 0.5693(3) 0.058(3) Uani 1 1 d . . . H228 H 0.1054 0.3760 0.5973 0.069 Uiso 1 1 calc R . . C229 C -0.0640(6) 0.2135(3) 0.6926(2) 0.041(2) Uani 1 1 d . . . H22A H -0.0702 0.2287 0.7212 0.062 Uiso 1 1 calc R . . H22B H -0.0129 0.2011 0.6950 0.062 Uiso 1 1 calc R . . H22C H -0.1081 0.1878 0.6829 0.062 Uiso 1 1 calc R . . C230 C 0.1696(6) 0.1646(3) 0.6175(3) 0.047(2) Uani 1 1 d . . . H23A H 0.2278 0.1699 0.6267 0.071 Uiso 1 1 calc R . . H23B H 0.1534 0.1333 0.6015 0.071 Uiso 1 1 calc R . . H23C H 0.1427 0.1672 0.6433 0.071 Uiso 1 1 calc R . . N301 N 0.2559(4) 0.3091(2) 0.56768(19) 0.0310(15) Uani 1 1 d . . . C302 C 0.3009(5) 0.3109(3) 0.6084(3) 0.043(2) Uani 1 1 d . . . H302 H 0.3037 0.2854 0.6253 0.051 Uiso 1 1 calc R . . C303 C 0.3409(6) 0.3549(3) 0.6207(3) 0.054(3) Uani 1 1 d . . . H303 H 0.3764 0.3658 0.6471 0.064 Uiso 1 1 calc R . . N304 N 0.3188(5) 0.3803(3) 0.5865(2) 0.060(2) Uani 1 1 d . . . H304 H 0.3350 0.4101 0.5854 0.072 Uiso 1 1 calc R . . C305 C 0.2693(5) 0.3520(3) 0.5558(3) 0.041(2) Uani 1 1 d . . . C306 C 0.2295(6) 0.3630(3) 0.5139(3) 0.047(2) Uani 1 1 d . . . H306 H 0.2402 0.3924 0.5031 0.057 Uiso 1 1 calc R . . N307 N 0.1795(4) 0.3295(2) 0.49352(19) 0.0317(15) Uani 1 1 d . . . N308 N 0.1359(4) 0.3325(2) 0.4536(2) 0.0349(16) Uani 1 1 d . . . C309 C 0.0844(5) 0.2930(3) 0.4359(2) 0.0314(18) Uani 1 1 d . . . C310 C 0.0370(5) 0.2908(3) 0.3953(2) 0.0328(18) Uani 1 1 d . . . H310 H 0.0375 0.3172 0.3792 0.039 Uiso 1 1 calc R . . C311 C -0.0102(5) 0.2496(3) 0.3794(2) 0.0288(17) Uani 1 1 d . . . N312 N -0.0558(4) 0.2426(2) 0.33861(19) 0.0331(16) Uani 1 1 d . . . N313 N -0.1033(4) 0.2004(2) 0.32753(19) 0.0278(14) Uani 1 1 d . . . C314 C -0.1495(5) 0.1885(3) 0.2906(2) 0.0343(19) Uani 1 1 d . . . H314 H -0.1545 0.2086 0.2682 0.041 Uiso 1 1 calc R . . C315 C -0.1925(5) 0.1424(3) 0.2862(2) 0.039(2) Uani 1 1 d . . . N316 N -0.2494(5) 0.1213(3) 0.2536(2) 0.051(2) Uani 1 1 d . . . H316 H -0.2690 0.1340 0.2305 0.061 Uiso 1 1 calc R . . C317 C -0.2714(7) 0.0770(4) 0.2625(3) 0.067(3) Uani 1 1 d . . . H317 H -0.3104 0.0539 0.2450 0.080 Uiso 1 1 calc R . . C318 C -0.2275(6) 0.0720(3) 0.3008(3) 0.053(3) Uani 1 1 d . . . H318 H -0.2305 0.0441 0.3147 0.063 Uiso 1 1 calc R . . N319 N -0.1773(4) 0.1130(2) 0.3173(2) 0.0401(17) Uani 1 1 d . . . N320 N -0.0152(4) 0.2111(2) 0.40364(18) 0.0279(14) Uani 1 1 d . . . C321 C 0.0353(5) 0.2170(3) 0.4415(2) 0.0318(19) Uani 1 1 d . . . N322 N 0.0836(4) 0.2557(2) 0.45969(18) 0.0288(15) Uani 1 1 d . . . C323 C 0.0394(5) 0.1743(3) 0.4645(2) 0.0284(17) Uani 1 1 d . . . C324 C -0.0096(5) 0.1620(3) 0.4950(2) 0.0354(19) Uani 1 1 d . . . H324 H -0.0494 0.1807 0.5011 0.043 Uiso 1 1 calc R . . C325 C -0.0010(6) 0.1228(3) 0.5165(3) 0.049(2) Uani 1 1 d . . . H325 H -0.0345 0.1148 0.5375 0.059 Uiso 1 1 calc R . . C326 C 0.0553(6) 0.0957(3) 0.5075(3) 0.050(2) Uani 1 1 d . . . H326 H 0.0602 0.0685 0.5219 0.060 Uiso 1 1 calc R . . C327 C 0.1053(6) 0.1074(3) 0.4777(3) 0.046(2) Uani 1 1 d . . . H327 H 0.1445 0.0882 0.4716 0.055 Uiso 1 1 calc R . . C328 C 0.0983(5) 0.1466(3) 0.4569(3) 0.041(2) Uani 1 1 d . . . H328 H 0.1340 0.1551 0.4371 0.049 Uiso 1 1 calc R . . C329 C 0.1485(6) 0.3750(3) 0.4318(3) 0.051(2) Uani 1 1 d . . . H32A H 0.1016 0.3761 0.4099 0.076 Uiso 1 1 calc R . . H32B H 0.1960 0.3747 0.4174 0.076 Uiso 1 1 calc R . . H32C H 0.1564 0.4025 0.4536 0.076 Uiso 1 1 calc R . . C330 C -0.0517(5) 0.2773(3) 0.3074(2) 0.037(2) Uani 1 1 d . . . H33A H -0.0431 0.2624 0.2791 0.056 Uiso 1 1 calc R . . H33B H -0.0071 0.3024 0.3186 0.056 Uiso 1 1 calc R . . H33C H -0.1020 0.2905 0.3035 0.056 Uiso 1 1 calc R . . N401 N 0.0108(4) 0.1276(2) 0.3518(2) 0.0409(18) Uani 1 1 d . . . C402 C 0.0802(6) 0.1452(3) 0.3358(3) 0.049(2) Uani 1 1 d . . . H402 H 0.0877 0.1733 0.3226 0.059 Uiso 1 1 calc R . . C403 C 0.1358(6) 0.1149(3) 0.3422(3) 0.057(3) Uani 1 1 d . . . H403 H 0.1879 0.1182 0.3343 0.068 Uiso 1 1 calc R . . N404 N 0.1008(5) 0.0790(3) 0.3626(2) 0.048(2) Uani 1 1 d . . . H404 H 0.1225 0.0545 0.3704 0.057 Uiso 1 1 calc R . . C405 C 0.0266(5) 0.0883(3) 0.3683(3) 0.043(2) Uani 1 1 d . . . C406 C -0.0274(5) 0.0642(3) 0.3942(2) 0.0340(19) Uani 1 1 d . . . H406 H -0.0218 0.0346 0.4042 0.041 Uiso 1 1 calc R . . N407 N -0.0834(4) 0.0880(2) 0.40186(19) 0.0297(15) Uani 1 1 d . . . N408 N -0.1382(4) 0.0739(2) 0.4279(2) 0.0338(16) Uani 1 1 d . . . C409 C -0.1871(5) 0.1059(3) 0.4377(2) 0.0311(18) Uani 1 1 d . . . C410 C -0.2407(5) 0.0996(3) 0.4667(3) 0.0357(19) Uani 1 1 d . . . H410 H -0.2453 0.0722 0.4813 0.043 Uiso 1 1 calc R . . C411 C -0.2872(5) 0.1335(3) 0.4738(2) 0.0327(18) Uani 1 1 d . . . N412 N -0.3431(4) 0.1291(2) 0.5014(2) 0.0353(16) Uani 1 1 d . . . N413 N -0.3857(4) 0.1658(2) 0.5052(2) 0.0378(17) Uani 1 1 d . . . C414 C -0.4404(5) 0.1674(3) 0.5302(3) 0.043(2) Uani 1 1 d . . . H414 H -0.4550 0.1436 0.5478 0.051 Uiso 1 1 calc R . . C415 C -0.4769(5) 0.2100(4) 0.5280(3) 0.045(2) Uani 1 1 d . . . N416 N -0.5337(5) 0.2234(3) 0.5492(3) 0.061(2) Uani 1 1 d . . . H416 H -0.5568 0.2080 0.5683 0.073 Uiso 1 1 calc R . . C417 C -0.5502(6) 0.2654(5) 0.5364(4) 0.072(4) Uani 1 1 d . . . H417 H -0.5883 0.2833 0.5463 0.087 Uiso 1 1 calc R . . C418 C -0.5016(6) 0.2764(4) 0.5067(3) 0.057(3) Uani 1 1 d . . . H418 H -0.4995 0.3037 0.4920 0.069 Uiso 1 1 calc R . . N419 N -0.4564(4) 0.2415(3) 0.5018(2) 0.0456(19) Uani 1 1 d . . . N420 N -0.2837(4) 0.1727(2) 0.45233(19) 0.0312(15) Uani 1 1 d . . . C421 C -0.2319(4) 0.1750(3) 0.4233(2) 0.0278(17) Uani 1 1 d . . . N422 N -0.1819(4) 0.1451(2) 0.41614(19) 0.0286(14) Uani 1 1 d . . . C423 C -0.2359(5) 0.2141(3) 0.3954(2) 0.0299(18) Uani 1 1 d . . . C424 C -0.1895(6) 0.2572(3) 0.4075(3) 0.047(2) Uani 1 1 d . . . H424 H -0.1536 0.2630 0.4344 0.056 Uiso 1 1 calc R . . C425 C -0.1961(7) 0.2926(3) 0.3791(4) 0.055(3) Uani 1 1 d . . . H425 H -0.1645 0.3224 0.3873 0.065 Uiso 1 1 calc R . . C426 C -0.2462(7) 0.2846(4) 0.3412(4) 0.063(3) Uani 1 1 d . . . H426 H -0.2496 0.3088 0.3226 0.076 Uiso 1 1 calc R . . C427 C -0.2935(7) 0.2415(4) 0.3284(3) 0.054(3) Uani 1 1 d . . . H427 H -0.3289 0.2363 0.3013 0.064 Uiso 1 1 calc R . . C428 C -0.2890(6) 0.2060(3) 0.3553(3) 0.043(2) Uani 1 1 d . . . H428 H -0.3214 0.1765 0.3468 0.051 Uiso 1 1 calc R . . C429 C -0.1370(5) 0.0301(3) 0.4469(3) 0.039(2) Uani 1 1 d . . . H42A H -0.1838 0.0241 0.4617 0.059 Uiso 1 1 calc R . . H42B H -0.0880 0.0320 0.4681 0.059 Uiso 1 1 calc R . . H42C H -0.1384 0.0046 0.4236 0.059 Uiso 1 1 calc R . . C430 C -0.3617(6) 0.0875(3) 0.5248(3) 0.049(2) Uani 1 1 d . . . H43A H -0.3561 0.0973 0.5563 0.074 Uiso 1 1 calc R . . H43B H -0.3244 0.0653 0.5195 0.074 Uiso 1 1 calc R . . H43C H -0.4167 0.0725 0.5139 0.074 Uiso 1 1 calc R . . Co5 Co 0.36240(7) 0.26968(4) 1.02767(3) 0.0352(3) Uani 1 1 d . . . Co6 Co 0.07684(6) 0.16357(4) 0.88038(3) 0.0291(3) Uani 1 1 d . . . Co7 Co -0.17612(7) 0.23772(4) 0.99323(4) 0.0371(3) Uani 1 1 d . . . Co8 Co 0.11150(8) 0.35340(4) 1.13290(4) 0.0414(3) Uani 1 1 d . . . N501 N 0.4426(4) 0.3014(3) 1.0846(2) 0.0443(19) Uani 1 1 d . . . C502 C 0.4819(6) 0.3437(4) 1.1052(3) 0.058(3) Uani 1 1 d . . . H502 H 0.4832 0.3729 1.0935 0.070 Uiso 1 1 calc R . . C503 C 0.5187(6) 0.3361(5) 1.1455(3) 0.069(3) Uani 1 1 d . . . H503 H 0.5497 0.3594 1.1670 0.083 Uiso 1 1 calc R . . N504 N 0.5036(5) 0.2907(4) 1.1497(2) 0.058(2) Uani 1 1 d . . . H504 H 0.5207 0.2766 1.1724 0.070 Uiso 1 1 calc R . . C505 C 0.4567(5) 0.2702(4) 1.1121(3) 0.043(2) Uani 1 1 d . . . C506 C 0.4213(6) 0.2231(3) 1.1029(3) 0.047(2) Uani 1 1 d . . . H506 H 0.4339 0.1996 1.1211 0.056 Uiso 1 1 calc R . . N507 N 0.3700(4) 0.2149(3) 1.06727(19) 0.0379(17) Uani 1 1 d . . . N508 N 0.3277(4) 0.1724(3) 1.0528(2) 0.0406(18) Uani 1 1 d . . . C509 C 0.2698(5) 0.1709(3) 1.0161(2) 0.0311(18) Uani 1 1 d . . . C510 C 0.2203(5) 0.1303(3) 0.9996(2) 0.0347(19) Uani 1 1 d . . . H510 H 0.2244 0.1023 1.0128 0.042 Uiso 1 1 calc R . . C511 C 0.1637(5) 0.1314(3) 0.9629(2) 0.0334(19) Uani 1 1 d . . . N512 N 0.1117(4) 0.0930(2) 0.9436(2) 0.0347(16) Uani 1 1 d . . . N513 N 0.0664(4) 0.0990(2) 0.9055(2) 0.0304(15) Uani 1 1 d . . . C514 C 0.0218(5) 0.0646(3) 0.8809(3) 0.037(2) Uani 1 1 d . . . H514 H 0.0163 0.0334 0.8883 0.045 Uiso 1 1 calc R . . C515 C -0.0191(6) 0.0778(3) 0.8410(3) 0.043(2) Uani 1 1 d . . . N516 N -0.0679(5) 0.0485(3) 0.8081(2) 0.054(2) Uani 1 1 d . . . H516 H -0.0822 0.0183 0.8080 0.065 Uiso 1 1 calc R . . C517 C -0.0905(7) 0.0747(4) 0.7754(3) 0.060(3) Uani 1 1 d . . . H517 H -0.1234 0.0641 0.7480 0.072 Uiso 1 1 calc R . . C518 C -0.0554(6) 0.1201(3) 0.7906(3) 0.050(2) Uani 1 1 d . . . H518 H -0.0619 0.1465 0.7753 0.060 Uiso 1 1 calc R . . N519 N -0.0095(4) 0.1216(2) 0.8313(2) 0.0377(16) Uani 1 1 d . . . N520 N 0.1599(4) 0.1725(2) 0.9436(2) 0.0305(15) Uani 1 1 d . . . C521 C 0.2137(4) 0.2087(3) 0.9609(2) 0.0256(17) Uani 1 1 d . . . N522 N 0.2681(4) 0.2108(2) 0.99731(19) 0.0300(15) Uani 1 1 d . . . C523 C 0.2171(5) 0.2499(3) 0.9364(2) 0.0300(18) Uani 1 1 d . . . C524 C 0.1648(5) 0.2832(3) 0.9404(3) 0.039(2) Uani 1 1 d . . . H524 H 0.1271 0.2799 0.9601 0.047 Uiso 1 1 calc R . . C525 C 0.1676(6) 0.3205(3) 0.9162(3) 0.052(3) Uani 1 1 d . . . H525 H 0.1319 0.3427 0.9191 0.062 Uiso 1 1 calc R . . C526 C 0.2212(7) 0.3254(3) 0.8881(3) 0.056(3) Uani 1 1 d . . . H526 H 0.2226 0.3513 0.8714 0.067 Uiso 1 1 calc R . . C527 C 0.2733(6) 0.2940(3) 0.8833(3) 0.051(2) Uani 1 1 d . . . H527 H 0.3101 0.2978 0.8631 0.061 Uiso 1 1 calc R . . C528 C 0.2722(6) 0.2561(3) 0.9083(3) 0.044(2) Uani 1 1 d . . . H528 H 0.3094 0.2347 0.9058 0.052 Uiso 1 1 calc R . . C529 C 0.3395(6) 0.1327(3) 1.0779(3) 0.053(3) Uani 1 1 d . . . H52A H 0.3964 0.1292 1.0825 0.079 Uiso 1 1 calc R . . H52B H 0.3083 0.1040 1.0616 0.079 Uiso 1 1 calc R . . H52C H 0.3216 0.1383 1.1063 0.079 Uiso 1 1 calc R . . C530 C 0.1091(6) 0.0471(3) 0.9583(3) 0.046(2) Uani 1 1 d . . . H53A H 0.0550 0.0363 0.9640 0.069 Uiso 1 1 calc R . . H53B H 0.1475 0.0486 0.9853 0.069 Uiso 1 1 calc R . . H53C H 0.1232 0.0252 0.9356 0.069 Uiso 1 1 calc R . . N601 N 0.1776(4) 0.1533(2) 0.8509(2) 0.0338(16) Uani 1 1 d . . . C602 C 0.2371(5) 0.1257(3) 0.8504(3) 0.041(2) Uani 1 1 d . . . H602 H 0.2459 0.1020 0.8689 0.050 Uiso 1 1 calc R . . C603 C 0.2809(6) 0.1377(3) 0.8193(3) 0.048(2) Uani 1 1 d . . . H603 H 0.3256 0.1240 0.8119 0.058 Uiso 1 1 calc R . . N604 N 0.2495(4) 0.1731(3) 0.8004(2) 0.0435(19) Uani 1 1 d . . . H604 H 0.2671 0.1878 0.7793 0.052 Uiso 1 1 calc R . . C605 C 0.1865(5) 0.1815(3) 0.8200(2) 0.0355(19) Uani 1 1 d . . . C606 C 0.1368(4) 0.2172(3) 0.8135(2) 0.0304(18) Uani 1 1 d . . . H606 H 0.1408 0.2377 0.7915 0.037 Uiso 1 1 calc R . . N607 N 0.0863(4) 0.2188(2) 0.84045(18) 0.0280(14) Uani 1 1 d . . . N608 N 0.0341(4) 0.2506(2) 0.84153(19) 0.0314(15) Uani 1 1 d . . . C609 C -0.0087(4) 0.2491(3) 0.8754(2) 0.0254(16) Uani 1 1 d . . . C610 C -0.0557(5) 0.2827(3) 0.8851(2) 0.0338(19) Uani 1 1 d . . . H610 H -0.0590 0.3084 0.8684 0.041 Uiso 1 1 calc R . . C611 C -0.0977(5) 0.2780(3) 0.9194(3) 0.0343(19) Uani 1 1 d . . . N612 N -0.1472(5) 0.3098(3) 0.9301(2) 0.048(2) Uani 1 1 d . . . N613 N -0.1891(4) 0.2988(3) 0.9628(2) 0.0452(19) Uani 1 1 d . . . C614 C -0.2409(6) 0.3244(3) 0.9756(3) 0.052(3) Uani 1 1 d . . . H614 H -0.2523 0.3521 0.9633 0.063 Uiso 1 1 calc R . . C615 C -0.2790(6) 0.3060(3) 1.0105(3) 0.049(2) Uani 1 1 d . . . N616 N -0.3336(5) 0.3247(3) 1.0305(3) 0.064(3) Uani 1 1 d . . . H616 H -0.3540 0.3502 1.0247 0.077 Uiso 1 1 calc R . . C617 C -0.3518(6) 0.2959(4) 1.0622(3) 0.062(3) Uani 1 1 d . . . H617 H -0.3875 0.3005 1.0826 0.074 Uiso 1 1 calc R . . C618 C -0.3089(5) 0.2599(3) 1.0584(3) 0.046(2) Uani 1 1 d . . . H618 H -0.3102 0.2344 1.0756 0.056 Uiso 1 1 calc R . . N619 N -0.2632(4) 0.2662(3) 1.0256(2) 0.0429(18) Uani 1 1 d . . . N620 N -0.0937(4) 0.2413(2) 0.9440(2) 0.0325(16) Uani 1 1 d . . . C621 C -0.0477(4) 0.2101(3) 0.9322(2) 0.0250(16) Uani 1 1 d . . . N622 N -0.0036(4) 0.2118(2) 0.89963(18) 0.0269(14) Uani 1 1 d . . . C623 C -0.0501(5) 0.1674(3) 0.9556(2) 0.0306(18) Uani 1 1 d . . . C624 C -0.0063(5) 0.1686(3) 0.9974(2) 0.042(2) Uani 1 1 d . . . H624 H 0.0272 0.1963 1.0113 0.051 Uiso 1 1 calc R . . C625 C -0.0134(6) 0.1275(4) 1.0183(3) 0.057(3) Uani 1 1 d . . . H625 H 0.0182 0.1272 1.0461 0.069 Uiso 1 1 calc R . . C626 C -0.0639(6) 0.0884(3) 1.0000(3) 0.052(3) Uani 1 1 d . . . H626 H -0.0684 0.0615 1.0153 0.063 Uiso 1 1 calc R . . C627 C -0.1097(6) 0.0876(3) 0.9581(3) 0.053(3) Uani 1 1 d . . . H627 H -0.1458 0.0605 0.9453 0.063 Uiso 1 1 calc R . . C628 C -0.1010(5) 0.1276(3) 0.9359(3) 0.041(2) Uani 1 1 d . . . H628 H -0.1300 0.1274 0.9073 0.049 Uiso 1 1 calc R . . C629 C 0.0334(5) 0.2861(3) 0.8124(2) 0.039(2) Uani 1 1 d . . . H62A H 0.0476 0.2739 0.7844 0.059 Uiso 1 1 calc R . . H62B H 0.0724 0.3134 0.8254 0.059 Uiso 1 1 calc R . . H62C H -0.0202 0.2953 0.8073 0.059 Uiso 1 1 calc R . . C630 C -0.1607(7) 0.3503(3) 0.9069(3) 0.065(3) Uani 1 1 d . . . H63A H -0.1750 0.3748 0.9269 0.098 Uiso 1 1 calc R . . H63B H -0.2044 0.3411 0.8822 0.098 Uiso 1 1 calc R . . H63C H -0.1117 0.3622 0.8958 0.098 Uiso 1 1 calc R . . N701 N -0.2580(4) 0.1904(3) 0.9465(2) 0.0389(17) Uani 1 1 d . . . C702 C -0.2956(6) 0.1832(3) 0.9038(3) 0.045(2) Uani 1 1 d . . . H702 H -0.2933 0.2057 0.8834 0.054 Uiso 1 1 calc R . . C703 C -0.3355(6) 0.1403(4) 0.8950(3) 0.053(3) Uani 1 1 d . . . H703 H -0.3661 0.1267 0.8678 0.064 Uiso 1 1 calc R . . N704 N -0.3242(5) 0.1190(3) 0.9327(2) 0.048(2) Uani 1 1 d . . . H704 H -0.3449 0.0905 0.9363 0.058 Uiso 1 1 calc R . . C705 C -0.2753(5) 0.1501(3) 0.9632(3) 0.039(2) Uani 1 1 d . . . C706 C -0.2391(5) 0.1425(3) 1.0063(3) 0.040(2) Uani 1 1 d . . . H706 H -0.2523 0.1148 1.0195 0.048 Uiso 1 1 calc R . . N707 N -0.1871(4) 0.1769(3) 1.0249(2) 0.0407(18) Uani 1 1 d . . . N708 N -0.1459(5) 0.1770(3) 1.0652(2) 0.0441(18) Uani 1 1 d . . . C709 C -0.0871(5) 0.2148(3) 1.0791(3) 0.040(2) Uani 1 1 d . . . C710 C -0.0349(5) 0.2163(3) 1.1176(3) 0.039(2) Uani 1 1 d . . . H710 H -0.0352 0.1905 1.1345 0.047 Uiso 1 1 calc R . . C711 C 0.0179(5) 0.2570(3) 1.1303(3) 0.038(2) Uani 1 1 d . . . N712 N 0.0705(5) 0.2630(3) 1.1697(2) 0.0435(18) Uani 1 1 d . . . N713 N 0.1217(5) 0.3035(2) 1.1778(2) 0.0416(18) Uani 1 1 d . . . C714 C 0.1723(7) 0.3146(3) 1.2126(3) 0.054(3) Uani 1 1 d . A . H714 H 0.1762 0.2960 1.2363 0.065 Uiso 1 1 calc R . . C715 C 0.2213(7) 0.3565(4) 1.2123(3) 0.079(4) Uani 1 1 d D . . N716 N 0.3031(8) 0.3701(5) 1.2352(4) 0.055(4) Uiso 0.50 1 d PD A 1 H716 H 0.3241 0.3575 1.2581 0.067 Uiso 0.50 1 calc PR A 1 C717 C 0.3446(14) 0.4066(7) 1.2156(6) 0.076(7) Uiso 0.50 1 d PD A 1 H717 H 0.3982 0.4217 1.2240 0.091 Uiso 0.50 1 calc PR A 1 C718 C 0.2898(10) 0.4144(6) 1.1825(6) 0.057(5) Uiso 0.50 1 d PD A 1 H718 H 0.2995 0.4372 1.1631 0.069 Uiso 0.50 1 calc PR A 1 N76' N 0.2659(8) 0.3869(6) 1.2502(5) 0.071(5) Uiso 0.50 1 d PD A 2 H76' H 0.2791 0.3781 1.2763 0.085 Uiso 0.50 1 calc PR A 2 C77' C 0.2851(13) 0.4330(9) 1.2388(8) 0.104(9) Uiso 0.50 1 d PD A 2 H77' H 0.3138 0.4596 1.2572 0.125 Uiso 0.50 1 calc PR A 2 C78' C 0.2539(10) 0.4306(6) 1.1963(7) 0.086(8) Uiso 0.50 1 d PD A 2 H78' H 0.2574 0.4562 1.1794 0.103 Uiso 0.50 1 calc PR A 2 N719 N 0.2144(5) 0.3842(3) 1.1798(2) 0.066(3) Uani 1 1 d D A . N720 N 0.0239(4) 0.2930(2) 1.1050(2) 0.0373(17) Uani 1 1 d . . . C721 C -0.0292(6) 0.2881(3) 1.0691(3) 0.041(2) Uani 1 1 d . . . N722 N -0.0843(4) 0.2500(3) 1.0528(2) 0.0381(17) Uani 1 1 d . . . C723 C -0.0332(5) 0.3301(3) 1.0442(3) 0.043(2) Uani 1 1 d . . . C724 C 0.0130(6) 0.3375(3) 1.0113(3) 0.050(2) Uani 1 1 d . . . H724 H 0.0465 0.3155 1.0033 0.060 Uiso 1 1 calc R . . C725 C 0.0095(7) 0.3765(4) 0.9907(3) 0.068(3) Uani 1 1 d . . . H725 H 0.0417 0.3823 0.9686 0.082 Uiso 1 1 calc R . . C726 C -0.0421(9) 0.4089(4) 1.0020(4) 0.089(4) Uani 1 1 d . . . H726 H -0.0465 0.4355 0.9865 0.107 Uiso 1 1 calc R . . C727 C -0.0851(8) 0.4016(4) 1.0351(4) 0.083(4) Uani 1 1 d . . . H727 H -0.1177 0.4239 1.0438 0.100 Uiso 1 1 calc R . . C728 C -0.0815(6) 0.3612(3) 1.0563(3) 0.058(3) Uani 1 1 d . . . H728 H -0.1124 0.3556 1.0790 0.069 Uiso 1 1 calc R . . C729 C -0.1626(6) 0.1376(3) 1.0909(3) 0.056(3) Uani 1 1 d . . . H72A H -0.2205 0.1306 1.0908 0.083 Uiso 1 1 calc R . . H72B H -0.1353 0.1461 1.1212 0.083 Uiso 1 1 calc R . . H72C H -0.1431 0.1100 1.0780 0.083 Uiso 1 1 calc R . . C730 C 0.0663(6) 0.2295(3) 1.2020(3) 0.053(3) Uani 1 1 d . . . H73A H 0.0533 0.2447 1.2291 0.079 Uiso 1 1 calc R . . H73B H 0.1182 0.2183 1.2083 0.079 Uiso 1 1 calc R . . H73C H 0.0247 0.2029 1.1904 0.079 Uiso 1 1 calc R . . N801 N 0.0334(5) 0.3855(3) 1.1676(3) 0.057(2) Uani 1 1 d . . . C802 C -0.0079(6) 0.3825(4) 1.2014(3) 0.058(3) Uani 1 1 d . . . H802 H -0.0151 0.3556 1.2164 0.070 Uiso 1 1 calc R . . C803 C -0.0384(8) 0.4231(4) 1.2115(4) 0.080(4) Uani 1 1 d . . . H803 H -0.0685 0.4298 1.2342 0.096 Uiso 1 1 calc R . . N804 N -0.0150(5) 0.4519(3) 1.1809(3) 0.059(2) Uani 1 1 d . . . H804 H -0.0268 0.4803 1.1785 0.071 Uiso 1 1 calc R . . C805 C 0.0286(6) 0.4290(4) 1.1557(3) 0.056(3) Uani 1 1 d . . . C806 C 0.0674(7) 0.4458(3) 1.1203(4) 0.067(3) Uani 1 1 d . . . H806 H 0.0644 0.4757 1.1104 0.080 Uiso 1 1 calc R . . N807 N 0.1071(5) 0.4147(3) 1.1037(2) 0.049(2) Uani 1 1 d . . . N808 N 0.1519(5) 0.4249(2) 1.0720(2) 0.047(2) Uani 1 1 d . . . C809 C 0.1950(5) 0.3912(3) 1.0600(3) 0.039(2) Uani 1 1 d . . . C810 C 0.2470(6) 0.3959(3) 1.0290(3) 0.045(2) Uani 1 1 d . . . H810 H 0.2534 0.4231 1.0143 0.054 Uiso 1 1 calc R . . C811 C 0.2877(5) 0.3594(3) 1.0209(2) 0.036(2) Uani 1 1 d . . . N812 N 0.3423(5) 0.3618(3) 0.9919(2) 0.0426(18) Uani 1 1 d . . . N813 N 0.3834(4) 0.3241(3) 0.9886(2) 0.0383(17) Uani 1 1 d . . . C814 C 0.4390(6) 0.3215(4) 0.9646(3) 0.053(3) Uani 1 1 d . . . H814 H 0.4560 0.3455 0.9477 0.063 Uiso 1 1 calc R . . C815 C 0.4721(6) 0.2790(4) 0.9660(3) 0.052(3) Uani 1 1 d . . . N816 N 0.5288(6) 0.2649(4) 0.9447(3) 0.079(3) Uani 1 1 d . . . H816 H 0.5520 0.2801 0.9255 0.095 Uiso 1 1 calc R . . C817 C 0.5451(8) 0.2224(6) 0.9577(4) 0.093(5) Uani 1 1 d . . . H817 H 0.5845 0.2048 0.9489 0.112 Uiso 1 1 calc R . . C818 C 0.4928(6) 0.2111(4) 0.9860(4) 0.067(3) Uani 1 1 d . . . H818 H 0.4878 0.1831 0.9996 0.080 Uiso 1 1 calc R . . N819 N 0.4487(4) 0.2470(3) 0.9914(2) 0.048(2) Uani 1 1 d . . . N820 N 0.2822(4) 0.3206(2) 1.04230(18) 0.0298(15) Uani 1 1 d . . . C821 C 0.2336(4) 0.3190(3) 1.0722(2) 0.0270(17) Uani 1 1 d . . . N822 N 0.1886(4) 0.3517(2) 1.08157(19) 0.0349(16) Uani 1 1 d . . . C823 C 0.2336(5) 0.2798(3) 1.0990(2) 0.0302(18) Uani 1 1 d . . . C824 C 0.1833(6) 0.2389(3) 1.0855(3) 0.048(2) Uani 1 1 d . . . H824 H 0.1474 0.2354 1.0586 0.058 Uiso 1 1 calc R . . C825 C 0.1853(8) 0.2014(4) 1.1124(5) 0.076(4) Uani 1 1 d . . . H825 H 0.1501 0.1729 1.1035 0.091 Uiso 1 1 calc R . . C826 C 0.2377(7) 0.2064(4) 1.1508(4) 0.064(3) Uani 1 1 d . . . H826 H 0.2400 0.1813 1.1684 0.077 Uiso 1 1 calc R . . C827 C 0.2857(7) 0.2471(4) 1.1632(3) 0.058(3) Uani 1 1 d . . . H827 H 0.3211 0.2508 1.1902 0.070 Uiso 1 1 calc R . . C828 C 0.2853(6) 0.2845(3) 1.1376(3) 0.044(2) Uani 1 1 d . . . H828 H 0.3206 0.3129 1.1470 0.053 Uiso 1 1 calc R . . C829 C 0.1543(7) 0.4706(3) 1.0548(3) 0.068(3) Uani 1 1 d . . . H82A H 0.0995 0.4768 1.0458 0.102 Uiso 1 1 calc R . . H82B H 0.1827 0.4702 1.0294 0.102 Uiso 1 1 calc R . . H82C H 0.1824 0.4952 1.0775 0.102 Uiso 1 1 calc R . . C830 C 0.3620(7) 0.4023(3) 0.9682(3) 0.059(3) Uani 1 1 d . . . H83A H 0.3495 0.3928 0.9366 0.089 Uiso 1 1 calc R . . H83B H 0.4193 0.4143 0.9761 0.089 Uiso 1 1 calc R . . H83C H 0.3305 0.4268 0.9762 0.089 Uiso 1 1 calc R . . S1 S -0.5430(3) 0.16887(17) 0.21478(12) 0.1051(13) Uani 1 1 d . . . O11 O -0.5765(6) 0.1884(4) 0.2509(3) 0.115(3) Uani 1 1 d . . . O12 O -0.4812(6) 0.1977(5) 0.2005(3) 0.139(5) Uani 1 1 d . . . O13 O -0.6039(6) 0.1416(4) 0.1823(3) 0.121(4) Uani 1 1 d . . . C1 C -0.4918(11) 0.1258(6) 0.2377(5) 0.100(5) Uani 1 1 d . . . F13 F -0.4340(7) 0.1457(5) 0.2702(3) 0.172(5) Uani 1 1 d . . . F12 F -0.5448(7) 0.0949(4) 0.2539(3) 0.149(4) Uani 1 1 d . . . F11 F -0.4585(7) 0.1010(4) 0.2103(3) 0.168(4) Uani 1 1 d . . . S2 S 0.03454(19) 0.56756(9) 0.63594(10) 0.0653(8) Uani 1 1 d . . . O21 O 0.0357(5) 0.5452(3) 0.6754(3) 0.083(2) Uani 1 1 d . . . O22 O 0.0314(5) 0.6160(3) 0.6394(3) 0.091(3) Uani 1 1 d . . . O23 O -0.0177(5) 0.5414(3) 0.6001(3) 0.091(3) Uani 1 1 d . . . C2 C 0.1289(9) 0.5620(5) 0.6194(6) 0.104(5) Uani 1 1 d . . . F21 F 0.1374(5) 0.5812(3) 0.5825(3) 0.126(3) Uani 1 1 d . . . F22 F 0.1419(6) 0.5184(3) 0.6152(4) 0.149(4) Uani 1 1 d . . . F23 F 0.1900(5) 0.5861(3) 0.6484(4) 0.155(4) Uani 1 1 d . . . S3 S -0.24328(18) 0.25665(13) 0.79712(9) 0.0729(9) Uani 1 1 d . . . O31 O -0.3067(5) 0.2562(4) 0.7611(3) 0.100(3) Uani 1 1 d . . . O32 O -0.2626(5) 0.2649(3) 0.8398(2) 0.080(2) Uani 1 1 d . . . O33 O -0.1682(5) 0.2813(4) 0.7905(3) 0.105(3) Uani 1 1 d . . . C3 C -0.2273(7) 0.1994(6) 0.7926(3) 0.109(6) Uani 1 1 d . . . F31 F -0.1696(4) 0.1898(3) 0.8256(2) 0.098(2) Uani 1 1 d . . . F32 F -0.2082(5) 0.1811(4) 0.7556(2) 0.131(3) Uani 1 1 d . . . F33 F -0.2936(5) 0.1663(3) 0.7980(2) 0.088(2) Uani 1 1 d . . . S4 S 0.33265(18) 0.05993(10) 0.53269(10) 0.0630(7) Uani 1 1 d . . . O41 O 0.3747(5) 0.0922(3) 0.5077(3) 0.080(2) Uani 1 1 d . . . O42 O 0.3034(5) 0.0143(3) 0.5114(3) 0.086(3) Uani 1 1 d . . . O43 O 0.2798(6) 0.0808(3) 0.5586(3) 0.103(3) Uani 1 1 d . . . C4 C 0.4119(9) 0.0491(8) 0.5723(6) 0.116(6) Uani 1 1 d . . . F41 F 0.3870(7) 0.0223(4) 0.6004(3) 0.182(5) Uani 1 1 d . . . F42 F 0.4515(8) 0.0891(5) 0.5937(4) 0.196(6) Uani 1 1 d . . . F43 F 0.4654(6) 0.0297(4) 0.5517(5) 0.187(6) Uani 1 1 d . . . S5 S 0.3072(3) 0.49613(19) 0.52725(19) 0.0543(10) Uiso 0.475(5) 1 d PD B 1 O51 O 0.3453(8) 0.4712(4) 0.5603(4) 0.0885(18) Uiso 0.475(5) 1 d PD B 1 O52 O 0.2786(9) 0.5383(4) 0.5446(5) 0.0885(18) Uiso 0.475(5) 1 d PD B 1 O53 O 0.2522(8) 0.4685(5) 0.4924(4) 0.0885(18) Uiso 0.475(5) 1 d PD B 1 C5 C 0.3886(7) 0.5201(5) 0.5005(4) 0.25(2) Uiso 0.475(5) 1 d PD B 1 F51 F 0.3582(10) 0.5472(6) 0.4717(5) 0.185(4) Uiso 0.475(5) 1 d PD B 1 F52 F 0.4166(10) 0.4851(6) 0.4808(6) 0.185(4) Uiso 0.475(5) 1 d PD B 1 F53 F 0.4433(7) 0.5452(6) 0.5316(6) 0.185(4) Uiso 0.475(5) 1 d PD B 1 S17 S 0.2915(3) 0.49810(18) 0.54438(18) 0.0543(10) Uiso 0.525(5) 1 d PD B 2 O171 O 0.2896(8) 0.4709(4) 0.5813(3) 0.0885(18) Uiso 0.525(5) 1 d PD B 2 O172 O 0.2645(8) 0.5426(4) 0.5507(5) 0.0885(18) Uiso 0.525(5) 1 d PD B 2 O173 O 0.2605(8) 0.4716(5) 0.5024(3) 0.0885(18) Uiso 0.525(5) 1 d PD B 2 C17 C 0.3975(5) 0.5125(4) 0.5433(4) 0.25(2) Uiso 0.525(5) 1 d PD B 2 F171 F 0.4073(8) 0.5350(6) 0.5090(5) 0.185(4) Uiso 0.525(5) 1 d PD B 2 F172 F 0.4281(7) 0.4724(5) 0.5411(6) 0.185(4) Uiso 0.525(5) 1 d PD B 2 F173 F 0.4294(7) 0.5391(6) 0.5808(5) 0.185(4) Uiso 0.525(5) 1 d PD B 2 S6 S 0.16990(15) 0.29817(9) 0.70012(7) 0.0469(6) Uani 1 1 d . . . O61 O 0.1491(4) 0.3299(2) 0.6689(2) 0.0578(18) Uani 1 1 d . . . O62 O 0.1080(4) 0.2803(2) 0.72285(18) 0.0524(17) Uani 1 1 d . . . O63 O 0.2179(4) 0.2635(2) 0.6858(2) 0.0568(18) Uani 1 1 d . . . C6 C 0.2381(7) 0.3348(4) 0.7439(4) 0.068(3) Uani 1 1 d . . . F61 F 0.2653(4) 0.3107(3) 0.77530(19) 0.094(2) Uani 1 1 d . . . F62 F 0.3027(4) 0.3554(3) 0.7277(2) 0.094(2) Uani 1 1 d . . . F63 F 0.2040(5) 0.3690(3) 0.7615(2) 0.109(3) Uani 1 1 d . . . S7 S 0.11733(15) -0.03119(8) 0.41846(7) 0.0441(6) Uani 1 1 d . . . O71 O 0.1618(4) 0.0086(2) 0.4044(2) 0.0646(19) Uani 1 1 d . . . O72 O 0.0504(4) -0.0202(3) 0.4388(2) 0.067(2) Uani 1 1 d . . . O73 O 0.1638(4) -0.0620(2) 0.44070(19) 0.0504(16) Uani 1 1 d . . . C7 C 0.0670(7) -0.0646(3) 0.3696(3) 0.060(3) Uani 1 1 d . . . F71 F 0.0266(6) -0.1041(3) 0.3754(2) 0.116(3) Uani 1 1 d . . . F72 F 0.1243(6) -0.0797(3) 0.3454(2) 0.128(3) Uani 1 1 d . . . F73 F 0.0268(5) -0.0411(2) 0.3425(2) 0.096(2) Uani 1 1 d . . . S8 S -0.5443(2) 0.20827(13) 0.65736(11) 0.0775(10) Uani 1 1 d . . . O81 O -0.6103(5) 0.2069(3) 0.6224(2) 0.078(2) Uani 1 1 d . . . O82 O -0.4740(6) 0.1943(4) 0.6422(3) 0.113(4) Uani 1 1 d . . . O83 O -0.5645(5) 0.1891(3) 0.6959(3) 0.098(3) Uani 1 1 d . . . C8 C -0.5158(8) 0.2702(6) 0.6772(4) 0.092(5) Uani 1 1 d . . . F81 F -0.4551(5) 0.2763(3) 0.7095(3) 0.123(3) Uani 1 1 d . . . F82 F -0.5776(5) 0.2876(3) 0.6908(2) 0.095(2) Uani 1 1 d . . . F83 F -0.4933(5) 0.2931(3) 0.6446(2) 0.114(3) Uani 1 1 d . . . S9 S 0.4983(5) 0.3397(3) 1.2814(3) 0.0901(15) Uiso 0.392(4) 1 d PD C 1 O91 O 0.4459(9) 0.3716(6) 1.2977(6) 0.114(3) Uiso 0.392(4) 1 d PD C 1 O92 O 0.4726(10) 0.3187(6) 1.2378(4) 0.114(3) Uiso 0.392(4) 1 d PD C 1 O93 O 0.5269(11) 0.3104(6) 1.3133(5) 0.114(3) Uiso 0.392(4) 1 d PD C 1 C9 C 0.5871(7) 0.3807(5) 1.2782(5) 0.140(9) Uiso 0.392(4) 1 d PD C 1 F91 F 0.6383(8) 0.3570(6) 1.2611(6) 0.150(3) Uiso 0.392(4) 1 d PD C 1 F92 F 0.6160(9) 0.4001(6) 1.3189(5) 0.150(3) Uiso 0.392(4) 1 d PD C 1 F93 F 0.5641(11) 0.4129(5) 1.2532(6) 0.150(3) Uiso 0.392(4) 1 d PD C 1 S18 S 0.5427(3) 0.3193(2) 1.27704(18) 0.0901(15) Uiso 0.608(4) 1 d PD C 2 O181 O 0.5750(7) 0.3109(4) 1.2376(3) 0.114(3) Uiso 0.608(4) 1 d PD C 2 O182 O 0.5963(6) 0.3524(4) 1.3110(3) 0.114(3) Uiso 0.608(4) 1 d PD C 2 O183 O 0.5059(7) 0.2789(3) 1.2939(4) 0.114(3) Uiso 0.608(4) 1 d PD C 2 C18 C 0.4612(6) 0.3516(4) 1.2624(4) 0.140(9) Uiso 0.608(4) 1 d PD C 2 F181 F 0.4282(7) 0.3601(5) 1.2984(4) 0.150(3) Uiso 0.608(4) 1 d PD C 2 F182 F 0.4093(6) 0.3258(4) 1.2309(4) 0.150(3) Uiso 0.608(4) 1 d PD C 2 F183 F 0.4919(8) 0.3916(3) 1.2494(4) 0.150(3) Uiso 0.608(4) 1 d PD C 2 S10 S -0.04703(16) -0.07144(9) 0.86722(8) 0.0494(6) Uani 1 1 d . . . O102 O 0.0215(5) -0.0519(3) 0.8998(2) 0.080(2) Uani 1 1 d . . . O101 O -0.0561(5) -0.0465(2) 0.8301(2) 0.069(2) Uani 1 1 d . . . O103 O -0.0567(5) -0.1206(2) 0.8599(3) 0.082(3) Uani 1 1 d . . . C10 C -0.1263(6) -0.0574(3) 0.8945(3) 0.040(2) Uani 1 1 d . . . F102 F -0.2006(4) -0.0749(3) 0.8695(2) 0.088(2) Uani 1 1 d . . . F101 F -0.1335(4) -0.0812(2) 0.92959(19) 0.0756(19) Uani 1 1 d . . . F103 F -0.1274(5) -0.0137(2) 0.9047(3) 0.111(3) Uani 1 1 d . . . S11 S -0.16961(17) 0.27092(10) 1.17056(8) 0.0563(7) Uani 1 1 d . . . O111 O -0.1505(5) 0.3044(3) 1.1403(2) 0.073(2) Uani 1 1 d . . . O112 O -0.1070(5) 0.2658(3) 1.2041(2) 0.080(3) Uani 1 1 d . . . O113 O -0.2145(4) 0.2245(3) 1.1526(3) 0.082(3) Uani 1 1 d . . . C11 C -0.2412(7) 0.2969(4) 1.1997(4) 0.067(3) Uani 1 1 d . . . F111 F -0.2664(5) 0.2690(3) 1.2298(2) 0.095(2) Uani 1 1 d . . . F112 F -0.3022(4) 0.3029(3) 1.1743(2) 0.095(2) Uani 1 1 d . . . F113 F -0.2067(5) 0.3388(3) 1.2224(3) 0.110(3) Uani 1 1 d . . . S12 S -0.3222(6) 0.4466(3) 0.9884(3) 0.108(2) Uiso 0.457(5) 1 d PD D 1 O121 O -0.3765(10) 0.4135(6) 1.0065(6) 0.141(3) Uiso 0.457(5) 1 d PD D 1 O122 O -0.2493(8) 0.4310(7) 0.9798(6) 0.141(3) Uiso 0.457(5) 1 d PD D 1 O123 O -0.3144(12) 0.4945(4) 1.0074(5) 0.141(3) Uiso 0.457(5) 1 d PD D 1 C12 C -0.3774(10) 0.4475(6) 0.9336(4) 0.238(17) Uiso 0.457(5) 1 d PD D 1 F121 F -0.3484(17) 0.4858(8) 0.9184(6) 0.281(7) Uiso 0.457(5) 1 d PD D 1 F122 F -0.4539(9) 0.4463(11) 0.9381(7) 0.281(7) Uiso 0.457(5) 1 d PD D 1 F123 F -0.3663(17) 0.4091(8) 0.9095(5) 0.281(7) Uiso 0.457(5) 1 d PD D 1 S19 S -0.3493(5) 0.4469(3) 1.0056(2) 0.108(2) Uiso 0.543(5) 1 d PD D 2 O191 O -0.4080(8) 0.4149(5) 0.9777(4) 0.141(3) Uiso 0.543(5) 1 d PD D 2 O192 O -0.3265(10) 0.4917(4) 0.9889(5) 0.141(3) Uiso 0.543(5) 1 d PD D 2 O193 O -0.2809(7) 0.4282(6) 1.0269(5) 0.141(3) Uiso 0.543(5) 1 d PD D 2 C19 C -0.3978(9) 0.4650(5) 1.0516(4) 0.238(17) Uiso 0.543(5) 1 d PD D 2 F191 F -0.3462(13) 0.4978(7) 1.0774(5) 0.281(7) Uiso 0.543(5) 1 d PD D 2 F192 F -0.4139(15) 0.4274(7) 1.0723(6) 0.281(7) Uiso 0.543(5) 1 d PD D 2 F193 F -0.4641(10) 0.4809(9) 1.0362(7) 0.281(7) Uiso 0.543(5) 1 d PD D 2 S13 S -0.30337(15) 0.00562(8) 0.99073(8) 0.0467(6) Uani 1 1 d . . . O131 O -0.3536(4) 0.0297(2) 0.9625(2) 0.0623(19) Uani 1 1 d . . . O132 O -0.2556(5) 0.0344(2) 1.0275(2) 0.074(2) Uani 1 1 d . . . O133 O -0.2634(4) -0.0276(2) 0.9691(2) 0.0580(18) Uani 1 1 d . . . C13 C -0.3741(8) -0.0312(4) 1.0161(4) 0.070(3) Uani 1 1 d . . . F131 F -0.3345(5) -0.0558(3) 1.0441(2) 0.108(3) Uani 1 1 d . . . F132 F -0.4234(5) -0.0615(3) 0.9867(3) 0.118(3) Uani 1 1 d . . . F133 F -0.4164(5) -0.0063(3) 1.0387(3) 0.114(3) Uani 1 1 d . . . S14 S 0.21643(17) 0.29068(11) 1.33141(8) 0.0626(8) Uani 1 1 d . . . O141 O 0.2486(6) 0.3311(4) 1.3132(3) 0.116(3) Uani 1 1 d . . . O142 O 0.1414(5) 0.2683(4) 1.3070(3) 0.110(4) Uani 1 1 d . . . O143 O 0.2203(5) 0.2980(3) 1.3779(2) 0.078(2) Uani 1 1 d . . . C14 C 0.2836(10) 0.2489(7) 1.3230(5) 0.102(5) Uani 1 1 d . . . F141 F 0.2660(6) 0.2092(3) 1.3376(3) 0.109(3) Uani 1 1 d . . . F142 F 0.3585(5) 0.2670(4) 1.3462(4) 0.142(4) Uani 1 1 d . . . F143 F 0.2940(7) 0.2447(4) 1.2813(3) 0.163(5) Uani 1 1 d . . . S15 S -0.04114(18) 0.56112(10) 1.12188(9) 0.0690(8) Uani 1 1 d D . . O151 O -0.0296(5) 0.5422(2) 1.16260(16) 0.076(2) Uani 1 1 d D . . O152 O -0.0001(5) 0.5378(3) 1.0885(2) 0.128(4) Uani 1 1 d D . . O153 O -0.0274(4) 0.61080(16) 1.1232(2) 0.064(2) Uani 1 1 d D . . C15 C -0.1437(4) 0.5438(2) 1.0988(2) 0.099(4) Uani 1 1 d DU . . F151 F -0.1599(4) 0.5609(2) 1.06113(18) 0.106(2) Uani 1 1 d D . . F152 F -0.1883(5) 0.5638(3) 1.1275(3) 0.188(6) Uani 1 1 d D . . F153 F -0.1628(4) 0.49824(19) 1.0964(2) 0.114(3) Uani 1 1 d D . . S16 S 0.4574(2) 0.04988(13) 0.80323(10) 0.0761(9) Uani 1 1 d . . . O161 O 0.4078(6) 0.0755(4) 0.7789(3) 0.127(4) Uani 1 1 d . . . O162 O 0.5409(5) 0.0661(4) 0.8050(3) 0.112(3) Uani 1 1 d . . . O163 O 0.4345(7) 0.0005(4) 0.7996(4) 0.141(4) Uani 1 1 d . . . C16 C 0.4443(8) 0.0651(5) 0.8595(4) 0.077(4) Uani 1 1 d . . . F161 F 0.4934(5) 0.0473(3) 0.8880(3) 0.125(3) Uani 1 1 d . . . F162 F 0.3715(5) 0.0553(3) 0.8664(2) 0.103(3) Uani 1 1 d . . . F163 F 0.4615(5) 0.1122(3) 0.8698(3) 0.118(3) Uani 1 1 d . . . N1 N 0.1813(9) 0.0285(5) 0.6555(4) 0.106(4) Uani 1 1 d . . . C1A C 0.2359(10) 0.0561(5) 0.6655(4) 0.077(4) Uani 1 1 d . . . C1B C 0.2995(10) 0.0926(6) 0.6800(5) 0.119(5) Uani 1 1 d . . . H1BA H 0.3436 0.0886 0.6634 0.178 Uiso 1 1 calc R . . H1BB H 0.3183 0.0921 0.7112 0.178 Uiso 1 1 calc R . . H1BC H 0.2811 0.1226 0.6753 0.178 Uiso 1 1 calc R . . N2 N 0.0870(6) 0.1472(3) 0.7120(3) 0.064(2) Uani 1 1 d . . . C2A C 0.0951(7) 0.1137(4) 0.7272(3) 0.060(3) Uani 1 1 d . . . C2B C 0.1049(8) 0.0703(4) 0.7472(4) 0.083(4) Uani 1 1 d . . . H2BA H 0.0982 0.0440 0.7242 0.124 Uiso 1 1 calc R . . H2BB H 0.0645 0.0645 0.7664 0.124 Uiso 1 1 calc R . . H2BC H 0.1586 0.0734 0.7645 0.124 Uiso 1 1 calc R . . N3 N -0.0758(8) 0.1340(4) 0.2097(5) 0.111(5) Uani 1 1 d . . . C3A C -0.0608(8) 0.1032(5) 0.2257(4) 0.081(4) Uani 1 1 d . . . C3B C -0.0387(8) 0.0611(4) 0.2490(4) 0.083(4) Uani 1 1 d . . . H3BA H -0.0346 0.0353 0.2272 0.125 Uiso 1 1 calc R . . H3BB H -0.0803 0.0512 0.2664 0.125 Uiso 1 1 calc R . . H3BC H 0.0128 0.0700 0.2684 0.125 Uiso 1 1 calc R . . N4 N -0.2343(9) 0.0562(6) 0.8544(5) 0.127(5) Uani 1 1 d . . . C4A C -0.2825(11) 0.0260(7) 0.8517(6) 0.102(5) Uani 1 1 d . . . C4B C -0.3460(10) -0.0128(6) 0.8516(5) 0.126(6) Uani 1 1 d . . . H4BA H -0.3256 -0.0424 0.8458 0.189 Uiso 1 1 calc R . . H4BB H -0.3909 -0.0106 0.8288 0.189 Uiso 1 1 calc R . . H4BC H -0.3642 -0.0114 0.8802 0.189 Uiso 1 1 calc R . . N5 N 0.4257(8) 0.2352(5) 0.8482(5) 0.126(5) Uani 1 1 d . . . C5A C 0.4675(9) 0.2185(6) 0.8280(6) 0.104(5) Uani 1 1 d . . . C5B C 0.5180(9) 0.1988(5) 0.8048(4) 0.113(5) Uani 1 1 d . . . H5BA H 0.5707 0.2182 0.8106 0.169 Uiso 1 1 calc R . . H5BB H 0.4969 0.1961 0.7735 0.169 Uiso 1 1 calc R . . H5BC H 0.5233 0.1675 0.8135 0.169 Uiso 1 1 calc R . . N6 N 0.1501(7) 0.0158(4) 0.8382(4) 0.094(4) Uani 1 1 d . . . C6A C 0.1901(9) -0.0102(4) 0.8475(4) 0.075(4) Uani 1 1 d . . . C6B C 0.2458(8) -0.0442(4) 0.8580(4) 0.088(4) Uani 1 1 d . . . H6BA H 0.2182 -0.0761 0.8483 0.131 Uiso 1 1 calc R . . H6BB H 0.2639 -0.0409 0.8897 0.131 Uiso 1 1 calc R . . H6BC H 0.2923 -0.0382 0.8428 0.131 Uiso 1 1 calc R . . N7 N -0.3600(8) 0.0872(4) 0.3720(4) 0.097(4) Uani 1 1 d . . . C7A C -0.4025(10) 0.0589(6) 0.3453(5) 0.097(5) Uani 1 1 d . . . C7B C -0.4583(14) 0.0236(6) 0.3161(5) 0.181(10) Uani 1 1 d . . . H7BA H -0.4310 0.0105 0.2931 0.272 Uiso 1 1 calc R . . H7BB H -0.5036 0.0378 0.3028 0.272 Uiso 1 1 calc R . . H7BC H -0.4778 -0.0014 0.3328 0.272 Uiso 1 1 calc R . . N8 N -0.5874(17) -0.1406(9) 0.9351(9) 0.249(15) Uani 1 1 d . . . C8A C -0.5728(13) -0.1114(9) 0.9164(7) 0.131(8) Uani 1 1 d . . . C8B C -0.5423(13) -0.0762(7) 0.8920(5) 0.139(8) Uani 1 1 d . . . H8BA H -0.5862 -0.0679 0.8716 0.209 Uiso 1 1 calc R . . H8BB H -0.5026 -0.0878 0.8754 0.209 Uiso 1 1 calc R . . H8BC H -0.5169 -0.0485 0.9120 0.209 Uiso 1 1 calc R . . N9 N -0.1727(13) -0.0287(5) 0.7422(5) 0.167(8) Uani 1 1 d . . . C9A C -0.2016(13) -0.0660(8) 0.7500(5) 0.126(7) Uani 1 1 d . . . C9B C -0.2294(13) -0.1142(6) 0.7603(5) 0.169(10) Uani 1 1 d . . . H9BA H -0.2819 -0.1151 0.7698 0.254 Uiso 1 1 calc R . . H9BB H -0.1908 -0.1227 0.7838 0.254 Uiso 1 1 calc R . . H9BC H -0.2336 -0.1365 0.7341 0.254 Uiso 1 1 calc R . . N10 N -0.3608(14) 0.0889(6) 0.6480(7) 0.221(11) Uani 1 1 d . . . C10A C -0.3952(14) 0.0993(7) 0.6754(6) 0.153(8) Uani 1 1 d . . . C10B C -0.4317(10) 0.1172(7) 0.7129(5) 0.146(7) Uani 1 1 d . . . H10A H -0.4136 0.1020 0.7386 0.220 Uiso 1 1 calc R . . H10B H -0.4902 0.1104 0.7056 0.220 Uiso 1 1 calc R . . H10C H -0.4154 0.1511 0.7192 0.220 Uiso 1 1 calc R . . N11 N 0.3068(8) 0.0817(5) 0.3695(7) 0.46(3) Uani 1 1 d D . . C11A C 0.3268(8) 0.0515(6) 0.3873(7) 0.148(8) Uani 1 1 d D . . C11B C 0.3522(7) 0.0129(4) 0.4096(4) 0.098(5) Uani 1 1 d D . . H11A H 0.4045 0.0071 0.4024 0.147 Uiso 1 1 calc RD . . H11B H 0.3128 -0.0152 0.4001 0.147 Uiso 1 1 calc RD . . H11C H 0.3563 0.0208 0.4413 0.147 Uiso 1 1 calc RD . . N12 N -0.3473(13) 0.4288(8) 1.1507(7) 0.154(11) Uiso 0.50 1 d PD E 1 C12A C -0.2933(13) 0.4151(8) 1.1384(7) 0.073(6) Uiso 0.50 1 d PD E 1 C12B C -0.2280(13) 0.3965(8) 1.1212(7) 0.095(8) Uiso 0.50 1 d PD E 1 H12D H -0.1839 0.3964 1.1451 0.143 Uiso 0.50 1 calc PRD E 1 H12E H -0.2094 0.4160 1.0994 0.143 Uiso 0.50 1 calc PRD E 1 H12F H -0.2464 0.3645 1.1073 0.143 Uiso 0.50 1 calc PRD E 1 N13 N -0.1950(13) 0.4619(7) 0.8300(7) 0.167(13) Uiso 0.50 1 d PD . . C13A C -0.1717(17) 0.4348(9) 0.8080(9) 0.103(9) Uiso 0.50 1 d PD . . C13B C -0.1389(11) 0.3990(6) 0.7830(6) 0.059(5) Uiso 0.50 1 d PD . . H13D H -0.1775 0.3862 0.7568 0.088 Uiso 0.50 1 calc PRD . . H13E H -0.1281 0.3739 0.8011 0.088 Uiso 0.50 1 calc PRD . . H13F H -0.0889 0.4129 0.7741 0.088 Uiso 0.50 1 calc PRD . . O01W O -0.3191(7) 0.1625(3) 0.1826(3) 0.112(3) Uani 1 1 d . . . O02W O 0.3008(5) 0.2055(3) 0.7297(3) 0.104(3) Uani 1 1 d . . . O03W O 0.6160(7) 0.3118(6) 0.8875(4) 0.177(6) Uani 1 1 d . . . O04W O -0.1875(13) 0.4775(8) 1.2434(7) 0.126(7) Uiso 0.50 1 d P . . O05W O 0.159(3) 0.4355(15) 1.2977(14) 0.266(18) Uiso 0.50 1 d P F 1 O06W O 0.2503(19) 0.4532(10) 0.6755(9) 0.179(11) Uiso 0.50 1 d P G 1 O07W O -0.5271(18) 0.3312(10) 0.7945(9) 0.173(10) Uiso 0.50 1 d P H 1 O08W O -0.4705(15) 0.4405(9) 0.7197(8) 0.136(8) Uiso 0.50 1 d P I 1 O09W O 0.3923(11) 0.3640(6) 0.4759(6) 0.098(5) Uiso 0.50 1 d P J 1 O10W O -0.3801(15) 0.5892(9) 1.1488(8) 0.142(8) Uiso 0.50 1 d P K 1 O11W O 0.230(3) 0.4692(17) 1.3557(16) 0.29(2) Uiso 0.50 1 d P L 1 O12W O -0.4110(18) 0.3691(10) 0.5673(9) 0.175(10) Uiso 0.50 1 d P M 1 O13W O 0.385(2) 0.3895(14) 0.3995(13) 0.107(12) Uiso 0.25 1 d P N 1 O14W O 0.3480(19) 0.4639(10) 0.6931(10) 0.187(11) Uiso 0.50 1 d P O 2 O15W O 0.559(3) 0.3079(16) 0.8206(15) 0.29(2) Uiso 0.50 1 d P P 2 O16W O -0.4345(17) 0.6269(10) 1.1405(9) 0.163(10) Uiso 0.50 1 d P Q 2 O17W O 0.183(3) 0.4929(15) 1.3234(14) 0.246(17) Uiso 0.50 1 d P R 2 O18W O 0.4038(13) 0.3693(8) 0.4401(7) 0.118(7) Uiso 0.50 1 d P S 2 O19W O -0.482(2) 0.4016(14) 0.7025(12) 0.219(14) Uiso 0.50 1 d P T 2 O20W O -0.4810(17) 0.3996(10) 0.5805(9) 0.167(10) Uiso 0.50 1 d P U 2 O21W O -0.3596(15) 0.3473(9) 0.5641(7) 0.047(6) Uiso 0.25 1 d P V 2 O22W O 0.697(2) 0.4218(13) 1.2587(12) 0.106(12) Uiso 0.25 1 d P W 2 O23W O -0.338(2) 0.5435(14) 1.1843(12) 0.107(12) Uiso 0.25 1 d P X 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 0.0303(6) 0.0371(7) 0.0294(5) 0.0017(5) 0.0080(4) 0.0102(5) Co2 0.0402(7) 0.0267(6) 0.0287(5) 0.0061(4) 0.0045(5) 0.0079(5) Co3 0.0368(7) 0.0254(6) 0.0290(5) 0.0079(4) 0.0040(4) 0.0105(5) Co4 0.0340(6) 0.0261(6) 0.0324(5) 0.0067(4) 0.0111(5) 0.0100(5) N101 0.037(4) 0.053(5) 0.040(4) -0.004(4) -0.002(3) 0.010(4) C102 0.050(6) 0.053(7) 0.055(6) -0.019(5) 0.000(5) 0.008(5) C103 0.044(6) 0.087(9) 0.051(6) -0.016(6) -0.002(5) -0.003(6) N104 0.048(5) 0.080(7) 0.037(4) -0.002(4) -0.008(4) 0.005(5) C105 0.041(6) 0.062(7) 0.033(5) -0.011(4) 0.004(4) 0.012(5) C106 0.040(5) 0.057(6) 0.038(5) 0.004(4) 0.007(4) 0.023(5) N107 0.034(4) 0.044(5) 0.029(3) 0.000(3) 0.001(3) 0.020(3) N108 0.039(4) 0.033(4) 0.028(3) 0.004(3) -0.005(3) 0.009(3) C109 0.034(5) 0.034(5) 0.024(4) 0.009(3) 0.006(3) 0.016(4) C110 0.045(5) 0.024(5) 0.036(4) 0.009(3) 0.007(4) 0.009(4) C111 0.038(5) 0.034(5) 0.039(4) 0.011(4) 0.005(4) 0.018(4) N112 0.054(5) 0.026(4) 0.035(4) 0.010(3) -0.003(3) 0.005(4) N113 0.039(4) 0.032(4) 0.037(4) 0.008(3) 0.004(3) 0.003(3) C114 0.067(7) 0.022(5) 0.039(5) 0.004(4) 0.006(4) 0.006(4) C115 0.042(5) 0.035(5) 0.044(5) -0.005(4) -0.008(4) 0.004(4) N116 0.074(6) 0.033(5) 0.051(5) 0.004(4) -0.007(4) 0.011(4) C117 0.053(6) 0.049(6) 0.037(5) -0.001(4) -0.005(4) 0.010(5) C118 0.054(6) 0.055(7) 0.034(5) 0.004(4) -0.001(4) 0.019(5) N119 0.044(4) 0.023(4) 0.042(4) 0.007(3) 0.003(3) 0.010(3) N120 0.045(4) 0.030(4) 0.029(3) 0.011(3) 0.005(3) 0.018(3) C121 0.028(4) 0.022(4) 0.032(4) 0.002(3) 0.002(3) 0.007(4) N122 0.033(4) 0.029(4) 0.025(3) 0.001(3) 0.004(3) 0.010(3) C123 0.030(5) 0.025(4) 0.033(4) 0.006(3) -0.001(3) 0.006(4) C124 0.053(6) 0.028(5) 0.054(5) 0.011(4) 0.001(4) 0.012(4) C125 0.059(7) 0.023(5) 0.073(7) 0.010(4) -0.005(5) 0.020(5) C126 0.066(8) 0.044(7) 0.075(7) 0.029(5) -0.019(6) -0.008(6) C127 0.048(6) 0.056(7) 0.048(5) 0.026(5) -0.001(4) 0.000(5) C128 0.037(5) 0.034(5) 0.041(5) 0.005(4) 0.004(4) 0.008(4) C129 0.075(7) 0.038(6) 0.048(5) 0.015(4) -0.016(5) 0.006(5) C130 0.071(7) 0.023(5) 0.056(6) 0.011(4) -0.012(5) 0.005(5) N201 0.047(5) 0.049(5) 0.033(4) 0.008(3) 0.006(3) 0.012(4) C202 0.052(7) 0.071(8) 0.082(7) 0.042(6) 0.026(6) 0.034(6) C203 0.063(8) 0.102(10) 0.088(8) 0.044(7) 0.034(6) 0.048(7) N204 0.051(5) 0.081(7) 0.059(5) 0.032(4) 0.025(4) 0.021(5) C205 0.047(6) 0.052(6) 0.034(4) 0.016(4) 0.008(4) 0.014(5) C206 0.055(6) 0.039(5) 0.026(4) 0.007(3) 0.004(4) 0.013(4) N207 0.041(4) 0.034(4) 0.030(3) 0.004(3) 0.006(3) 0.010(3) N208 0.050(5) 0.039(4) 0.030(3) 0.013(3) 0.009(3) 0.018(4) C209 0.046(5) 0.030(5) 0.024(4) 0.004(3) 0.005(3) 0.008(4) C210 0.054(6) 0.030(5) 0.026(4) 0.011(3) 0.012(4) 0.013(4) C211 0.040(5) 0.019(4) 0.032(4) 0.008(3) 0.009(3) 0.011(4) N212 0.053(5) 0.031(4) 0.024(3) 0.012(3) 0.006(3) 0.020(3) N213 0.049(5) 0.027(4) 0.034(4) 0.011(3) 0.007(3) 0.011(3) C214 0.051(6) 0.034(5) 0.040(5) 0.009(4) 0.011(4) 0.024(4) C215 0.043(5) 0.040(5) 0.032(4) 0.012(4) 0.005(4) 0.019(4) N216 0.060(5) 0.039(4) 0.038(4) 0.011(3) 0.011(3) 0.025(4) C217 0.061(7) 0.060(7) 0.044(5) 0.016(4) 0.026(5) 0.029(5) C218 0.063(7) 0.050(6) 0.042(5) 0.014(4) 0.022(5) 0.023(5) N219 0.040(4) 0.044(4) 0.029(3) 0.012(3) 0.007(3) 0.021(3) N220 0.036(4) 0.025(4) 0.028(3) 0.011(3) 0.000(3) 0.006(3) C221 0.036(5) 0.028(5) 0.029(4) 0.007(3) 0.001(3) 0.008(4) N222 0.034(4) 0.027(4) 0.029(3) 0.007(3) 0.003(3) 0.012(3) C223 0.050(6) 0.032(5) 0.042(5) 0.017(4) 0.018(4) 0.022(4) C224 0.054(6) 0.058(7) 0.047(5) 0.027(4) 0.004(4) 0.030(5) C225 0.110(10) 0.115(11) 0.048(6) 0.058(7) 0.037(6) 0.079(9) C226 0.139(14) 0.071(10) 0.109(11) 0.069(9) 0.070(10) 0.061(10) C227 0.106(11) 0.032(6) 0.129(11) 0.036(7) 0.059(9) 0.012(7) C228 0.073(8) 0.038(6) 0.067(6) 0.021(5) 0.017(6) 0.007(5) C229 0.060(6) 0.039(5) 0.029(4) 0.016(4) 0.010(4) 0.011(5) C230 0.077(7) 0.035(5) 0.040(5) 0.022(4) 0.013(4) 0.028(5) N301 0.030(4) 0.033(4) 0.029(3) 0.004(3) -0.001(3) 0.004(3) C302 0.046(6) 0.044(6) 0.042(5) 0.005(4) 0.012(4) 0.014(5) C303 0.066(7) 0.048(6) 0.041(5) -0.001(4) -0.014(5) 0.014(5) N304 0.075(6) 0.030(5) 0.059(5) 0.002(4) -0.031(4) -0.003(4) C305 0.042(5) 0.028(5) 0.051(5) 0.013(4) -0.004(4) 0.003(4) C306 0.056(6) 0.030(5) 0.054(5) 0.017(4) -0.004(5) 0.002(5) N307 0.039(4) 0.023(4) 0.032(3) 0.010(3) -0.005(3) 0.006(3) N308 0.040(4) 0.026(4) 0.036(4) 0.013(3) -0.006(3) 0.003(3) C309 0.036(5) 0.026(5) 0.033(4) 0.005(3) 0.002(3) 0.012(4) C310 0.031(5) 0.031(5) 0.036(4) 0.012(3) 0.001(3) 0.005(4) C311 0.027(4) 0.034(5) 0.029(4) 0.012(3) 0.007(3) 0.010(4) N312 0.045(4) 0.031(4) 0.025(3) 0.015(3) 0.005(3) 0.002(3) N313 0.033(4) 0.024(4) 0.029(3) 0.006(3) 0.010(3) 0.006(3) C314 0.034(5) 0.044(5) 0.027(4) 0.006(3) 0.012(4) 0.007(4) C315 0.050(6) 0.039(5) 0.028(4) 0.004(4) 0.010(4) 0.006(4) N316 0.068(6) 0.054(5) 0.023(3) -0.001(3) -0.001(3) -0.009(4) C317 0.082(8) 0.065(8) 0.039(5) -0.010(5) 0.002(5) -0.026(6) C318 0.065(7) 0.033(6) 0.058(6) -0.002(4) 0.014(5) -0.005(5) N319 0.048(5) 0.033(4) 0.039(4) 0.000(3) 0.013(3) 0.000(4) N320 0.024(4) 0.036(4) 0.026(3) 0.010(3) 0.004(3) 0.007(3) C321 0.038(5) 0.033(5) 0.033(4) 0.014(3) 0.014(4) 0.020(4) N322 0.044(4) 0.021(4) 0.025(3) 0.008(3) 0.004(3) 0.013(3) C323 0.027(4) 0.023(4) 0.035(4) 0.010(3) 0.006(3) 0.000(3) C324 0.032(5) 0.041(5) 0.035(4) 0.011(4) 0.008(3) 0.006(4) C325 0.063(7) 0.042(6) 0.044(5) 0.028(4) 0.008(4) 0.000(5) C326 0.057(7) 0.035(6) 0.059(6) 0.022(4) -0.005(5) 0.008(5) C327 0.052(6) 0.028(5) 0.063(6) 0.015(4) 0.005(5) 0.021(4) C328 0.044(5) 0.028(5) 0.055(5) 0.018(4) 0.010(4) 0.011(4) C329 0.064(7) 0.026(5) 0.057(6) 0.019(4) -0.005(5) -0.006(5) C330 0.054(6) 0.030(5) 0.028(4) 0.014(3) 0.001(4) 0.004(4) N401 0.044(5) 0.035(4) 0.053(4) 0.015(3) 0.020(4) 0.020(4) C402 0.056(6) 0.047(6) 0.057(6) 0.023(5) 0.029(5) 0.017(5) C403 0.058(7) 0.050(6) 0.079(7) 0.020(5) 0.042(6) 0.026(5) N404 0.062(5) 0.040(5) 0.050(4) 0.009(3) 0.022(4) 0.023(4) C405 0.048(6) 0.040(5) 0.045(5) 0.004(4) 0.016(4) 0.015(5) C406 0.042(5) 0.026(4) 0.041(4) 0.009(3) 0.015(4) 0.017(4) N407 0.036(4) 0.024(4) 0.031(3) 0.002(3) 0.010(3) 0.005(3) N408 0.042(4) 0.022(4) 0.043(4) 0.014(3) 0.015(3) 0.009(3) C409 0.038(5) 0.016(4) 0.041(4) 0.006(3) 0.011(4) 0.004(4) C410 0.043(5) 0.029(5) 0.042(4) 0.017(4) 0.012(4) 0.015(4) C411 0.038(5) 0.027(5) 0.036(4) 0.007(3) 0.009(4) 0.011(4) N412 0.038(4) 0.032(4) 0.042(4) 0.011(3) 0.020(3) 0.006(3) N413 0.038(4) 0.046(5) 0.031(3) 0.003(3) 0.012(3) 0.004(4) C414 0.040(5) 0.050(6) 0.037(5) -0.003(4) 0.018(4) -0.007(5) C415 0.030(5) 0.069(7) 0.036(5) -0.009(4) 0.015(4) 0.007(5) N416 0.055(6) 0.064(6) 0.069(6) -0.005(5) 0.035(4) 0.010(5) C417 0.050(7) 0.084(9) 0.088(8) -0.013(7) 0.032(6) 0.022(7) C418 0.051(6) 0.065(7) 0.064(6) 0.003(5) 0.023(5) 0.023(6) N419 0.041(5) 0.057(5) 0.043(4) -0.001(4) 0.015(3) 0.020(4) N420 0.033(4) 0.030(4) 0.034(3) 0.007(3) 0.012(3) 0.007(3) C421 0.028(4) 0.028(4) 0.029(4) 0.002(3) 0.005(3) 0.008(4) N422 0.035(4) 0.025(4) 0.030(3) 0.009(3) 0.010(3) 0.010(3) C423 0.038(5) 0.020(4) 0.039(4) 0.008(3) 0.017(4) 0.013(4) C424 0.048(6) 0.032(5) 0.069(6) 0.014(4) 0.028(5) 0.014(5) C425 0.071(8) 0.020(5) 0.082(7) 0.011(5) 0.038(6) 0.010(5) C426 0.072(8) 0.071(8) 0.068(7) 0.041(6) 0.037(6) 0.043(7) C427 0.074(7) 0.056(7) 0.049(5) 0.034(5) 0.032(5) 0.033(6) C428 0.060(6) 0.041(5) 0.037(5) 0.012(4) 0.022(4) 0.023(5) C429 0.042(5) 0.030(5) 0.051(5) 0.016(4) 0.013(4) 0.010(4) C430 0.061(7) 0.038(5) 0.059(6) 0.016(4) 0.035(5) 0.007(5) Co5 0.0321(6) 0.0438(7) 0.0309(6) 0.0013(5) 0.0059(5) 0.0113(5) Co6 0.0345(6) 0.0275(6) 0.0295(5) 0.0073(4) 0.0095(4) 0.0117(5) Co7 0.0389(7) 0.0377(7) 0.0446(6) 0.0190(5) 0.0198(5) 0.0179(6) Co8 0.0628(9) 0.0304(7) 0.0401(6) 0.0096(5) 0.0237(6) 0.0196(6) N501 0.033(4) 0.056(5) 0.042(4) -0.003(4) 0.007(3) 0.005(4) C502 0.053(7) 0.064(8) 0.057(6) -0.004(5) 0.011(5) 0.009(6) C503 0.046(7) 0.102(11) 0.045(6) -0.010(6) -0.004(5) -0.021(7) N504 0.039(5) 0.086(7) 0.047(5) 0.004(4) -0.003(4) 0.013(5) C505 0.034(5) 0.064(7) 0.031(4) -0.005(4) 0.003(4) 0.014(5) C506 0.052(6) 0.058(7) 0.035(5) 0.004(4) 0.013(4) 0.021(5) N507 0.034(4) 0.057(5) 0.025(3) 0.001(3) -0.004(3) 0.023(4) N508 0.049(5) 0.041(5) 0.035(4) 0.003(3) 0.002(3) 0.022(4) C509 0.031(5) 0.043(5) 0.023(4) 0.007(3) 0.008(3) 0.016(4) C510 0.045(5) 0.031(5) 0.034(4) 0.013(3) 0.007(4) 0.019(4) C511 0.039(5) 0.037(5) 0.032(4) 0.014(4) 0.014(4) 0.022(4) N512 0.047(4) 0.027(4) 0.032(3) 0.009(3) 0.004(3) 0.011(3) N513 0.032(4) 0.025(4) 0.037(4) 0.008(3) 0.010(3) 0.006(3) C514 0.038(5) 0.030(5) 0.047(5) 0.012(4) 0.012(4) 0.005(4) C515 0.048(6) 0.035(5) 0.044(5) 0.012(4) 0.003(4) 0.003(4) N516 0.063(6) 0.046(5) 0.051(5) 0.017(4) 0.005(4) 0.000(4) C517 0.077(8) 0.061(7) 0.038(5) 0.012(5) -0.006(5) 0.012(6) C518 0.049(6) 0.043(6) 0.054(6) 0.015(4) -0.009(5) 0.005(5) N519 0.035(4) 0.035(4) 0.042(4) 0.011(3) 0.003(3) 0.001(3) N520 0.026(4) 0.034(4) 0.037(3) 0.015(3) 0.010(3) 0.013(3) C521 0.023(4) 0.033(5) 0.023(4) 0.001(3) 0.002(3) 0.013(4) N522 0.035(4) 0.031(4) 0.027(3) 0.007(3) 0.005(3) 0.015(3) C523 0.029(4) 0.027(5) 0.031(4) 0.001(3) -0.004(3) 0.003(4) C524 0.047(6) 0.031(5) 0.041(5) 0.007(4) -0.001(4) 0.019(4) C525 0.064(7) 0.028(5) 0.062(6) 0.012(4) -0.012(5) 0.021(5) C526 0.081(8) 0.032(6) 0.046(5) 0.022(4) -0.025(5) 0.000(5) C527 0.059(7) 0.052(6) 0.040(5) 0.017(4) 0.003(4) -0.002(5) C528 0.058(6) 0.041(6) 0.034(4) 0.010(4) 0.006(4) 0.011(5) C529 0.068(7) 0.047(6) 0.043(5) 0.015(4) -0.008(5) 0.023(5) C530 0.059(6) 0.041(6) 0.042(5) 0.016(4) 0.006(4) 0.018(5) N601 0.028(4) 0.038(4) 0.039(4) 0.010(3) 0.012(3) 0.006(3) C602 0.038(5) 0.041(5) 0.053(5) 0.017(4) 0.014(4) 0.017(4) C603 0.044(6) 0.055(6) 0.057(6) 0.015(5) 0.020(5) 0.026(5) N604 0.036(4) 0.061(5) 0.043(4) 0.015(4) 0.017(3) 0.022(4) C605 0.038(5) 0.040(5) 0.033(4) 0.008(4) 0.010(4) 0.013(4) C606 0.029(4) 0.038(5) 0.028(4) 0.007(3) 0.009(3) 0.010(4) N607 0.030(4) 0.027(4) 0.028(3) 0.004(3) 0.004(3) 0.008(3) N608 0.039(4) 0.036(4) 0.028(3) 0.013(3) 0.012(3) 0.023(3) C609 0.025(4) 0.030(4) 0.025(4) 0.012(3) 0.003(3) 0.012(3) C610 0.036(5) 0.036(5) 0.039(4) 0.021(4) 0.017(4) 0.016(4) C611 0.034(5) 0.029(5) 0.048(5) 0.016(4) 0.017(4) 0.018(4) N612 0.055(5) 0.051(5) 0.053(4) 0.028(4) 0.036(4) 0.025(4) N613 0.050(5) 0.048(5) 0.052(4) 0.020(4) 0.029(4) 0.028(4) C614 0.064(7) 0.049(6) 0.069(6) 0.039(5) 0.042(5) 0.045(5) C615 0.049(6) 0.057(6) 0.058(6) 0.022(5) 0.034(5) 0.031(5) N616 0.070(6) 0.083(7) 0.066(5) 0.034(5) 0.041(5) 0.055(5) C617 0.059(7) 0.086(8) 0.056(6) 0.022(6) 0.034(5) 0.031(6) C618 0.038(5) 0.059(6) 0.050(5) 0.015(4) 0.021(4) 0.011(5) N619 0.038(4) 0.048(5) 0.055(4) 0.016(4) 0.026(3) 0.024(4) N620 0.038(4) 0.030(4) 0.039(4) 0.015(3) 0.020(3) 0.018(3) C621 0.017(4) 0.025(4) 0.035(4) 0.007(3) 0.004(3) 0.009(3) N622 0.030(4) 0.028(4) 0.026(3) 0.005(3) 0.007(3) 0.008(3) C623 0.032(5) 0.029(5) 0.039(4) 0.012(3) 0.018(4) 0.015(4) C624 0.046(6) 0.059(6) 0.029(4) 0.015(4) 0.009(4) 0.023(5) C625 0.055(7) 0.079(8) 0.056(6) 0.044(6) 0.018(5) 0.036(6) C626 0.073(8) 0.036(6) 0.066(6) 0.031(5) 0.036(6) 0.026(5) C627 0.064(7) 0.027(5) 0.076(7) 0.014(5) 0.032(6) 0.010(5) C628 0.048(6) 0.035(5) 0.046(5) 0.010(4) 0.023(4) 0.008(4) C629 0.056(6) 0.038(5) 0.034(4) 0.017(4) 0.019(4) 0.022(4) C630 0.101(9) 0.056(7) 0.066(6) 0.038(5) 0.048(6) 0.055(6) N701 0.035(4) 0.047(5) 0.039(4) 0.012(3) 0.015(3) 0.012(4) C702 0.048(6) 0.038(6) 0.057(6) 0.012(4) 0.025(5) 0.012(5) C703 0.054(6) 0.075(8) 0.038(5) 0.011(5) 0.018(4) 0.019(6) N704 0.062(5) 0.038(5) 0.054(5) 0.018(4) 0.022(4) 0.022(4) C705 0.039(5) 0.034(5) 0.046(5) 0.005(4) 0.010(4) 0.008(4) C706 0.045(6) 0.042(6) 0.038(5) 0.013(4) 0.010(4) 0.019(5) N707 0.042(5) 0.044(5) 0.043(4) 0.015(3) 0.020(3) 0.014(4) N708 0.051(5) 0.048(5) 0.041(4) 0.027(3) 0.009(3) 0.014(4) C709 0.048(6) 0.037(5) 0.046(5) 0.020(4) 0.023(4) 0.016(5) C710 0.043(5) 0.038(5) 0.047(5) 0.027(4) 0.014(4) 0.019(4) C711 0.041(5) 0.034(5) 0.046(5) 0.013(4) 0.019(4) 0.015(4) N712 0.055(5) 0.037(5) 0.047(4) 0.019(3) 0.017(4) 0.020(4) N713 0.055(5) 0.029(4) 0.050(4) 0.014(3) 0.024(4) 0.015(4) C714 0.083(8) 0.048(6) 0.033(5) 0.014(4) 0.012(5) 0.008(6) C715 0.113(11) 0.062(8) 0.052(6) 0.021(5) -0.001(6) -0.017(7) N719 0.094(7) 0.046(5) 0.052(5) 0.019(4) 0.002(5) -0.003(5) N720 0.043(4) 0.039(4) 0.037(4) 0.018(3) 0.013(3) 0.016(3) C721 0.053(6) 0.038(5) 0.047(5) 0.016(4) 0.031(5) 0.021(5) N722 0.042(4) 0.041(5) 0.041(4) 0.026(3) 0.014(3) 0.017(4) C723 0.048(6) 0.030(5) 0.059(5) 0.018(4) 0.014(4) 0.016(4) C724 0.073(7) 0.044(6) 0.038(5) 0.014(4) 0.019(5) 0.004(5) C725 0.089(9) 0.064(8) 0.057(6) 0.033(5) 0.016(6) 0.005(7) C726 0.123(12) 0.056(8) 0.095(9) 0.045(7) 0.005(9) 0.023(8) C727 0.119(11) 0.060(8) 0.089(9) 0.036(7) 0.026(8) 0.050(8) C728 0.076(8) 0.033(6) 0.077(7) 0.021(5) 0.030(6) 0.023(5) C729 0.059(7) 0.047(6) 0.058(6) 0.032(5) -0.005(5) -0.006(5) C730 0.082(8) 0.037(6) 0.048(5) 0.021(4) 0.021(5) 0.017(5) N801 0.065(6) 0.050(5) 0.069(5) 0.014(4) 0.032(5) 0.028(5) C802 0.065(7) 0.051(7) 0.069(7) 0.017(5) 0.024(6) 0.024(6) C803 0.095(10) 0.078(9) 0.087(8) 0.018(7) 0.054(7) 0.039(8) N804 0.068(6) 0.050(5) 0.067(5) 0.002(4) 0.020(4) 0.032(5) C805 0.059(7) 0.046(6) 0.066(6) 0.000(5) 0.015(5) 0.017(5) C806 0.092(9) 0.040(6) 0.091(8) 0.025(5) 0.053(7) 0.041(6) N807 0.076(6) 0.038(5) 0.047(4) 0.015(3) 0.029(4) 0.027(4) N808 0.076(6) 0.030(4) 0.050(4) 0.019(3) 0.029(4) 0.026(4) C809 0.044(5) 0.043(5) 0.034(4) 0.007(4) 0.009(4) 0.014(4) C810 0.073(7) 0.033(5) 0.034(4) 0.010(4) 0.021(4) 0.015(5) C811 0.046(5) 0.037(5) 0.030(4) 0.007(4) 0.012(4) 0.013(4) N812 0.054(5) 0.041(5) 0.039(4) 0.012(3) 0.020(3) 0.008(4) N813 0.037(4) 0.048(5) 0.030(3) -0.001(3) 0.007(3) 0.007(4) C814 0.051(6) 0.070(7) 0.038(5) 0.004(5) 0.020(4) -0.004(5) C815 0.033(5) 0.073(8) 0.048(5) -0.002(5) 0.012(4) 0.004(5) N816 0.058(6) 0.102(9) 0.084(7) -0.004(6) 0.040(5) 0.015(6) C817 0.065(9) 0.134(14) 0.092(9) 0.001(9) 0.043(7) 0.033(9) C818 0.057(7) 0.072(8) 0.081(7) 0.004(6) 0.026(6) 0.034(6) N819 0.037(4) 0.067(6) 0.044(4) -0.005(4) 0.008(3) 0.026(4) N820 0.031(4) 0.034(4) 0.024(3) 0.004(3) 0.004(3) 0.004(3) C821 0.028(4) 0.030(4) 0.021(4) -0.002(3) 0.003(3) 0.000(4) N822 0.047(4) 0.036(4) 0.028(3) 0.010(3) 0.013(3) 0.015(3) C823 0.038(5) 0.024(4) 0.033(4) 0.007(3) 0.014(4) 0.010(4) C824 0.042(6) 0.043(6) 0.066(6) 0.011(5) 0.023(5) 0.004(5) C825 0.074(9) 0.023(6) 0.143(12) 0.005(7) 0.064(9) 0.004(6) C826 0.073(9) 0.051(7) 0.090(8) 0.036(6) 0.046(7) 0.034(7) C827 0.071(8) 0.072(8) 0.046(5) 0.027(5) 0.024(5) 0.032(7) C828 0.057(6) 0.034(5) 0.047(5) 0.010(4) 0.015(4) 0.020(5) C829 0.108(10) 0.043(6) 0.074(7) 0.034(5) 0.046(7) 0.037(6) C830 0.087(8) 0.044(6) 0.055(6) 0.021(5) 0.032(6) 0.006(6) S1 0.125(4) 0.134(4) 0.071(2) 0.037(2) 0.019(2) 0.050(3) O11 0.140(9) 0.133(9) 0.090(6) 0.019(6) 0.039(6) 0.055(7) O12 0.102(8) 0.204(13) 0.107(7) 0.042(8) 0.039(6) -0.038(8) O13 0.112(8) 0.183(11) 0.055(5) 0.009(6) -0.025(5) 0.010(7) C1 0.123(14) 0.126(14) 0.062(8) 0.010(8) 0.024(9) 0.055(12) F13 0.148(9) 0.240(13) 0.123(8) 0.004(8) -0.025(7) 0.071(9) F12 0.169(10) 0.129(9) 0.162(9) 0.038(7) 0.062(8) 0.017(7) F11 0.215(12) 0.171(10) 0.140(8) 0.014(7) 0.067(8) 0.076(9) S2 0.079(2) 0.0312(15) 0.0802(19) 0.0173(13) -0.0136(15) 0.0068(14) O21 0.122(7) 0.047(5) 0.082(5) 0.021(4) 0.002(5) 0.019(5) O22 0.108(7) 0.046(5) 0.114(6) 0.016(4) -0.018(5) 0.024(5) O23 0.113(7) 0.052(5) 0.090(6) 0.022(4) -0.030(5) -0.016(5) C2 0.082(11) 0.069(10) 0.172(15) 0.081(10) 0.009(10) 0.022(8) F21 0.131(7) 0.113(7) 0.162(8) 0.087(6) 0.049(6) 0.046(6) F22 0.164(9) 0.104(7) 0.225(10) 0.096(7) 0.080(8) 0.083(7) F23 0.074(6) 0.124(8) 0.254(12) 0.093(8) -0.050(7) -0.004(5) S3 0.0574(19) 0.102(3) 0.0585(17) 0.0337(16) 0.0040(14) -0.0022(18) O31 0.063(5) 0.149(9) 0.083(6) 0.073(6) -0.020(4) -0.016(5) O32 0.102(7) 0.083(6) 0.064(5) 0.036(4) 0.023(4) 0.014(5) O33 0.063(6) 0.162(9) 0.077(5) 0.042(6) -0.005(4) -0.031(6) C3 0.046(7) 0.226(18) 0.043(6) -0.064(9) 0.023(6) 0.017(10) F31 0.080(5) 0.117(6) 0.100(5) 0.006(5) 0.010(4) 0.037(5) F32 0.140(7) 0.199(10) 0.076(5) 0.016(5) 0.047(5) 0.077(7) F33 0.092(6) 0.102(6) 0.074(4) 0.026(4) 0.015(4) 0.016(5) S4 0.0673(19) 0.0499(17) 0.0787(18) 0.0222(14) 0.0163(15) 0.0180(15) O41 0.093(6) 0.061(5) 0.107(6) 0.047(4) 0.039(5) 0.033(5) O42 0.098(7) 0.066(6) 0.083(5) -0.002(4) 0.015(5) -0.021(5) O43 0.119(8) 0.060(5) 0.161(9) 0.037(5) 0.082(7) 0.046(5) C4 0.056(10) 0.164(18) 0.131(13) 0.075(13) 0.009(9) -0.008(11) F41 0.200(11) 0.231(13) 0.167(9) 0.156(9) 0.064(8) 0.084(10) F42 0.192(12) 0.215(14) 0.137(9) 0.033(9) -0.031(8) -0.081(11) F43 0.092(7) 0.200(12) 0.330(16) 0.163(12) 0.094(9) 0.083(8) S6 0.0476(15) 0.0571(16) 0.0387(12) 0.0121(11) 0.0111(10) 0.0084(12) O61 0.063(5) 0.069(5) 0.050(4) 0.027(3) 0.012(3) 0.024(4) O62 0.055(4) 0.063(5) 0.039(3) 0.008(3) 0.014(3) -0.002(3) O63 0.059(4) 0.056(4) 0.064(4) 0.024(3) 0.013(3) 0.020(4) C6 0.061(8) 0.073(9) 0.064(7) 0.014(6) -0.004(6) 0.001(7) F61 0.102(6) 0.123(6) 0.053(4) 0.035(4) -0.014(4) 0.010(5) F62 0.065(5) 0.105(6) 0.101(5) 0.031(4) -0.004(4) -0.023(4) F63 0.124(7) 0.092(6) 0.090(5) -0.029(4) -0.015(5) 0.003(5) S7 0.0541(15) 0.0353(13) 0.0470(12) 0.0165(10) 0.0088(11) 0.0119(11) O71 0.054(5) 0.050(4) 0.090(5) 0.031(4) 0.004(4) -0.001(4) O72 0.076(5) 0.071(5) 0.071(4) 0.028(4) 0.037(4) 0.036(4) O73 0.058(4) 0.048(4) 0.048(3) 0.016(3) 0.001(3) 0.018(3) C7 0.097(9) 0.029(6) 0.044(5) 0.016(4) -0.021(5) 0.002(6) F71 0.160(8) 0.073(5) 0.085(5) 0.013(4) -0.052(5) -0.014(5) F72 0.206(10) 0.143(8) 0.059(4) 0.003(4) 0.037(5) 0.100(7) F73 0.129(6) 0.062(5) 0.081(4) 0.019(3) -0.043(4) 0.009(4) S8 0.069(2) 0.092(3) 0.092(2) 0.0458(19) 0.0402(18) 0.0338(19) O81 0.064(5) 0.102(7) 0.071(5) 0.020(4) 0.024(4) 0.003(5) O82 0.102(7) 0.151(9) 0.125(7) 0.075(7) 0.065(6) 0.073(7) O83 0.093(7) 0.115(7) 0.118(7) 0.073(6) 0.058(6) 0.044(6) C8 0.060(9) 0.136(14) 0.086(9) 0.072(9) 0.004(7) 0.009(9) F81 0.070(5) 0.182(9) 0.104(6) 0.047(6) -0.023(4) -0.007(5) F82 0.091(6) 0.103(6) 0.087(5) 0.008(4) 0.001(4) 0.015(5) F83 0.114(7) 0.127(7) 0.092(5) 0.042(5) 0.001(5) -0.021(5) S10 0.0608(17) 0.0390(14) 0.0557(14) 0.0162(11) 0.0210(12) 0.0134(12) O102 0.060(5) 0.101(7) 0.078(5) 0.033(5) 0.001(4) 0.004(5) O101 0.105(6) 0.058(5) 0.052(4) 0.017(3) 0.033(4) 0.015(4) O103 0.128(7) 0.035(4) 0.105(6) 0.014(4) 0.075(6) 0.026(4) C10 0.059(6) 0.034(5) 0.037(5) 0.015(4) 0.010(4) 0.029(5) F102 0.071(5) 0.092(5) 0.106(5) 0.030(4) 0.013(4) 0.017(4) F101 0.097(5) 0.082(5) 0.070(4) 0.034(3) 0.045(4) 0.041(4) F103 0.142(7) 0.056(5) 0.157(7) 0.008(4) 0.091(6) 0.024(5) S11 0.0640(18) 0.0676(19) 0.0427(13) 0.0132(12) 0.0137(12) 0.0184(15) O111 0.075(5) 0.083(6) 0.065(4) 0.018(4) 0.028(4) 0.004(4) O112 0.090(6) 0.128(7) 0.036(4) 0.019(4) 0.004(4) 0.067(5) O113 0.046(4) 0.048(5) 0.145(7) -0.019(5) 0.018(5) 0.004(4) C11 0.062(8) 0.069(9) 0.078(8) 0.023(7) 0.016(6) 0.020(7) F111 0.123(6) 0.129(6) 0.062(4) 0.038(4) 0.053(4) 0.061(5) F112 0.084(5) 0.138(7) 0.073(4) 0.029(4) 0.012(4) 0.044(5) F113 0.127(7) 0.086(6) 0.125(6) -0.019(5) 0.053(5) 0.024(5) S13 0.0558(16) 0.0380(14) 0.0509(13) 0.0108(10) 0.0109(11) 0.0170(12) O131 0.069(5) 0.047(4) 0.076(5) 0.021(3) 0.005(4) 0.025(4) O132 0.087(6) 0.048(5) 0.077(5) 0.007(4) -0.017(4) 0.008(4) O133 0.081(5) 0.046(4) 0.059(4) 0.018(3) 0.024(4) 0.032(4) C13 0.079(9) 0.068(9) 0.070(7) 0.014(6) 0.026(7) 0.017(7) F131 0.153(8) 0.092(6) 0.099(5) 0.049(5) 0.058(5) 0.026(5) F132 0.107(7) 0.112(7) 0.120(6) -0.010(5) 0.035(5) -0.037(5) F133 0.124(7) 0.127(7) 0.114(6) 0.016(5) 0.079(5) 0.034(5) S14 0.0599(18) 0.082(2) 0.0541(15) 0.0303(14) 0.0084(13) 0.0260(16) O141 0.126(8) 0.115(8) 0.112(7) 0.074(6) 0.004(6) 0.011(7) O142 0.059(6) 0.209(11) 0.061(5) 0.019(6) 0.002(4) 0.022(6) O143 0.090(6) 0.099(6) 0.050(4) 0.014(4) 0.000(4) 0.043(5) C14 0.099(12) 0.147(16) 0.076(9) 0.013(9) 0.031(9) 0.055(11) F141 0.155(8) 0.077(6) 0.109(6) 0.038(5) 0.039(5) 0.031(5) F142 0.078(6) 0.181(10) 0.189(10) 0.069(8) 0.026(6) 0.061(6) F143 0.199(10) 0.230(12) 0.114(7) 0.062(7) 0.104(7) 0.115(9) S15 0.086(2) 0.0569(19) 0.0690(18) 0.0241(14) 0.0091(16) 0.0187(16) O151 0.129(7) 0.045(4) 0.051(4) 0.016(3) -0.004(4) 0.009(5) O152 0.230(12) 0.092(7) 0.125(7) 0.067(6) 0.121(8) 0.116(8) O153 0.086(6) 0.029(4) 0.077(5) 0.016(3) 0.008(4) 0.002(4) C15 0.132(8) 0.051(6) 0.087(7) 0.044(5) -0.059(6) -0.027(6) F151 0.112(6) 0.109(6) 0.092(5) 0.020(5) -0.002(5) 0.011(5) F152 0.187(11) 0.153(10) 0.287(14) 0.084(9) 0.147(11) 0.095(8) F153 0.126(7) 0.068(5) 0.141(7) 0.041(5) -0.013(5) 0.004(5) S16 0.076(2) 0.087(3) 0.0732(19) 0.0049(17) 0.0125(16) 0.044(2) O161 0.134(8) 0.219(12) 0.070(5) 0.055(6) 0.037(6) 0.130(9) O162 0.073(6) 0.167(10) 0.123(8) 0.062(7) 0.046(6) 0.048(6) O163 0.138(10) 0.115(9) 0.150(10) -0.045(8) -0.031(8) 0.038(8) C16 0.078(10) 0.083(10) 0.077(8) 0.040(7) 0.005(7) 0.022(8) F161 0.112(7) 0.182(9) 0.107(6) 0.078(6) 0.019(5) 0.071(6) F162 0.076(5) 0.140(7) 0.104(5) 0.031(5) 0.038(4) 0.024(5) F163 0.128(7) 0.126(8) 0.104(6) 0.017(5) 0.009(5) 0.041(6) N1 0.139(13) 0.090(10) 0.086(8) 0.001(7) 0.010(8) 0.015(9) C1A 0.088(11) 0.079(10) 0.061(7) 0.004(7) 0.002(7) 0.014(8) C1B 0.113(13) 0.131(15) 0.119(12) 0.051(11) 0.003(10) 0.032(12) N2 0.074(7) 0.070(7) 0.048(5) 0.021(4) -0.002(4) 0.009(5) C2A 0.074(8) 0.069(8) 0.037(5) 0.005(5) 0.004(5) 0.016(6) C2B 0.114(11) 0.064(8) 0.077(8) 0.027(6) 0.013(7) 0.023(8) N3 0.141(12) 0.071(9) 0.149(11) 0.037(8) 0.081(10) 0.042(8) C3A 0.096(10) 0.064(9) 0.091(9) -0.010(7) 0.054(8) 0.014(8) C3B 0.106(11) 0.083(10) 0.066(7) -0.008(7) 0.040(7) 0.013(8) N4 0.101(12) 0.160(16) 0.113(10) -0.012(10) 0.012(9) 0.023(10) C4A 0.082(13) 0.103(15) 0.116(12) -0.013(11) -0.002(11) 0.035(10) C4B 0.100(13) 0.151(17) 0.124(12) -0.007(12) -0.033(10) 0.080(13) N5 0.091(10) 0.127(12) 0.151(12) -0.006(9) 0.017(9) -0.002(9) C5A 0.069(10) 0.117(13) 0.132(13) -0.007(10) 0.024(9) 0.035(9) C5B 0.141(14) 0.139(14) 0.089(10) 0.047(9) 0.051(10) 0.075(12) N6 0.087(9) 0.076(9) 0.128(10) 0.012(7) 0.042(7) 0.014(7) C6A 0.092(11) 0.051(8) 0.090(9) 0.017(7) 0.037(8) 0.009(7) C6B 0.111(11) 0.067(9) 0.084(8) 0.027(7) 0.008(8) 0.006(8) N7 0.119(11) 0.092(9) 0.093(8) 0.015(7) 0.028(8) 0.048(8) C7A 0.115(13) 0.102(13) 0.077(10) 0.021(8) 0.005(9) 0.025(10) C7B 0.29(3) 0.130(17) 0.093(12) 0.012(11) -0.040(15) -0.024(18) N8 0.24(3) 0.21(3) 0.24(3) 0.058(19) -0.08(2) -0.09(2) C8A 0.106(16) 0.15(2) 0.123(17) -0.014(15) -0.022(12) 0.033(16) C8B 0.20(2) 0.144(18) 0.083(11) 0.026(11) -0.014(12) 0.088(16) N9 0.27(2) 0.071(10) 0.124(12) -0.011(9) -0.051(13) -0.001(13) C9A 0.156(18) 0.123(16) 0.090(11) -0.017(12) -0.016(11) 0.048(15) C9B 0.25(3) 0.123(16) 0.106(13) 0.020(11) 0.031(14) -0.076(17) N10 0.34(3) 0.156(15) 0.24(2) 0.047(14) 0.23(2) 0.086(16) C10A 0.21(2) 0.121(15) 0.152(16) 0.025(12) 0.113(16) 0.005(14) C10B 0.134(15) 0.21(2) 0.123(13) 0.019(13) 0.061(12) 0.073(14) N11 0.087(13) 0.29(3) 0.98(8) 0.45(4) -0.15(3) -0.060(15) C11A 0.035(8) 0.172(19) 0.23(2) 0.111(16) -0.018(10) -0.027(10) C11B 0.090(10) 0.114(12) 0.111(10) 0.062(9) 0.022(8) 0.050(9) O01W 0.160(10) 0.095(7) 0.073(5) 0.040(5) -0.002(6) -0.011(7) O02W 0.103(7) 0.155(9) 0.100(6) 0.089(6) 0.070(5) 0.079(6) O03W 0.120(10) 0.274(17) 0.155(11) 0.070(11) 0.070(9) 0.004(10) _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 N107 2.097(7) . ? Co1 N413 2.098(7) . ? Co1 N419 2.116(6) . ? Co1 N101 2.139(7) . ? Co1 N420 2.174(6) . ? Co1 N122 2.238(6) . ? Co2 N207 2.082(7) . ? Co2 N113 2.095(7) . ? Co2 N119 2.118(7) . ? Co2 N201 2.143(7) . ? Co2 N222 2.207(6) . ? Co2 N120 2.215(6) . ? Co3 N213 2.090(6) . ? Co3 N307 2.094(6) . ? Co3 N301 2.105(6) . ? Co3 N219 2.113(6) . ? Co3 N322 2.195(6) . ? Co3 N220 2.227(6) . ? Co4 N319 2.101(7) . ? Co4 N407 2.097(6) . ? Co4 N401 2.100(6) . ? Co4 N313 2.108(6) . ? Co4 N320 2.196(6) . ? Co4 N422 2.201(6) . ? N101 C105 1.354(12) . ? N101 C102 1.388(11) . ? C102 C103 1.353(14) . ? C102 H102 0.9500 . ? C103 N104 1.386(13) . ? C103 H103 0.9500 . ? N104 C105 1.358(11) . ? N104 H104 0.8800 . ? C105 C106 1.433(13) . ? C106 N107 1.282(10) . ? C106 H106 0.9500 . ? N107 N108 1.350(9) . ? N108 C109 1.387(9) . ? N108 C129 1.456(10) . ? C109 N122 1.360(9) . ? C109 C110 1.377(11) . ? C110 C111 1.382(11) . ? C110 H110 0.9500 . ? C111 N120 1.363(10) . ? C111 N112 1.384(10) . ? N112 N113 1.365(9) . ? N112 C130 1.454(10) . ? N113 C114 1.293(10) . ? C114 C115 1.430(11) . ? C114 H114 0.9500 . ? C115 N116 1.339(10) . ? C115 N119 1.339(10) . ? N116 C117 1.376(11) . ? N116 H116 0.8800 . ? C117 C118 1.360(12) . ? C117 H117 0.9500 . ? C118 N119 1.385(10) . ? C118 H118 0.9500 . ? N120 C121 1.313(10) . ? C121 N122 1.343(9) . ? C121 C123 1.505(10) . ? C123 C124 1.369(11) . ? C123 C128 1.379(11) . ? C124 C125 1.392(12) . ? C124 H124 0.9500 . ? C125 C126 1.352(14) . ? C125 H125 0.9500 . ? C126 C127 1.387(14) . ? C126 H126 0.9500 . ? C127 C128 1.397(12) . ? C127 H127 0.9500 . ? C128 H128 0.9500 . ? C129 H12A 0.9800 . ? C129 H12B 0.9800 . ? C129 H12C 0.9800 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? N201 C205 1.338(10) . ? N201 C202 1.360(11) . ? C202 C203 1.349(13) . ? C202 H202 0.9500 . ? C203 N204 1.375(13) . ? C203 H203 0.9500 . ? N204 C205 1.345(11) . ? N204 H204 0.8800 . ? C205 C206 1.414(11) . ? C206 N207 1.292(10) . ? C206 H206 0.9500 . ? N207 N208 1.382(9) . ? N208 C209 1.387(10) . ? N208 C229 1.433(9) . ? C209 N222 1.359(9) . ? C209 C210 1.380(11) . ? C210 C211 1.389(10) . ? C210 H210 0.9500 . ? C211 N220 1.358(9) . ? C211 N212 1.369(9) . ? N212 N213 1.367(8) . ? N212 C230 1.483(9) . ? N213 C214 1.301(10) . ? C214 C215 1.443(11) . ? C214 H214 0.9500 . ? C215 N216 1.343(10) . ? C215 N219 1.339(10) . ? N216 C217 1.394(11) . ? N216 H216 0.8800 . ? C217 C218 1.368(12) . ? C217 H217 0.9500 . ? C218 N219 1.367(10) . ? C218 H218 0.9500 . ? N220 C221 1.345(10) . ? C221 N222 1.348(9) . ? C221 C223 1.472(10) . ? C223 C224 1.375(12) . ? C223 C228 1.403(13) . ? C224 C225 1.404(14) . ? C224 H224 0.9500 . ? C225 C226 1.401(18) . ? C225 H225 0.9500 . ? C226 C227 1.357(18) . ? C226 H226 0.9500 . ? C227 C228 1.395(14) . ? C227 H227 0.9500 . ? C228 H228 0.9500 . ? C229 H22A 0.9800 . ? C229 H22B 0.9800 . ? C229 H22C 0.9800 . ? C230 H23A 0.9800 . ? C230 H23B 0.9800 . ? C230 H23C 0.9800 . ? N301 C305 1.331(10) . ? N301 C302 1.374(10) . ? C302 C303 1.359(12) . ? C302 H302 0.9500 . ? C303 N304 1.382(11) . ? C303 H303 0.9500 . ? N304 C305 1.320(11) . ? N304 H304 0.8800 . ? C305 C306 1.463(11) . ? C306 N307 1.261(10) . ? C306 H306 0.9500 . ? N307 N308 1.369(8) . ? N308 C309 1.367(10) . ? N308 C329 1.464(10) . ? C309 N322 1.365(9) . ? C309 C310 1.389(10) . ? C310 C311 1.362(11) . ? C310 H310 0.9500 . ? C311 N312 1.371(9) . ? C311 N320 1.402(9) . ? N312 N313 1.363(9) . ? N312 C330 1.464(9) . ? N313 C314 1.286(10) . ? C314 C315 1.425(11) . ? C314 H314 0.9500 . ? C315 N316 1.338(11) . ? C315 N319 1.365(10) . ? N316 C317 1.358(12) . ? N316 H316 0.8800 . ? C317 C318 1.342(14) . ? C317 H317 0.9500 . ? C318 N319 1.381(11) . ? C318 H318 0.9500 . ? N320 C321 1.337(10) . ? C321 N322 1.330(10) . ? C321 C323 1.492(10) . ? C323 C324 1.389(10) . ? C323 C328 1.396(11) . ? C324 C325 1.385(11) . ? C324 H324 0.9500 . ? C325 C326 1.359(13) . ? C325 H325 0.9500 . ? C326 C327 1.379(13) . ? C326 H326 0.9500 . ? C327 C328 1.369(11) . ? C327 H327 0.9500 . ? C328 H328 0.9500 . ? C329 H32A 0.9800 . ? C329 H32B 0.9800 . ? C329 H32C 0.9800 . ? C330 H33A 0.9800 . ? C330 H33B 0.9800 . ? C330 H33C 0.9800 . ? N401 C405 1.336(10) . ? N401 C402 1.401(11) . ? C402 C403 1.379(12) . ? C402 H402 0.9500 . ? C403 N404 1.382(11) . ? C403 H403 0.9500 . ? N404 C405 1.358(11) . ? N404 H404 0.8800 . ? C405 C406 1.459(11) . ? C406 N407 1.286(9) . ? C406 H406 0.9500 . ? N407 N408 1.365(8) . ? N408 C409 1.368(9) . ? N408 C429 1.451(9) . ? C409 N422 1.370(9) . ? C409 C410 1.377(10) . ? C410 C411 1.363(10) . ? C410 H410 0.9500 . ? C411 N420 1.369(10) . ? C411 N412 1.367(9) . ? N412 N413 1.370(9) . ? N412 C430 1.488(10) . ? N413 C414 1.296(9) . ? C414 C415 1.457(13) . ? C414 H414 0.9500 . ? C415 N416 1.323(10) . ? C415 N419 1.325(12) . ? N416 C417 1.366(14) . ? N416 H416 0.8800 . ? C417 C418 1.354(14) . ? C417 H417 0.9500 . ? C418 N419 1.360(11) . ? C418 H418 0.9500 . ? N420 C421 1.347(9) . ? C421 N422 1.320(9) . ? C421 C423 1.492(10) . ? C423 C424 1.378(12) . ? C423 C428 1.411(12) . ? C424 C425 1.419(12) . ? C424 H424 0.9500 . ? C425 C426 1.335(14) . ? C425 H425 0.9500 . ? C426 C427 1.390(15) . ? C426 H426 0.9500 . ? C427 C428 1.386(11) . ? C427 H427 0.9500 . ? C428 H428 0.9500 . ? C429 H42A 0.9800 . ? C429 H42B 0.9800 . ? C429 H42C 0.9800 . ? C430 H43A 0.9800 . ? C430 H43B 0.9800 . ? C430 H43C 0.9800 . ? Co5 N813 2.102(7) . ? Co5 N507 2.103(7) . ? Co5 N819 2.109(7) . ? Co5 N501 2.128(7) . ? Co5 N820 2.198(6) . ? Co5 N522 2.224(7) . ? Co6 N513 2.091(6) . ? Co6 N601 2.098(6) . ? Co6 N607 2.118(6) . ? Co6 N519 2.128(7) . ? Co6 N622 2.184(6) . ? Co6 N520 2.224(6) . ? Co7 N707 2.098(7) . ? Co7 N613 2.105(7) . ? Co7 N619 2.116(6) . ? Co7 N701 2.121(7) . ? Co7 N722 2.215(7) . ? Co7 N620 2.217(6) . ? Co8 N807 2.074(7) . ? Co8 N801 2.085(7) . ? Co8 N713 2.105(7) . ? Co8 N719 2.150(9) . ? Co8 N720 2.174(8) . ? Co8 N822 2.205(6) . ? N501 C505 1.319(11) . ? N501 C502 1.373(12) . ? C502 C503 1.369(14) . ? C502 H502 0.9500 . ? C503 N504 1.333(14) . ? C503 H503 0.9500 . ? N504 C505 1.355(11) . ? N504 H504 0.8800 . ? C505 C506 1.407(13) . ? C506 N507 1.290(10) . ? C506 H506 0.9500 . ? N507 N508 1.348(10) . ? N508 C509 1.389(10) . ? N508 C529 1.469(10) . ? C509 N522 1.348(10) . ? C509 C510 1.367(11) . ? C510 C511 1.391(11) . ? C510 H510 0.9500 . ? C511 N512 1.362(10) . ? C511 N520 1.385(9) . ? N512 N513 1.354(8) . ? N512 C530 1.447(10) . ? N513 C514 1.289(10) . ? C514 C515 1.441(11) . ? C514 H514 0.9500 . ? C515 N519 1.327(10) . ? C515 N516 1.368(11) . ? N516 C517 1.363(11) . ? N516 H516 0.8800 . ? C517 C518 1.384(13) . ? C517 H517 0.9500 . ? C518 N519 1.380(11) . ? C518 H518 0.9500 . ? N520 C521 1.319(10) . ? C521 N522 1.347(9) . ? C521 C523 1.473(10) . ? C523 C528 1.375(11) . ? C523 C524 1.407(11) . ? C524 C525 1.371(12) . ? C524 H524 0.9500 . ? C525 C526 1.351(14) . ? C525 H525 0.9500 . ? C526 C527 1.367(14) . ? C526 H526 0.9500 . ? C527 C528 1.403(12) . ? C527 H527 0.9500 . ? C528 H528 0.9500 . ? C529 H52A 0.9800 . ? C529 H52B 0.9800 . ? C529 H52C 0.9800 . ? C530 H53A 0.9800 . ? C530 H53B 0.9800 . ? C530 H53C 0.9800 . ? N601 C605 1.328(10) . ? N601 C602 1.373(10) . ? C602 C603 1.344(11) . ? C602 H602 0.9500 . ? C603 N604 1.361(11) . ? C603 H603 0.9500 . ? N604 C605 1.343(9) . ? N604 H604 0.8800 . ? C605 C606 1.433(11) . ? C606 N607 1.285(9) . ? C606 H606 0.9500 . ? N607 N608 1.364(8) . ? N608 C609 1.362(9) . ? N608 C629 1.433(9) . ? C609 N622 1.379(9) . ? C609 C610 1.379(10) . ? C610 C611 1.371(10) . ? C610 H610 0.9500 . ? C611 N620 1.369(9) . ? C611 N612 1.378(10) . ? N612 N613 1.359(9) . ? N612 C630 1.461(10) . ? N613 C614 1.304(10) . ? C614 C615 1.449(11) . ? C614 H614 0.9500 . ? C615 N616 1.332(10) . ? C615 N619 1.331(11) . ? N616 C617 1.390(12) . ? N616 H616 0.8800 . ? C617 C618 1.358(13) . ? C617 H617 0.9500 . ? C618 N619 1.378(10) . ? C618 H618 0.9500 . ? N620 C621 1.333(9) . ? C621 N622 1.342(9) . ? C621 C623 1.493(10) . ? C623 C628 1.385(11) . ? C623 C624 1.398(11) . ? C624 C625 1.408(12) . ? C624 H624 0.9500 . ? C625 C626 1.357(14) . ? C625 H625 0.9500 . ? C626 C627 1.414(14) . ? C626 H626 0.9500 . ? C627 C628 1.407(12) . ? C627 H627 0.9500 . ? C628 H628 0.9500 . ? C629 H62A 0.9800 . ? C629 H62B 0.9800 . ? C629 H62C 0.9800 . ? C630 H63A 0.9800 . ? C630 H63B 0.9800 . ? C630 H63C 0.9800 . ? N701 C705 1.337(10) . ? N701 C702 1.373(11) . ? C702 C703 1.324(13) . ? C702 H702 0.9500 . ? C703 N704 1.373(11) . ? C703 H703 0.9500 . ? N704 C705 1.353(11) . ? N704 H704 0.8800 . ? C705 C706 1.440(11) . ? C706 N707 1.279(11) . ? C706 H706 0.9500 . ? N707 N708 1.343(9) . ? N708 C709 1.379(11) . ? N708 C729 1.475(10) . ? C709 N722 1.365(10) . ? C709 C710 1.379(12) . ? C710 C711 1.378(12) . ? C710 H710 0.9500 . ? C711 N720 1.364(10) . ? C711 N712 1.394(11) . ? N712 N713 1.349(10) . ? N712 C730 1.463(10) . ? N713 C714 1.272(12) . ? C714 C715 1.386(14) . ? C714 H714 0.9500 . ? C715 N719 1.348(12) . ? C715 N76' 1.455(15) . ? C715 N716 1.459(15) . ? N716 C717 1.43(2) . ? N716 H716 0.8800 . ? C717 C718 1.34(2) . ? C717 H717 0.9500 . ? C718 N719 1.446(16) . ? C718 H718 0.9500 . ? N76' C77' 1.42(2) . ? N76' H76' 0.8800 . ? C77' C78' 1.34(2) . ? C77' H77' 0.9500 . ? C78' N719 1.439(17) . ? C78' H78' 0.9500 . ? N720 C721 1.315(11) . ? C721 N722 1.360(11) . ? C721 C723 1.507(11) . ? C723 C728 1.360(12) . ? C723 C724 1.391(11) . ? C724 C725 1.354(13) . ? C724 H724 0.9500 . ? C725 C726 1.420(16) . ? C725 H725 0.9500 . ? C726 C727 1.360(17) . ? C726 H726 0.9500 . ? C727 C728 1.401(13) . ? C727 H727 0.9500 . ? C728 H728 0.9500 . ? C729 H72A 0.9800 . ? C729 H72B 0.9800 . ? C729 H72C 0.9800 . ? C730 H73A 0.9800 . ? C730 H73B 0.9800 . ? C730 H73C 0.9800 . ? N801 C802 1.345(11) . ? N801 C805 1.358(12) . ? C802 C803 1.375(14) . ? C802 H802 0.9500 . ? C803 N804 1.387(13) . ? C803 H803 0.9500 . ? N804 C805 1.344(11) . ? N804 H804 0.8800 . ? C805 C806 1.450(13) . ? C806 N807 1.308(11) . ? C806 H806 0.9500 . ? N807 N808 1.358(9) . ? N808 C809 1.355(10) . ? N808 C829 1.473(11) . ? C809 N822 1.379(10) . ? C809 C810 1.402(11) . ? C810 C811 1.361(11) . ? C810 H810 0.9500 . ? C811 N820 1.359(10) . ? C811 N812 1.383(10) . ? N812 N813 1.376(10) . ? N812 C830 1.472(10) . ? N813 C814 1.291(10) . ? C814 C815 1.424(14) . ? C814 H814 0.9500 . ? C815 N816 1.332(11) . ? C815 N819 1.331(12) . ? N816 C817 1.382(16) . ? N816 H816 0.8800 . ? C817 C818 1.367(15) . ? C817 H817 0.9500 . ? C818 N819 1.372(12) . ? C818 H818 0.9500 . ? N820 C821 1.330(9) . ? C821 N822 1.330(9) . ? C821 C823 1.470(10) . ? C823 C824 1.364(12) . ? C823 C828 1.367(12) . ? C824 C825 1.433(15) . ? C824 H824 0.9500 . ? C825 C826 1.367(16) . ? C825 H825 0.9500 . ? C826 C827 1.338(15) . ? C826 H826 0.9500 . ? C827 C828 1.403(12) . ? C827 H827 0.9500 . ? C828 H828 0.9500 . ? C829 H82A 0.9800 . ? C829 H82B 0.9800 . ? C829 H82C 0.9800 . ? C830 H83A 0.9800 . ? C830 H83B 0.9800 . ? C830 H83C 0.9800 . ? S1 O12 1.407(9) . ? S1 O13 1.435(9) . ? S1 O11 1.431(9) . ? S1 C1 1.760(16) . ? C1 F11 1.301(14) . ? C1 F13 1.337(17) . ? C1 F12 1.370(18) . ? S2 O22 1.410(8) . ? S2 O23 1.412(8) . ? S2 O21 1.436(8) . ? S2 C2 1.778(15) . ? C2 F22 1.309(15) . ? C2 F23 1.345(18) . ? C2 F21 1.336(15) . ? S3 O32 1.416(7) . ? S3 O31 1.438(8) . ? S3 O33 1.433(8) . ? S3 C3 1.714(18) . ? C3 F32 1.324(10) . ? C3 F31 1.389(14) . ? C3 F33 1.424(15) . ? S4 O42 1.418(8) . ? S4 O43 1.442(8) . ? S4 O41 1.453(7) . ? S4 C4 1.774(16) . ? C4 F41 1.298(16) . ? C4 F42 1.33(2) . ? C4 F43 1.34(2) . ? S5 O53 1.432(7) . ? S5 O51 1.437(7) . ? S5 O52 1.460(8) . ? S5 C5 1.812(8) . ? C5 F52 1.314(9) . ? C5 F53 1.331(9) . ? C5 F51 1.337(9) . ? S17 O172 1.433(7) . ? S17 O173 1.443(7) . ? S17 O171 1.451(7) . ? S17 C17 1.806(8) . ? C17 F171 1.318(9) . ? C17 F172 1.335(9) . ? C17 F173 1.339(9) . ? S6 O62 1.420(6) . ? S6 O61 1.436(6) . ? S6 O63 1.455(7) . ? S6 C6 1.813(12) . ? C6 F61 1.318(12) . ? C6 F63 1.327(13) . ? C6 F62 1.365(13) . ? S7 O71 1.434(7) . ? S7 O72 1.435(6) . ? S7 O73 1.431(6) . ? S7 C7 1.767(9) . ? C7 F71 1.301(11) . ? C7 F73 1.306(10) . ? C7 F72 1.401(13) . ? S8 O83 1.430(8) . ? S8 O82 1.438(8) . ? S8 O81 1.441(8) . ? S8 C8 1.825(17) . ? C8 F81 1.316(13) . ? C8 F82 1.331(15) . ? C8 F83 1.334(13) . ? S9 O92 1.415(8) . ? S9 O93 1.439(8) . ? S9 O91 1.472(8) . ? S9 C9 1.819(8) . ? C9 F91 1.319(9) . ? C9 F93 1.330(9) . ? C9 F92 1.332(9) . ? S18 O181 1.426(7) . ? S18 O183 1.434(7) . ? S18 O182 1.477(7) . ? S18 C18 1.803(8) . ? C18 F182 1.319(8) . ? C18 F183 1.333(8) . ? C18 F181 1.338(8) . ? S10 O103 1.409(7) . ? S10 O101 1.416(7) . ? S10 O102 1.447(8) . ? S10 C10 1.764(9) . ? C10 F103 1.280(10) . ? C10 F101 1.353(9) . ? C10 F102 1.395(11) . ? S11 O112 1.414(7) . ? S11 O111 1.451(7) . ? S11 O113 1.476(7) . ? S11 C11 1.817(11) . ? C11 F112 1.251(12) . ? C11 F111 1.370(12) . ? C11 F113 1.363(13) . ? S12 O122 1.428(8) . ? S12 O123 1.441(8) . ? S12 O121 1.453(8) . ? S12 C12 1.825(8) . ? C12 F121 1.314(9) . ? C12 F122 1.326(9) . ? C12 F123 1.335(9) . ? S19 O191 1.406(8) . ? S19 O193 1.450(8) . ? S19 O192 1.472(8) . ? S19 C19 1.816(8) . ? C19 F193 1.319(9) . ? C19 F191 1.329(9) . ? C19 F192 1.333(9) . ? S13 O133 1.423(6) . ? S13 O131 1.430(7) . ? S13 O132 1.430(7) . ? S13 C13 1.817(12) . ? C13 F133 1.311(12) . ? C13 F132 1.323(13) . ? C13 F131 1.341(13) . ? S14 O141 1.427(9) . ? S14 O142 1.431(9) . ? S14 O143 1.429(7) . ? S14 C14 1.798(15) . ? C14 F141 1.292(18) . ? C14 F143 1.326(14) . ? C14 F142 1.386(17) . ? S15 O151 1.422(5) . ? S15 O153 1.426(5) . ? S15 O152 1.489(5) . ? S15 C15 1.781(6) . ? C15 F153 1.314(7) . ? C15 F151 1.318(7) . ? C15 F152 1.385(8) . ? S16 O161 1.387(8) . ? S16 O163 1.426(12) . ? S16 O162 1.432(9) . ? S16 C16 1.814(13) . ? C16 F162 1.288(14) . ? C16 F161 1.317(12) . ? C16 F163 1.357(14) . ? N1 C1A 1.132(16) . ? C1A C1B 1.406(19) . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? N2 C2A 1.133(12) . ? C2A C2B 1.476(15) . ? C2B H2BA 0.9800 . ? C2B H2BB 0.9800 . ? C2B H2BC 0.9800 . ? N3 C3A 1.105(16) . ? C3A C3B 1.535(18) . ? C3B H3BA 0.9800 . ? C3B H3BB 0.9800 . ? C3B H3BC 0.9800 . ? N4 C4A 1.11(2) . ? C4A C4B 1.45(2) . ? C4B H4BA 0.9800 . ? C4B H4BB 0.9800 . ? C4B H4BC 0.9800 . ? N5 C5A 1.139(16) . ? C5A C5B 1.348(17) . ? C5B H5BA 0.9800 . ? C5B H5BB 0.9800 . ? C5B H5BC 0.9800 . ? N6 C6A 1.112(15) . ? C6A C6B 1.483(17) . ? C6B H6BA 0.9800 . ? C6B H6BB 0.9800 . ? C6B H6BC 0.9800 . ? N7 C7A 1.197(17) . ? C7A C7B 1.45(2) . ? C7B H7BA 0.9800 . ? C7B H7BB 0.9800 . ? C7B H7BC 0.9800 . ? N8 C8A 1.09(3) . ? C8A C8B 1.42(3) . ? C8B H8BA 0.9800 . ? C8B H8BB 0.9800 . ? C8B H8BC 0.9800 . ? N9 C9A 1.19(2) . ? C9A C9B 1.49(2) . ? C9B H9BA 0.9800 . ? C9B H9BB 0.9800 . ? C9B H9BC 0.9800 . ? N10 C10A 1.137(18) . ? C10A C10B 1.48(2) . ? C10B H10A 0.9800 . ? C10B H10B 0.9800 . ? C10B H10C 0.9800 . ? N11 C11A 1.142(8) . ? C11A C11B 1.450(8) . ? C11B H11A 0.9800 . ? C11B H11B 0.9800 . ? C11B H11C 0.9800 . ? N12 C12A 1.148(8) . ? C12A C12B 1.444(8) . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? N13 C13A 1.140(8) . ? C13A C13B 1.458(8) . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? 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 N107 Co1 N413 168.9(3) . . ? N107 Co1 N419 93.4(3) . . ? N413 Co1 N419 77.7(3) . . ? N107 Co1 N101 77.7(3) . . ? N413 Co1 N101 96.0(3) . . ? N419 Co1 N101 93.2(3) . . ? N107 Co1 N420 115.5(2) . . ? N413 Co1 N420 73.5(2) . . ? N419 Co1 N420 151.0(3) . . ? N101 Co1 N420 92.5(3) . . ? N107 Co1 N122 72.5(2) . . ? N413 Co1 N122 113.8(2) . . ? N419 Co1 N122 91.1(3) . . ? N101 Co1 N122 150.1(3) . . ? N420 Co1 N122 98.0(2) . . ? N207 Co2 N113 166.1(2) . . ? N207 Co2 N119 92.8(3) . . ? N113 Co2 N119 77.4(3) . . ? N207 Co2 N201 76.7(3) . . ? N113 Co2 N201 93.8(3) . . ? N119 Co2 N201 93.2(3) . . ? N207 Co2 N222 73.0(2) . . ? N113 Co2 N222 117.3(2) . . ? N119 Co2 N222 95.9(2) . . ? N201 Co2 N222 148.7(3) . . ? N207 Co2 N120 116.5(3) . . ? N113 Co2 N120 73.0(3) . . ? N119 Co2 N120 150.3(3) . . ? N201 Co2 N120 89.7(2) . . ? N222 Co2 N120 96.9(2) . . ? N213 Co3 N307 168.0(3) . . ? N213 Co3 N301 91.8(3) . . ? N307 Co3 N301 77.7(3) . . ? N213 Co3 N219 77.3(3) . . ? N307 Co3 N219 98.1(3) . . ? N301 Co3 N219 97.3(3) . . ? N213 Co3 N322 117.4(3) . . ? N307 Co3 N322 73.2(2) . . ? N301 Co3 N322 150.8(2) . . ? N219 Co3 N322 89.0(2) . . ? N213 Co3 N220 73.2(2) . . ? N307 Co3 N220 112.4(2) . . ? N301 Co3 N220 91.2(2) . . ? N219 Co3 N220 149.5(2) . . ? N322 Co3 N220 97.7(2) . . ? N319 Co4 N407 94.0(3) . . ? N319 Co4 N401 98.9(3) . . ? N407 Co4 N401 77.3(2) . . ? N319 Co4 N313 78.1(3) . . ? N407 Co4 N313 168.7(2) . . ? N401 Co4 N313 95.9(2) . . ? N319 Co4 N320 151.8(3) . . ? N407 Co4 N320 114.1(2) . . ? N401 Co4 N320 85.0(3) . . ? N313 Co4 N320 73.7(2) . . ? N319 Co4 N422 93.5(2) . . ? N407 Co4 N422 73.0(2) . . ? N401 Co4 N422 148.4(3) . . ? N313 Co4 N422 115.1(2) . . ? N320 Co4 N422 97.5(2) . . ? C105 N101 C102 107.2(8) . . ? C105 N101 Co1 109.2(6) . . ? C102 N101 Co1 143.7(7) . . ? C103 C102 N101 108.7(10) . . ? C103 C102 H102 125.6 . . ? N101 C102 H102 125.6 . . ? C102 C103 N104 107.1(9) . . ? C102 C103 H103 126.5 . . ? N104 C103 H103 126.5 . . ? C105 N104 C103 108.2(9) . . ? C105 N104 H104 125.9 . . ? C103 N104 H104 125.9 . . ? N101 C105 N104 108.9(9) . . ? N101 C105 C106 121.7(8) . . ? N104 C105 C106 129.4(10) . . ? N107 C106 C105 113.5(9) . . ? N107 C106 H106 123.3 . . ? C105 C106 H106 123.3 . . ? C106 N107 N108 121.3(8) . . ? C106 N107 Co1 117.8(7) . . ? N108 N107 Co1 120.7(5) . . ? N107 N108 C109 115.3(7) . . ? N107 N108 C129 120.0(6) . . ? C109 N108 C129 124.6(7) . . ? N122 C109 C110 122.8(7) . . ? N122 C109 N108 116.2(7) . . ? C110 C109 N108 120.9(7) . . ? C109 C110 C111 116.6(7) . . ? C109 C110 H110 121.7 . . ? C111 C110 H110 121.7 . . ? N120 C111 N112 116.4(7) . . ? N120 C111 C110 122.1(8) . . ? N112 C111 C110 121.5(7) . . ? N113 N112 C111 114.9(6) . . ? N113 N112 C130 120.9(7) . . ? C111 N112 C130 124.0(7) . . ? C114 N113 N112 121.5(7) . . ? C114 N113 Co2 117.8(6) . . ? N112 N113 Co2 120.4(5) . . ? N113 C114 C115 112.2(8) . . ? N113 C114 H114 123.9 . . ? C115 C114 H114 123.9 . . ? N116 C115 N119 110.4(8) . . ? N116 C115 C114 127.4(8) . . ? N119 C115 C114 122.2(7) . . ? C115 N116 C117 108.1(8) . . ? C115 N116 H116 126.0 . . ? C117 N116 H116 126.0 . . ? C118 C117 N116 106.5(8) . . ? C118 C117 H117 126.8 . . ? N116 C117 H117 126.8 . . ? C117 C118 N119 108.9(8) . . ? C117 C118 H118 125.5 . . ? N119 C118 H118 125.5 . . ? C115 N119 C118 106.1(7) . . ? C115 N119 Co2 109.9(5) . . ? C118 N119 Co2 143.5(6) . . ? C121 N120 C111 115.9(7) . . ? C121 N120 Co2 128.6(5) . . ? C111 N120 Co2 115.3(5) . . ? N120 C121 N122 127.7(7) . . ? N120 C121 C123 116.6(7) . . ? N122 C121 C123 115.7(7) . . ? C121 N122 C109 114.9(7) . . ? C121 N122 Co1 129.9(5) . . ? C109 N122 Co1 114.8(5) . . ? C124 C123 C128 119.1(8) . . ? C124 C123 C121 121.2(7) . . ? C128 C123 C121 119.8(7) . . ? C123 C124 C125 120.7(9) . . ? C123 C124 H124 119.6 . . ? C125 C124 H124 119.6 . . ? C126 C125 C124 120.9(9) . . ? C126 C125 H125 119.6 . . ? C124 C125 H125 119.6 . . ? C125 C126 C127 119.1(9) . . ? C125 C126 H126 120.4 . . ? C127 C126 H126 120.4 . . ? C126 C127 C128 120.3(9) . . ? C126 C127 H127 119.9 . . ? C128 C127 H127 119.9 . . ? C123 C128 C127 119.9(8) . . ? C123 C128 H128 120.0 . . ? C127 C128 H128 120.0 . . ? N108 C129 H12A 109.5 . . ? N108 C129 H12B 109.5 . . ? H12A C129 H12B 109.5 . . ? N108 C129 H12C 109.5 . . ? H12A C129 H12C 109.5 . . ? H12B C129 H12C 109.5 . . ? N112 C130 H13A 109.5 . . ? N112 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? N112 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? C205 N201 C202 107.1(8) . . ? C205 N201 Co2 109.7(6) . . ? C202 N201 Co2 143.1(7) . . ? C203 C202 N201 109.0(9) . . ? C203 C202 H202 125.5 . . ? N201 C202 H202 125.5 . . ? C202 C203 N204 106.9(9) . . ? C202 C203 H203 126.5 . . ? N204 C203 H203 126.5 . . ? C205 N204 C203 107.4(8) . . ? C205 N204 H204 126.3 . . ? C203 N204 H204 126.3 . . ? N201 C205 N204 109.5(8) . . ? N201 C205 C206 122.1(8) . . ? N204 C205 C206 128.3(8) . . ? N207 C206 C205 112.5(7) . . ? N207 C206 H206 123.8 . . ? C205 C206 H206 123.8 . . ? C206 N207 N208 120.4(7) . . ? C206 N207 Co2 118.8(6) . . ? N208 N207 Co2 120.7(5) . . ? N207 N208 C209 113.3(6) . . ? N207 N208 C229 121.2(6) . . ? C209 N208 C229 125.5(7) . . ? N222 C209 C210 122.5(7) . . ? N222 C209 N208 117.1(7) . . ? C210 C209 N208 120.4(7) . . ? C209 C210 C211 116.9(7) . . ? C209 C210 H210 121.6 . . ? C211 C210 H210 121.6 . . ? N220 C211 N212 117.0(6) . . ? N220 C211 C210 122.2(7) . . ? N212 C211 C210 120.8(7) . . ? N213 N212 C211 115.3(6) . . ? N213 N212 C230 119.6(6) . . ? C211 N212 C230 125.1(6) . . ? C214 N213 N212 121.9(7) . . ? C214 N213 Co3 118.5(6) . . ? N212 N213 Co3 119.2(5) . . ? N213 C214 C215 111.3(7) . . ? N213 C214 H214 124.3 . . ? C215 C214 H214 124.3 . . ? N216 C215 N219 111.7(7) . . ? N216 C215 C214 125.9(8) . . ? N219 C215 C214 121.8(7) . . ? C215 N216 C217 105.9(7) . . ? C215 N216 H216 127.0 . . ? C217 N216 H216 127.0 . . ? C218 C217 N216 107.1(7) . . ? C218 C217 H217 126.4 . . ? N216 C217 H217 126.4 . . ? N219 C218 C217 108.8(8) . . ? N219 C218 H218 125.6 . . ? C217 C218 H218 125.6 . . ? C215 N219 C218 106.3(7) . . ? C215 N219 Co3 110.6(5) . . ? C218 N219 Co3 142.8(6) . . ? C221 N220 C211 116.3(6) . . ? C221 N220 Co3 129.3(5) . . ? C211 N220 Co3 114.2(5) . . ? N220 C221 N222 125.9(7) . . ? N220 C221 C223 117.6(7) . . ? N222 C221 C223 116.3(7) . . ? C221 N222 C209 116.1(6) . . ? C221 N222 Co2 128.6(5) . . ? C209 N222 Co2 115.2(5) . . ? C224 C223 C228 120.9(9) . . ? C224 C223 C221 121.1(8) . . ? C228 C223 C221 118.0(8) . . ? C223 C224 C225 119.2(11) . . ? C223 C224 H224 120.4 . . ? C225 C224 H224 120.4 . . ? C224 C225 C226 121.4(11) . . ? C224 C225 H225 119.3 . . ? C226 C225 H225 119.3 . . ? C227 C226 C225 116.9(11) . . ? C227 C226 H226 121.6 . . ? C225 C226 H226 121.6 . . ? C226 C227 C228 124.3(13) . . ? C226 C227 H227 117.9 . . ? C228 C227 H227 117.9 . . ? C227 C228 C223 117.3(11) . . ? C227 C228 H228 121.4 . . ? C223 C228 H228 121.4 . . ? N208 C229 H22A 109.5 . . ? N208 C229 H22B 109.5 . . ? H22A C229 H22B 109.5 . . ? N208 C229 H22C 109.5 . . ? H22A C229 H22C 109.5 . . ? H22B C229 H22C 109.5 . . ? N212 C230 H23A 109.5 . . ? N212 C230 H23B 109.5 . . ? H23A C230 H23B 109.5 . . ? N212 C230 H23C 109.5 . . ? H23A C230 H23C 109.5 . . ? H23B C230 H23C 109.5 . . ? C305 N301 C302 105.6(7) . . ? C305 N301 Co3 110.6(5) . . ? C302 N301 Co3 143.5(6) . . ? C303 C302 N301 109.6(8) . . ? C303 C302 H302 125.2 . . ? N301 C302 H302 125.2 . . ? C302 C303 N304 105.3(8) . . ? C302 C303 H303 127.3 . . ? N304 C303 H303 127.3 . . ? C305 N304 C303 108.2(8) . . ? C305 N304 H304 125.9 . . ? C303 N304 H304 125.9 . . ? N304 C305 N301 111.1(8) . . ? N304 C305 C306 128.2(8) . . ? N301 C305 C306 120.6(8) . . ? N307 C306 C305 113.0(8) . . ? N307 C306 H306 123.5 . . ? C305 C306 H306 123.5 . . ? C306 N307 N308 122.3(7) . . ? C306 N307 Co3 117.9(6) . . ? N308 N307 Co3 119.6(5) . . ? C309 N308 N307 115.0(6) . . ? C309 N308 C329 124.6(7) . . ? N307 N308 C329 120.4(6) . . ? N322 C309 N308 116.7(7) . . ? N322 C309 C310 121.9(7) . . ? N308 C309 C310 121.4(7) . . ? C311 C310 C309 117.5(7) . . ? C311 C310 H310 121.2 . . ? C309 C310 H310 121.2 . . ? C310 C311 N312 122.5(7) . . ? C310 C311 N320 122.2(7) . . ? N312 C311 N320 115.4(7) . . ? N313 N312 C311 116.5(6) . . ? N313 N312 C330 121.0(6) . . ? C311 N312 C330 122.4(7) . . ? C314 N313 N312 124.1(7) . . ? C314 N313 Co4 116.6(6) . . ? N312 N313 Co4 119.0(5) . . ? N313 C314 C315 113.9(7) . . ? N313 C314 H314 123.0 . . ? C315 C314 H314 123.0 . . ? N316 C315 N319 110.8(8) . . ? N316 C315 C314 128.3(8) . . ? N319 C315 C314 120.9(8) . . ? C315 N316 C317 107.9(8) . . ? C315 N316 H316 126.0 . . ? C317 N316 H316 126.0 . . ? C318 C317 N316 106.9(9) . . ? C318 C317 H317 126.6 . . ? N316 C317 H317 126.6 . . ? C317 C318 N319 110.7(9) . . ? C317 C318 H318 124.6 . . ? N319 C318 H318 124.6 . . ? C315 N319 C318 103.7(8) . . ? C315 N319 Co4 110.1(6) . . ? C318 N319 Co4 146.1(7) . . ? C321 N320 C311 114.4(7) . . ? C321 N320 Co4 130.1(5) . . ? C311 N320 Co4 115.1(5) . . ? N322 C321 N320 127.6(7) . . ? N322 C321 C323 117.3(7) . . ? N320 C321 C323 115.1(7) . . ? C321 N322 C309 116.1(6) . . ? C321 N322 Co3 128.4(5) . . ? C309 N322 Co3 115.3(5) . . ? C324 C323 C328 118.2(7) . . ? C324 C323 C321 123.2(7) . . ? C328 C323 C321 118.6(7) . . ? C325 C324 C323 120.6(8) . . ? C325 C324 H324 119.7 . . ? C323 C324 H324 119.7 . . ? C326 C325 C324 119.9(8) . . ? C326 C325 H325 120.0 . . ? C324 C325 H325 120.0 . . ? C325 C326 C327 120.7(9) . . ? C325 C326 H326 119.7 . . ? C327 C326 H326 119.7 . . ? C328 C327 C326 119.9(8) . . ? C328 C327 H327 120.1 . . ? C326 C327 H327 120.1 . . ? C327 C328 C323 120.7(8) . . ? C327 C328 H328 119.6 . . ? C323 C328 H328 119.6 . . ? N308 C329 H32A 109.5 . . ? N308 C329 H32B 109.5 . . ? H32A C329 H32B 109.5 . . ? N308 C329 H32C 109.5 . . ? H32A C329 H32C 109.5 . . ? H32B C329 H32C 109.5 . . ? N312 C330 H33A 109.5 . . ? N312 C330 H33B 109.5 . . ? H33A C330 H33B 109.5 . . ? N312 C330 H33C 109.5 . . ? H33A C330 H33C 109.5 . . ? H33B C330 H33C 109.5 . . ? C405 N401 C402 105.6(7) . . ? C405 N401 Co4 111.4(5) . . ? C402 N401 Co4 141.2(6) . . ? C403 C402 N401 109.1(8) . . ? C403 C402 H402 125.5 . . ? N401 C402 H402 125.5 . . ? C402 C403 N404 106.4(8) . . ? C402 C403 H403 126.8 . . ? N404 C403 H403 126.8 . . ? C405 N404 C403 107.5(8) . . ? C405 N404 H404 126.3 . . ? C403 N404 H404 126.3 . . ? N401 C405 N404 111.5(8) . . ? N401 C405 C406 121.0(7) . . ? N404 C405 C406 127.0(8) . . ? N407 C406 C405 111.5(7) . . ? N407 C406 H406 124.3 . . ? C405 C406 H406 124.3 . . ? C406 N407 N408 122.0(7) . . ? C406 N407 Co4 118.5(5) . . ? N408 N407 Co4 119.4(5) . . ? N407 N408 C409 115.0(6) . . ? N407 N408 C429 120.9(6) . . ? C409 N408 C429 123.7(6) . . ? N422 C409 N408 116.3(6) . . ? N422 C409 C410 120.4(7) . . ? N408 C409 C410 123.2(7) . . ? C411 C410 C409 118.5(7) . . ? C411 C410 H410 120.8 . . ? C409 C410 H410 120.8 . . ? C410 C411 N420 122.1(7) . . ? C410 C411 N412 121.7(7) . . ? N420 C411 N412 116.1(7) . . ? N413 N412 C411 115.3(6) . . ? N413 N412 C430 119.9(6) . . ? C411 N412 C430 124.7(7) . . ? C414 N413 N412 123.1(7) . . ? C414 N413 Co1 117.7(6) . . ? N412 N413 Co1 119.0(4) . . ? N413 C414 C415 112.1(8) . . ? N413 C414 H414 124.0 . . ? C415 C414 H414 124.0 . . ? N416 C415 N419 109.6(9) . . ? N416 C415 C414 128.6(9) . . ? N419 C415 C414 121.8(7) . . ? C415 N416 C417 108.2(9) . . ? C415 N416 H416 125.9 . . ? C417 N416 H416 125.9 . . ? C418 C417 N416 106.7(9) . . ? C418 C417 H417 126.7 . . ? N416 C417 H417 126.7 . . ? C417 C418 N419 107.9(10) . . ? C417 C418 H418 126.0 . . ? N419 C418 H418 126.0 . . ? C415 N419 C418 107.6(8) . . ? C415 N419 Co1 110.7(6) . . ? C418 N419 Co1 141.7(7) . . ? C421 N420 C411 115.3(6) . . ? C421 N420 Co1 128.6(5) . . ? C411 N420 Co1 115.9(5) . . ? N422 C421 N420 126.3(7) . . ? N422 C421 C423 118.1(6) . . ? N420 C421 C423 115.5(6) . . ? C421 N422 C409 117.2(6) . . ? C421 N422 Co4 127.6(5) . . ? C409 N422 Co4 115.2(5) . . ? C424 C423 C428 119.8(8) . . ? C424 C423 C421 122.1(8) . . ? C428 C423 C421 118.1(7) . . ? C423 C424 C425 119.1(10) . . ? C423 C424 H424 120.5 . . ? C425 C424 H424 120.5 . . ? C426 C425 C424 120.8(10) . . ? C426 C425 H425 119.6 . . ? C424 C425 H425 119.6 . . ? C425 C426 C427 121.0(10) . . ? C425 C426 H426 119.5 . . ? C427 C426 H426 119.5 . . ? C426 C427 C428 119.9(10) . . ? C426 C427 H427 120.1 . . ? C428 C427 H427 120.1 . . ? C427 C428 C423 119.5(9) . . ? C427 C428 H428 120.3 . . ? C423 C428 H428 120.3 . . ? N408 C429 H42A 109.5 . . ? N408 C429 H42B 109.5 . . ? H42A C429 H42B 109.5 . . ? N408 C429 H42C 109.5 . . ? H42A C429 H42C 109.5 . . ? H42B C429 H42C 109.5 . . ? N412 C430 H43A 109.5 . . ? N412 C430 H43B 109.5 . . ? H43A C430 H43B 109.5 . . ? N412 C430 H43C 109.5 . . ? H43A C430 H43C 109.5 . . ? H43B C430 H43C 109.5 . . ? N813 Co5 N507 166.7(3) . . ? N813 Co5 N819 77.3(3) . . ? N507 Co5 N819 92.0(3) . . ? N813 Co5 N501 96.8(3) . . ? N507 Co5 N501 76.6(3) . . ? N819 Co5 N501 97.5(3) . . ? N813 Co5 N820 73.1(2) . . ? N507 Co5 N820 117.6(2) . . ? N819 Co5 N820 150.3(3) . . ? N501 Co5 N820 87.9(3) . . ? N813 Co5 N522 115.4(2) . . ? N507 Co5 N522 72.6(3) . . ? N819 Co5 N522 93.5(3) . . ? N501 Co5 N522 147.6(3) . . ? N820 Co5 N522 97.4(2) . . ? N513 Co6 N601 95.2(3) . . ? N513 Co6 N607 166.2(2) . . ? N601 Co6 N607 76.9(2) . . ? N513 Co6 N519 78.1(3) . . ? N601 Co6 N519 96.7(3) . . ? N607 Co6 N519 91.4(2) . . ? N513 Co6 N622 116.6(2) . . ? N601 Co6 N622 147.6(3) . . ? N607 Co6 N622 73.0(2) . . ? N519 Co6 N622 95.6(2) . . ? N513 Co6 N520 73.0(2) . . ? N601 Co6 N520 85.9(2) . . ? N607 Co6 N520 117.1(2) . . ? N519 Co6 N520 151.1(3) . . ? N622 Co6 N520 97.4(2) . . ? N707 Co7 N613 168.6(3) . . ? N707 Co7 N619 92.4(3) . . ? N613 Co7 N619 77.6(3) . . ? N707 Co7 N701 77.6(3) . . ? N613 Co7 N701 97.6(3) . . ? N619 Co7 N701 96.4(3) . . ? N707 Co7 N722 73.0(3) . . ? N613 Co7 N722 112.9(3) . . ? N619 Co7 N722 93.4(3) . . ? N701 Co7 N722 149.3(3) . . ? N707 Co7 N620 117.1(2) . . ? N613 Co7 N620 72.7(2) . . ? N619 Co7 N620 150.3(3) . . ? N701 Co7 N620 87.7(2) . . ? N722 Co7 N620 97.9(2) . . ? N807 Co8 N801 78.8(3) . . ? N807 Co8 N713 164.9(3) . . ? N801 Co8 N713 91.2(3) . . ? N807 Co8 N719 92.3(3) . . ? N801 Co8 N719 92.6(3) . . ? N713 Co8 N719 76.7(3) . . ? N807 Co8 N720 117.8(3) . . ? N801 Co8 N720 94.9(3) . . ? N713 Co8 N720 74.0(3) . . ? N719 Co8 N720 149.9(3) . . ? N807 Co8 N822 72.7(3) . . ? N801 Co8 N822 151.5(3) . . ? N713 Co8 N822 116.8(3) . . ? N719 Co8 N822 89.2(3) . . ? N720 Co8 N822 97.7(2) . . ? C505 N501 C502 106.5(8) . . ? C505 N501 Co5 110.5(6) . . ? C502 N501 Co5 142.8(7) . . ? C503 C502 N501 107.3(10) . . ? C503 C502 H502 126.3 . . ? N501 C502 H502 126.3 . . ? N504 C503 C502 108.5(9) . . ? N504 C503 H503 125.8 . . ? C502 C503 H503 125.8 . . ? C503 N504 C505 106.7(9) . . ? C503 N504 H504 126.6 . . ? C505 N504 H504 126.6 . . ? N501 C505 N504 110.9(9) . . ? N501 C505 C506 122.1(8) . . ? N504 C505 C506 126.9(10) . . ? N507 C506 C505 113.3(9) . . ? N507 C506 H506 123.3 . . ? C505 C506 H506 123.3 . . ? C506 N507 N508 123.2(8) . . ? C506 N507 Co5 117.0(7) . . ? N508 N507 Co5 119.5(5) . . ? N507 N508 C509 115.4(7) . . ? N507 N508 C529 119.8(7) . . ? C509 N508 C529 124.5(8) . . ? N522 C509 C510 122.8(7) . . ? N522 C509 N508 116.1(8) . . ? C510 C509 N508 121.0(8) . . ? C509 C510 C511 117.8(8) . . ? C509 C510 H510 121.1 . . ? C511 C510 H510 121.1 . . ? N512 C511 N520 117.2(7) . . ? N512 C511 C510 122.7(8) . . ? N520 C511 C510 120.1(8) . . ? N513 N512 C511 115.0(6) . . ? N513 N512 C530 120.0(7) . . ? C511 N512 C530 124.6(7) . . ? C514 N513 N512 122.1(7) . . ? C514 N513 Co6 116.6(6) . . ? N512 N513 Co6 120.9(5) . . ? N513 C514 C515 113.7(8) . . ? N513 C514 H514 123.2 . . ? C515 C514 H514 123.2 . . ? N519 C515 N516 111.6(8) . . ? N519 C515 C514 121.7(8) . . ? N516 C515 C514 126.6(8) . . ? C517 N516 C515 107.7(8) . . ? C517 N516 H516 126.1 . . ? C515 N516 H516 126.1 . . ? N516 C517 C518 105.3(8) . . ? N516 C517 H517 127.3 . . ? C518 C517 H517 127.3 . . ? N519 C518 C517 110.5(8) . . ? N519 C518 H518 124.7 . . ? C517 C518 H518 124.7 . . ? C515 N519 C518 104.8(7) . . ? C515 N519 Co6 109.5(6) . . ? C518 N519 Co6 145.2(6) . . ? C521 N520 C511 116.7(7) . . ? C521 N520 Co6 128.6(5) . . ? C511 N520 Co6 113.6(5) . . ? N520 C521 N522 126.4(7) . . ? N520 C521 C523 116.3(6) . . ? N522 C521 C523 117.1(7) . . ? C521 N522 C509 115.8(7) . . ? C521 N522 Co5 128.8(5) . . ? C509 N522 Co5 115.2(5) . . ? C528 C523 C524 118.4(8) . . ? C528 C523 C521 119.6(7) . . ? C524 C523 C521 122.0(7) . . ? C525 C524 C523 120.8(9) . . ? C525 C524 H524 119.6 . . ? C523 C524 H524 119.6 . . ? C526 C525 C524 119.8(9) . . ? C526 C525 H525 120.1 . . ? C524 C525 H525 120.1 . . ? C525 C526 C527 121.4(9) . . ? C525 C526 H526 119.3 . . ? C527 C526 H526 119.3 . . ? C526 C527 C528 119.6(9) . . ? C526 C527 H527 120.2 . . ? C528 C527 H527 120.2 . . ? C523 C528 C527 120.0(9) . . ? C523 C528 H528 120.0 . . ? C527 C528 H528 120.0 . . ? N508 C529 H52A 109.5 . . ? N508 C529 H52B 109.5 . . ? H52A C529 H52B 109.5 . . ? N508 C529 H52C 109.5 . . ? H52A C529 H52C 109.5 . . ? H52B C529 H52C 109.5 . . ? N512 C530 H53A 109.5 . . ? N512 C530 H53B 109.5 . . ? H53A C530 H53B 109.5 . . ? N512 C530 H53C 109.5 . . ? H53A C530 H53C 109.5 . . ? H53B C530 H53C 109.5 . . ? C605 N601 C602 106.2(6) . . ? C605 N601 Co6 111.4(5) . . ? C602 N601 Co6 142.3(6) . . ? C603 C602 N601 108.8(8) . . ? C603 C602 H602 125.6 . . ? N601 C602 H602 125.6 . . ? C602 C603 N604 107.4(7) . . ? C602 C603 H603 126.3 . . ? N604 C603 H603 126.3 . . ? C605 N604 C603 107.2(7) . . ? C605 N604 H604 126.4 . . ? C603 N604 H604 126.4 . . ? N601 C605 N604 110.5(7) . . ? N601 C605 C606 120.9(7) . . ? N604 C605 C606 128.5(7) . . ? N607 C606 C605 113.3(7) . . ? N607 C606 H606 123.4 . . ? C605 C606 H606 123.4 . . ? C606 N607 N608 124.1(6) . . ? C606 N607 Co6 116.4(5) . . ? N608 N607 Co6 119.1(4) . . ? C609 N608 N607 114.6(6) . . ? C609 N608 C629 123.8(6) . . ? N607 N608 C629 121.1(6) . . ? N608 C609 N622 116.7(6) . . ? N608 C609 C610 122.3(7) . . ? N622 C609 C610 121.0(6) . . ? C611 C610 C609 118.3(7) . . ? C611 C610 H610 120.8 . . ? C609 C610 H610 120.8 . . ? N620 C611 N612 117.0(6) . . ? N620 C611 C610 121.9(7) . . ? N612 C611 C610 121.2(7) . . ? N613 N612 C611 114.5(7) . . ? N613 N612 C630 120.7(7) . . ? C611 N612 C630 124.6(6) . . ? C614 N613 N612 121.9(7) . . ? C614 N613 Co7 117.3(6) . . ? N612 N613 Co7 120.8(5) . . ? N613 C614 C615 112.5(8) . . ? N613 C614 H614 123.7 . . ? C615 C614 H614 123.7 . . ? N616 C615 N619 112.1(7) . . ? N616 C615 C614 126.3(9) . . ? N619 C615 C614 121.6(7) . . ? C615 N616 C617 106.4(8) . . ? C615 N616 H616 126.8 . . ? C617 N616 H616 126.8 . . ? C618 C617 N616 106.8(8) . . ? C618 C617 H617 126.6 . . ? N616 C617 H617 126.6 . . ? C617 C618 N619 109.0(8) . . ? C617 C618 H618 125.5 . . ? N619 C618 H618 125.5 . . ? C615 N619 C618 105.6(7) . . ? C615 N619 Co7 111.0(5) . . ? C618 N619 Co7 143.3(6) . . ? C621 N620 C611 116.1(6) . . ? C621 N620 Co7 128.5(5) . . ? C611 N620 Co7 115.0(5) . . ? N620 C621 N622 126.6(7) . . ? N620 C621 C623 116.3(6) . . ? N622 C621 C623 116.9(6) . . ? C621 N622 C609 116.1(6) . . ? C621 N622 Co6 128.5(5) . . ? C609 N622 Co6 115.4(4) . . ? C628 C623 C624 121.3(8) . . ? C628 C623 C621 117.9(7) . . ? C624 C623 C621 120.7(8) . . ? C623 C624 C625 117.8(9) . . ? C623 C624 H624 121.1 . . ? C625 C624 H624 121.1 . . ? C626 C625 C624 122.0(9) . . ? C626 C625 H625 119.0 . . ? C624 C625 H625 119.0 . . ? C625 C626 C627 120.1(9) . . ? C625 C626 H626 120.0 . . ? C627 C626 H626 120.0 . . ? C628 C627 C626 118.9(9) . . ? C628 C627 H627 120.6 . . ? C626 C627 H627 120.6 . . ? C623 C628 C627 119.9(9) . . ? C623 C628 H628 120.0 . . ? C627 C628 H628 120.0 . . ? N608 C629 H62A 109.5 . . ? N608 C629 H62B 109.5 . . ? H62A C629 H62B 109.5 . . ? N608 C629 H62C 109.5 . . ? H62A C629 H62C 109.5 . . ? H62B C629 H62C 109.5 . . ? N612 C630 H63A 109.5 . . ? N612 C630 H63B 109.5 . . ? H63A C630 H63B 109.5 . . ? N612 C630 H63C 109.5 . . ? H63A C630 H63C 109.5 . . ? H63B C630 H63C 109.5 . . ? C705 N701 C702 105.8(7) . . ? C705 N701 Co7 109.6(6) . . ? C702 N701 Co7 144.2(6) . . ? C703 C702 N701 110.1(9) . . ? C703 C702 H702 125.0 . . ? N701 C702 H702 125.0 . . ? C702 C703 N704 107.2(9) . . ? C702 C703 H703 126.4 . . ? N704 C703 H703 126.4 . . ? C705 N704 C703 107.1(8) . . ? C705 N704 H704 126.4 . . ? C703 N704 H704 126.4 . . ? N701 C705 N704 109.8(8) . . ? N701 C705 C706 122.1(8) . . ? N704 C705 C706 128.0(8) . . ? N707 C706 C705 112.7(8) . . ? N707 C706 H706 123.6 . . ? C705 C706 H706 123.6 . . ? C706 N707 N708 122.5(8) . . ? C706 N707 Co7 117.6(6) . . ? N708 N707 Co7 119.6(6) . . ? N707 N708 C709 115.6(7) . . ? N707 N708 C729 120.4(8) . . ? C709 N708 C729 124.0(7) . . ? N722 C709 N708 116.3(8) . . ? N722 C709 C710 122.9(9) . . ? N708 C709 C710 120.8(8) . . ? C709 C710 C711 116.3(8) . . ? C709 C710 H710 121.8 . . ? C711 C710 H710 121.8 . . ? N720 C711 C710 123.0(8) . . ? N720 C711 N712 116.0(8) . . ? C710 C711 N712 121.0(8) . . ? N713 N712 C711 115.7(7) . . ? N713 N712 C730 121.9(8) . . ? C711 N712 C730 122.2(8) . . ? C714 N713 N712 123.3(8) . . ? C714 N713 Co8 117.9(7) . . ? N712 N713 Co8 118.6(6) . . ? N713 C714 C715 112.8(9) . . ? N713 C714 H714 123.6 . . ? C715 C714 H714 123.6 . . ? N719 C715 C714 124.3(10) . . ? N719 C715 N76' 105.1(11) . . ? C714 C715 N76' 127.0(11) . . ? N719 C715 N716 104.9(10) . . ? C714 C715 N716 126.9(11) . . ? N76' C715 N716 39.7(6) . . ? C717 N716 C715 111.0(15) . . ? C717 N716 H716 124.5 . . ? C715 N716 H716 124.5 . . ? C718 C717 N716 103.5(19) . . ? C718 C717 H717 128.3 . . ? N716 C717 H717 128.3 . . ? C717 C718 N719 112.4(18) . . ? C717 C718 H718 123.8 . . ? N719 C718 H718 123.8 . . ? C77' N76' C715 110.0(17) . . ? C77' N76' H76' 125.0 . . ? C715 N76' H76' 125.0 . . ? C78' C77' N76' 105(2) . . ? C78' C77' H77' 127.6 . . ? N76' C77' H77' 127.6 . . ? C77' C78' N719 111(2) . . ? C77' C78' H78' 124.4 . . ? N719 C78' H78' 124.4 . . ? C715 N719 C78' 108.8(12) . . ? C715 N719 C718 108.2(11) . . ? C78' N719 C718 38.2(7) . . ? C715 N719 Co8 107.6(7) . . ? C78' N719 Co8 136.8(10) . . ? C718 N719 Co8 140.5(9) . . ? C721 N720 C711 115.4(8) . . ? C721 N720 Co8 128.8(6) . . ? C711 N720 Co8 115.5(6) . . ? N720 C721 N722 127.5(8) . . ? N720 C721 C723 116.8(9) . . ? N722 C721 C723 115.6(8) . . ? C721 N722 C709 114.5(8) . . ? C721 N722 Co7 130.8(6) . . ? C709 N722 Co7 114.6(6) . . ? C728 C723 C724 121.6(9) . . ? C728 C723 C721 117.3(8) . . ? C724 C723 C721 121.1(8) . . ? C725 C724 C723 119.0(10) . . ? C725 C724 H724 120.5 . . ? C723 C724 H724 120.5 . . ? C724 C725 C726 120.4(10) . . ? C724 C725 H725 119.8 . . ? C726 C725 H725 119.8 . . ? C727 C726 C725 119.5(11) . . ? C727 C726 H726 120.3 . . ? C725 C726 H726 120.3 . . ? C726 C727 C728 120.0(11) . . ? C726 C727 H727 120.0 . . ? C728 C727 H727 120.0 . . ? C723 C728 C727 119.3(10) . . ? C723 C728 H728 120.3 . . ? C727 C728 H728 120.3 . . ? N708 C729 H72A 109.5 . . ? N708 C729 H72B 109.5 . . ? H72A C729 H72B 109.5 . . ? N708 C729 H72C 109.5 . . ? H72A C729 H72C 109.5 . . ? H72B C729 H72C 109.5 . . ? N712 C730 H73A 109.5 . . ? N712 C730 H73B 109.5 . . ? H73A C730 H73B 109.5 . . ? N712 C730 H73C 109.5 . . ? H73A C730 H73C 109.5 . . ? H73B C730 H73C 109.5 . . ? C802 N801 C805 105.1(8) . . ? C802 N801 Co8 144.3(7) . . ? C805 N801 Co8 109.9(6) . . ? N801 C802 C803 111.9(10) . . ? N801 C802 H802 124.0 . . ? C803 C802 H802 124.0 . . ? C802 C803 N804 104.2(9) . . ? C802 C803 H803 127.9 . . ? N804 C803 H803 127.9 . . ? C805 N804 C803 108.2(9) . . ? C805 N804 H804 125.9 . . ? C803 N804 H804 125.9 . . ? N804 C805 N801 110.6(9) . . ? N804 C805 C806 127.8(10) . . ? N801 C805 C806 121.6(8) . . ? N807 C806 C805 111.3(9) . . ? N807 C806 H806 124.3 . . ? C805 C806 H806 124.3 . . ? C806 N807 N808 120.4(8) . . ? C806 N807 Co8 117.9(6) . . ? N808 N807 Co8 121.2(5) . . ? C809 N808 N807 114.7(7) . . ? C809 N808 C829 124.6(7) . . ? N807 N808 C829 120.6(7) . . ? N808 C809 N822 116.5(7) . . ? N808 C809 C810 123.2(8) . . ? N822 C809 C810 120.2(7) . . ? C811 C810 C809 116.6(8) . . ? C811 C810 H810 121.7 . . ? C809 C810 H810 121.7 . . ? N820 C811 C810 123.5(7) . . ? N820 C811 N812 115.8(7) . . ? C810 C811 N812 120.5(8) . . ? N813 N812 C811 115.2(7) . . ? N813 N812 C830 120.2(7) . . ? C811 N812 C830 124.4(7) . . ? C814 N813 N812 123.2(8) . . ? C814 N813 Co5 117.1(7) . . ? N812 N813 Co5 119.5(5) . . ? N813 C814 C815 113.0(9) . . ? N813 C814 H814 123.5 . . ? C815 C814 H814 123.5 . . ? N816 C815 N819 109.9(10) . . ? N816 C815 C814 128.4(10) . . ? N819 C815 C814 121.7(8) . . ? C815 N816 C817 108.5(10) . . ? C815 N816 H816 125.7 . . ? C817 N816 H816 125.7 . . ? C818 C817 N816 105.6(11) . . ? C818 C817 H817 127.2 . . ? N816 C817 H817 127.2 . . ? C817 C818 N819 108.7(12) . . ? C817 C818 H818 125.6 . . ? N819 C818 H818 125.6 . . ? C815 N819 C818 107.2(8) . . ? C815 N819 Co5 110.7(6) . . ? C818 N819 Co5 142.0(8) . . ? C821 N820 C811 116.6(7) . . ? C821 N820 Co5 126.7(5) . . ? C811 N820 Co5 116.4(5) . . ? N822 C821 N820 125.0(7) . . ? N822 C821 C823 117.5(6) . . ? N820 C821 C823 117.3(7) . . ? C821 N822 C809 117.9(6) . . ? C821 N822 Co8 127.1(5) . . ? C809 N822 Co8 114.7(5) . . ? C824 C823 C828 120.1(8) . . ? C824 C823 C821 120.8(8) . . ? C828 C823 C821 119.2(8) . . ? C823 C824 C825 119.1(10) . . ? C823 C824 H824 120.4 . . ? C825 C824 H824 120.4 . . ? C826 C825 C824 120.3(11) . . ? C826 C825 H825 119.8 . . ? C824 C825 H825 119.8 . . ? C827 C826 C825 118.9(11) . . ? C827 C826 H826 120.5 . . ? C825 C826 H826 120.5 . . ? C826 C827 C828 122.2(11) . . ? C826 C827 H827 118.9 . . ? C828 C827 H827 118.9 . . ? C823 C828 C827 119.3(10) . . ? C823 C828 H828 120.3 . . ? C827 C828 H828 120.3 . . ? N808 C829 H82A 109.5 . . ? N808 C829 H82B 109.5 . . ? H82A C829 H82B 109.5 . . ? N808 C829 H82C 109.5 . . ? H82A C829 H82C 109.5 . . ? H82B C829 H82C 109.5 . . ? N812 C830 H83A 109.5 . . ? N812 C830 H83B 109.5 . . ? H83A C830 H83B 109.5 . . ? N812 C830 H83C 109.5 . . ? H83A C830 H83C 109.5 . . ? H83B C830 H83C 109.5 . . ? O12 S1 O13 118.2(6) . . ? O12 S1 O11 116.7(8) . . ? O13 S1 O11 111.4(7) . . ? O12 S1 C1 102.2(9) . . ? O13 S1 C1 102.5(8) . . ? O11 S1 C1 102.8(6) . . ? F11 C1 F13 107.3(14) . . ? F11 C1 F12 106.3(15) . . ? F13 C1 F12 109.2(13) . . ? F11 C1 S1 114.8(11) . . ? F13 C1 S1 110.0(13) . . ? F12 C1 S1 109.2(12) . . ? O22 S2 O23 114.4(5) . . ? O22 S2 O21 117.5(5) . . ? O23 S2 O21 112.7(5) . . ? O22 S2 C2 104.5(6) . . ? O23 S2 C2 100.6(8) . . ? O21 S2 C2 104.6(6) . . ? F22 C2 F23 107.1(12) . . ? F22 C2 F21 110.2(15) . . ? F23 C2 F21 102.7(12) . . ? F22 C2 S2 112.3(10) . . ? F23 C2 S2 111.9(13) . . ? F21 C2 S2 112.2(10) . . ? O32 S3 O31 116.7(6) . . ? O32 S3 O33 115.2(5) . . ? O31 S3 O33 113.4(5) . . ? O32 S3 C3 104.4(5) . . ? O31 S3 C3 101.7(6) . . ? O33 S3 C3 102.9(6) . . ? F32 C3 F31 105.5(10) . . ? F32 C3 F33 101.4(11) . . ? F31 C3 F33 100.3(13) . . ? F32 C3 S3 118.7(13) . . ? F31 C3 S3 113.4(9) . . ? F33 C3 S3 115.3(8) . . ? O42 S4 O43 115.8(5) . . ? O42 S4 O41 116.7(5) . . ? O43 S4 O41 114.1(5) . . ? O42 S4 C4 101.8(8) . . ? O43 S4 C4 103.7(8) . . ? O41 S4 C4 101.7(6) . . ? F41 C4 F42 109.2(17) . . ? F41 C4 F43 110.2(17) . . ? F42 C4 F43 105.4(13) . . ? F41 C4 S4 112.5(11) . . ? F42 C4 S4 110.5(15) . . ? F43 C4 S4 108.8(13) . . ? O53 S5 O51 116.5(6) . . ? O53 S5 O52 114.1(6) . . ? O51 S5 O52 114.1(6) . . ? O53 S5 C5 103.8(5) . . ? O51 S5 C5 104.0(5) . . ? O52 S5 C5 102.1(5) . . ? F52 C5 F53 112.2(8) . . ? F52 C5 F51 111.5(8) . . ? F53 C5 F51 111.1(8) . . ? F52 C5 S5 108.1(7) . . ? F53 C5 S5 106.7(7) . . ? F51 C5 S5 106.9(7) . . ? O172 S17 O173 114.8(6) . . ? O172 S17 O171 114.7(6) . . ? O173 S17 O171 114.2(6) . . ? O172 S17 C17 104.2(5) . . ? O173 S17 C17 104.3(5) . . ? O171 S17 C17 102.8(5) . . ? F171 C17 F172 111.6(8) . . ? F171 C17 F173 111.5(8) . . ? F172 C17 F173 110.1(8) . . ? F171 C17 S17 108.8(7) . . ? F172 C17 S17 107.5(7) . . ? F173 C17 S17 107.2(7) . . ? O62 S6 O61 116.2(4) . . ? O62 S6 O63 114.0(4) . . ? O61 S6 O63 115.2(4) . . ? O62 S6 C6 101.5(5) . . ? O61 S6 C6 104.0(5) . . ? O63 S6 C6 103.2(5) . . ? F61 C6 F63 108.4(10) . . ? F61 C6 F62 107.4(10) . . ? F63 C6 F62 106.9(10) . . ? F61 C6 S6 112.2(9) . . ? F63 C6 S6 111.9(8) . . ? F62 C6 S6 109.8(8) . . ? O71 S7 O72 113.5(4) . . ? O71 S7 O73 116.0(4) . . ? O72 S7 O73 114.3(4) . . ? O71 S7 C7 105.0(5) . . ? O72 S7 C7 100.6(5) . . ? O73 S7 C7 105.3(4) . . ? F71 C7 F73 113.3(10) . . ? F71 C7 F72 101.7(9) . . ? F73 C7 F72 102.9(8) . . ? F71 C7 S7 114.2(7) . . ? F73 C7 S7 114.5(7) . . ? F72 C7 S7 108.6(8) . . ? O83 S8 O82 115.5(5) . . ? O83 S8 O81 115.3(5) . . ? O82 S8 O81 112.9(6) . . ? O83 S8 C8 101.8(6) . . ? O82 S8 C8 104.6(7) . . ? O81 S8 C8 104.7(6) . . ? F81 C8 F82 109.5(13) . . ? F81 C8 F83 108.3(11) . . ? F82 C8 F83 109.1(12) . . ? F81 C8 S8 110.7(10) . . ? F82 C8 S8 110.1(9) . . ? F83 C8 S8 109.0(11) . . ? O92 S9 O93 117.4(7) . . ? O92 S9 O91 114.8(7) . . ? O93 S9 O91 113.2(7) . . ? O92 S9 C9 104.4(6) . . ? O93 S9 C9 103.3(6) . . ? O91 S9 C9 101.0(6) . . ? F91 C9 F93 111.7(8) . . ? F91 C9 F92 112.2(8) . . ? F93 C9 F92 110.5(8) . . ? F91 C9 S9 107.8(7) . . ? F93 C9 S9 107.4(7) . . ? F92 C9 S9 107.0(7) . . ? O181 S18 O183 116.4(6) . . ? O181 S18 O182 113.9(6) . . ? O183 S18 O182 113.3(6) . . ? O181 S18 C18 104.8(5) . . ? O183 S18 C18 104.2(5) . . ? O182 S18 C18 102.4(5) . . ? F182 C18 F183 111.8(8) . . ? F182 C18 F181 111.3(8) . . ? F183 C18 F181 110.1(7) . . ? F182 C18 S18 108.3(6) . . ? F183 C18 S18 107.7(6) . . ? F181 C18 S18 107.3(6) . . ? O103 S10 O101 117.7(5) . . ? O103 S10 O102 113.0(5) . . ? O101 S10 O102 113.8(5) . . ? O103 S10 C10 106.3(4) . . ? O101 S10 C10 102.7(4) . . ? O102 S10 C10 100.9(5) . . ? F103 C10 F101 110.5(7) . . ? F103 C10 F102 106.3(8) . . ? F101 C10 F102 98.4(8) . . ? F103 C10 S10 115.9(7) . . ? F101 C10 S10 112.8(6) . . ? F102 C10 S10 111.3(6) . . ? O112 S11 O111 116.5(5) . . ? O112 S11 O113 109.7(5) . . ? O111 S11 O113 118.6(5) . . ? O112 S11 C11 104.0(5) . . ? O111 S11 C11 103.3(5) . . ? O113 S11 C11 102.3(5) . . ? F112 C11 F111 107.4(10) . . ? F112 C11 F113 109.1(11) . . ? F111 C11 F113 106.7(10) . . ? F112 C11 S11 112.0(9) . . ? F111 C11 S11 110.9(8) . . ? F113 C11 S11 110.5(8) . . ? O122 S12 O123 115.3(7) . . ? O122 S12 O121 115.7(7) . . ? O123 S12 O121 115.2(7) . . ? O122 S12 C12 103.2(6) . . ? O123 S12 C12 103.1(6) . . ? O121 S12 C12 101.4(6) . . ? F121 C12 F122 112.6(8) . . ? F121 C12 F123 111.9(8) . . ? F122 C12 F123 110.9(8) . . ? F121 C12 S12 107.8(7) . . ? F122 C12 S12 106.5(7) . . ? F123 C12 S12 106.8(7) . . ? O191 S19 O193 116.6(7) . . ? O191 S19 O192 115.7(7) . . ? O193 S19 O192 112.6(6) . . ? O191 S19 C19 105.1(6) . . ? O193 S19 C19 102.4(6) . . ? O192 S19 C19 101.9(5) . . ? F193 C19 F191 111.8(8) . . ? F193 C19 F192 111.3(8) . . ? F191 C19 F192 110.9(8) . . ? F193 C19 S19 108.4(7) . . ? F191 C19 S19 107.1(7) . . ? F192 C19 S19 107.2(7) . . ? O133 S13 O131 115.3(4) . . ? O133 S13 O132 115.2(5) . . ? O131 S13 O132 114.9(4) . . ? O133 S13 C13 102.6(5) . . ? O131 S13 C13 103.4(5) . . ? O132 S13 C13 102.8(5) . . ? F133 C13 F132 109.0(11) . . ? F133 C13 F131 107.0(10) . . ? F132 C13 F131 107.4(11) . . ? F133 C13 S13 111.6(9) . . ? F132 C13 S13 111.9(8) . . ? F131 C13 S13 109.8(9) . . ? O141 S14 O142 112.7(6) . . ? O141 S14 O143 113.3(6) . . ? O142 S14 O143 116.3(5) . . ? O141 S14 C14 104.9(8) . . ? O142 S14 C14 103.7(8) . . ? O143 S14 C14 104.5(6) . . ? F141 C14 F143 113.2(14) . . ? F141 C14 F142 104.4(13) . . ? F143 C14 F142 104.9(13) . . ? F141 C14 S14 115.5(11) . . ? F143 C14 S14 109.7(11) . . ? F142 C14 S14 108.3(11) . . ? O151 S15 O153 117.1(4) . . ? O151 S15 O152 112.3(4) . . ? O153 S15 O152 111.9(4) . . ? O151 S15 C15 106.7(4) . . ? O153 S15 C15 105.7(4) . . ? O152 S15 C15 101.5(4) . . ? F153 C15 F151 113.9(6) . . ? F153 C15 F152 107.4(6) . . ? F151 C15 F152 107.4(6) . . ? F153 C15 S15 110.6(5) . . ? F151 C15 S15 110.6(5) . . ? F152 C15 S15 106.6(5) . . ? O161 S16 O163 117.7(8) . . ? O161 S16 O162 113.5(7) . . ? O163 S16 O162 116.5(7) . . ? O161 S16 C16 104.6(6) . . ? O163 S16 C16 99.7(7) . . ? O162 S16 C16 101.4(6) . . ? F162 C16 F161 110.4(10) . . ? F162 C16 F163 104.1(11) . . ? F161 C16 F163 105.5(12) . . ? F162 C16 S16 113.7(10) . . ? F161 C16 S16 112.9(10) . . ? F163 C16 S16 109.5(9) . . ? N1 C1A C1B 175.0(16) . . ? C1A C1B H1BA 109.5 . . ? C1A C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? C1A C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? N2 C2A C2B 179.3(13) . . ? C2A C2B H2BA 109.5 . . ? C2A C2B H2BB 109.5 . . ? H2BA C2B H2BB 109.5 . . ? C2A C2B H2BC 109.5 . . ? H2BA C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? N3 C3A C3B 178.5(18) . . ? C3A C3B H3BA 109.5 . . ? C3A C3B H3BB 109.5 . . ? H3BA C3B H3BB 109.5 . . ? C3A C3B H3BC 109.5 . . ? H3BA C3B H3BC 109.5 . . ? H3BB C3B H3BC 109.5 . . ? N4 C4A C4B 176(2) . . ? C4A C4B H4BA 109.5 . . ? C4A C4B H4BB 109.5 . . ? H4BA C4B H4BB 109.5 . . ? C4A C4B H4BC 109.5 . . ? H4BA C4B H4BC 109.5 . . ? H4BB C4B H4BC 109.5 . . ? N5 C5A C5B 179(2) . . ? C5A C5B H5BA 109.5 . . ? C5A C5B H5BB 109.5 . . ? H5BA C5B H5BB 109.5 . . ? C5A C5B H5BC 109.5 . . ? H5BA C5B H5BC 109.5 . . ? H5BB C5B H5BC 109.5 . . ? N6 C6A C6B 177.0(14) . . ? C6A C6B H6BA 109.5 . . ? C6A C6B H6BB 109.5 . . ? H6BA C6B H6BB 109.5 . . ? C6A C6B H6BC 109.5 . . ? H6BA C6B H6BC 109.5 . . ? H6BB C6B H6BC 109.5 . . ? N7 C7A C7B 174.8(18) . . ? C7A C7B H7BA 109.5 . . ? C7A C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C7A C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N8 C8A C8B 171(3) . . ? C8A C8B H8BA 109.5 . . ? C8A C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? C8A C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? N9 C9A C9B 174(2) . . ? C9A C9B H9BA 109.5 . . ? C9A C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C9A C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? N10 C10A C10B 173(2) . . ? C10A C10B H10A 109.5 . . ? C10A C10B H10B 109.5 . . ? H10A C10B H10B 109.5 . . ? C10A C10B H10C 109.5 . . ? H10A C10B H10C 109.5 . . ? H10B C10B H10C 109.5 . . ? N11 C11A C11B 180(3) . . ? C11A C11B H11A 109.5 . . ? C11A C11B H11B 109.5 . . ? H11A C11B H11B 109.5 . . ? C11A C11B H11C 109.5 . . ? H11A C11B H11C 109.5 . . ? H11B C11B H11C 109.5 . . ? N12 C12A C12B 177(3) . . ? C12A C12B H12D 109.5 . . ? C12A C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C12A C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? N13 C13A C13B 176(3) . . ? C13A C13B H13D 109.5 . . ? C13A C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C13A C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? 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 N107 Co1 N101 C105 0.6(5) . . . . ? N413 Co1 N101 C105 171.4(5) . . . . ? N419 Co1 N101 C105 93.4(6) . . . . ? N420 Co1 N101 C105 -115.0(6) . . . . ? N122 Co1 N101 C105 -4.2(9) . . . . ? N107 Co1 N101 C102 -179.7(10) . . . . ? N413 Co1 N101 C102 -9.0(10) . . . . ? N419 Co1 N101 C102 -86.9(10) . . . . ? N420 Co1 N101 C102 64.7(10) . . . . ? N122 Co1 N101 C102 175.4(8) . . . . ? C105 N101 C102 C103 1.9(10) . . . . ? Co1 N101 C102 C103 -177.8(7) . . . . ? N101 C102 C103 N104 -2.4(11) . . . . ? C102 C103 N104 C105 2.0(11) . . . . ? C102 N101 C105 N104 -0.6(9) . . . . ? Co1 N101 C105 N104 179.1(5) . . . . ? C102 N101 C105 C106 176.8(8) . . . . ? Co1 N101 C105 C106 -3.4(10) . . . . ? C103 N104 C105 N101 -0.8(10) . . . . ? C103 N104 C105 C106 -178.0(9) . . . . ? N101 C105 C106 N107 5.6(11) . . . . ? N104 C105 C106 N107 -177.6(8) . . . . ? C105 C106 N107 N108 -178.4(7) . . . . ? C105 C106 N107 Co1 -4.7(9) . . . . ? N413 Co1 N107 C106 -53.8(15) . . . . ? N419 Co1 N107 C106 -90.1(6) . . . . ? N101 Co1 N107 C106 2.4(6) . . . . ? N420 Co1 N107 C106 89.3(6) . . . . ? N122 Co1 N107 C106 179.9(6) . . . . ? N413 Co1 N107 N108 120.0(13) . . . . ? N419 Co1 N107 N108 83.7(6) . . . . ? N101 Co1 N107 N108 176.2(6) . . . . ? N420 Co1 N107 N108 -97.0(5) . . . . ? N122 Co1 N107 N108 -6.4(5) . . . . ? C106 N107 N108 C109 179.8(7) . . . . ? Co1 N107 N108 C109 6.3(8) . . . . ? C106 N107 N108 C129 2.2(11) . . . . ? Co1 N107 N108 C129 -171.3(6) . . . . ? N107 N108 C109 N122 -0.8(9) . . . . ? C129 N108 C109 N122 176.7(7) . . . . ? N107 N108 C109 C110 -179.4(6) . . . . ? C129 N108 C109 C110 -1.9(12) . . . . ? N122 C109 C110 C111 -0.9(11) . . . . ? N108 C109 C110 C111 177.7(7) . . . . ? C109 C110 C111 N120 1.6(11) . . . . ? C109 C110 C111 N112 -178.4(7) . . . . ? N120 C111 N112 N113 -1.2(10) . . . . ? C110 C111 N112 N113 178.8(7) . . . . ? N120 C111 N112 C130 -175.6(8) . . . . ? C110 C111 N112 C130 4.4(12) . . . . ? C111 N112 N113 C114 -174.1(7) . . . . ? C130 N112 N113 C114 0.5(12) . . . . ? C111 N112 N113 Co2 -0.5(9) . . . . ? C130 N112 N113 Co2 174.1(6) . . . . ? N207 Co2 N113 C114 40.2(15) . . . . ? N119 Co2 N113 C114 -5.8(6) . . . . ? N201 Co2 N113 C114 86.6(7) . . . . ? N222 Co2 N113 C114 -95.9(6) . . . . ? N120 Co2 N113 C114 175.1(7) . . . . ? N207 Co2 N113 N112 -133.6(10) . . . . ? N119 Co2 N113 N112 -179.7(6) . . . . ? N201 Co2 N113 N112 -87.3(6) . . . . ? N222 Co2 N113 N112 90.2(6) . . . . ? N120 Co2 N113 N112 1.2(5) . . . . ? N112 N113 C114 C115 178.7(7) . . . . ? Co2 N113 C114 C115 4.9(10) . . . . ? N113 C114 C115 N116 -178.6(9) . . . . ? N113 C114 C115 N119 0.3(12) . . . . ? N119 C115 N116 C117 -0.1(11) . . . . ? C114 C115 N116 C117 178.9(9) . . . . ? C115 N116 C117 C118 -0.2(11) . . . . ? N116 C117 C118 N119 0.4(10) . . . . ? N116 C115 N119 C118 0.4(10) . . . . ? C114 C115 N119 C118 -178.7(8) . . . . ? N116 C115 N119 Co2 174.2(6) . . . . ? C114 C115 N119 Co2 -4.9(10) . . . . ? C117 C118 N119 C115 -0.5(10) . . . . ? C117 C118 N119 Co2 -170.6(7) . . . . ? N207 Co2 N119 C115 -164.8(6) . . . . ? N113 Co2 N119 C115 5.3(6) . . . . ? N201 Co2 N119 C115 -88.0(6) . . . . ? N222 Co2 N119 C115 122.0(6) . . . . ? N120 Co2 N119 C115 7.0(9) . . . . ? N207 Co2 N119 C118 5.2(9) . . . . ? N113 Co2 N119 C118 175.2(10) . . . . ? N201 Co2 N119 C118 82.0(9) . . . . ? N222 Co2 N119 C118 -68.0(9) . . . . ? N120 Co2 N119 C118 177.0(8) . . . . ? N112 C111 N120 C121 177.4(7) . . . . ? C110 C111 N120 C121 -2.6(11) . . . . ? N112 C111 N120 Co2 2.2(9) . . . . ? C110 C111 N120 Co2 -177.8(6) . . . . ? N207 Co2 N120 C121 -7.2(7) . . . . ? N113 Co2 N120 C121 -176.2(7) . . . . ? N119 Co2 N120 C121 -178.0(6) . . . . ? N201 Co2 N120 C121 -82.1(7) . . . . ? N222 Co2 N120 C121 67.2(7) . . . . ? N207 Co2 N120 C111 167.3(5) . . . . ? N113 Co2 N120 C111 -1.8(5) . . . . ? N119 Co2 N120 C111 -3.5(8) . . . . ? N201 Co2 N120 C111 92.3(6) . . . . ? N222 Co2 N120 C111 -118.3(5) . . . . ? C111 N120 C121 N122 3.2(11) . . . . ? Co2 N120 C121 N122 177.7(5) . . . . ? C111 N120 C121 C123 -174.8(6) . . . . ? Co2 N120 C121 C123 -0.4(10) . . . . ? N120 C121 N122 C109 -2.5(11) . . . . ? C123 C121 N122 C109 175.5(6) . . . . ? N120 C121 N122 Co1 -174.2(5) . . . . ? C123 C121 N122 Co1 3.8(9) . . . . ? C110 C109 N122 C121 1.2(10) . . . . ? N108 C109 N122 C121 -177.4(6) . . . . ? C110 C109 N122 Co1 174.2(6) . . . . ? N108 C109 N122 Co1 -4.4(8) . . . . ? N107 Co1 N122 C121 177.3(6) . . . . ? N413 Co1 N122 C121 7.0(7) . . . . ? N419 Co1 N122 C121 84.0(6) . . . . ? N101 Co1 N122 C121 -177.7(6) . . . . ? N420 Co1 N122 C121 -68.3(6) . . . . ? N107 Co1 N122 C109 5.6(5) . . . . ? N413 Co1 N122 C109 -164.7(5) . . . . ? N419 Co1 N122 C109 -87.7(5) . . . . ? N101 Co1 N122 C109 10.6(8) . . . . ? N420 Co1 N122 C109 119.9(5) . . . . ? N120 C121 C123 C124 -91.3(9) . . . . ? N122 C121 C123 C124 90.4(9) . . . . ? N120 C121 C123 C128 89.2(9) . . . . ? N122 C121 C123 C128 -89.1(9) . . . . ? C128 C123 C124 C125 -1.6(13) . . . . ? C121 C123 C124 C125 178.9(8) . . . . ? C123 C124 C125 C126 1.9(14) . . . . ? C124 C125 C126 C127 -1.1(15) . . . . ? C125 C126 C127 C128 0.1(15) . . . . ? C124 C123 C128 C127 0.6(12) . . . . ? C121 C123 C128 C127 -179.9(7) . . . . ? C126 C127 C128 C123 0.1(13) . . . . ? N207 Co2 N201 C205 1.3(6) . . . . ? N113 Co2 N201 C205 -168.4(6) . . . . ? N119 Co2 N201 C205 -90.9(6) . . . . ? N222 Co2 N201 C205 15.8(9) . . . . ? N120 Co2 N201 C205 118.7(6) . . . . ? N207 Co2 N201 C202 -179.9(12) . . . . ? N113 Co2 N201 C202 10.4(11) . . . . ? N119 Co2 N201 C202 88.0(11) . . . . ? N222 Co2 N201 C202 -165.3(10) . . . . ? N120 Co2 N201 C202 -62.5(11) . . . . ? C205 N201 C202 C203 0.9(12) . . . . ? Co2 N201 C202 C203 -177.9(8) . . . . ? N201 C202 C203 N204 -0.6(14) . . . . ? C202 C203 N204 C205 0.1(13) . . . . ? C202 N201 C205 N204 -0.8(11) . . . . ? Co2 N201 C205 N204 178.4(6) . . . . ? C202 N201 C205 C206 -179.1(9) . . . . ? Co2 N201 C205 C206 0.2(11) . . . . ? C203 N204 C205 N201 0.4(12) . . . . ? C203 N204 C205 C206 178.6(10) . . . . ? N201 C205 C206 N207 -2.5(12) . . . . ? N204 C205 C206 N207 179.6(9) . . . . ? C205 C206 N207 N208 -179.3(7) . . . . ? C205 C206 N207 Co2 3.7(9) . . . . ? N113 Co2 N207 C206 45.0(15) . . . . ? N119 Co2 N207 C206 89.7(6) . . . . ? N201 Co2 N207 C206 -2.9(6) . . . . ? N222 Co2 N207 C206 -175.0(7) . . . . ? N120 Co2 N207 C206 -85.7(6) . . . . ? N113 Co2 N207 N208 -132.0(10) . . . . ? N119 Co2 N207 N208 -87.3(6) . . . . ? N201 Co2 N207 N208 -179.9(6) . . . . ? N222 Co2 N207 N208 8.0(5) . . . . ? N120 Co2 N207 N208 97.3(6) . . . . ? C206 N207 N208 C209 174.6(7) . . . . ? Co2 N207 N208 C209 -8.4(9) . . . . ? C206 N207 N208 C229 -6.9(11) . . . . ? Co2 N207 N208 C229 170.0(6) . . . . ? N207 N208 C209 N222 2.3(10) . . . . ? C229 N208 C209 N222 -176.1(8) . . . . ? N207 N208 C209 C210 -177.2(7) . . . . ? C229 N208 C209 C210 4.4(12) . . . . ? N222 C209 C210 C211 0.3(12) . . . . ? N208 C209 C210 C211 179.7(7) . . . . ? C209 C210 C211 N220 -1.9(12) . . . . ? C209 C210 C211 N212 176.2(7) . . . . ? N220 C211 N212 N213 -7.8(10) . . . . ? C210 C211 N212 N213 174.1(7) . . . . ? N220 C211 N212 C230 172.2(8) . . . . ? C210 C211 N212 C230 -6.0(12) . . . . ? C211 N212 N213 C214 -175.1(8) . . . . ? C230 N212 N213 C214 4.9(11) . . . . ? C211 N212 N213 Co3 12.5(9) . . . . ? C230 N212 N213 Co3 -167.5(6) . . . . ? N307 Co3 N213 C214 -62.5(14) . . . . ? N301 Co3 N213 C214 -91.1(6) . . . . ? N219 Co3 N213 C214 6.0(6) . . . . ? N322 Co3 N213 C214 88.1(7) . . . . ? N220 Co3 N213 C214 178.2(7) . . . . ? N307 Co3 N213 N212 110.1(12) . . . . ? N301 Co3 N213 N212 81.6(6) . . . . ? N219 Co3 N213 N212 178.7(6) . . . . ? N322 Co3 N213 N212 -99.2(6) . . . . ? N220 Co3 N213 N212 -9.2(5) . . . . ? N212 N213 C214 C215 -179.5(7) . . . . ? Co3 N213 C214 C215 -7.1(10) . . . . ? N213 C214 C215 N216 -166.1(8) . . . . ? N213 C214 C215 N219 4.2(12) . . . . ? N219 C215 N216 C217 3.7(10) . . . . ? C214 C215 N216 C217 174.9(9) . . . . ? C215 N216 C217 C218 -2.6(11) . . . . ? N216 C217 C218 N219 0.7(11) . . . . ? N216 C215 N219 C218 -3.3(10) . . . . ? C214 C215 N219 C218 -174.9(8) . . . . ? N216 C215 N219 Co3 172.2(6) . . . . ? C214 C215 N219 Co3 0.6(10) . . . . ? C217 C218 N219 C215 1.5(11) . . . . ? C217 C218 N219 Co3 -171.5(8) . . . . ? N213 Co3 N219 C215 -3.2(6) . . . . ? N307 Co3 N219 C215 165.5(6) . . . . ? N301 Co3 N219 C215 87.0(6) . . . . ? N322 Co3 N219 C215 -121.6(6) . . . . ? N220 Co3 N219 C215 -18.1(9) . . . . ? N213 Co3 N219 C218 169.7(10) . . . . ? N307 Co3 N219 C218 -21.6(10) . . . . ? N301 Co3 N219 C218 -100.1(10) . . . . ? N322 Co3 N219 C218 51.3(10) . . . . ? N220 Co3 N219 C218 154.8(9) . . . . ? N212 C211 N220 C221 -175.5(7) . . . . ? C210 C211 N220 C221 2.6(11) . . . . ? N212 C211 N220 Co3 0.1(9) . . . . ? C210 C211 N220 Co3 178.2(6) . . . . ? N213 Co3 N220 C221 179.6(7) . . . . ? N307 Co3 N220 C221 10.9(7) . . . . ? N301 Co3 N220 C221 88.1(7) . . . . ? N219 Co3 N220 C221 -165.2(6) . . . . ? N322 Co3 N220 C221 -64.0(7) . . . . ? N213 Co3 N220 C211 4.7(5) . . . . ? N307 Co3 N220 C211 -164.0(5) . . . . ? N301 Co3 N220 C211 -86.8(6) . . . . ? N219 Co3 N220 C211 19.9(8) . . . . ? N322 Co3 N220 C211 121.0(5) . . . . ? C211 N220 C221 N222 -1.9(11) . . . . ? Co3 N220 C221 N222 -176.8(5) . . . . ? C211 N220 C221 C223 173.1(7) . . . . ? Co3 N220 C221 C223 -1.8(10) . . . . ? N220 C221 N222 C209 0.5(11) . . . . ? C223 C221 N222 C209 -174.6(7) . . . . ? N220 C221 N222 Co2 176.7(6) . . . . ? C223 C221 N222 Co2 1.6(10) . . . . ? C210 C209 N222 C221 0.4(11) . . . . ? N208 C209 N222 C221 -179.1(7) . . . . ? C210 C209 N222 Co2 -176.4(6) . . . . ? N208 C209 N222 Co2 4.2(9) . . . . ? N207 Co2 N222 C221 177.5(7) . . . . ? N113 Co2 N222 C221 -12.5(7) . . . . ? N119 Co2 N222 C221 -91.3(6) . . . . ? N201 Co2 N222 C221 162.7(6) . . . . ? N120 Co2 N222 C221 61.8(7) . . . . ? N207 Co2 N222 C209 -6.3(5) . . . . ? N113 Co2 N222 C209 163.7(5) . . . . ? N119 Co2 N222 C209 84.9(6) . . . . ? N201 Co2 N222 C209 -21.1(8) . . . . ? N120 Co2 N222 C209 -122.0(6) . . . . ? N220 C221 C223 C224 87.2(10) . . . . ? N222 C221 C223 C224 -97.4(9) . . . . ? N220 C221 C223 C228 -91.8(9) . . . . ? N222 C221 C223 C228 83.7(10) . . . . ? C228 C223 C224 C225 -1.1(13) . . . . ? C221 C223 C224 C225 180.0(8) . . . . ? C223 C224 C225 C226 3.1(15) . . . . ? C224 C225 C226 C227 -4.6(17) . . . . ? C225 C226 C227 C228 4.3(19) . . . . ? C226 C227 C228 C223 -2.5(17) . . . . ? C224 C223 C228 C227 0.8(14) . . . . ? C221 C223 C228 C227 179.7(8) . . . . ? N213 Co3 N301 C305 174.7(6) . . . . ? N307 Co3 N301 C305 0.5(5) . . . . ? N219 Co3 N301 C305 97.3(6) . . . . ? N322 Co3 N301 C305 -3.8(8) . . . . ? N220 Co3 N301 C305 -112.1(6) . . . . ? N213 Co3 N301 C302 -11.6(9) . . . . ? N307 Co3 N301 C302 174.2(9) . . . . ? N219 Co3 N301 C302 -89.0(9) . . . . ? N322 Co3 N301 C302 169.9(7) . . . . ? N220 Co3 N301 C302 61.6(9) . . . . ? C305 N301 C302 C303 0.1(9) . . . . ? Co3 N301 C302 C303 -173.8(7) . . . . ? N301 C302 C303 N304 0.4(10) . . . . ? C302 C303 N304 C305 -0.8(11) . . . . ? C303 N304 C305 N301 0.9(11) . . . . ? C303 N304 C305 C306 179.2(9) . . . . ? C302 N301 C305 N304 -0.6(10) . . . . ? Co3 N301 C305 N304 175.5(6) . . . . ? C302 N301 C305 C306 -179.0(8) . . . . ? Co3 N301 C305 C306 -2.9(10) . . . . ? N304 C305 C306 N307 -173.3(9) . . . . ? N301 C305 C306 N307 4.8(13) . . . . ? C305 C306 N307 N308 -179.8(7) . . . . ? C305 C306 N307 Co3 -4.1(10) . . . . ? N213 Co3 N307 C306 -27.1(16) . . . . ? N301 Co3 N307 C306 2.2(7) . . . . ? N219 Co3 N307 C306 -93.6(7) . . . . ? N322 Co3 N307 C306 180.0(7) . . . . ? N220 Co3 N307 C306 88.4(7) . . . . ? N213 Co3 N307 N308 148.7(10) . . . . ? N301 Co3 N307 N308 178.0(6) . . . . ? N219 Co3 N307 N308 82.2(6) . . . . ? N322 Co3 N307 N308 -4.2(5) . . . . ? N220 Co3 N307 N308 -95.8(5) . . . . ? C306 N307 N308 C309 179.9(8) . . . . ? Co3 N307 N308 C309 4.3(8) . . . . ? C306 N307 N308 C329 2.7(12) . . . . ? Co3 N307 N308 C329 -173.0(6) . . . . ? N307 N308 C309 N322 -0.8(10) . . . . ? C329 N308 C309 N322 176.3(7) . . . . ? N307 N308 C309 C310 -179.3(7) . . . . ? C329 N308 C309 C310 -2.1(12) . . . . ? N322 C309 C310 C311 -0.9(11) . . . . ? N308 C309 C310 C311 177.5(7) . . . . ? C309 C310 C311 N312 -176.0(7) . . . . ? C309 C310 C311 N320 3.6(11) . . . . ? C310 C311 N312 N313 -176.9(7) . . . . ? N320 C311 N312 N313 3.5(9) . . . . ? C310 C311 N312 C330 5.8(11) . . . . ? N320 C311 N312 C330 -173.8(7) . . . . ? C311 N312 N313 C314 180.0(7) . . . . ? C330 N312 N313 C314 -2.7(11) . . . . ? C311 N312 N313 Co4 -6.0(8) . . . . ? C330 N312 N313 Co4 171.3(5) . . . . ? N319 Co4 N313 C314 -1.9(5) . . . . ? N407 Co4 N313 C314 44.1(15) . . . . ? N401 Co4 N313 C314 96.0(6) . . . . ? N320 Co4 N313 C314 179.0(6) . . . . ? N422 Co4 N313 C314 -90.2(5) . . . . ? N319 Co4 N313 N312 -176.3(5) . . . . ? N407 Co4 N313 N312 -130.4(12) . . . . ? N401 Co4 N313 N312 -78.4(5) . . . . ? N320 Co4 N313 N312 4.6(5) . . . . ? N422 Co4 N313 N312 95.3(5) . . . . ? N312 N313 C314 C315 179.1(6) . . . . ? Co4 N313 C314 C315 4.9(8) . . . . ? N313 C314 C315 N316 174.2(8) . . . . ? N313 C314 C315 N319 -6.9(11) . . . . ? N319 C315 N316 C317 -1.2(10) . . . . ? C314 C315 N316 C317 177.8(9) . . . . ? C315 N316 C317 C318 0.4(11) . . . . ? N316 C317 C318 N319 0.5(12) . . . . ? N316 C315 N319 C318 1.4(9) . . . . ? C314 C315 N319 C318 -177.6(7) . . . . ? N316 C315 N319 Co4 -175.8(5) . . . . ? C314 C315 N319 Co4 5.1(9) . . . . ? C317 C318 N319 C315 -1.2(10) . . . . ? C317 C318 N319 Co4 174.2(8) . . . . ? N407 Co4 N319 C315 -173.6(5) . . . . ? N401 Co4 N319 C315 -95.9(6) . . . . ? N313 Co4 N319 C315 -1.7(5) . . . . ? N320 Co4 N319 C315 0.1(9) . . . . ? N422 Co4 N319 C315 113.2(5) . . . . ? N407 Co4 N319 C318 11.2(11) . . . . ? N401 Co4 N319 C318 88.9(11) . . . . ? N313 Co4 N319 C318 -176.9(11) . . . . ? N320 Co4 N319 C318 -175.1(9) . . . . ? N422 Co4 N319 C318 -62.0(11) . . . . ? C310 C311 N320 C321 -5.7(10) . . . . ? N312 C311 N320 C321 173.9(6) . . . . ? C310 C311 N320 Co4 -179.2(6) . . . . ? N312 C311 N320 Co4 0.4(8) . . . . ? N319 Co4 N320 C321 -176.7(6) . . . . ? N407 Co4 N320 C321 -3.6(7) . . . . ? N401 Co4 N320 C321 -77.2(6) . . . . ? N313 Co4 N320 C321 -174.8(6) . . . . ? N422 Co4 N320 C321 71.1(6) . . . . ? N319 Co4 N320 C311 -4.4(8) . . . . ? N407 Co4 N320 C311 168.7(5) . . . . ? N401 Co4 N320 C311 95.1(5) . . . . ? N313 Co4 N320 C311 -2.5(5) . . . . ? N422 Co4 N320 C311 -116.6(5) . . . . ? C311 N320 C321 N322 5.7(10) . . . . ? Co4 N320 C321 N322 178.1(5) . . . . ? C311 N320 C321 C323 -171.4(6) . . . . ? Co4 N320 C321 C323 0.9(9) . . . . ? N320 C321 N322 C309 -3.3(11) . . . . ? C323 C321 N322 C309 173.8(6) . . . . ? N320 C321 N322 Co3 -177.7(5) . . . . ? C323 C321 N322 Co3 -0.6(9) . . . . ? N308 C309 N322 C321 -177.8(6) . . . . ? C310 C309 N322 C321 0.6(10) . . . . ? N308 C309 N322 Co3 -2.7(8) . . . . ? C310 C309 N322 Co3 175.7(6) . . . . ? N213 Co3 N322 C321 4.1(7) . . . . ? N307 Co3 N322 C321 178.0(7) . . . . ? N301 Co3 N322 C321 -177.6(5) . . . . ? N219 Co3 N322 C321 79.2(6) . . . . ? N220 Co3 N322 C321 -70.9(6) . . . . ? N213 Co3 N322 C309 -170.3(5) . . . . ? N307 Co3 N322 C309 3.6(5) . . . . ? N301 Co3 N322 C309 8.0(8) . . . . ? N219 Co3 N322 C309 -95.2(5) . . . . ? N220 Co3 N322 C309 114.7(5) . . . . ? N322 C321 C323 C324 92.3(9) . . . . ? N320 C321 C323 C324 -90.2(9) . . . . ? N322 C321 C323 C328 -84.0(9) . . . . ? N320 C321 C323 C328 93.4(9) . . . . ? C328 C323 C324 C325 -1.2(12) . . . . ? C321 C323 C324 C325 -177.6(8) . . . . ? C323 C324 C325 C326 -0.7(13) . . . . ? C324 C325 C326 C327 1.3(14) . . . . ? C325 C326 C327 C328 0.0(14) . . . . ? C326 C327 C328 C323 -1.9(14) . . . . ? C324 C323 C328 C327 2.5(13) . . . . ? C321 C323 C328 C327 179.1(8) . . . . ? N319 Co4 N401 C405 -90.6(6) . . . . ? N407 Co4 N401 C405 1.5(6) . . . . ? N313 Co4 N401 C405 -169.4(6) . . . . ? N320 Co4 N401 C405 117.6(6) . . . . ? N422 Co4 N401 C405 21.4(9) . . . . ? N319 Co4 N401 C402 108.1(10) . . . . ? N407 Co4 N401 C402 -159.9(10) . . . . ? N313 Co4 N401 C402 29.2(10) . . . . ? N320 Co4 N401 C402 -43.8(10) . . . . ? N422 Co4 N401 C402 -139.9(9) . . . . ? C405 N401 C402 C403 1.4(10) . . . . ? Co4 N401 C402 C403 163.4(8) . . . . ? N401 C402 C403 N404 -0.5(11) . . . . ? C402 C403 N404 C405 -0.6(11) . . . . ? C402 N401 C405 N404 -1.8(10) . . . . ? Co4 N401 C405 N404 -169.8(6) . . . . ? C402 N401 C405 C406 170.1(8) . . . . ? Co4 N401 C405 C406 2.1(10) . . . . ? C403 N404 C405 N401 1.6(10) . . . . ? C403 N404 C405 C406 -169.8(9) . . . . ? N401 C405 C406 N407 -6.5(12) . . . . ? N404 C405 C406 N407 164.1(8) . . . . ? C405 C406 N407 N408 -175.8(7) . . . . ? C405 C406 N407 Co4 7.7(9) . . . . ? N319 Co4 N407 C406 92.8(6) . . . . ? N401 Co4 N407 C406 -5.5(6) . . . . ? N313 Co4 N407 C406 47.9(16) . . . . ? N320 Co4 N407 C406 -84.0(6) . . . . ? N422 Co4 N407 C406 -174.7(6) . . . . ? N319 Co4 N407 N408 -83.8(5) . . . . ? N401 Co4 N407 N408 177.9(6) . . . . ? N313 Co4 N407 N408 -128.6(12) . . . . ? N320 Co4 N407 N408 99.5(5) . . . . ? N422 Co4 N407 N408 8.7(5) . . . . ? C406 N407 N408 C409 171.4(7) . . . . ? Co4 N407 N408 C409 -12.1(9) . . . . ? C406 N407 N408 C429 -2.2(11) . . . . ? Co4 N407 N408 C429 174.2(6) . . . . ? N407 N408 C409 N422 7.9(10) . . . . ? C429 N408 C409 N422 -178.7(7) . . . . ? N407 N408 C409 C410 -173.8(7) . . . . ? C429 N408 C409 C410 -0.4(13) . . . . ? N422 C409 C410 C411 -1.2(12) . . . . ? N408 C409 C410 C411 -179.4(8) . . . . ? C409 C410 C411 N420 1.9(13) . . . . ? C409 C410 C411 N412 178.5(7) . . . . ? C410 C411 N412 N413 -179.7(7) . . . . ? N420 C411 N412 N413 -2.9(10) . . . . ? C410 C411 N412 C430 -2.4(13) . . . . ? N420 C411 N412 C430 174.4(8) . . . . ? C411 N412 N413 C414 -179.5(7) . . . . ? C430 N412 N413 C414 3.0(12) . . . . ? C411 N412 N413 Co1 4.9(9) . . . . ? C430 N412 N413 Co1 -172.5(6) . . . . ? N107 Co1 N413 C414 -34.0(16) . . . . ? N419 Co1 N413 C414 3.2(6) . . . . ? N101 Co1 N413 C414 -88.7(6) . . . . ? N420 Co1 N413 C414 -179.5(7) . . . . ? N122 Co1 N413 C414 88.9(6) . . . . ? N107 Co1 N413 N412 141.9(12) . . . . ? N419 Co1 N413 N412 179.1(6) . . . . ? N101 Co1 N413 N412 87.1(6) . . . . ? N420 Co1 N413 N412 -3.7(5) . . . . ? N122 Co1 N413 N412 -95.2(6) . . . . ? N412 N413 C414 C415 -179.5(7) . . . . ? Co1 N413 C414 C415 -3.8(9) . . . . ? N413 C414 C415 N416 -179.3(9) . . . . ? N413 C414 C415 N419 2.3(12) . . . . ? N419 C415 N416 C417 -0.3(11) . . . . ? C414 C415 N416 C417 -178.9(9) . . . . ? C415 N416 C417 C418 0.2(12) . . . . ? N416 C417 C418 N419 0.0(12) . . . . ? N416 C415 N419 C418 0.3(11) . . . . ? C414 C415 N419 C418 179.0(8) . . . . ? N416 C415 N419 Co1 -178.4(6) . . . . ? C414 C415 N419 Co1 0.4(10) . . . . ? C417 C418 N419 C415 -0.2(11) . . . . ? C417 C418 N419 Co1 177.8(8) . . . . ? N107 Co1 N419 C415 171.6(6) . . . . ? N413 Co1 N419 C415 -1.7(6) . . . . ? N101 Co1 N419 C415 93.7(6) . . . . ? N420 Co1 N419 C415 -7.2(10) . . . . ? N122 Co1 N419 C415 -115.9(6) . . . . ? N107 Co1 N419 C418 -6.4(11) . . . . ? N413 Co1 N419 C418 -179.7(11) . . . . ? N101 Co1 N419 C418 -84.2(11) . . . . ? N420 Co1 N419 C418 174.8(9) . . . . ? N122 Co1 N419 C418 66.2(11) . . . . ? C410 C411 N420 C421 0.7(11) . . . . ? N412 C411 N420 C421 -176.1(7) . . . . ? C410 C411 N420 Co1 176.6(6) . . . . ? N412 C411 N420 Co1 -0.2(9) . . . . ? N107 Co1 N420 C421 4.2(7) . . . . ? N413 Co1 N420 C421 177.3(7) . . . . ? N419 Co1 N420 C421 -177.1(6) . . . . ? N101 Co1 N420 C421 81.7(7) . . . . ? N122 Co1 N420 C421 -70.2(7) . . . . ? N107 Co1 N420 C411 -171.1(5) . . . . ? N413 Co1 N420 C411 2.0(5) . . . . ? N419 Co1 N420 C411 7.6(9) . . . . ? N101 Co1 N420 C411 -93.5(6) . . . . ? N122 Co1 N420 C411 114.6(6) . . . . ? C411 N420 C421 N422 -4.5(11) . . . . ? Co1 N420 C421 N422 -179.7(6) . . . . ? C411 N420 C421 C423 171.8(7) . . . . ? Co1 N420 C421 C423 -3.4(10) . . . . ? N420 C421 N422 C409 5.2(11) . . . . ? C423 C421 N422 C409 -171.0(7) . . . . ? N420 C421 N422 Co4 -178.4(5) . . . . ? C423 C421 N422 Co4 5.4(10) . . . . ? N408 C409 N422 C421 176.2(7) . . . . ? C410 C409 N422 C421 -2.1(11) . . . . ? N408 C409 N422 Co4 -0.6(9) . . . . ? C410 C409 N422 Co4 -178.9(6) . . . . ? N319 Co4 N422 C421 -87.5(7) . . . . ? N407 Co4 N422 C421 179.4(7) . . . . ? N401 Co4 N422 C421 159.0(6) . . . . ? N313 Co4 N422 C421 -9.0(7) . . . . ? N320 Co4 N422 C421 66.5(7) . . . . ? N319 Co4 N422 C409 88.9(6) . . . . ? N407 Co4 N422 C409 -4.1(5) . . . . ? N401 Co4 N422 C409 -24.5(8) . . . . ? N313 Co4 N422 C409 167.4(5) . . . . ? N320 Co4 N422 C409 -117.1(5) . . . . ? N422 C421 C423 C424 -92.3(9) . . . . ? N420 C421 C423 C424 91.1(9) . . . . ? N422 C421 C423 C428 87.3(9) . . . . ? N420 C421 C423 C428 -89.2(8) . . . . ? C428 C423 C424 C425 0.0(11) . . . . ? C421 C423 C424 C425 179.6(7) . . . . ? C423 C424 C425 C426 -0.2(13) . . . . ? C424 C425 C426 C427 0.2(14) . . . . ? C425 C426 C427 C428 0.0(14) . . . . ? C426 C427 C428 C423 -0.3(12) . . . . ? C424 C423 C428 C427 0.3(11) . . . . ? C421 C423 C428 C427 -179.4(7) . . . . ? N813 Co5 N501 C505 -165.0(6) . . . . ? N507 Co5 N501 C505 3.2(5) . . . . ? N819 Co5 N501 C505 -87.1(6) . . . . ? N820 Co5 N501 C505 122.3(6) . . . . ? N522 Co5 N501 C505 21.8(8) . . . . ? N813 Co5 N501 C502 21.3(10) . . . . ? N507 Co5 N501 C502 -170.5(10) . . . . ? N819 Co5 N501 C502 99.2(10) . . . . ? N820 Co5 N501 C502 -51.4(10) . . . . ? N522 Co5 N501 C502 -151.9(9) . . . . ? C505 N501 C502 C503 -0.4(10) . . . . ? Co5 N501 C502 C503 173.4(7) . . . . ? N501 C502 C503 N504 0.7(11) . . . . ? C502 C503 N504 C505 -0.7(11) . . . . ? C502 N501 C505 N504 0.0(10) . . . . ? Co5 N501 C505 N504 -176.0(5) . . . . ? C502 N501 C505 C506 175.8(8) . . . . ? Co5 N501 C505 C506 -0.2(10) . . . . ? C503 N504 C505 N501 0.4(10) . . . . ? C503 N504 C505 C506 -175.1(9) . . . . ? N501 C505 C506 N507 -5.2(12) . . . . ? N504 C505 C506 N507 169.9(8) . . . . ? C505 C506 N507 N508 -178.5(7) . . . . ? C505 C506 N507 Co5 8.0(9) . . . . ? N813 Co5 N507 C506 55.0(13) . . . . ? N819 Co5 N507 C506 90.9(6) . . . . ? N501 Co5 N507 C506 -6.4(6) . . . . ? N820 Co5 N507 C506 -86.8(6) . . . . ? N522 Co5 N507 C506 -176.1(6) . . . . ? N813 Co5 N507 N508 -118.8(11) . . . . ? N819 Co5 N507 N508 -82.9(6) . . . . ? N501 Co5 N507 N508 179.8(6) . . . . ? N820 Co5 N507 N508 99.4(5) . . . . ? N522 Co5 N507 N508 10.1(5) . . . . ? C506 N507 N508 C509 174.3(7) . . . . ? Co5 N507 N508 C509 -12.3(8) . . . . ? C506 N507 N508 C529 -0.3(11) . . . . ? Co5 N507 N508 C529 173.1(6) . . . . ? N507 N508 C509 N522 5.9(9) . . . . ? C529 N508 C509 N522 -179.9(7) . . . . ? N507 N508 C509 C510 -176.8(7) . . . . ? C529 N508 C509 C510 -2.5(11) . . . . ? N522 C509 C510 C511 -2.9(11) . . . . ? N508 C509 C510 C511 179.9(6) . . . . ? C509 C510 C511 N512 179.7(7) . . . . ? C509 C510 C511 N520 1.4(11) . . . . ? N520 C511 N512 N513 5.0(9) . . . . ? C510 C511 N512 N513 -173.4(6) . . . . ? N520 C511 N512 C530 177.8(7) . . . . ? C510 C511 N512 C530 -0.5(12) . . . . ? C511 N512 N513 C514 171.3(7) . . . . ? C530 N512 N513 C514 -1.9(11) . . . . ? C511 N512 N513 Co6 -0.9(8) . . . . ? C530 N512 N513 Co6 -174.2(5) . . . . ? N601 Co6 N513 C514 -90.5(6) . . . . ? N607 Co6 N513 C514 -35.8(14) . . . . ? N519 Co6 N513 C514 5.2(6) . . . . ? N622 Co6 N513 C514 95.6(6) . . . . ? N520 Co6 N513 C514 -174.5(6) . . . . ? N601 Co6 N513 N512 82.2(5) . . . . ? N607 Co6 N513 N512 136.9(10) . . . . ? N519 Co6 N513 N512 177.9(6) . . . . ? N622 Co6 N513 N512 -91.7(5) . . . . ? N520 Co6 N513 N512 -1.8(5) . . . . ? N512 N513 C514 C515 -177.5(7) . . . . ? Co6 N513 C514 C515 -4.9(9) . . . . ? N513 C514 C515 N519 0.8(12) . . . . ? N513 C514 C515 N516 177.6(8) . . . . ? N519 C515 N516 C517 0.5(11) . . . . ? C514 C515 N516 C517 -176.6(9) . . . . ? C515 N516 C517 C518 -1.6(11) . . . . ? N516 C517 C518 N519 2.2(11) . . . . ? N516 C515 N519 C518 0.9(10) . . . . ? C514 C515 N519 C518 178.1(8) . . . . ? N516 C515 N519 Co6 -173.8(6) . . . . ? C514 C515 N519 Co6 3.4(10) . . . . ? C517 C518 N519 C515 -1.9(10) . . . . ? C517 C518 N519 Co6 169.2(8) . . . . ? N513 Co6 N519 C515 -4.3(6) . . . . ? N601 Co6 N519 C515 89.7(6) . . . . ? N607 Co6 N519 C515 166.7(6) . . . . ? N622 Co6 N519 C515 -120.3(6) . . . . ? N520 Co6 N519 C515 -3.9(9) . . . . ? N513 Co6 N519 C518 -175.3(11) . . . . ? N601 Co6 N519 C518 -81.3(10) . . . . ? N607 Co6 N519 C518 -4.3(10) . . . . ? N622 Co6 N519 C518 68.7(10) . . . . ? N520 Co6 N519 C518 -174.8(9) . . . . ? N512 C511 N520 C521 -175.9(6) . . . . ? C510 C511 N520 C521 2.5(10) . . . . ? N512 C511 N520 Co6 -6.4(8) . . . . ? C510 C511 N520 Co6 172.0(5) . . . . ? N513 Co6 N520 C521 172.3(6) . . . . ? N601 Co6 N520 C521 75.5(6) . . . . ? N607 Co6 N520 C521 2.5(7) . . . . ? N519 Co6 N520 C521 171.8(6) . . . . ? N622 Co6 N520 C521 -72.1(6) . . . . ? N513 Co6 N520 C511 4.2(5) . . . . ? N601 Co6 N520 C511 -92.5(5) . . . . ? N607 Co6 N520 C511 -165.6(4) . . . . ? N519 Co6 N520 C511 3.8(8) . . . . ? N622 Co6 N520 C511 119.8(5) . . . . ? C511 N520 C521 N522 -5.4(10) . . . . ? Co6 N520 C521 N522 -173.2(5) . . . . ? C511 N520 C521 C523 171.1(6) . . . . ? Co6 N520 C521 C523 3.3(9) . . . . ? N520 C521 N522 C509 4.0(10) . . . . ? C523 C521 N522 C509 -172.4(6) . . . . ? N520 C521 N522 Co5 178.4(5) . . . . ? C523 C521 N522 Co5 2.0(9) . . . . ? C510 C509 N522 C521 0.4(10) . . . . ? N508 C509 N522 C521 177.8(6) . . . . ? C510 C509 N522 Co5 -174.7(6) . . . . ? N508 C509 N522 Co5 2.6(8) . . . . ? N813 Co5 N522 C521 -12.4(7) . . . . ? N507 Co5 N522 C521 179.1(6) . . . . ? N819 Co5 N522 C521 -89.9(6) . . . . ? N501 Co5 N522 C521 160.1(6) . . . . ? N820 Co5 N522 C521 62.3(6) . . . . ? N813 Co5 N522 C509 162.1(5) . . . . ? N507 Co5 N522 C509 -6.5(5) . . . . ? N819 Co5 N522 C509 84.5(5) . . . . ? N501 Co5 N522 C509 -25.4(7) . . . . ? N820 Co5 N522 C509 -123.2(5) . . . . ? N520 C521 C523 C528 -96.2(9) . . . . ? N522 C521 C523 C528 80.6(9) . . . . ? N520 C521 C523 C524 83.1(9) . . . . ? N522 C521 C523 C524 -100.1(9) . . . . ? C528 C523 C524 C525 1.3(12) . . . . ? C521 C523 C524 C525 -178.0(8) . . . . ? C523 C524 C525 C526 -0.1(14) . . . . ? C524 C525 C526 C527 -0.1(14) . . . . ? C525 C526 C527 C528 -0.9(14) . . . . ? C524 C523 C528 C527 -2.3(12) . . . . ? C521 C523 C528 C527 177.0(8) . . . . ? C526 C527 C528 C523 2.1(13) . . . . ? N513 Co6 N601 C605 160.2(6) . . . . ? N607 Co6 N601 C605 -8.2(6) . . . . ? N519 Co6 N601 C605 81.6(6) . . . . ? N622 Co6 N601 C605 -30.0(8) . . . . ? N520 Co6 N601 C605 -127.3(6) . . . . ? N513 Co6 N601 C602 -15.0(10) . . . . ? N607 Co6 N601 C602 176.5(10) . . . . ? N519 Co6 N601 C602 -93.6(9) . . . . ? N622 Co6 N601 C602 154.7(8) . . . . ? N520 Co6 N601 C602 57.4(9) . . . . ? C605 N601 C602 C603 0.1(10) . . . . ? Co6 N601 C602 C603 175.5(7) . . . . ? N601 C602 C603 N604 0.4(11) . . . . ? C602 C603 N604 C605 -0.8(11) . . . . ? C602 N601 C605 N604 -0.6(10) . . . . ? Co6 N601 C605 N604 -177.6(5) . . . . ? C602 N601 C605 C606 -176.1(7) . . . . ? Co6 N601 C605 C606 6.9(10) . . . . ? C603 N604 C605 N601 0.9(10) . . . . ? C603 N604 C605 C606 175.9(8) . . . . ? N601 C605 C606 N607 1.0(11) . . . . ? N604 C605 C606 N607 -173.5(8) . . . . ? C605 C606 N607 N608 178.1(7) . . . . ? C605 C606 N607 Co6 -8.7(9) . . . . ? N513 Co6 N607 C606 -46.9(13) . . . . ? N601 Co6 N607 C606 9.6(5) . . . . ? N519 Co6 N607 C606 -86.9(6) . . . . ? N622 Co6 N607 C606 177.6(6) . . . . ? N520 Co6 N607 C606 87.9(6) . . . . ? N513 Co6 N607 N608 126.6(10) . . . . ? N601 Co6 N607 N608 -176.9(6) . . . . ? N519 Co6 N607 N608 86.6(5) . . . . ? N622 Co6 N607 N608 -8.9(5) . . . . ? N520 Co6 N607 N608 -98.5(5) . . . . ? C606 N607 N608 C609 -173.8(7) . . . . ? Co6 N607 N608 C609 13.2(8) . . . . ? C606 N607 N608 C629 -1.4(11) . . . . ? Co6 N607 N608 C629 -174.4(6) . . . . ? N607 N608 C609 N622 -9.9(10) . . . . ? C629 N608 C609 N622 178.0(7) . . . . ? N607 N608 C609 C610 170.8(7) . . . . ? C629 N608 C609 C610 -1.3(12) . . . . ? N608 C609 C610 C611 179.1(7) . . . . ? N622 C609 C610 C611 -0.2(12) . . . . ? C609 C610 C611 N620 0.1(13) . . . . ? C609 C610 C611 N612 -178.4(8) . . . . ? N620 C611 N612 N613 -3.1(12) . . . . ? C610 C611 N612 N613 175.5(8) . . . . ? N620 C611 N612 C630 -178.2(9) . . . . ? C610 C611 N612 C630 0.4(15) . . . . ? C611 N612 N613 C614 -177.3(9) . . . . ? C630 N612 N613 C614 -2.0(14) . . . . ? C611 N612 N613 Co7 0.1(11) . . . . ? C630 N612 N613 Co7 175.4(7) . . . . ? N707 Co7 N613 C614 29.4(19) . . . . ? N619 Co7 N613 C614 -0.9(7) . . . . ? N701 Co7 N613 C614 94.0(8) . . . . ? N722 Co7 N613 C614 -89.4(8) . . . . ? N620 Co7 N613 C614 179.2(8) . . . . ? N707 Co7 N613 N612 -148.1(13) . . . . ? N619 Co7 N613 N612 -178.5(7) . . . . ? N701 Co7 N613 N612 -83.5(7) . . . . ? N722 Co7 N613 N612 93.1(7) . . . . ? N620 Co7 N613 N612 1.7(6) . . . . ? N612 N613 C614 C615 179.4(9) . . . . ? Co7 N613 C614 C615 1.9(12) . . . . ? N613 C614 C615 N616 179.2(10) . . . . ? N613 C614 C615 N619 -2.4(15) . . . . ? N619 C615 N616 C617 2.7(12) . . . . ? C614 C615 N616 C617 -178.8(11) . . . . ? C615 N616 C617 C618 -2.3(12) . . . . ? N616 C617 C618 N619 1.2(12) . . . . ? N616 C615 N619 C618 -2.0(12) . . . . ? C614 C615 N619 C618 179.4(9) . . . . ? N616 C615 N619 Co7 -179.8(7) . . . . ? C614 C615 N619 Co7 1.6(12) . . . . ? C617 C618 N619 C615 0.4(11) . . . . ? C617 C618 N619 Co7 177.0(8) . . . . ? N707 Co7 N619 C615 -174.7(7) . . . . ? N613 Co7 N619 C615 -0.4(7) . . . . ? N701 Co7 N619 C615 -96.8(7) . . . . ? N722 Co7 N619 C615 112.3(7) . . . . ? N620 Co7 N619 C615 -0.2(10) . . . . ? N707 Co7 N619 C618 8.9(11) . . . . ? N613 Co7 N619 C618 -176.8(11) . . . . ? N701 Co7 N619 C618 86.7(11) . . . . ? N722 Co7 N619 C618 -64.2(11) . . . . ? N620 Co7 N619 C618 -176.6(9) . . . . ? N612 C611 N620 C621 177.7(7) . . . . ? C610 C611 N620 C621 -0.9(12) . . . . ? N612 C611 N620 Co7 4.4(10) . . . . ? C610 C611 N620 Co7 -174.1(6) . . . . ? N707 Co7 N620 C621 -1.8(8) . . . . ? N613 Co7 N620 C621 -175.4(7) . . . . ? N619 Co7 N620 C621 -175.6(6) . . . . ? N701 Co7 N620 C621 -76.7(7) . . . . ? N722 Co7 N620 C621 73.0(7) . . . . ? N707 Co7 N620 C611 170.4(6) . . . . ? N613 Co7 N620 C611 -3.2(6) . . . . ? N619 Co7 N620 C611 -3.4(10) . . . . ? N701 Co7 N620 C611 95.5(6) . . . . ? N722 Co7 N620 C611 -114.7(6) . . . . ? C611 N620 C621 N622 1.9(12) . . . . ? Co7 N620 C621 N622 174.1(5) . . . . ? C611 N620 C621 C623 -173.6(7) . . . . ? Co7 N620 C621 C623 -1.4(10) . . . . ? N620 C621 N622 C609 -2.0(11) . . . . ? C623 C621 N622 C609 173.5(7) . . . . ? N620 C621 N622 Co6 177.1(6) . . . . ? C623 C621 N622 Co6 -7.4(10) . . . . ? N608 C609 N622 C621 -178.3(6) . . . . ? C610 C609 N622 C621 1.0(11) . . . . ? N608 C609 N622 Co6 2.5(9) . . . . ? C610 C609 N622 Co6 -178.2(6) . . . . ? N513 Co6 N622 C621 14.9(7) . . . . ? N601 Co6 N622 C621 -153.6(6) . . . . ? N607 Co6 N622 C621 -175.9(7) . . . . ? N519 Co6 N622 C621 94.4(6) . . . . ? N520 Co6 N622 C621 -59.7(6) . . . . ? N513 Co6 N622 C609 -166.0(5) . . . . ? N601 Co6 N622 C609 25.4(8) . . . . ? N607 Co6 N622 C609 3.2(5) . . . . ? N519 Co6 N622 C609 -86.5(5) . . . . ? N520 Co6 N622 C609 119.4(5) . . . . ? N620 C621 C623 C628 96.1(8) . . . . ? N622 C621 C623 C628 -79.8(9) . . . . ? N620 C621 C623 C624 -79.7(9) . . . . ? N622 C621 C623 C624 104.3(8) . . . . ? C628 C623 C624 C625 2.2(11) . . . . ? C621 C623 C624 C625 177.9(7) . . . . ? C623 C624 C625 C626 -3.4(13) . . . . ? C624 C625 C626 C627 1.8(14) . . . . ? C625 C626 C627 C628 0.9(13) . . . . ? C624 C623 C628 C627 0.5(12) . . . . ? C621 C623 C628 C627 -175.3(7) . . . . ? C626 C627 C628 C623 -2.1(12) . . . . ? N707 Co7 N701 C705 3.8(5) . . . . ? N613 Co7 N701 C705 -165.7(5) . . . . ? N619 Co7 N701 C705 -87.4(6) . . . . ? N722 Co7 N701 C705 20.5(8) . . . . ? N620 Co7 N701 C705 122.2(5) . . . . ? N707 Co7 N701 C702 -167.6(10) . . . . ? N613 Co7 N701 C702 23.0(9) . . . . ? N619 Co7 N701 C702 101.3(9) . . . . ? N722 Co7 N701 C702 -150.9(8) . . . . ? N620 Co7 N701 C702 -49.2(9) . . . . ? C705 N701 C702 C703 1.1(9) . . . . ? Co7 N701 C702 C703 172.6(7) . . . . ? N701 C702 C703 N704 0.3(10) . . . . ? C702 C703 N704 C705 -1.5(10) . . . . ? C702 N701 C705 N704 -2.1(9) . . . . ? Co7 N701 C705 N704 -176.8(5) . . . . ? C702 N701 C705 C706 173.1(7) . . . . ? Co7 N701 C705 C706 -1.7(9) . . . . ? C703 N704 C705 N701 2.3(9) . . . . ? C703 N704 C705 C706 -172.5(8) . . . . ? N701 C705 C706 N707 -3.3(11) . . . . ? N704 C705 C706 N707 170.9(8) . . . . ? C705 C706 N707 N708 -179.6(7) . . . . ? C705 C706 N707 Co7 6.8(9) . . . . ? N613 Co7 N707 C706 60.3(17) . . . . ? N619 Co7 N707 C706 89.9(6) . . . . ? N701 Co7 N707 C706 -6.1(6) . . . . ? N722 Co7 N707 C706 -177.3(6) . . . . ? N620 Co7 N707 C706 -87.0(6) . . . . ? N613 Co7 N707 N708 -113.4(15) . . . . ? N619 Co7 N707 N708 -83.9(6) . . . . ? N701 Co7 N707 N708 -179.9(6) . . . . ? N722 Co7 N707 N708 8.9(5) . . . . ? N620 Co7 N707 N708 99.2(6) . . . . ? C706 N707 N708 C709 174.5(7) . . . . ? Co7 N707 N708 C709 -12.1(9) . . . . ? C706 N707 N708 C729 -3.6(12) . . . . ? Co7 N707 N708 C729 169.9(6) . . . . ? N707 N708 C709 N722 7.5(10) . . . . ? C729 N708 C709 N722 -174.5(8) . . . . ? N707 N708 C709 C710 -172.6(7) . . . . ? C729 N708 C709 C710 5.4(12) . . . . ? N722 C709 C710 C711 4.5(12) . . . . ? N708 C709 C710 C711 -175.4(7) . . . . ? C709 C710 C711 N720 -5.3(12) . . . . ? C709 C710 C711 N712 176.8(7) . . . . ? N720 C711 N712 N713 -0.7(10) . . . . ? C710 C711 N712 N713 177.2(7) . . . . ? N720 C711 N712 C730 174.3(7) . . . . ? C710 C711 N712 C730 -7.7(11) . . . . ? C711 N712 N713 C714 178.6(8) . . . . ? C730 N712 N713 C714 3.6(12) . . . . ? C711 N712 N713 Co8 3.7(8) . . . . ? C730 N712 N713 Co8 -171.4(6) . . . . ? N807 Co8 N713 C714 -35.9(15) . . . . ? N801 Co8 N713 C714 -84.1(7) . . . . ? N719 Co8 N713 C714 8.2(7) . . . . ? N720 Co8 N713 C714 -178.9(7) . . . . ? N822 Co8 N713 C714 90.5(7) . . . . ? N807 Co8 N713 N712 139.3(11) . . . . ? N801 Co8 N713 N712 91.1(6) . . . . ? N719 Co8 N713 N712 -176.5(6) . . . . ? N720 Co8 N713 N712 -3.6(5) . . . . ? N822 Co8 N713 N712 -94.3(6) . . . . ? N712 N713 C714 C715 176.5(8) . . . . ? Co8 N713 C714 C715 -8.5(11) . . . . ? N713 C714 C715 N719 3.0(14) . . . . ? N713 C714 C715 N76' 158.2(10) . . . . ? N713 C714 C715 N716 -151.6(9) . . . . ? N719 C715 N716 C717 0.2(2) . . . . ? C714 C715 N716 C717 158.6(11) . . . . ? N76' C715 N716 C717 -95.6(16) . . . . ? C715 N716 C717 C718 0.0(2) . . . . ? N716 C717 C718 N719 -0.3(4) . . . . ? N719 C715 N76' C77' -0.3(2) . . . . ? C714 C715 N76' C77' -159.2(14) . . . . ? N716 C715 N76' C77' 95.1(15) . . . . ? C715 N76' C77' C78' 0.0(2) . . . . ? N76' C77' C78' N719 0.3(4) . . . . ? C714 C715 N719 C78' 160.1(12) . . . . ? N76' C715 N719 C78' 0.4(4) . . . . ? N716 C715 N719 C78' -40.7(6) . . . . ? C714 C715 N719 C718 -159.5(11) . . . . ? N76' C715 N719 C718 40.8(6) . . . . ? N716 C715 N719 C718 -0.3(4) . . . . ? C714 C715 N719 Co8 3.7(11) . . . . ? N76' C715 N719 Co8 -156.0(7) . . . . ? N716 C715 N719 Co8 162.8(6) . . . . ? C77' C78' N719 C715 -0.5(5) . . . . ? C77' C78' N719 C718 -96.2(19) . . . . ? C77' C78' N719 Co8 145.7(11) . . . . ? C717 C718 N719 C715 0.4(5) . . . . ? C717 C718 N719 C78' 98(2) . . . . ? C717 C718 N719 Co8 -153.8(10) . . . . ? N807 Co8 N719 C715 163.9(6) . . . . ? N801 Co8 N719 C715 85.0(6) . . . . ? N713 Co8 N719 C715 -5.6(5) . . . . ? N720 Co8 N719 C715 -19.4(9) . . . . ? N822 Co8 N719 C715 -123.5(6) . . . . ? N807 Co8 N719 C78' 17.4(12) . . . . ? N801 Co8 N719 C78' -61.5(12) . . . . ? N713 Co8 N719 C78' -152.1(12) . . . . ? N720 Co8 N719 C78' -165.9(12) . . . . ? N822 Co8 N719 C78' 90.1(12) . . . . ? N807 Co8 N719 C718 -41.8(11) . . . . ? N801 Co8 N719 C718 -120.7(11) . . . . ? N713 Co8 N719 C718 148.7(11) . . . . ? N720 Co8 N719 C718 135.0(11) . . . . ? N822 Co8 N719 C718 30.9(11) . . . . ? C710 C711 N720 C721 5.9(11) . . . . ? N712 C711 N720 C721 -176.2(7) . . . . ? C710 C711 N720 Co8 179.7(6) . . . . ? N712 C711 N720 Co8 -2.3(9) . . . . ? N807 Co8 N720 C721 6.2(8) . . . . ? N801 Co8 N720 C721 86.1(7) . . . . ? N713 Co8 N720 C721 176.0(7) . . . . ? N719 Co8 N720 C721 -170.1(6) . . . . ? N822 Co8 N720 C721 -68.3(7) . . . . ? N807 Co8 N720 C711 -166.6(5) . . . . ? N801 Co8 N720 C711 -86.7(6) . . . . ? N713 Co8 N720 C711 3.1(5) . . . . ? N719 Co8 N720 C711 17.0(9) . . . . ? N822 Co8 N720 C711 118.9(5) . . . . ? C711 N720 C721 N722 -5.9(12) . . . . ? Co8 N720 C721 N722 -178.8(5) . . . . ? C711 N720 C721 C723 170.4(7) . . . . ? Co8 N720 C721 C723 -2.5(10) . . . . ? N720 C721 N722 C709 5.1(11) . . . . ? C723 C721 N722 C709 -171.2(7) . . . . ? N720 C721 N722 Co7 -180.0(6) . . . . ? C723 C721 N722 Co7 3.7(10) . . . . ? N708 C709 N722 C721 175.7(7) . . . . ? C710 C709 N722 C721 -4.2(11) . . . . ? N708 C709 N722 Co7 0.0(9) . . . . ? C710 C709 N722 Co7 -179.9(6) . . . . ? N707 Co7 N722 C721 -179.4(7) . . . . ? N613 Co7 N722 C721 -9.8(7) . . . . ? N619 Co7 N722 C721 -87.8(7) . . . . ? N701 Co7 N722 C721 163.5(6) . . . . ? N620 Co7 N722 C721 64.6(7) . . . . ? N707 Co7 N722 C709 -4.5(5) . . . . ? N613 Co7 N722 C709 165.0(5) . . . . ? N619 Co7 N722 C709 87.0(6) . . . . ? N701 Co7 N722 C709 -21.6(8) . . . . ? N620 Co7 N722 C709 -120.5(5) . . . . ? N720 C721 C723 C728 -87.4(11) . . . . ? N722 C721 C723 C728 89.4(10) . . . . ? N720 C721 C723 C724 90.4(10) . . . . ? N722 C721 C723 C724 -92.8(10) . . . . ? C728 C723 C724 C725 -0.2(16) . . . . ? C721 C723 C724 C725 -177.9(10) . . . . ? C723 C724 C725 C726 -1.5(17) . . . . ? C724 C725 C726 C727 3(2) . . . . ? C725 C726 C727 C728 -3(2) . . . . ? C724 C723 C728 C727 0.2(17) . . . . ? C721 C723 C728 C727 178.0(10) . . . . ? C726 C727 C728 C723 2(2) . . . . ? N807 Co8 N801 C802 -174.0(13) . . . . ? N713 Co8 N801 C802 -5.4(13) . . . . ? N719 Co8 N801 C802 -82.1(13) . . . . ? N720 Co8 N801 C802 68.7(13) . . . . ? N822 Co8 N801 C802 -175.3(10) . . . . ? N807 Co8 N801 C805 -5.7(7) . . . . ? N713 Co8 N801 C805 162.9(7) . . . . ? N719 Co8 N801 C805 86.2(7) . . . . ? N720 Co8 N801 C805 -123.1(7) . . . . ? N822 Co8 N801 C805 -7.0(11) . . . . ? C805 N801 C802 C803 -0.4(13) . . . . ? Co8 N801 C802 C803 168.2(10) . . . . ? N801 C802 C803 N804 1.3(14) . . . . ? C802 C803 N804 C805 -1.8(13) . . . . ? C803 N804 C805 N801 1.6(13) . . . . ? C803 N804 C805 C806 -178.1(12) . . . . ? C802 N801 C805 N804 -0.8(12) . . . . ? Co8 N801 C805 N804 -173.7(7) . . . . ? C802 N801 C805 C806 179.0(10) . . . . ? Co8 N801 C805 C806 6.0(13) . . . . ? N804 C805 C806 N807 177.9(10) . . . . ? N801 C805 C806 N807 -1.8(16) . . . . ? C805 C806 N807 N808 -175.8(9) . . . . ? C805 C806 N807 Co8 -3.7(13) . . . . ? N801 Co8 N807 C806 5.4(8) . . . . ? N713 Co8 N807 C806 -44.0(17) . . . . ? N719 Co8 N807 C806 -86.7(9) . . . . ? N720 Co8 N807 C806 95.1(9) . . . . ? N822 Co8 N807 C806 -175.2(9) . . . . ? N801 Co8 N807 N808 177.5(8) . . . . ? N713 Co8 N807 N808 128.0(11) . . . . ? N719 Co8 N807 N808 85.3(7) . . . . ? N720 Co8 N807 N808 -92.9(7) . . . . ? N822 Co8 N807 N808 -3.2(7) . . . . ? C806 N807 N808 C809 175.1(10) . . . . ? Co8 N807 N808 C809 3.2(11) . . . . ? C806 N807 N808 C829 -2.0(15) . . . . ? Co8 N807 N808 C829 -173.9(7) . . . . ? N807 N808 C809 N822 -0.6(12) . . . . ? C829 N808 C809 N822 176.3(9) . . . . ? N807 N808 C809 C810 -177.7(8) . . . . ? C829 N808 C809 C810 -0.8(15) . . . . ? N808 C809 C810 C811 178.6(9) . . . . ? N822 C809 C810 C811 1.6(13) . . . . ? C809 C810 C811 N820 -2.3(13) . . . . ? C809 C810 C811 N812 -177.7(8) . . . . ? N820 C811 N812 N813 0.3(11) . . . . ? C810 C811 N812 N813 176.0(8) . . . . ? N820 C811 N812 C830 -174.9(8) . . . . ? C810 C811 N812 C830 0.8(13) . . . . ? C811 N812 N813 C814 -176.9(8) . . . . ? C830 N812 N813 C814 -1.5(12) . . . . ? C811 N812 N813 Co5 -1.6(9) . . . . ? C830 N812 N813 Co5 173.9(6) . . . . ? N507 Co5 N813 C814 32.2(14) . . . . ? N819 Co5 N813 C814 -4.7(6) . . . . ? N501 Co5 N813 C814 91.5(6) . . . . ? N820 Co5 N813 C814 177.2(7) . . . . ? N522 Co5 N813 C814 -92.5(6) . . . . ? N507 Co5 N813 N812 -143.5(10) . . . . ? N819 Co5 N813 N812 179.6(6) . . . . ? N501 Co5 N813 N812 -84.1(6) . . . . ? N820 Co5 N813 N812 1.6(5) . . . . ? N522 Co5 N813 N812 91.8(6) . . . . ? N812 N813 C814 C815 -179.2(8) . . . . ? Co5 N813 C814 C815 5.3(10) . . . . ? N813 C814 C815 N816 178.7(10) . . . . ? N813 C814 C815 N819 -2.6(13) . . . . ? N819 C815 N816 C817 -2.0(13) . . . . ? C814 C815 N816 C817 176.9(11) . . . . ? C815 N816 C817 C818 2.9(14) . . . . ? N816 C817 C818 N819 -2.8(14) . . . . ? N816 C815 N819 C818 0.1(11) . . . . ? C814 C815 N819 C818 -178.8(9) . . . . ? N816 C815 N819 Co5 177.6(7) . . . . ? C814 C815 N819 Co5 -1.3(11) . . . . ? C817 C818 N819 C815 1.7(13) . . . . ? C817 C818 N819 Co5 -174.4(9) . . . . ? N813 Co5 N819 C815 3.0(6) . . . . ? N507 Co5 N819 C815 -169.1(6) . . . . ? N501 Co5 N819 C815 -92.3(7) . . . . ? N820 Co5 N819 C815 6.7(10) . . . . ? N522 Co5 N819 C815 118.2(6) . . . . ? N813 Co5 N819 C818 179.0(11) . . . . ? N507 Co5 N819 C818 7.0(11) . . . . ? N501 Co5 N819 C818 83.7(11) . . . . ? N820 Co5 N819 C818 -177.2(9) . . . . ? N522 Co5 N819 C818 -65.7(11) . . . . ? C810 C811 N820 C821 0.5(12) . . . . ? N812 C811 N820 C821 176.1(7) . . . . ? C810 C811 N820 Co5 -174.5(7) . . . . ? N812 C811 N820 Co5 1.0(9) . . . . ? N813 Co5 N820 C821 -175.8(6) . . . . ? N507 Co5 N820 C821 -4.4(7) . . . . ? N819 Co5 N820 C821 -179.6(6) . . . . ? N501 Co5 N820 C821 -78.1(6) . . . . ? N522 Co5 N820 C821 69.8(6) . . . . ? N813 Co5 N820 C811 -1.4(5) . . . . ? N507 Co5 N820 C811 170.1(5) . . . . ? N819 Co5 N820 C811 -5.2(9) . . . . ? N501 Co5 N820 C811 96.4(6) . . . . ? N522 Co5 N820 C811 -115.8(6) . . . . ? C811 N820 C821 N822 2.3(11) . . . . ? Co5 N820 C821 N822 176.7(6) . . . . ? C811 N820 C821 C823 -173.5(7) . . . . ? Co5 N820 C821 C823 0.9(9) . . . . ? N820 C821 N822 C809 -2.9(12) . . . . ? C823 C821 N822 C809 172.9(7) . . . . ? N820 C821 N822 Co8 -176.6(5) . . . . ? C823 C821 N822 Co8 -0.8(10) . . . . ? N808 C809 N822 C821 -176.4(7) . . . . ? C810 C809 N822 C821 0.8(12) . . . . ? N808 C809 N822 Co8 -2.0(10) . . . . ? C810 C809 N822 Co8 175.2(6) . . . . ? N807 Co8 N822 C821 176.4(7) . . . . ? N801 Co8 N822 C821 177.8(7) . . . . ? N713 Co8 N822 C821 9.2(8) . . . . ? N719 Co8 N822 C821 83.8(7) . . . . ? N720 Co8 N822 C821 -66.8(7) . . . . ? N807 Co8 N822 C809 2.6(6) . . . . ? N801 Co8 N822 C809 4.0(10) . . . . ? N713 Co8 N822 C809 -164.7(6) . . . . ? N719 Co8 N822 C809 -90.0(6) . . . . ? N720 Co8 N822 C809 119.4(6) . . . . ? N822 C821 C823 C824 94.7(9) . . . . ? N820 C821 C823 C824 -89.2(9) . . . . ? N822 C821 C823 C828 -85.8(9) . . . . ? N820 C821 C823 C828 90.3(9) . . . . ? C828 C823 C824 C825 0.3(12) . . . . ? C821 C823 C824 C825 179.8(7) . . . . ? C823 C824 C825 C826 -0.8(14) . . . . ? C824 C825 C826 C827 1.4(15) . . . . ? C825 C826 C827 C828 -1.5(15) . . . . ? C824 C823 C828 C827 -0.4(12) . . . . ? C821 C823 C828 C827 -179.9(7) . . . . ? C826 C827 C828 C823 1.0(13) . . . . ? O12 S1 C1 F11 -61.6(16) . . . . ? O13 S1 C1 F11 61.3(16) . . . . ? O11 S1 C1 F11 177.0(14) . . . . ? O12 S1 C1 F13 59.4(12) . . . . ? O13 S1 C1 F13 -177.7(11) . . . . ? O11 S1 C1 F13 -62.0(13) . . . . ? O12 S1 C1 F12 179.1(10) . . . . ? O13 S1 C1 F12 -57.9(11) . . . . ? O11 S1 C1 F12 57.8(12) . . . . ? O22 S2 C2 F22 179.2(12) . . . . ? O23 S2 C2 F22 -62.0(13) . . . . ? O21 S2 C2 F22 55.1(14) . . . . ? O22 S2 C2 F23 58.7(10) . . . . ? O23 S2 C2 F23 177.6(9) . . . . ? O21 S2 C2 F23 -65.3(10) . . . . ? O22 S2 C2 F21 -56.1(14) . . . . ? O23 S2 C2 F21 62.7(13) . . . . ? O21 S2 C2 F21 179.8(11) . . . . ? O32 S3 C3 F32 179.7(9) . . . . ? O31 S3 C3 F32 57.9(11) . . . . ? O33 S3 C3 F32 -59.7(11) . . . . ? O32 S3 C3 F31 -55.7(9) . . . . ? O31 S3 C3 F31 -177.5(8) . . . . ? O33 S3 C3 F31 65.0(9) . . . . ? O32 S3 C3 F33 59.2(9) . . . . ? O31 S3 C3 F33 -62.6(9) . . . . ? O33 S3 C3 F33 179.8(7) . . . . ? O42 S4 C4 F41 -62.7(17) . . . . ? O43 S4 C4 F41 57.9(18) . . . . ? O41 S4 C4 F41 176.5(15) . . . . ? O42 S4 C4 F42 175.0(12) . . . . ? O43 S4 C4 F42 -64.4(13) . . . . ? O41 S4 C4 F42 54.3(14) . . . . ? O42 S4 C4 F43 59.7(13) . . . . ? O43 S4 C4 F43 -179.7(12) . . . . ? O41 S4 C4 F43 -61.0(14) . . . . ? O53 S5 C5 F52 -57.2(12) . . . . ? O51 S5 C5 F52 65.1(11) . . . . ? O52 S5 C5 F52 -176.1(11) . . . . ? O53 S5 C5 F53 -178.1(11) . . . . ? O51 S5 C5 F53 -55.8(11) . . . . ? O52 S5 C5 F53 63.0(11) . . . . ? O53 S5 C5 F51 62.9(11) . . . . ? O51 S5 C5 F51 -174.8(10) . . . . ? O52 S5 C5 F51 -55.9(11) . . . . ? O172 S17 C17 F171 -64.1(11) . . . . ? O173 S17 C17 F171 56.6(11) . . . . ? O171 S17 C17 F171 176.0(10) . . . . ? O172 S17 C17 F172 175.0(10) . . . . ? O173 S17 C17 F172 -64.3(11) . . . . ? O171 S17 C17 F172 55.1(10) . . . . ? O172 S17 C17 F173 56.6(11) . . . . ? O173 S17 C17 F173 177.3(10) . . . . ? O171 S17 C17 F173 -63.4(10) . . . . ? O62 S6 C6 F61 60.7(9) . . . . ? O61 S6 C6 F61 -178.2(8) . . . . ? O63 S6 C6 F61 -57.6(9) . . . . ? O62 S6 C6 F63 -61.4(10) . . . . ? O61 S6 C6 F63 59.7(9) . . . . ? O63 S6 C6 F63 -179.7(8) . . . . ? O62 S6 C6 F62 -179.9(8) . . . . ? O61 S6 C6 F62 -58.8(9) . . . . ? O63 S6 C6 F62 61.8(9) . . . . ? O71 S7 C7 F71 176.1(9) . . . . ? O72 S7 C7 F71 -65.8(10) . . . . ? O73 S7 C7 F71 53.2(10) . . . . ? O71 S7 C7 F73 -51.0(10) . . . . ? O72 S7 C7 F73 67.1(10) . . . . ? O73 S7 C7 F73 -173.9(8) . . . . ? O71 S7 C7 F72 63.4(7) . . . . ? O72 S7 C7 F72 -178.6(7) . . . . ? O73 S7 C7 F72 -59.5(7) . . . . ? O83 S8 C8 F81 59.7(10) . . . . ? O82 S8 C8 F81 -60.9(10) . . . . ? O81 S8 C8 F81 -179.9(8) . . . . ? O83 S8 C8 F82 -61.5(9) . . . . ? O82 S8 C8 F82 177.8(8) . . . . ? O81 S8 C8 F82 58.9(9) . . . . ? O83 S8 C8 F83 178.8(9) . . . . ? O82 S8 C8 F83 58.1(10) . . . . ? O81 S8 C8 F83 -60.8(10) . . . . ? O92 S9 C9 F91 -56.5(12) . . . . ? O93 S9 C9 F91 66.8(12) . . . . ? O91 S9 C9 F91 -175.9(12) . . . . ? O92 S9 C9 F93 64.0(12) . . . . ? O93 S9 C9 F93 -172.7(12) . . . . ? O91 S9 C9 F93 -55.4(12) . . . . ? O92 S9 C9 F92 -177.3(12) . . . . ? O93 S9 C9 F92 -54.0(12) . . . . ? O91 S9 C9 F92 63.3(12) . . . . ? O181 S18 C18 F182 59.4(9) . . . . ? O183 S18 C18 F182 -63.4(9) . . . . ? O182 S18 C18 F182 178.4(9) . . . . ? O181 S18 C18 F183 -61.8(9) . . . . ? O183 S18 C18 F183 175.5(9) . . . . ? O182 S18 C18 F183 57.3(9) . . . . ? O181 S18 C18 F181 179.6(9) . . . . ? O183 S18 C18 F181 56.9(9) . . . . ? O182 S18 C18 F181 -61.3(9) . . . . ? O103 S10 C10 F103 179.1(8) . . . . ? O101 S10 C10 F103 -56.7(9) . . . . ? O102 S10 C10 F103 61.0(8) . . . . ? O103 S10 C10 F101 50.3(9) . . . . ? O101 S10 C10 F101 174.5(7) . . . . ? O102 S10 C10 F101 -67.8(8) . . . . ? O103 S10 C10 F102 -59.3(7) . . . . ? O101 S10 C10 F102 64.9(7) . . . . ? O102 S10 C10 F102 -177.4(6) . . . . ? O112 S11 C11 F112 -178.4(9) . . . . ? O111 S11 C11 F112 59.5(10) . . . . ? O113 S11 C11 F112 -64.2(10) . . . . ? O112 S11 C11 F111 -58.5(10) . . . . ? O111 S11 C11 F111 179.4(8) . . . . ? O113 S11 C11 F111 55.7(10) . . . . ? O112 S11 C11 F113 59.7(9) . . . . ? O111 S11 C11 F113 -62.5(9) . . . . ? O113 S11 C11 F113 173.8(8) . . . . ? O122 S12 C12 F121 -79.2(15) . . . . ? O123 S12 C12 F121 41.2(15) . . . . ? O121 S12 C12 F121 160.8(15) . . . . ? O122 S12 C12 F122 159.8(15) . . . . ? O123 S12 C12 F122 -79.9(15) . . . . ? O121 S12 C12 F122 39.7(15) . . . . ? O122 S12 C12 F123 41.2(15) . . . . ? O123 S12 C12 F123 161.5(15) . . . . ? O121 S12 C12 F123 -78.9(15) . . . . ? O191 S19 C19 F193 -54.9(13) . . . . ? O193 S19 C19 F193 -177.2(13) . . . . ? O192 S19 C19 F193 66.1(13) . . . . ? O191 S19 C19 F191 -175.7(13) . . . . ? O193 S19 C19 F191 62.0(13) . . . . ? O192 S19 C19 F191 -54.7(13) . . . . ? O191 S19 C19 F192 65.3(13) . . . . ? O193 S19 C19 F192 -57.0(13) . . . . ? O192 S19 C19 F192 -173.7(13) . . . . ? O133 S13 C13 F133 178.8(9) . . . . ? O131 S13 C13 F133 -60.9(10) . . . . ? O132 S13 C13 F133 58.9(10) . . . . ? O133 S13 C13 F132 -58.8(10) . . . . ? O131 S13 C13 F132 61.4(10) . . . . ? O132 S13 C13 F132 -178.7(9) . . . . ? O133 S13 C13 F131 60.4(9) . . . . ? O131 S13 C13 F131 -179.4(8) . . . . ? O132 S13 C13 F131 -59.5(9) . . . . ? O141 S14 C14 F141 179.4(11) . . . . ? O142 S14 C14 F141 -62.3(13) . . . . ? O143 S14 C14 F141 60.0(14) . . . . ? O141 S14 C14 F143 -51.3(15) . . . . ? O142 S14 C14 F143 67.1(14) . . . . ? O143 S14 C14 F143 -170.6(12) . . . . ? O141 S14 C14 F142 62.8(11) . . . . ? O142 S14 C14 F142 -178.8(10) . . . . ? O143 S14 C14 F142 -56.6(12) . . . . ? O151 S15 C15 F153 -54.2(7) . . . . ? O153 S15 C15 F153 -179.6(6) . . . . ? O152 S15 C15 F153 63.5(6) . . . . ? O151 S15 C15 F151 178.7(6) . . . . ? O153 S15 C15 F151 53.3(6) . . . . ? O152 S15 C15 F151 -63.6(6) . . . . ? O151 S15 C15 F152 62.3(6) . . . . ? O153 S15 C15 F152 -63.1(6) . . . . ? O152 S15 C15 F152 180.0(5) . . . . ? O161 S16 C16 F162 59.6(12) . . . . ? O163 S16 C16 F162 -62.5(11) . . . . ? O162 S16 C16 F162 177.7(10) . . . . ? O161 S16 C16 F161 -173.7(11) . . . . ? O163 S16 C16 F161 64.2(12) . . . . ? O162 S16 C16 F161 -55.5(12) . . . . ? O161 S16 C16 F163 -56.4(11) . . . . ? O163 S16 C16 F163 -178.5(9) . . . . ? O162 S16 C16 F163 61.8(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N104 H104 O11 0.88 2.27 2.969(12) 135.9 . N116 H116 O21 0.88 2.04 2.866(11) 156.4 . N204 H204 O31 0.88 1.99 2.813(11) 156.3 . N204 H204 F81 0.88 2.56 3.088(11) 119.8 . N216 H216 O41 0.88 1.93 2.796(10) 169.7 . N304 H304 O51 0.88 2.00 2.832(14) 157.7 . N304 H304 O171 0.88 2.02 2.754(14) 139.9 . N316 H316 O01W 0.88 1.92 2.795(12) 175.2 . N404 H404 O71 0.88 1.91 2.756(10) 162.2 . N416 H416 O81 0.88 2.02 2.825(10) 150.8 . N504 H504 O181 0.88 2.19 2.801(13) 126.2 . N516 H516 O101 0.88 2.14 2.927(11) 148.9 . N604 H604 O02W 0.88 1.81 2.678(10) 167.7 . N616 H616 O121 0.88 2.04 2.904(19) 166.7 . N616 H616 O193 0.88 2.43 3.039(19) 126.8 . N704 H704 O131 0.88 2.01 2.838(10) 157.4 . N716 H716 O91 0.88 2.23 2.88(2) 131.1 . N716 H716 O141 0.88 2.41 2.979(18) 123.2 . N76' H76' O141 0.88 1.93 2.67(2) 141.9 . N804 H804 O151 0.88 1.91 2.765(10) 163.7 . N816 H816 O03W 0.88 1.93 2.806(15) 172.4 . _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 2.248 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.150 # Attachment '- as827.cif' data_as827 _database_code_depnum_ccdc_archive 'CCDC 826153' _publ_section_title_footnote ; ? #<< paper footnote text ; # 4. TEXT _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; #Barbour, L. J. (2001). J. Supramol. Chem., 1, 189-191. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # 5. CHEMICAL DATA _publ_section_figure_captions ; ? #<< figure captions ; #============================================================================== # 6. CRYSTALLOGRAPHY _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C80 H80 N40 Zn4), 16(Cl O4), 5(C2 H3 N), 8(H2 O)' _chemical_formula_sum 'C170 H191 Cl16 N85 O72 Zn8' _chemical_formula_weight 5667.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 24.517(5) _cell_length_b 19.460(4) _cell_length_c 24.071(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.50(3) _cell_angle_gamma 90.00 _cell_volume 11481(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5628 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 29.9 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5788 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25520 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.0921 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10110 _reflns_number_gt 6359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0680P)^2^+120.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10110 _refine_ls_number_parameters 853 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1271 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1986 _refine_ls_wR_factor_gt 0.1644 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.020 _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 Zn1 Zn 0.38438(3) 0.22741(4) 0.10611(3) 0.0288(2) Uani 1 1 d . . . Zn2 Zn 0.35766(3) 0.26696(4) 0.36764(3) 0.0321(2) Uani 1 1 d . . . Cl1 Cl 0.51940(9) 0.37856(11) 0.96011(9) 0.0560(6) Uani 1 1 d . . . Cl2 Cl 0.21827(9) 0.09993(12) 0.22669(9) 0.0594(6) Uani 1 1 d . . . Cl3A Cl 0.09490(18) 0.3695(2) 0.20587(17) 0.0544(12) Uani 0.65 1 d PD A 1 O31A O 0.0514(3) 0.3694(6) 0.1684(3) 0.088(5) Uani 0.65 1 d PD A 1 O32A O 0.0911(4) 0.3137(4) 0.2407(4) 0.103(6) Uani 0.65 1 d PD A 1 O33A O 0.1429(2) 0.3658(6) 0.1776(4) 0.100(4) Uani 0.65 1 d PD A 1 O34A O 0.0942(5) 0.4291(4) 0.2367(4) 0.166(9) Uani 0.65 1 d PD A 1 Cl3B Cl 0.0766(3) 0.3851(4) 0.2202(3) 0.0399(19) Uani 0.35 1 d PD B 2 O31B O 0.0375(6) 0.4315(7) 0.2359(10) 0.22(2) Uani 0.35 1 d PD B 2 O32B O 0.0909(7) 0.3438(11) 0.2647(7) 0.141(18) Uani 0.35 1 d PD B 2 O33B O 0.0561(7) 0.3451(12) 0.1773(7) 0.20(3) Uani 0.35 1 d PD B 2 O34B O 0.1220(5) 0.4201(8) 0.2028(8) 0.113(11) Uani 0.35 1 d PD B 2 Cl4 Cl 0.24880(8) 0.99820(10) 0.01401(9) 0.0455(5) Uani 1 1 d . . . O11 O 0.5298(4) 0.3831(5) 0.9034(3) 0.132(4) Uani 1 1 d . . . O12 O 0.5544(3) 0.4246(4) 0.9898(3) 0.083(2) Uani 1 1 d . . . O13 O 0.5288(2) 0.3115(3) 0.9803(3) 0.0687(18) Uani 1 1 d . . . O14 O 0.4633(3) 0.3954(4) 0.9693(3) 0.093(2) Uani 1 1 d . . . O21 O 0.2417(3) 0.1655(3) 0.2169(3) 0.0649(17) Uani 1 1 d . . . O22 O 0.2447(4) 0.0506(4) 0.1935(4) 0.109(3) Uani 1 1 d . . . O23 O 0.2251(3) 0.0819(4) 0.2842(3) 0.079(2) Uani 1 1 d . . . O24 O 0.1620(3) 0.0985(4) 0.2130(3) 0.103(3) Uani 1 1 d . . . O41 O 0.2782(5) 0.9511(5) 0.0436(4) 0.146(4) Uani 1 1 d . . . O42 O 0.2231(4) 0.9667(5) -0.0328(4) 0.138(4) Uani 1 1 d . . . O43 O 0.2097(3) 1.0356(5) 0.0413(4) 0.117(3) Uani 1 1 d . . . O44 O 0.2836(4) 1.0434(6) -0.0113(5) 0.152(4) Uani 1 1 d . . . O45 O 0.1071(3) 0.1700(4) 0.1217(3) 0.106(3) Uani 1 1 d . . . H45A H 0.1211 0.1434 0.1461 0.160 Uiso 1 1 d . . . H45B H 0.0886 0.1459 0.0986 0.160 Uiso 1 1 d . . . O46 O 0.3585(5) 0.3536(5) 0.6417(4) 0.095(3) Uani 0.75 1 d P C 1 H46A H 0.3889 0.3719 0.6342 0.142 Uiso 0.75 1 d P D 1 H46B H 0.3416 0.3804 0.6631 0.142 Uiso 0.75 1 d P E 1 O47 O 0.2983(12) 0.3852(17) 0.6081(13) 0.094(9) Uiso 0.25 1 d P F 2 H47A H 0.2902 0.3995 0.6403 0.141 Uiso 0.25 1 d P G 2 H47B H 0.2899 0.4166 0.5847 0.141 Uiso 0.25 1 d P H 2 N1A N 0.4042(2) 0.2010(3) 0.0235(2) 0.0327(13) Uani 1 1 d . . . N1B N 0.2983(2) 0.2265(3) 0.0910(2) 0.0361(14) Uani 1 1 d . . . N3A N 0.4196(2) 0.1834(4) -0.0642(3) 0.0465(16) Uani 1 1 d . . . H3A H 0.4263 0.1916 -0.0985 0.056 Uiso 1 1 calc R . . N3B N 0.2100(2) 0.2184(4) 0.0795(3) 0.0537(19) Uani 1 1 d . . . H3B H 0.1779 0.2005 0.0777 0.064 Uiso 1 1 calc R . . N7A N 0.3875(2) 0.1170(3) 0.1060(2) 0.0307(13) Uani 1 1 d . . . N7B N 0.3639(2) 0.3328(3) 0.0897(2) 0.0336(14) Uani 1 1 d . . . N8A N 0.3778(2) 0.0819(3) 0.1540(2) 0.0385(14) Uani 1 1 d . . . N8B N 0.4040(2) 0.3817(3) 0.0917(3) 0.0362(14) Uani 1 1 d . . . N11A N 0.3771(2) 0.1914(3) 0.1935(2) 0.0278(12) Uani 1 1 d . . . N11B N 0.4603(2) 0.2880(3) 0.1135(2) 0.0271(12) Uani 1 1 d . . . N13A N 0.3656(2) 0.2056(3) 0.2909(2) 0.0291(13) Uani 1 1 d . . . N13B N 0.5567(2) 0.3016(3) 0.1236(2) 0.0270(12) Uani 1 1 d . . . N22A N 0.3468(2) 0.1131(3) 0.3487(2) 0.0382(14) Uani 1 1 d . . . N22B N 0.5971(2) 0.4106(3) 0.1235(3) 0.0384(15) Uani 1 1 d . . . N24B N 0.6435(2) 0.3763(3) 0.1386(2) 0.0345(14) Uani 1 1 d . . . N28A N 0.3218(3) 0.2828(4) 0.5413(3) 0.0562(19) Uani 1 1 d . . . H28A H 0.3168 0.3021 0.5729 0.067 Uiso 1 1 calc R . . N28N N 0.8039(3) 0.3073(5) 0.1978(3) 0.063(2) Uani 1 1 d . . . H28N H 0.8355 0.2990 0.2126 0.076 Uiso 1 1 calc R . . N30A N 0.3422(2) 0.2706(3) 0.4541(2) 0.0411(15) Uani 1 1 d . . . N30B N 0.7241(2) 0.2901(3) 0.1582(2) 0.0399(15) Uani 1 1 d . . . N31 N 0.9363(4) 0.4073(5) 0.0585(4) 0.093(3) Uani 1 1 d . . . N34 N 0.5000 0.5531(6) 0.2500 0.098(11) Uani 0.50 2 d SPD . . C2A C 0.4151(3) 0.2306(4) -0.0238(3) 0.0397(18) Uani 1 1 d . . . H2A H 0.4192 0.2777 -0.0288 0.048 Uiso 1 1 calc R . . C2B C 0.2561(3) 0.1853(4) 0.0921(3) 0.0438(19) Uani 1 1 d . . . H2B H 0.2581 0.1387 0.1006 0.053 Uiso 1 1 calc R . . C4A C 0.4116(3) 0.1205(4) -0.0414(3) 0.0450(19) Uani 1 1 d . . . H4A H 0.4123 0.0784 -0.0597 0.054 Uiso 1 1 calc R . . C4B C 0.2223(3) 0.2853(5) 0.0700(4) 0.055(2) Uani 1 1 d . . . H4B H 0.1980 0.3204 0.0606 0.066 Uiso 1 1 calc R . . C5A C 0.4023(3) 0.1311(4) 0.0134(3) 0.0350(16) Uani 1 1 d . . . C5B C 0.2775(3) 0.2904(4) 0.0772(3) 0.0375(17) Uani 1 1 d . . . C6A C 0.3930(3) 0.0852(4) 0.0597(3) 0.0368(17) Uani 1 1 d . . . H6A H 0.3911 0.0377 0.0562 0.044 Uiso 1 1 calc R . . C6B C 0.3145(3) 0.3475(4) 0.0753(3) 0.0393(18) Uani 1 1 d . . . H6B H 0.3035 0.3914 0.0646 0.047 Uiso 1 1 calc R . . C9A C 0.3750(4) 0.0071(4) 0.1532(3) 0.055(2) Uani 1 1 d . . . H9A1 H 0.3730 -0.0098 0.1905 0.082 Uiso 1 1 calc R . . H9A2 H 0.4069 -0.0110 0.1362 0.082 Uiso 1 1 calc R . . H9A3 H 0.3431 -0.0071 0.1322 0.082 Uiso 1 1 calc R . . C9B C 0.3919(3) 0.4526(4) 0.0757(4) 0.053(2) Uani 1 1 d . . . H9B1 H 0.3788 0.4537 0.0378 0.079 Uiso 1 1 calc R . . H9B2 H 0.4245 0.4797 0.0794 0.079 Uiso 1 1 calc R . . H9B3 H 0.3646 0.4709 0.0994 0.079 Uiso 1 1 calc R . . C10A C 0.3735(3) 0.1215(3) 0.2005(3) 0.0305(15) Uani 1 1 d . . . C10B C 0.4556(3) 0.3579(3) 0.1045(3) 0.0302(15) Uani 1 1 d . . . C12A C 0.3723(2) 0.2290(4) 0.2393(3) 0.0300(15) Uani 1 1 d . . . C12B C 0.5114(2) 0.2646(3) 0.1199(2) 0.0240(14) Uani 1 1 d . . . C14A C 0.3593(3) 0.1367(4) 0.2961(3) 0.0318(16) Uani 1 1 d . . . C14B C 0.5503(3) 0.3711(3) 0.1193(3) 0.0300(15) Uani 1 1 d . . . C15A C 0.3650(3) 0.0926(4) 0.2521(3) 0.0342(16) Uani 1 1 d . . . H15A H 0.3633 0.0452 0.2568 0.041 Uiso 1 1 calc R . . C15B C 0.5000(3) 0.4010(3) 0.1097(3) 0.0336(16) Uani 1 1 d . . . H15B H 0.4961 0.4485 0.1069 0.040 Uiso 1 1 calc R . . C16A C 0.3726(3) 0.3048(4) 0.2330(3) 0.0365(17) Uani 1 1 d . . . C16B C 0.5166(2) 0.1881(3) 0.1219(3) 0.0285(15) Uani 1 1 d . . . C17A C 0.4195(3) 0.3433(4) 0.2432(3) 0.0442(19) Uani 1 1 d . . . H17A H 0.4519 0.3215 0.2536 0.053 Uiso 1 1 calc R . . C17B C 0.5297(3) 0.1534(4) 0.0737(3) 0.0362(17) Uani 1 1 d . . . H17B H 0.5367 0.1778 0.0415 0.043 Uiso 1 1 calc R . . C18A C 0.4179(5) 0.4140(5) 0.2380(4) 0.071(3) Uani 1 1 d . . . H18A H 0.4493 0.4397 0.2450 0.086 Uiso 1 1 calc R . . C18B C 0.5322(3) 0.0822(4) 0.0737(4) 0.045(2) Uani 1 1 d . . . H18B H 0.5412 0.0590 0.0414 0.054 Uiso 1 1 calc R . . C19A C 0.3711(6) 0.4460(5) 0.2227(4) 0.084(4) Uani 1 1 d . . . H19A H 0.3705 0.4937 0.2197 0.101 Uiso 1 1 calc R . . C19B C 0.5216(3) 0.0457(4) 0.1213(4) 0.051(2) Uani 1 1 d . . . H19B H 0.5223 -0.0021 0.1209 0.061 Uiso 1 1 calc R . . C20A C 0.3247(5) 0.4096(6) 0.2117(4) 0.077(3) Uani 1 1 d . . . H20A H 0.2930 0.4327 0.2010 0.092 Uiso 1 1 calc R . . C20B C 0.5099(3) 0.0801(4) 0.1694(3) 0.0440(19) Uani 1 1 d . . . H20B H 0.5041 0.0556 0.2019 0.053 Uiso 1 1 calc R . . C21A C 0.3241(3) 0.3370(4) 0.2162(3) 0.048(2) Uani 1 1 d . . . H21A H 0.2926 0.3119 0.2083 0.058 Uiso 1 1 calc R . . C21B C 0.5066(3) 0.1516(4) 0.1695(3) 0.0361(17) Uani 1 1 d . . . H21B H 0.4976 0.1747 0.2018 0.043 Uiso 1 1 calc R . . C23A C 0.3318(4) 0.0419(4) 0.3609(4) 0.056(2) Uani 1 1 d . . . H23A H 0.3542 0.0252 0.3913 0.084 Uiso 1 1 calc R . . H23B H 0.3374 0.0139 0.3287 0.084 Uiso 1 1 calc R . . H23C H 0.2942 0.0401 0.3706 0.084 Uiso 1 1 calc R . . C23B C 0.5969(3) 0.4850(4) 0.1169(4) 0.054(2) Uani 1 1 d . . . H23D H 0.5914 0.5064 0.1522 0.081 Uiso 1 1 calc R . . H23E H 0.5680 0.4981 0.0914 0.081 Uiso 1 1 calc R . . H23F H 0.6312 0.4996 0.1027 0.081 Uiso 1 1 calc R . . N24A N 0.3430(2) 0.1614(3) 0.3887(2) 0.0356(14) Uani 1 1 d . . . C25A C 0.3280(3) 0.1487(4) 0.4382(3) 0.0428(19) Uani 1 1 d . . . H25A H 0.3182 0.1049 0.4497 0.051 Uiso 1 1 calc R . . C25B C 0.6889(3) 0.4061(4) 0.1500(3) 0.0407(18) Uani 1 1 d . . . H25B H 0.6931 0.4535 0.1489 0.049 Uiso 1 1 calc R . . C26A C 0.3274(3) 0.2074(4) 0.4750(3) 0.044(2) Uani 1 1 d . . . C26B C 0.7329(3) 0.3602(4) 0.1647(3) 0.044(2) Uani 1 1 d . . . C27A C 0.3138(3) 0.2154(5) 0.5293(4) 0.056(2) Uani 1 1 d . . . H27A H 0.3015 0.1815 0.5532 0.067 Uiso 1 1 calc R . . C27B C 0.7823(3) 0.3703(5) 0.1892(4) 0.058(2) Uani 1 1 d . . . H27B H 0.7982 0.4123 0.1983 0.070 Uiso 1 1 calc R . . C29A C 0.3389(3) 0.3144(5) 0.4953(3) 0.050(2) Uani 1 1 d . . . H29A H 0.3472 0.3609 0.4930 0.060 Uiso 1 1 calc R . . C29B C 0.7680(3) 0.2596(5) 0.1794(3) 0.048(2) Uani 1 1 d . . . H29B H 0.7733 0.2123 0.1814 0.058 Uiso 1 1 calc R . . C32 C 0.9369(4) 0.3599(6) 0.0848(5) 0.062(3) Uani 1 1 d . . . C33 C 0.9393(4) 0.3013(6) 0.1200(5) 0.087(4) Uani 1 1 d . . . H33A H 0.9628 0.2674 0.1043 0.131 Uiso 1 1 calc R . . H33B H 0.9034 0.2824 0.1234 0.131 Uiso 1 1 calc R . . H33C H 0.9534 0.3144 0.1561 0.131 Uiso 1 1 calc R . . C35 C 0.5000 0.6137(6) 0.2500 0.046(6) Uani 0.50 2 d SPD . . C36 C 0.5000 0.6872(6) 0.2500 0.15(2) Uani 0.50 2 d SPD . . H36A H 0.5108 0.7036 0.2143 0.219 Uiso 0.25 1 calc PR . . H36B H 0.5252 0.7036 0.2782 0.219 Uiso 0.25 1 calc PR . . H36C H 0.4640 0.7036 0.2575 0.219 Uiso 0.25 1 calc PR . . 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 Zn1 0.0303(4) 0.0232(4) 0.0328(5) 0.0016(4) 0.0005(3) -0.0014(3) Zn2 0.0319(4) 0.0334(5) 0.0309(5) 0.0035(4) 0.0001(3) 0.0015(3) Cl1 0.0670(14) 0.0470(13) 0.0538(14) 0.0062(11) -0.0036(10) -0.0006(11) Cl2 0.0707(14) 0.0560(14) 0.0506(13) 0.0035(11) -0.0139(11) -0.0279(11) Cl3A 0.070(3) 0.054(3) 0.039(3) 0.006(2) -0.010(2) -0.015(2) O31A 0.076(10) 0.136(12) 0.052(9) -0.012(8) -0.020(7) 0.048(9) O32A 0.086(9) 0.113(10) 0.107(13) 0.070(10) -0.046(9) -0.044(8) O33A 0.072(8) 0.124(12) 0.104(10) 0.020(9) -0.002(7) -0.019(7) O34A 0.31(3) 0.094(13) 0.098(14) -0.053(11) -0.027(15) -0.054(17) Cl3B 0.053(4) 0.044(5) 0.023(4) 0.004(3) 0.013(3) 0.003(3) O31B 0.11(2) 0.10(2) 0.45(7) 0.05(3) 0.10(3) 0.077(19) O32B 0.045(13) 0.33(5) 0.048(16) 0.10(2) -0.014(10) -0.02(2) O33B 0.10(2) 0.45(7) 0.066(18) -0.15(3) 0.042(15) -0.16(3) O34B 0.17(2) 0.032(12) 0.15(3) -0.007(14) 0.10(2) -0.058(14) Cl4 0.0421(10) 0.0418(11) 0.0528(13) 0.0041(10) 0.0029(9) 0.0044(8) O11 0.186(10) 0.156(9) 0.053(5) -0.004(5) -0.001(5) 0.004(7) O12 0.095(5) 0.067(5) 0.087(5) 0.003(4) 0.008(4) -0.043(4) O13 0.059(4) 0.042(4) 0.105(5) 0.008(4) -0.005(3) -0.001(3) O14 0.085(5) 0.074(5) 0.119(7) -0.002(5) -0.015(4) 0.033(4) O21 0.086(4) 0.047(4) 0.062(4) -0.004(3) 0.004(3) -0.032(3) O22 0.146(7) 0.071(5) 0.110(7) -0.036(5) 0.013(6) -0.039(5) O23 0.102(5) 0.072(5) 0.061(4) 0.016(4) -0.026(4) -0.026(4) O24 0.080(5) 0.130(7) 0.097(6) 0.047(5) -0.046(4) -0.046(5) O41 0.223(11) 0.117(8) 0.096(7) 0.029(6) -0.034(7) 0.075(8) O42 0.113(7) 0.143(9) 0.156(9) -0.066(7) -0.049(6) 0.043(6) O43 0.106(6) 0.148(8) 0.100(7) -0.031(6) 0.031(5) 0.024(6) O44 0.100(7) 0.155(10) 0.201(11) 0.074(8) 0.029(7) -0.031(6) O45 0.090(5) 0.116(7) 0.111(6) 0.069(5) -0.043(5) -0.046(5) O46 0.151(9) 0.083(7) 0.052(6) -0.011(5) 0.050(6) -0.011(7) N1A 0.029(3) 0.032(3) 0.037(4) -0.001(3) -0.003(2) -0.005(2) N1B 0.036(3) 0.033(3) 0.040(4) 0.002(3) 0.003(3) -0.005(3) N3A 0.047(4) 0.053(4) 0.040(4) -0.005(3) 0.010(3) -0.009(3) N3B 0.032(3) 0.056(5) 0.073(5) 0.020(4) -0.006(3) -0.009(3) N7A 0.038(3) 0.023(3) 0.032(3) -0.002(3) 0.001(2) 0.001(2) N7B 0.035(3) 0.024(3) 0.041(4) -0.002(3) 0.003(3) 0.000(3) N8A 0.058(4) 0.020(3) 0.038(4) -0.002(3) 0.003(3) -0.009(3) N8B 0.029(3) 0.022(3) 0.057(4) 0.011(3) -0.003(3) -0.001(2) N11A 0.030(3) 0.022(3) 0.031(3) 0.002(3) 0.002(2) -0.004(2) N11B 0.029(3) 0.024(3) 0.029(3) 0.001(2) 0.001(2) 0.000(2) N13A 0.031(3) 0.026(3) 0.030(3) 0.002(3) 0.002(2) -0.001(2) N13B 0.029(3) 0.020(3) 0.031(3) 0.003(2) -0.002(2) -0.003(2) N22A 0.044(3) 0.037(4) 0.034(4) 0.007(3) -0.002(3) -0.004(3) N22B 0.043(4) 0.022(3) 0.050(4) 0.003(3) -0.004(3) -0.010(3) N24B 0.034(3) 0.037(3) 0.032(3) 0.000(3) 0.001(2) -0.006(3) N28A 0.062(4) 0.069(6) 0.038(4) -0.002(4) 0.009(3) 0.015(4) N28N 0.033(4) 0.096(6) 0.059(5) 0.021(4) -0.012(3) -0.014(4) N30A 0.038(3) 0.053(4) 0.033(4) 0.005(3) 0.006(3) 0.002(3) N30B 0.034(3) 0.053(4) 0.033(3) 0.009(3) 0.003(3) -0.007(3) N31 0.120(8) 0.069(7) 0.091(8) -0.029(6) 0.027(6) -0.016(6) N34 0.028(10) 0.009(10) 0.25(3) 0.000 -0.031(14) 0.000 C2A 0.035(4) 0.046(5) 0.039(4) 0.003(4) 0.003(3) -0.006(3) C2B 0.039(4) 0.047(5) 0.045(5) 0.010(4) -0.002(3) -0.006(4) C4A 0.047(5) 0.039(5) 0.049(5) -0.006(4) 0.002(4) -0.003(4) C4B 0.037(4) 0.056(6) 0.071(6) 0.019(5) -0.009(4) 0.004(4) C5A 0.029(4) 0.038(4) 0.038(4) -0.009(3) 0.002(3) 0.004(3) C5B 0.035(4) 0.037(4) 0.041(5) 0.008(3) 0.006(3) 0.000(3) C6A 0.040(4) 0.024(4) 0.046(5) 0.002(4) -0.001(3) -0.006(3) C6B 0.041(4) 0.038(4) 0.038(4) 0.010(4) -0.001(3) 0.007(3) C9A 0.099(7) 0.023(4) 0.042(5) -0.001(4) 0.007(4) -0.017(4) C9B 0.044(5) 0.030(4) 0.084(7) 0.024(4) -0.007(4) 0.000(3) C10A 0.030(3) 0.021(4) 0.040(4) 0.001(3) -0.002(3) -0.007(3) C10B 0.037(4) 0.023(4) 0.031(4) 0.001(3) 0.004(3) 0.000(3) C12A 0.024(3) 0.030(4) 0.036(4) 0.000(3) -0.002(3) -0.001(3) C12B 0.031(3) 0.018(3) 0.023(3) -0.002(3) -0.002(3) -0.006(3) C14A 0.033(4) 0.030(4) 0.032(4) 0.010(3) -0.007(3) -0.002(3) C14B 0.033(4) 0.021(4) 0.037(4) 0.004(3) -0.001(3) -0.007(3) C15A 0.045(4) 0.019(4) 0.039(4) 0.005(3) 0.001(3) -0.005(3) C15B 0.042(4) 0.016(3) 0.043(4) 0.000(3) 0.000(3) -0.003(3) C16A 0.054(5) 0.022(4) 0.034(4) -0.001(3) 0.015(3) 0.001(3) C16B 0.025(3) 0.019(3) 0.041(4) 0.000(3) -0.006(3) -0.001(3) C17A 0.063(5) 0.030(4) 0.041(5) -0.008(4) 0.022(4) -0.007(4) C17B 0.038(4) 0.033(4) 0.038(4) -0.006(3) 0.000(3) -0.002(3) C18A 0.117(9) 0.042(6) 0.057(6) -0.013(5) 0.039(6) -0.027(6) C18B 0.044(4) 0.033(4) 0.058(5) -0.020(4) -0.003(4) 0.001(3) C19A 0.162(12) 0.028(5) 0.064(7) 0.004(5) 0.045(8) 0.007(7) C19B 0.049(5) 0.020(4) 0.085(7) -0.007(4) -0.005(4) 0.004(3) C20A 0.120(9) 0.061(7) 0.051(6) 0.012(5) 0.020(6) 0.049(7) C20B 0.052(5) 0.035(4) 0.044(5) 0.010(4) -0.011(4) -0.004(4) C21A 0.065(5) 0.041(5) 0.039(5) 0.007(4) 0.006(4) 0.019(4) C21B 0.039(4) 0.031(4) 0.038(4) -0.002(3) -0.001(3) -0.005(3) C23A 0.072(6) 0.039(5) 0.055(6) 0.018(4) -0.001(4) -0.010(4) C23B 0.050(5) 0.029(4) 0.082(7) 0.007(4) -0.006(4) -0.011(4) N24A 0.028(3) 0.048(4) 0.031(3) 0.009(3) -0.001(2) -0.001(3) C25A 0.040(4) 0.050(5) 0.038(5) 0.010(4) -0.001(3) -0.003(4) C25B 0.045(4) 0.038(4) 0.039(5) 0.004(4) 0.000(3) -0.016(4) C26A 0.035(4) 0.063(6) 0.035(5) 0.008(4) 0.001(3) 0.004(4) C26B 0.036(4) 0.064(6) 0.033(4) 0.015(4) -0.001(3) -0.015(4) C27A 0.055(5) 0.066(7) 0.049(5) 0.011(5) 0.009(4) 0.008(4) C27B 0.041(5) 0.065(6) 0.069(6) 0.017(5) -0.009(4) -0.018(4) C29A 0.042(4) 0.069(6) 0.038(5) -0.003(5) -0.002(3) 0.010(4) C29B 0.040(4) 0.067(6) 0.039(5) 0.005(4) 0.002(3) -0.003(4) C32 0.061(6) 0.057(7) 0.069(7) -0.035(6) 0.024(5) -0.016(5) C33 0.088(8) 0.087(9) 0.088(9) -0.020(7) 0.028(6) -0.023(7) C35 0.028(11) 0.024(12) 0.085(18) 0.000 0.000(10) 0.000 C36 0.35(7) 0.021(15) 0.07(2) 0.000 0.08(3) 0.000 _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 Zn1 N1A 2.123(6) . ? Zn1 N1B 2.132(5) . ? Zn1 N7B 2.146(6) . ? Zn1 N7A 2.150(5) . ? Zn1 N11B 2.207(5) . ? Zn1 N11A 2.228(5) . ? Zn2 N30A 2.127(6) . ? Zn2 N30B 2.131(6) 2_655 ? Zn2 N24B 2.134(6) 2_655 ? Zn2 N24A 2.149(6) . ? Zn2 N13B 2.211(5) 2_655 ? Zn2 N13A 2.213(6) . ? Cl1 O11 1.398(8) . ? Cl1 O13 1.409(6) . ? Cl1 O12 1.422(7) . ? Cl1 O14 1.436(7) . ? Cl2 O24 1.409(7) . ? Cl2 O22 1.417(8) . ? Cl2 O21 1.422(6) . ? Cl2 O23 1.434(6) . ? Cl3A O32A 1.3769(10) . ? Cl3A O34A 1.3772(10) . ? Cl3A O31A 1.3773(10) . ? Cl3A O33A 1.3778(10) . ? Cl3B O31B 1.3772(10) . ? Cl3B O32B 1.3773(10) . ? Cl3B O33B 1.3773(10) . ? Cl3B O34B 1.3773(10) . ? Cl4 O41 1.356(8) . ? Cl4 O44 1.377(8) . ? Cl4 O43 1.382(8) . ? Cl4 O42 1.417(9) . ? O45 H45A 0.8496 . ? O45 H45B 0.8499 . ? O46 H46A 0.8498 . ? O46 H46B 0.8497 . ? O47 H47A 0.8519 . ? O47 H47B 0.8517 . ? N1A C2A 1.311(9) . ? N1A C5A 1.381(9) . ? N1B C2B 1.311(9) . ? N1B C5B 1.382(9) . ? N3A C2A 1.343(9) . ? N3A C4A 1.359(10) . ? N3A H3A 0.8600 . ? N3B C2B 1.329(9) . ? N3B C4B 1.357(10) . ? N3B H3B 0.8600 . ? N7A C6A 1.284(9) . ? N7A N8A 1.369(8) . ? N7B C6B 1.285(8) . ? N7B N8B 1.367(7) . ? N8A C10A 1.367(9) . ? N8A C9A 1.457(9) . ? N8B C10B 1.377(8) . ? N8B C9B 1.459(9) . ? N11A C12A 1.333(8) . ? N11A C10A 1.373(8) . ? N11B C12B 1.339(8) . ? N11B C10B 1.380(8) . ? N13A C12A 1.337(8) . ? N13A C14A 1.355(8) . ? N13B C12B 1.323(8) . ? N13B C14B 1.364(8) . ? N13B Zn2 2.211(5) 2_655 ? N22A N24A 1.352(8) . ? N22A C14A 1.389(9) . ? N22A C23A 1.464(9) . ? N22B N24B 1.360(8) . ? N22B C14B 1.382(8) . ? N22B C23B 1.457(9) . ? N24B C25B 1.278(8) . ? N24B Zn2 2.134(6) 2_655 ? N28A C29A 1.342(10) . ? N28A C27A 1.358(11) . ? N28A H28A 0.8600 . ? N28N C29B 1.347(10) . ? N28N C27B 1.350(11) . ? N28N H28N 0.8600 . ? N30A C29A 1.312(10) . ? N30A C26A 1.381(10) . ? N30B C29B 1.320(9) . ? N30B C26B 1.389(10) . ? N30B Zn2 2.131(6) 2_655 ? N31 C32 1.120(13) . ? N34 C35 1.1797(11) . ? C2A H2A 0.9300 . ? C2B H2B 0.9300 . ? C4A C5A 1.360(10) . ? C4A H4A 0.9300 . ? C4B C5B 1.363(10) . ? C4B H4B 0.9300 . ? C5A C6A 1.452(10) . ? C5B C6B 1.436(10) . ? C6A H6A 0.9300 . ? C6B H6B 0.9300 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C10A C15A 1.384(9) . ? C10B C15B 1.377(9) . ? C12A C16A 1.483(10) . ? C12B C16B 1.495(8) . ? C14A C15A 1.372(10) . ? C14B C15B 1.379(9) . ? C15A H15A 0.9300 . ? C15B H15B 0.9300 . ? C16A C17A 1.387(10) . ? C16A C21A 1.396(10) . ? C16B C21B 1.375(9) . ? C16B C17B 1.387(9) . ? C17A C18A 1.382(12) . ? C17A H17A 0.9300 . ? C17B C18B 1.386(10) . ? C17B H17B 0.9300 . ? C18A C19A 1.349(15) . ? C18A H18A 0.9300 . ? C18B C19B 1.380(11) . ? C18B H18B 0.9300 . ? C19A C20A 1.359(15) . ? C19A H19A 0.9300 . ? C19B C20B 1.373(11) . ? C19B H19B 0.9300 . ? C20A C21A 1.416(13) . ? C20A H20A 0.9300 . ? C20B C21B 1.395(10) . ? C20B H20B 0.9300 . ? C21A H21A 0.9300 . ? C21B H21B 0.9300 . ? C23A H23A 0.9600 . ? C23A H23B 0.9600 . ? C23A H23C 0.9600 . ? C23B H23D 0.9600 . ? C23B H23E 0.9600 . ? C23B H23F 0.9600 . ? N24A C25A 1.281(9) . ? C25A C26A 1.444(11) . ? C25A H25A 0.9300 . ? C25B C26B 1.437(11) . ? C25B H25B 0.9300 . ? C26A C27A 1.367(11) . ? C26B C27B 1.347(10) . ? C27A H27A 0.9300 . ? C27B H27B 0.9300 . ? C29A H29A 0.9300 . ? C29B H29B 0.9300 . ? C32 C33 1.421(16) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C35 C36 1.4298(11) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Zn1 N1B 95.1(2) . . ? N1A Zn1 N7B 96.8(2) . . ? N1B Zn1 N7B 75.6(2) . . ? N1A Zn1 N7A 75.3(2) . . ? N1B Zn1 N7A 91.5(2) . . ? N7B Zn1 N7A 164.4(2) . . ? N1A Zn1 N11B 89.5(2) . . ? N1B Zn1 N11B 147.9(2) . . ? N7B Zn1 N11B 72.3(2) . . ? N7A Zn1 N11B 120.3(2) . . ? N1A Zn1 N11A 146.5(2) . . ? N1B Zn1 N11A 93.2(2) . . ? N7B Zn1 N11A 116.8(2) . . ? N7A Zn1 N11A 72.0(2) . . ? N11B Zn1 N11A 100.37(19) . . ? N30A Zn2 N30B 95.0(2) . 2_655 ? N30A Zn2 N24B 91.9(2) . 2_655 ? N30B Zn2 N24B 76.0(2) 2_655 2_655 ? N30A Zn2 N24A 76.4(2) . . ? N30B Zn2 N24A 96.3(2) 2_655 . ? N24B Zn2 N24A 165.5(2) 2_655 . ? N30A Zn2 N13B 95.2(2) . 2_655 ? N30B Zn2 N13B 147.9(2) 2_655 2_655 ? N24B Zn2 N13B 73.3(2) 2_655 2_655 ? N24A Zn2 N13B 115.7(2) . 2_655 ? N30A Zn2 N13A 149.0(2) . . ? N30B Zn2 N13A 88.4(2) 2_655 . ? N24B Zn2 N13A 118.7(2) 2_655 . ? N24A Zn2 N13A 72.5(2) . . ? N13B Zn2 N13A 98.06(19) 2_655 . ? O11 Cl1 O13 111.2(5) . . ? O11 Cl1 O12 109.2(5) . . ? O13 Cl1 O12 108.6(4) . . ? O11 Cl1 O14 109.6(6) . . ? O13 Cl1 O14 107.9(4) . . ? O12 Cl1 O14 110.3(5) . . ? O24 Cl2 O22 108.3(5) . . ? O24 Cl2 O21 112.1(5) . . ? O22 Cl2 O21 108.8(4) . . ? O24 Cl2 O23 108.0(4) . . ? O22 Cl2 O23 109.6(5) . . ? O21 Cl2 O23 110.0(4) . . ? O32A Cl3A O34A 109.51(9) . . ? O32A Cl3A O31A 109.50(9) . . ? O34A Cl3A O31A 109.48(9) . . ? O32A Cl3A O33A 109.46(9) . . ? O34A Cl3A O33A 109.43(9) . . ? O31A Cl3A O33A 109.44(9) . . ? O31B Cl3B O32B 109.47(9) . . ? O31B Cl3B O33B 109.47(9) . . ? O32B Cl3B O33B 109.47(9) . . ? O31B Cl3B O34B 109.48(9) . . ? O32B Cl3B O34B 109.45(9) . . ? O33B Cl3B O34B 109.47(9) . . ? O41 Cl4 O44 109.6(7) . . ? O41 Cl4 O43 118.2(6) . . ? O44 Cl4 O43 108.6(7) . . ? O41 Cl4 O42 110.1(6) . . ? O44 Cl4 O42 101.1(7) . . ? O43 Cl4 O42 107.8(5) . . ? H45A O45 H45B 108.4 . . ? H46A O46 H46B 108.4 . . ? H47A O47 H47B 108.0 . . ? C2A N1A C5A 106.6(6) . . ? C2A N1A Zn1 139.9(5) . . ? C5A N1A Zn1 113.4(5) . . ? C2B N1B C5B 105.5(6) . . ? C2B N1B Zn1 141.3(5) . . ? C5B N1B Zn1 113.1(4) . . ? C2A N3A C4A 108.0(7) . . ? C2A N3A H3A 126.0 . . ? C4A N3A H3A 126.0 . . ? C2B N3B C4B 108.2(6) . . ? C2B N3B H3B 125.9 . . ? C4B N3B H3B 125.9 . . ? C6A N7A N8A 121.1(6) . . ? C6A N7A Zn1 119.2(5) . . ? N8A N7A Zn1 119.4(4) . . ? C6B N7B N8B 121.8(6) . . ? C6B N7B Zn1 118.5(5) . . ? N8B N7B Zn1 119.7(4) . . ? C10A N8A N7A 115.5(5) . . ? C10A N8A C9A 124.7(6) . . ? N7A N8A C9A 119.8(6) . . ? N7B N8B C10B 115.4(5) . . ? N7B N8B C9B 120.6(5) . . ? C10B N8B C9B 123.8(6) . . ? C12A N11A C10A 115.7(6) . . ? C12A N11A Zn1 128.3(4) . . ? C10A N11A Zn1 115.8(4) . . ? C12B N11B C10B 115.2(5) . . ? C12B N11B Zn1 127.8(4) . . ? C10B N11B Zn1 116.6(4) . . ? C12A N13A C14A 116.1(6) . . ? C12A N13A Zn2 127.4(5) . . ? C14A N13A Zn2 116.4(4) . . ? C12B N13B C14B 116.1(5) . . ? C12B N13B Zn2 129.3(4) . 2_655 ? C14B N13B Zn2 114.5(4) . 2_655 ? N24A N22A C14A 116.1(6) . . ? N24A N22A C23A 119.5(6) . . ? C14A N22A C23A 124.0(6) . . ? N24B N22B C14B 115.7(5) . . ? N24B N22B C23B 121.1(6) . . ? C14B N22B C23B 123.0(6) . . ? C25B N24B N22B 123.6(6) . . ? C25B N24B Zn2 118.5(5) . 2_655 ? N22B N24B Zn2 117.4(4) . 2_655 ? C29A N28A C27A 108.3(7) . . ? C29A N28A H28A 125.8 . . ? C27A N28A H28A 125.8 . . ? C29B N28N C27B 109.0(7) . . ? C29B N28N H28N 125.5 . . ? C27B N28N H28N 125.5 . . ? C29A N30A C26A 106.4(7) . . ? C29A N30A Zn2 141.1(6) . . ? C26A N30A Zn2 112.4(5) . . ? C29B N30B C26B 106.0(6) . . ? C29B N30B Zn2 140.2(6) . 2_655 ? C26B N30B Zn2 112.5(5) . 2_655 ? N1A C2A N3A 110.6(7) . . ? N1A C2A H2A 124.7 . . ? N3A C2A H2A 124.7 . . ? N1B C2B N3B 111.5(7) . . ? N1B C2B H2B 124.2 . . ? N3B C2B H2B 124.2 . . ? N3A C4A C5A 106.4(7) . . ? N3A C4A H4A 126.8 . . ? C5A C4A H4A 126.8 . . ? N3B C4B C5B 105.8(7) . . ? N3B C4B H4B 127.1 . . ? C5B C4B H4B 127.1 . . ? C4A C5A N1A 108.4(7) . . ? C4A C5A C6A 133.2(7) . . ? N1A C5A C6A 118.3(6) . . ? C4B C5B N1B 109.0(7) . . ? C4B C5B C6B 132.7(7) . . ? N1B C5B C6B 118.3(6) . . ? N7A C6A C5A 113.1(6) . . ? N7A C6A H6A 123.5 . . ? C5A C6A H6A 123.5 . . ? N7B C6B C5B 114.3(7) . . ? N7B C6B H6B 122.8 . . ? C5B C6B H6B 122.8 . . ? N8A C9A H9A1 109.5 . . ? N8A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? N8A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? N8B C9B H9B1 109.5 . . ? N8B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? N8B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? N8A C10A N11A 116.7(6) . . ? N8A C10A C15A 121.6(6) . . ? N11A C10A C15A 121.7(6) . . ? N8B C10B C15B 122.3(6) . . ? N8B C10B N11B 116.0(6) . . ? C15B C10B N11B 121.6(6) . . ? N11A C12A N13A 126.7(6) . . ? N11A C12A C16A 117.5(6) . . ? N13A C12A C16A 115.8(6) . . ? N13B C12B N11B 127.1(6) . . ? N13B C12B C16B 118.0(5) . . ? N11B C12B C16B 114.9(5) . . ? N13A C14A C15A 122.2(6) . . ? N13A C14A N22A 116.1(6) . . ? C15A C14A N22A 121.7(6) . . ? N13B C14B C15B 122.1(6) . . ? N13B C14B N22B 116.9(6) . . ? C15B C14B N22B 120.9(6) . . ? C14A C15A C10A 117.3(6) . . ? C14A C15A H15A 121.3 . . ? C10A C15A H15A 121.3 . . ? C10B C15B C14B 117.3(6) . . ? C10B C15B H15B 121.4 . . ? C14B C15B H15B 121.4 . . ? C17A C16A C21A 120.3(7) . . ? C17A C16A C12A 121.7(7) . . ? C21A C16A C12A 118.0(7) . . ? C21B C16B C17B 119.6(6) . . ? C21B C16B C12B 121.7(6) . . ? C17B C16B C12B 118.6(6) . . ? C18A C17A C16A 120.0(9) . . ? C18A C17A H17A 120.0 . . ? C16A C17A H17A 120.0 . . ? C18B C17B C16B 119.9(7) . . ? C18B C17B H17B 120.0 . . ? C16B C17B H17B 120.0 . . ? C19A C18A C17A 120.4(10) . . ? C19A C18A H18A 119.8 . . ? C17A C18A H18A 119.8 . . ? C19B C18B C17B 120.3(7) . . ? C19B C18B H18B 119.8 . . ? C17B C18B H18B 119.8 . . ? C18A C19A C20A 120.9(10) . . ? C18A C19A H19A 119.6 . . ? C20A C19A H19A 119.6 . . ? C20B C19B C18B 119.8(7) . . ? C20B C19B H19B 120.1 . . ? C18B C19B H19B 120.1 . . ? C19A C20A C21A 121.1(10) . . ? C19A C20A H20A 119.4 . . ? C21A C20A H20A 119.4 . . ? C19B C20B C21B 120.1(7) . . ? C19B C20B H20B 120.0 . . ? C21B C20B H20B 120.0 . . ? C16A C21A C20A 117.3(9) . . ? C16A C21A H21A 121.4 . . ? C20A C21A H21A 121.4 . . ? C16B C21B C20B 120.2(7) . . ? C16B C21B H21B 119.9 . . ? C20B C21B H21B 119.9 . . ? N22A C23A H23A 109.5 . . ? N22A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? N22A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? N22B C23B H23D 109.5 . . ? N22B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? N22B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C25A N24A N22A 123.8(7) . . ? C25A N24A Zn2 117.3(6) . . ? N22A N24A Zn2 118.8(4) . . ? N24A C25A C26A 115.1(7) . . ? N24A C25A H25A 122.4 . . ? C26A C25A H25A 122.4 . . ? N24B C25B C26B 114.6(7) . . ? N24B C25B H25B 122.7 . . ? C26B C25B H25B 122.7 . . ? C27A C26A N30A 108.6(8) . . ? C27A C26A C25A 133.0(8) . . ? N30A C26A C25A 118.4(7) . . ? C27B C26B N30B 109.2(8) . . ? C27B C26B C25B 132.6(9) . . ? N30B C26B C25B 118.0(6) . . ? N28A C27A C26A 106.0(8) . . ? N28A C27A H27A 127.0 . . ? C26A C27A H27A 127.0 . . ? C26B C27B N28N 106.2(8) . . ? C26B C27B H27B 126.9 . . ? N28N C27B H27B 126.9 . . ? N30A C29A N28A 110.6(8) . . ? N30A C29A H29A 124.7 . . ? N28A C29A H29A 124.7 . . ? N30B C29B N28N 109.6(8) . . ? N30B C29B H29B 125.2 . . ? N28N C29B H29B 125.2 . . ? N31 C32 C33 177.3(12) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N34 C35 C36 180.000(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? 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 N1B Zn1 N1A C2A 91.0(7) . . . . ? N7B Zn1 N1A C2A 14.9(7) . . . . ? N7A Zn1 N1A C2A -178.8(7) . . . . ? N11B Zn1 N1A C2A -57.2(7) . . . . ? N11A Zn1 N1A C2A -165.5(6) . . . . ? N1B Zn1 N1A C5A -83.6(5) . . . . ? N7B Zn1 N1A C5A -159.7(4) . . . . ? N7A Zn1 N1A C5A 6.7(4) . . . . ? N11B Zn1 N1A C5A 128.2(4) . . . . ? N11A Zn1 N1A C5A 19.9(6) . . . . ? N1A Zn1 N1B C2B 90.2(8) . . . . ? N7B Zn1 N1B C2B -174.1(9) . . . . ? N7A Zn1 N1B C2B 14.8(8) . . . . ? N11B Zn1 N1B C2B -172.6(7) . . . . ? N11A Zn1 N1B C2B -57.3(8) . . . . ? N1A Zn1 N1B C5B -93.2(5) . . . . ? N7B Zn1 N1B C5B 2.5(5) . . . . ? N7A Zn1 N1B C5B -168.6(5) . . . . ? N11B Zn1 N1B C5B 4.1(7) . . . . ? N11A Zn1 N1B C5B 119.4(5) . . . . ? N1A Zn1 N7A C6A -7.5(5) . . . . ? N1B Zn1 N7A C6A 87.3(5) . . . . ? N7B Zn1 N7A C6A 53.5(10) . . . . ? N11B Zn1 N7A C6A -88.1(5) . . . . ? N11A Zn1 N7A C6A -179.8(5) . . . . ? N1A Zn1 N7A N8A 179.6(5) . . . . ? N1B Zn1 N7A N8A -85.6(5) . . . . ? N7B Zn1 N7A N8A -119.4(8) . . . . ? N11B Zn1 N7A N8A 98.9(5) . . . . ? N11A Zn1 N7A N8A 7.2(4) . . . . ? N1A Zn1 N7B C6B 88.9(5) . . . . ? N1B Zn1 N7B C6B -4.6(5) . . . . ? N7A Zn1 N7B C6B 30.4(11) . . . . ? N11B Zn1 N7B C6B 176.2(6) . . . . ? N11A Zn1 N7B C6B -90.9(6) . . . . ? N1A Zn1 N7B N8B -87.4(5) . . . . ? N1B Zn1 N7B N8B 179.1(5) . . . . ? N7A Zn1 N7B N8B -145.8(7) . . . . ? N11B Zn1 N7B N8B -0.1(5) . . . . ? N11A Zn1 N7B N8B 92.9(5) . . . . ? C6A N7A N8A C10A 179.2(6) . . . . ? Zn1 N7A N8A C10A -8.0(7) . . . . ? C6A N7A N8A C9A 1.7(10) . . . . ? Zn1 N7A N8A C9A 174.5(5) . . . . ? C6B N7B N8B C10B -176.2(6) . . . . ? Zn1 N7B N8B C10B -0.1(8) . . . . ? C6B N7B N8B C9B -1.8(10) . . . . ? Zn1 N7B N8B C9B 174.3(6) . . . . ? N1A Zn1 N11A C12A 165.7(5) . . . . ? N1B Zn1 N11A C12A -90.2(5) . . . . ? N7B Zn1 N11A C12A -14.8(6) . . . . ? N7A Zn1 N11A C12A 179.2(5) . . . . ? N11B Zn1 N11A C12A 60.6(5) . . . . ? N1A Zn1 N11A C10A -19.1(6) . . . . ? N1B Zn1 N11A C10A 85.0(4) . . . . ? N7B Zn1 N11A C10A 160.5(4) . . . . ? N7A Zn1 N11A C10A -5.5(4) . . . . ? N11B Zn1 N11A C10A -124.2(4) . . . . ? N1A Zn1 N11B C12B -74.7(5) . . . . ? N1B Zn1 N11B C12B -173.6(5) . . . . ? N7B Zn1 N11B C12B -172.0(6) . . . . ? N7A Zn1 N11B C12B -2.1(6) . . . . ? N11A Zn1 N11B C12B 73.0(5) . . . . ? N1A Zn1 N11B C10B 97.4(5) . . . . ? N1B Zn1 N11B C10B -1.4(7) . . . . ? N7B Zn1 N11B C10B 0.2(4) . . . . ? N7A Zn1 N11B C10B 170.1(4) . . . . ? N11A Zn1 N11B C10B -114.8(5) . . . . ? N30A Zn2 N13A C12A 173.5(5) . . . . ? N30B Zn2 N13A C12A 76.3(5) 2_655 . . . ? N24B Zn2 N13A C12A 3.2(6) 2_655 . . . ? N24A Zn2 N13A C12A 173.3(5) . . . . ? N13B Zn2 N13A C12A -72.2(5) 2_655 . . . ? N30A Zn2 N13A C14A -1.8(7) . . . . ? N30B Zn2 N13A C14A -99.0(5) 2_655 . . . ? N24B Zn2 N13A C14A -172.1(4) 2_655 . . . ? N24A Zn2 N13A C14A -1.9(4) . . . . ? N13B Zn2 N13A C14A 112.5(4) 2_655 . . . ? C14B N22B N24B C25B -172.4(6) . . . . ? C23B N22B N24B C25B 2.8(11) . . . . ? C14B N22B N24B Zn2 15.9(8) . . . 2_655 ? C23B N22B N24B Zn2 -168.9(6) . . . 2_655 ? N30B Zn2 N30A C29A -84.4(8) 2_655 . . . ? N24B Zn2 N30A C29A -8.2(8) 2_655 . . . ? N24A Zn2 N30A C29A -179.6(8) . . . . ? N13B Zn2 N30A C29A 65.2(8) 2_655 . . . ? N13A Zn2 N30A C29A -179.8(7) . . . . ? N30B Zn2 N30A C26A 90.4(5) 2_655 . . . ? N24B Zn2 N30A C26A 166.5(5) 2_655 . . . ? N24A Zn2 N30A C26A -4.8(4) . . . . ? N13B Zn2 N30A C26A -120.0(5) 2_655 . . . ? N13A Zn2 N30A C26A -5.0(7) . . . . ? C5A N1A C2A N3A 0.9(7) . . . . ? Zn1 N1A C2A N3A -173.9(5) . . . . ? C4A N3A C2A N1A -0.5(8) . . . . ? C5B N1B C2B N3B 0.5(9) . . . . ? Zn1 N1B C2B N3B 177.3(6) . . . . ? C4B N3B C2B N1B -0.5(10) . . . . ? C2A N3A C4A C5A -0.1(8) . . . . ? C2B N3B C4B C5B 0.3(10) . . . . ? N3A C4A C5A N1A 0.6(8) . . . . ? N3A C4A C5A C6A -177.7(7) . . . . ? C2A N1A C5A C4A -0.9(7) . . . . ? Zn1 N1A C5A C4A 175.4(4) . . . . ? C2A N1A C5A C6A 177.7(6) . . . . ? Zn1 N1A C5A C6A -6.0(7) . . . . ? N3B C4B C5B N1B 0.0(9) . . . . ? N3B C4B C5B C6B -177.0(8) . . . . ? C2B N1B C5B C4B -0.3(9) . . . . ? Zn1 N1B C5B C4B -178.1(5) . . . . ? C2B N1B C5B C6B 177.2(7) . . . . ? Zn1 N1B C5B C6B -0.7(8) . . . . ? N8A N7A C6A C5A 179.3(6) . . . . ? Zn1 N7A C6A C5A 6.4(7) . . . . ? C4A C5A C6A N7A 178.0(7) . . . . ? N1A C5A C6A N7A -0.1(9) . . . . ? N8B N7B C6B C5B -178.2(6) . . . . ? Zn1 N7B C6B C5B 5.6(8) . . . . ? C4B C5B C6B N7B 173.5(8) . . . . ? N1B C5B C6B N7B -3.2(10) . . . . ? N7A N8A C10A N11A 2.7(8) . . . . ? C9A N8A C10A N11A -180.0(7) . . . . ? N7A N8A C10A C15A -178.4(6) . . . . ? C9A N8A C10A C15A -1.0(11) . . . . ? C12A N11A C10A N8A 179.3(5) . . . . ? Zn1 N11A C10A N8A 3.5(7) . . . . ? C12A N11A C10A C15A 0.4(9) . . . . ? Zn1 N11A C10A C15A -175.4(5) . . . . ? N7B N8B C10B C15B -178.0(6) . . . . ? C9B N8B C10B C15B 7.8(11) . . . . ? N7B N8B C10B N11B 0.2(9) . . . . ? C9B N8B C10B N11B -174.0(7) . . . . ? C12B N11B C10B N8B 172.9(6) . . . . ? Zn1 N11B C10B N8B -0.3(7) . . . . ? C12B N11B C10B C15B -8.9(9) . . . . ? Zn1 N11B C10B C15B 178.0(5) . . . . ? C10A N11A C12A N13A 1.5(9) . . . . ? Zn1 N11A C12A N13A 176.8(4) . . . . ? C10A N11A C12A C16A -176.4(6) . . . . ? Zn1 N11A C12A C16A -1.2(8) . . . . ? C14A N13A C12A N11A -4.9(9) . . . . ? Zn2 N13A C12A N11A 179.8(4) . . . . ? C14A N13A C12A C16A 173.1(6) . . . . ? Zn2 N13A C12A C16A -2.2(8) . . . . ? C14B N13B C12B N11B -1.6(10) . . . . ? Zn2 N13B C12B N11B -178.6(5) 2_655 . . . ? C14B N13B C12B C16B 177.4(6) . . . . ? Zn2 N13B C12B C16B 0.4(9) 2_655 . . . ? C10B N11B C12B N13B 6.9(9) . . . . ? Zn1 N11B C12B N13B 179.1(5) . . . . ? C10B N11B C12B C16B -172.1(6) . . . . ? Zn1 N11B C12B C16B 0.1(8) . . . . ? C12A N13A C14A C15A 6.4(9) . . . . ? Zn2 N13A C14A C15A -177.8(5) . . . . ? C12A N13A C14A N22A -173.7(5) . . . . ? Zn2 N13A C14A N22A 2.2(7) . . . . ? N24A N22A C14A N13A -0.8(8) . . . . ? C23A N22A C14A N13A 172.0(6) . . . . ? N24A N22A C14A C15A 179.1(6) . . . . ? C23A N22A C14A C15A -8.1(10) . . . . ? C12B N13B C14B C15B -2.1(10) . . . . ? Zn2 N13B C14B C15B 175.4(5) 2_655 . . . ? C12B N13B C14B N22B 179.6(6) . . . . ? Zn2 N13B C14B N22B -3.0(8) 2_655 . . . ? N24B N22B C14B N13B -8.1(9) . . . . ? C23B N22B C14B N13B 176.8(7) . . . . ? N24B N22B C14B C15B 173.5(6) . . . . ? C23B N22B C14B C15B -1.6(11) . . . . ? N13A C14A C15A C10A -4.8(10) . . . . ? N22A C14A C15A C10A 175.3(6) . . . . ? N8A C10A C15A C14A -177.7(6) . . . . ? N11A C10A C15A C14A 1.2(9) . . . . ? N8B C10B C15B C14B -176.0(6) . . . . ? N11B C10B C15B C14B 5.8(10) . . . . ? N13B C14B C15B C10B -0.1(10) . . . . ? N22B C14B C15B C10B 178.2(6) . . . . ? N11A C12A C16A C17A -98.3(8) . . . . ? N13A C12A C16A C17A 83.5(8) . . . . ? N11A C12A C16A C21A 81.4(8) . . . . ? N13A C12A C16A C21A -96.8(8) . . . . ? N13B C12B C16B C21B 101.1(7) . . . . ? N11B C12B C16B C21B -79.7(8) . . . . ? N13B C12B C16B C17B -81.5(8) . . . . ? N11B C12B C16B C17B 97.6(7) . . . . ? C21A C16A C17A C18A 1.5(11) . . . . ? C12A C16A C17A C18A -178.8(7) . . . . ? C21B C16B C17B C18B 0.4(10) . . . . ? C12B C16B C17B C18B -177.0(6) . . . . ? C16A C17A C18A C19A -0.3(13) . . . . ? C16B C17B C18B C19B 0.3(11) . . . . ? C17A C18A C19A C20A -0.7(15) . . . . ? C17B C18B C19B C20B -1.8(11) . . . . ? C18A C19A C20A C21A 0.4(16) . . . . ? C18B C19B C20B C21B 2.6(11) . . . . ? C17A C16A C21A C20A -1.7(11) . . . . ? C12A C16A C21A C20A 178.5(7) . . . . ? C19A C20A C21A C16A 0.8(13) . . . . ? C17B C16B C21B C20B 0.3(10) . . . . ? C12B C16B C21B C20B 177.7(6) . . . . ? C19B C20B C21B C16B -1.9(11) . . . . ? C14A N22A N24A C25A 174.8(6) . . . . ? C23A N22A N24A C25A 1.6(10) . . . . ? C14A N22A N24A Zn2 -1.0(7) . . . . ? C23A N22A N24A Zn2 -174.1(5) . . . . ? N30A Zn2 N24A C25A 5.6(5) . . . . ? N30B Zn2 N24A C25A -88.1(5) 2_655 . . . ? N24B Zn2 N24A C25A -31.4(11) 2_655 . . . ? N13B Zn2 N24A C25A 94.8(5) 2_655 . . . ? N13A Zn2 N24A C25A -174.5(5) . . . . ? N30A Zn2 N24A N22A -178.4(5) . . . . ? N30B Zn2 N24A N22A 87.9(5) 2_655 . . . ? N24B Zn2 N24A N22A 144.6(8) 2_655 . . . ? N13B Zn2 N24A N22A -89.2(5) 2_655 . . . ? N13A Zn2 N24A N22A 1.5(4) . . . . ? N22A N24A C25A C26A 179.2(6) . . . . ? Zn2 N24A C25A C26A -5.0(8) . . . . ? N22B N24B C25B C26B -179.7(6) . . . . ? Zn2 N24B C25B C26B -8.0(8) 2_655 . . . ? C29A N30A C26A C27A 1.7(8) . . . . ? Zn2 N30A C26A C27A -174.9(5) . . . . ? C29A N30A C26A C25A -179.3(6) . . . . ? Zn2 N30A C26A C25A 4.1(8) . . . . ? N24A C25A C26A C27A 179.3(8) . . . . ? N24A C25A C26A N30A 0.5(10) . . . . ? C29B N30B C26B C27B 0.8(9) . . . . ? Zn2 N30B C26B C27B 170.5(5) 2_655 . . . ? C29B N30B C26B C25B -173.9(6) . . . . ? Zn2 N30B C26B C25B -4.2(8) 2_655 . . . ? N24B C25B C26B C27B -165.1(8) . . . . ? N24B C25B C26B N30B 8.1(10) . . . . ? C29A N28A C27A C26A 0.9(9) . . . . ? N30A C26A C27A N28A -1.6(9) . . . . ? C25A C26A C27A N28A 179.6(8) . . . . ? N30B C26B C27B N28N 0.0(9) . . . . ? C25B C26B C27B N28N 173.6(8) . . . . ? C29B N28N C27B C26B -0.7(10) . . . . ? C26A N30A C29A N28A -1.1(8) . . . . ? Zn2 N30A C29A N28A 173.8(5) . . . . ? C27A N28A C29A N30A 0.1(9) . . . . ? C26B N30B C29B N28N -1.2(8) . . . . ? Zn2 N30B C29B N28N -166.2(6) 2_655 . . . ? C27B N28N C29B N30B 1.2(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O45 H45A O24 0.85 2.07 2.903(9) 167.3 . O45 H45B O14 0.85 2.20 3.032(11) 167.9 7_556 O46 H46A O11 0.85 2.22 3.028(15) 158.3 2_656 O46 H46B O23 0.85 2.22 3.024(12) 158.2 7_556 O47 H47A O23 0.85 1.90 2.74(3) 171.5 7_556 O47 H47B O42 0.85 1.61 2.45(3) 170.5 4_545 N3A H3A O33B 0.86 2.08 2.856(15) 149.2 7 N3A H3A O31A 0.86 2.14 2.819(11) 135.2 7 N3B H3B O45 0.86 2.14 2.901(10) 147.1 . N28A H28A O47 0.86 1.89 2.63(3) 144.3 . N28A H28A O46 0.86 2.17 2.904(12) 143.3 . N28N H28N O32B 0.86 2.06 2.801(17) 143.3 2_655 N28N H28N O32A 0.86 2.12 2.938(12) 160.0 2_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.970 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.105 data_as840 _database_code_depnum_ccdc_archive 'CCDC 826154' _publ_section_title_footnote ; ? #<< paper footnote text ; # 4. TEXT _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; #Barbour, L. J. (2001). J. Supramol. Chem., 1, 189-191. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # 5. CHEMICAL DATA _publ_section_figure_captions ; ? #<< figure captions ; #============================================================================== # 6. CRYSTALLOGRAPHY _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_melting_point ? _chemical_formula_moiety 'C80 H80 Co4 N40, 7(F6 P), Cl, 8(C2 H3 N)' _chemical_formula_sum 'C96 H104 Cl Co4 F42 N48 P7' _chemical_formula_weight 3216.23 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n n m' _symmetry_space_group_name_Hall '-P 4ac 2bc' _symmetry_int_tables_number 134 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z' '-y+1/2, -x+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z' 'y-1/2, x-1/2, z' _cell_length_a 19.069(4) _cell_length_b 19.069 _cell_length_c 24.440(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8888(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3587 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.1 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9002 _exptl_absorpt_correction_T_max 0.9384 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20391 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.52 _reflns_number_total 5846 _reflns_number_gt 3167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The structure contains solvent accessible voids of 687 A**3. Despite numerous attempts, the solvent was not able to be modelled satisfactorily. This electron density was effectively removed by use of the program Squeeze. ; _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^)+(0.0600P)^2^+57.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5846 _refine_ls_number_parameters 221 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1792 _refine_ls_R_factor_gt 0.1242 _refine_ls_wR_factor_ref 0.2835 _refine_ls_wR_factor_gt 0.2589 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _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 0.51313(6) 0.2500 0.2500 0.0434(3) Uani 1 2 d S . . C1 C 0.6337(3) 0.3663(3) 0.2623(3) 0.0390(17) Uani 1 2 d S . . N2 N 0.5893(2) 0.3217(3) 0.28680(16) 0.0410(10) Uani 1 1 d . . . C3 C 0.5864(3) 0.3258(3) 0.3429(2) 0.0485(14) Uani 1 1 d . . . C4 C 0.6284(4) 0.3716(4) 0.3722(3) 0.053(2) Uani 1 2 d S . . H4A H 0.6260 0.3740 0.4101 0.063 Uiso 1 2 calc SR . . N5 N 0.5391(3) 0.2833(3) 0.36856(17) 0.0550(14) Uani 1 1 d . . . N6 N 0.5011(3) 0.2395(3) 0.33503(18) 0.0468(12) Uani 1 1 d . . . C7 C 0.4543(3) 0.1986(3) 0.3527(2) 0.0544(16) Uani 1 1 d . . . H7A H 0.4432 0.1951 0.3896 0.065 Uiso 1 1 calc R . . C8 C 0.4194(4) 0.1578(3) 0.3115(3) 0.0548(15) Uani 1 1 d . . . C9 C 0.3671(4) 0.1093(4) 0.3133(3) 0.0670(19) Uani 1 1 d . . . H9A H 0.3445 0.0927 0.3444 0.080 Uiso 1 1 calc R . . N10 N 0.3545(3) 0.0899(3) 0.2609(2) 0.0741(18) Uani 1 1 d . . . H10A H 0.3242 0.0594 0.2504 0.089 Uiso 1 1 calc R . . C11 C 0.3982(4) 0.1271(4) 0.2281(3) 0.0611(17) Uani 1 1 d . . . H11A H 0.3994 0.1234 0.1902 0.073 Uiso 1 1 calc R . . N12 N 0.4387(3) 0.1690(3) 0.25698(19) 0.0499(12) Uani 1 1 d . . . C13 C 0.6328(3) 0.3672(3) 0.2013(3) 0.0417(17) Uani 1 2 d S . . C14 C 0.6735(4) 0.3265(4) 0.1704(3) 0.063(3) Uani 1 2 d S . . H14A H 0.7047 0.2953 0.1866 0.076 Uiso 1 2 calc SR . . C15 C 0.6687(6) 0.3313(6) 0.1118(4) 0.091(4) Uani 1 2 d S . . H15A H 0.6970 0.3030 0.0901 0.109 Uiso 1 2 calc SR . . C16 C 0.6240(7) 0.3760(7) 0.0881(4) 0.101(5) Uani 1 2 d S . . H16A H 0.6216 0.3784 0.0502 0.121 Uiso 1 2 calc SR . . C17 C 0.5809(5) 0.4191(5) 0.1196(4) 0.080(4) Uani 1 2 d S . . H17A H 0.5500 0.4500 0.1028 0.097 Uiso 1 2 calc SR . . C18 C 0.5848(4) 0.4152(4) 0.1771(3) 0.049(2) Uani 1 2 d S . . H18A H 0.5565 0.4435 0.1988 0.059 Uiso 1 2 calc SR . . C19 C 0.5305(4) 0.2812(4) 0.4286(2) 0.076(2) Uani 1 1 d . . . H19A H 0.5604 0.3157 0.4452 0.114 Uiso 1 1 calc R . . H19B H 0.5429 0.2354 0.4419 0.114 Uiso 1 1 calc R . . H19C H 0.4825 0.2910 0.4379 0.114 Uiso 1 1 calc R . . N20 N 0.4936(8) 0.2711(8) 0.6781(8) 0.214(6) Uiso 1 1 d . . . C21 C 0.4930(10) 0.2837(10) 0.6290(9) 0.200(7) Uiso 1 1 d . . . C22 C 0.5334(9) 0.2699(9) 0.5752(8) 0.207(7) Uiso 1 1 d . . . H22A H 0.5075 0.2889 0.5450 0.311 Uiso 1 1 calc R . . H22B H 0.5392 0.2203 0.5702 0.311 Uiso 1 1 calc R . . H22C H 0.5786 0.2919 0.5771 0.311 Uiso 1 1 calc R . . P1 P 0.7500 0.2500 0.5359(2) 0.125(2) Uani 1 4 d S . . F1 F 0.7924(3) 0.2076(3) 0.4885(4) 0.126(3) Uiso 1 2 d S . . F2 F 0.6901(4) 0.1901(4) 0.5363(4) 0.168(4) Uiso 1 2 d S . . F3 F 0.7913(5) 0.2087(5) 0.5821(6) 0.197(5) Uiso 1 2 d S . . P2 P 0.38833(12) 0.11167(12) 0.5000 0.0657(7) Uani 1 2 d S . . F4 F 0.3857(4) 0.1909(4) 0.4825(3) 0.097(2) Uiso 0.67 1 d P A 1 F5 F 0.4676(4) 0.1119(5) 0.4824(3) 0.108(3) Uiso 0.67 1 d P A 1 F6 F 0.3669(4) 0.0925(4) 0.4396(3) 0.094(2) Uiso 0.67 1 d P A 1 F4' F 0.4232(10) 0.0719(9) 0.4513(7) 0.109(5) Uiso 0.33 1 d P A 2 F5' F 0.3465(9) 0.1518(9) 0.4517(6) 0.099(4) Uiso 0.33 1 d P A 2 F6' F 0.4423(10) 0.1726(9) 0.4966(7) 0.111(5) Uiso 0.33 1 d P A 2 P3 P 0.5000 0.5000 0.5000 0.164(6) Uiso 0.50 4 d SPD . 1 F7 F 0.4945(9) 0.5055(9) 0.43504(13) 0.177(5) Uiso 0.50 2 d SPD B 1 F8 F 0.55884(11) 0.44116(11) 0.4937(10) 0.177(5) Uiso 0.50 2 d SPD C 1 F9 F 0.44088(8) 0.44088(8) 0.5000 0.177(5) Uiso 0.50 2 d SPD D 1 Cl1 Cl 0.4732(13) 0.4403(13) 0.3997(9) 0.120(7) Uiso 0.125 1 d P E 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 0.0469(7) 0.0502(7) 0.0332(5) -0.0008(5) 0.000 0.000 C1 0.042(3) 0.042(3) 0.033(4) -0.002(2) 0.002(2) 0.009(3) N2 0.040(3) 0.053(3) 0.030(2) -0.006(2) 0.0034(19) -0.001(2) C3 0.050(4) 0.062(4) 0.033(3) -0.001(3) 0.005(2) 0.000(3) C4 0.065(4) 0.065(4) 0.028(4) -0.007(3) 0.007(3) -0.021(5) N5 0.072(4) 0.067(4) 0.026(2) -0.003(2) 0.006(2) -0.016(3) N6 0.055(3) 0.048(3) 0.037(2) -0.003(2) 0.008(2) -0.004(2) C7 0.060(4) 0.066(4) 0.036(3) 0.003(3) 0.018(3) 0.001(3) C8 0.065(4) 0.044(4) 0.055(3) 0.005(3) 0.006(3) 0.000(3) C9 0.067(5) 0.061(4) 0.073(5) 0.002(4) 0.008(4) -0.013(4) N10 0.077(4) 0.070(4) 0.075(4) 0.009(3) -0.016(3) -0.022(3) C11 0.069(5) 0.057(4) 0.057(4) -0.003(3) 0.001(3) 0.005(4) N12 0.055(3) 0.050(3) 0.045(3) 0.004(2) -0.004(2) -0.003(2) C13 0.043(3) 0.043(3) 0.039(4) -0.007(3) 0.007(3) -0.009(3) C14 0.079(4) 0.079(4) 0.032(4) -0.007(3) 0.007(3) 0.002(6) C15 0.116(7) 0.116(7) 0.042(6) -0.031(5) 0.031(5) -0.023(9) C16 0.136(8) 0.136(8) 0.030(5) 0.013(6) -0.013(6) -0.052(10) C17 0.100(6) 0.100(6) 0.041(5) 0.022(5) -0.022(5) -0.034(7) C18 0.056(3) 0.056(3) 0.034(4) 0.010(3) -0.010(3) -0.010(4) C19 0.102(6) 0.101(6) 0.024(3) -0.004(3) 0.010(3) -0.026(5) P1 0.162(4) 0.162(4) 0.052(2) 0.000 0.000 -0.058(5) P2 0.0751(11) 0.0751(11) 0.0470(12) 0.0149(9) 0.0149(9) -0.0103(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 N6 2.100(4) 6 ? Co1 N6 2.100(4) . ? Co1 N12 2.104(5) 6 ? Co1 N12 2.104(5) . ? Co1 N2 2.189(5) . ? Co1 N2 2.189(4) 6 ? C1 N2 1.341(5) . ? C1 N2 1.341(5) 15_665 ? C1 C13 1.490(10) . ? N2 C3 1.374(6) . ? C3 N5 1.365(7) . ? C3 C4 1.385(7) . ? C4 C3 1.385(7) 15_665 ? C4 H4A 0.9300 . ? N5 N6 1.376(6) . ? N5 C19 1.478(7) . ? N6 C7 1.261(7) . ? C7 C8 1.434(9) . ? C7 H7A 0.9300 . ? C8 C9 1.361(9) . ? C8 N12 1.399(7) . ? C9 N10 1.353(9) . ? C9 H9A 0.9300 . ? N10 C11 1.355(9) . ? N10 H10A 0.8600 . ? C11 N12 1.317(8) . ? C11 H11A 0.9300 . ? C13 C14 1.332(12) . ? C13 C18 1.423(12) . ? C14 C15 1.438(13) . ? C14 H14A 0.9300 . ? C15 C16 1.338(19) . ? C15 H15A 0.9300 . ? C16 C17 1.393(19) . ? C16 H16A 0.9300 . ? C17 C18 1.409(12) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? N20 C21 1.22(2) . ? C21 C22 1.55(2) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? P1 F3 1.587(13) . ? P1 F3 1.587(13) 2_655 ? P1 F2 1.615(12) . ? P1 F2 1.615(12) 2_655 ? P1 F1 1.627(9) 2_655 ? P1 F1 1.627(9) . ? P2 F6' 1.555(17) . ? P2 F6' 1.555(17) 8_556 ? P2 F4' 1.561(16) 8_556 ? P2 F4' 1.561(16) . ? P2 F5 1.572(9) 8_556 ? P2 F5 1.572(9) . ? P2 F4 1.572(8) 8_556 ? P2 F4 1.572(8) . ? P2 F6 1.574(7) . ? P2 F6 1.574(8) 8_556 ? P2 F5' 1.618(15) 8_556 ? P2 F5' 1.618(15) . ? P3 F9 1.594(2) 9_666 ? P3 F9 1.594(2) . ? P3 F7 1.594(2) . ? P3 F7 1.594(2) 9_666 ? P3 F8 1.594(2) 9_666 ? P3 F8 1.594(2) . ? Cl1 Cl1 2.33(5) 15_665 ? 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 N6 Co1 N6 167.5(3) 6 . ? N6 Co1 N12 77.07(18) 6 6 ? N6 Co1 N12 94.38(19) . 6 ? N6 Co1 N12 94.38(19) 6 . ? N6 Co1 N12 77.06(18) . . ? N12 Co1 N12 95.2(3) 6 . ? N6 Co1 N2 114.80(18) 6 . ? N6 Co1 N2 74.07(17) . . ? N12 Co1 N2 91.30(18) 6 . ? N12 Co1 N2 150.81(17) . . ? N6 Co1 N2 74.07(17) 6 6 ? N6 Co1 N2 114.81(18) . 6 ? N12 Co1 N2 150.81(17) 6 6 ? N12 Co1 N2 91.30(18) . 6 ? N2 Co1 N2 96.8(2) . 6 ? N2 C1 N2 126.8(6) . 15_665 ? N2 C1 C13 116.6(3) . . ? N2 C1 C13 116.6(3) 15_665 . ? C1 N2 C3 115.9(5) . . ? C1 N2 Co1 129.1(4) . . ? C3 N2 Co1 114.7(4) . . ? N5 C3 N2 116.9(5) . . ? N5 C3 C4 121.3(5) . . ? N2 C3 C4 121.8(6) . . ? C3 C4 C3 117.6(7) 15_665 . ? C3 C4 H4A 121.2 15_665 . ? C3 C4 H4A 121.2 . . ? C3 N5 N6 115.7(4) . . ? C3 N5 C19 123.1(5) . . ? N6 N5 C19 121.1(5) . . ? C7 N6 N5 123.0(5) . . ? C7 N6 Co1 118.3(4) . . ? N5 N6 Co1 118.3(3) . . ? N6 C7 C8 115.1(5) . . ? N6 C7 H7A 122.5 . . ? C8 C7 H7A 122.5 . . ? C9 C8 N12 109.0(6) . . ? C9 C8 C7 133.3(6) . . ? N12 C8 C7 117.6(5) . . ? N10 C9 C8 106.6(6) . . ? N10 C9 H9A 126.7 . . ? C8 C9 H9A 126.7 . . ? C9 N10 C11 107.9(6) . . ? C9 N10 H10A 126.0 . . ? C11 N10 H10A 126.0 . . ? N12 C11 N10 111.2(6) . . ? N12 C11 H11A 124.4 . . ? N10 C11 H11A 124.4 . . ? C11 N12 C8 105.2(5) . . ? C11 N12 Co1 143.0(4) . . ? C8 N12 Co1 111.5(4) . . ? C14 C13 C18 120.9(8) . . ? C14 C13 C1 123.7(8) . . ? C18 C13 C1 115.4(7) . . ? C13 C14 C15 119.4(11) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C16 C15 C14 120.7(11) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 120.9(9) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C16 C17 C18 119.2(11) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C17 C18 C13 118.8(10) . . ? C17 C18 H18A 120.6 . . ? C13 C18 H18A 120.6 . . ? N5 C19 H19A 109.5 . . ? N5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N20 C21 C22 142.7(18) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? F3 P1 F3 89.1(10) . 2_655 ? F3 P1 F2 89.7(3) . . ? F3 P1 F2 89.7(3) 2_655 . ? F3 P1 F2 89.7(3) . 2_655 ? F3 P1 F2 89.7(3) 2_655 2_655 ? F2 P1 F2 179.3(9) . 2_655 ? F3 P1 F1 179.9(8) . 2_655 ? F3 P1 F1 90.8(6) 2_655 2_655 ? F2 P1 F1 90.3(3) . 2_655 ? F2 P1 F1 90.3(3) 2_655 2_655 ? F3 P1 F1 90.8(6) . . ? F3 P1 F1 179.9(8) 2_655 . ? F2 P1 F1 90.3(3) . . ? F2 P1 F1 90.3(3) 2_655 . ? F1 P1 F1 89.3(7) 2_655 . ? F6' P2 F6' 173.1(14) . 8_556 ? F6' P2 F4' 92.1(10) . 8_556 ? F6' P2 F4' 92.3(9) 8_556 8_556 ? F6' P2 F4' 92.3(9) . . ? F6' P2 F4' 92.1(10) 8_556 . ? F4' P2 F4' 99.7(13) 8_556 . ? F6' P2 F5 137.3(9) . 8_556 ? F6' P2 F5 49.2(7) 8_556 8_556 ? F4' P2 F5 51.9(7) 8_556 8_556 ? F4' P2 F5 75.0(7) . 8_556 ? F6' P2 F5 49.2(7) . . ? F6' P2 F5 137.3(9) 8_556 . ? F4' P2 F5 75.0(7) 8_556 . ? F4' P2 F5 51.9(7) . . ? F5 P2 F5 94.6(7) 8_556 . ? F6' P2 F4 128.9(9) . 8_556 ? F4' P2 F4 105.8(7) 8_556 8_556 ? F4' P2 F4 129.3(8) . 8_556 ? F5 P2 F4 87.3(4) 8_556 8_556 ? F5 P2 F4 178.1(5) . 8_556 ? F6' P2 F4 128.9(9) 8_556 . ? F4' P2 F4 129.3(8) 8_556 . ? F4' P2 F4 105.8(7) . . ? F5 P2 F4 178.1(5) 8_556 . ? F5 P2 F4 87.3(4) . . ? F4 P2 F4 90.8(6) 8_556 . ? F6' P2 F6 107.2(7) . . ? F6' P2 F6 72.7(7) 8_556 . ? F4' P2 F6 138.0(9) 8_556 . ? F5 P2 F6 91.9(4) 8_556 . ? F5 P2 F6 89.7(4) . . ? F4 P2 F6 90.8(4) 8_556 . ? F4 P2 F6 87.7(4) . . ? F6' P2 F6 72.7(7) . 8_556 ? F6' P2 F6 107.2(7) 8_556 8_556 ? F4' P2 F6 138.0(9) . 8_556 ? F5 P2 F6 89.7(4) 8_556 8_556 ? F5 P2 F6 91.9(4) . 8_556 ? F4 P2 F6 87.7(4) 8_556 8_556 ? F4 P2 F6 90.8(4) . 8_556 ? F6 P2 F6 177.8(7) . 8_556 ? F6' P2 F5' 89.0(9) . 8_556 ? F6' P2 F5' 86.2(9) 8_556 8_556 ? F4' P2 F5' 83.3(8) 8_556 8_556 ? F4' P2 F5' 176.7(10) . 8_556 ? F5 P2 F5' 105.9(6) 8_556 8_556 ? F5 P2 F5' 130.8(7) . 8_556 ? F4 P2 F5' 48.0(6) 8_556 8_556 ? F4 P2 F5' 73.1(6) . 8_556 ? F6 P2 F5' 132.5(8) . 8_556 ? F6 P2 F5' 45.3(6) 8_556 8_556 ? F6' P2 F5' 86.2(9) . . ? F6' P2 F5' 89.0(9) 8_556 . ? F4' P2 F5' 176.7(10) 8_556 . ? F4' P2 F5' 83.3(8) . . ? F5 P2 F5' 130.8(7) 8_556 . ? F5 P2 F5' 105.9(6) . . ? F4 P2 F5' 73.1(6) 8_556 . ? F4 P2 F5' 48.0(6) . . ? F6 P2 F5' 45.3(6) . . ? F6 P2 F5' 132.5(8) 8_556 . ? F5' P2 F5' 93.8(11) 8_556 . ? F9 P3 F9 180.0 9_666 . ? F9 P3 F7 90.000(2) 9_666 . ? F9 P3 F7 90.000(1) . . ? F9 P3 F7 90.001(1) 9_666 9_666 ? F9 P3 F7 89.998(2) . 9_666 ? F7 P3 F7 180.0(12) . 9_666 ? F9 P3 F8 90.000(12) 9_666 9_666 ? F9 P3 F8 89.998(12) . 9_666 ? F7 P3 F8 90.2(12) . 9_666 ? F7 P3 F8 89.8(12) 9_666 9_666 ? F9 P3 F8 90.002(12) 9_666 . ? F9 P3 F8 90.000(12) . . ? F7 P3 F8 89.8(12) . . ? F7 P3 F8 90.2(12) 9_666 . ? F8 P3 F8 180.00(11) 9_666 . ? 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 C1 N2 C3 4.7(11) 15_665 . . . ? C13 C1 N2 C3 -174.6(6) . . . . ? N2 C1 N2 Co1 178.1(4) 15_665 . . . ? C13 C1 N2 Co1 -1.2(10) . . . . ? N6 Co1 N2 C1 -7.0(6) 6 . . . ? N6 Co1 N2 C1 -177.5(6) . . . . ? N12 Co1 N2 C1 -83.3(6) 6 . . . ? N12 Co1 N2 C1 173.7(5) . . . . ? N2 Co1 N2 C1 68.6(5) 6 . . . ? N6 Co1 N2 C3 166.5(4) 6 . . . ? N6 Co1 N2 C3 -4.0(4) . . . . ? N12 Co1 N2 C3 90.2(4) 6 . . . ? N12 Co1 N2 C3 -12.8(7) . . . . ? N2 Co1 N2 C3 -117.9(5) 6 . . . ? C1 N2 C3 N5 176.9(6) . . . . ? Co1 N2 C3 N5 2.5(7) . . . . ? C1 N2 C3 C4 -2.0(10) . . . . ? Co1 N2 C3 C4 -176.4(6) . . . . ? N5 C3 C4 C3 -179.0(5) . . . 15_665 ? N2 C3 C4 C3 -0.2(13) . . . 15_665 ? N2 C3 N5 N6 1.9(8) . . . . ? C4 C3 N5 N6 -179.2(7) . . . . ? N2 C3 N5 C19 179.2(6) . . . . ? C4 C3 N5 C19 -1.8(11) . . . . ? C3 N5 N6 C7 -178.2(6) . . . . ? C19 N5 N6 C7 4.4(10) . . . . ? C3 N5 N6 Co1 -5.7(7) . . . . ? C19 N5 N6 Co1 176.9(5) . . . . ? N6 Co1 N6 C7 41.5(5) 6 . . . ? N12 Co1 N6 C7 87.9(5) 6 . . . ? N12 Co1 N6 C7 -6.4(5) . . . . ? N2 Co1 N6 C7 178.0(5) . . . . ? N2 Co1 N6 C7 -91.7(5) 6 . . . ? N6 Co1 N6 N5 -131.4(4) 6 . . . ? N12 Co1 N6 N5 -84.9(4) 6 . . . ? N12 Co1 N6 N5 -179.2(5) . . . . ? N2 Co1 N6 N5 5.2(4) . . . . ? N2 Co1 N6 N5 95.4(4) 6 . . . ? N5 N6 C7 C8 179.0(6) . . . . ? Co1 N6 C7 C8 6.5(8) . . . . ? N6 C7 C8 C9 -179.5(8) . . . . ? N6 C7 C8 N12 -2.1(9) . . . . ? N12 C8 C9 N10 0.7(8) . . . . ? C7 C8 C9 N10 178.3(7) . . . . ? C8 C9 N10 C11 -0.7(8) . . . . ? C9 N10 C11 N12 0.5(8) . . . . ? N10 C11 N12 C8 0.0(8) . . . . ? N10 C11 N12 Co1 -172.9(5) . . . . ? C9 C8 N12 C11 -0.4(8) . . . . ? C7 C8 N12 C11 -178.4(6) . . . . ? C9 C8 N12 Co1 174.9(5) . . . . ? C7 C8 N12 Co1 -3.1(7) . . . . ? N6 Co1 N12 C11 6.5(8) 6 . . . ? N6 Co1 N12 C11 177.2(8) . . . . ? N12 Co1 N12 C11 83.8(7) 6 . . . ? N2 Co1 N12 C11 -174.2(6) . . . . ? N2 Co1 N12 C11 -67.7(8) 6 . . . ? N6 Co1 N12 C8 -166.1(4) 6 . . . ? N6 Co1 N12 C8 4.6(4) . . . . ? N12 Co1 N12 C8 -88.7(4) 6 . . . ? N2 Co1 N12 C8 13.3(7) . . . . ? N2 Co1 N12 C8 119.8(4) 6 . . . ? N2 C1 C13 C14 -90.3(6) . . . . ? N2 C1 C13 C14 90.3(6) 15_665 . . . ? N2 C1 C13 C18 89.7(6) . . . . ? N2 C1 C13 C18 -89.7(6) 15_665 . . . ? C18 C13 C14 C15 0.000(2) . . . . ? C1 C13 C14 C15 180.000(2) . . . . ? C13 C14 C15 C16 0.000(3) . . . . ? C14 C15 C16 C17 0.000(3) . . . . ? C15 C16 C17 C18 0.000(2) . . . . ? C16 C17 C18 C13 0.000(3) . . . . ? C14 C13 C18 C17 0.000(2) . . . . ? C1 C13 C18 C17 180.000(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10A N20 0.86 2.27 3.027(17) 146.5 4_554 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.025 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.115