# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dongfeng Li' _publ_contact_author_email dfli@mail.ccnu.edu.cn loop_ _publ_author_name 'Lili Wen' 'Hua Qu' 'Bingguang Zhang' 'Li Zhou' 'Dongfeng Li' data_1 _database_code_depnum_ccdc_archive 'CCDC 866677' #TrackingRef '- new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H19 Mn N5 O4, 0.26(H0.40 O0.20)' _chemical_formula_sum 'C26 H19.20 Mn N5 O4.10' _chemical_formula_weight 522.20 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Cc ' _symmetry_space_group_name_Hall 'C -2yc ' 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' _cell_length_a 34.569(3) _cell_length_b 17.656(2) _cell_length_c 20.504(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.326(3) _cell_angle_gamma 90.00 _cell_volume 11880(2) _cell_formula_units_Z 20 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 8572 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 25.13 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5360 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8500 _exptl_absorpt_correction_T_max 0.8794 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 48525 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 22713 _reflns_number_gt 16911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.07P)^2^+1.88P] 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 0.027(12) _refine_ls_number_reflns 22713 _refine_ls_number_parameters 1639 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.56140(12) 0.0219(2) -0.15768(19) 0.0362(9) Uani 1 1 d . . . C2 C 0.52395(13) 0.0071(2) -0.2088(2) 0.0440(11) Uani 1 1 d . . . C3 C 0.52358(13) -0.0067(2) -0.2754(2) 0.0384(9) Uani 1 1 d . . . H3 H 0.4989 -0.0153 -0.3096 0.046 Uiso 1 1 calc R . . C4 C 0.56023(14) -0.0079(3) -0.2921(2) 0.0472(11) Uani 1 1 d . . . C5 C 0.59763(13) 0.0077(2) -0.2396(2) 0.0382(9) Uani 1 1 d . . . H5 H 0.6221 0.0083 -0.2494 0.046 Uiso 1 1 calc R . . C6 C 0.59660(13) 0.0219(2) -0.1741(2) 0.0425(10) Uani 1 1 d . . . H6 H 0.6210 0.0320 -0.1396 0.051 Uiso 1 1 calc R . . C7 C 0.56182(12) 0.0471(2) -0.0870(2) 0.0351(8) Uani 1 1 d . . . C8 C 0.55986(13) -0.0318(2) -0.36162(19) 0.0393(9) Uani 1 1 d . . . C9 C 0.64195(14) 0.1650(3) 0.1175(2) 0.0445(10) Uani 1 1 d . . . H9 H 0.6560 0.1202 0.1172 0.053 Uiso 1 1 calc R . . C10 C 0.59188(14) 0.2520(3) 0.1067(2) 0.0582(13) Uani 1 1 d . . . H10 H 0.5661 0.2733 0.0977 0.070 Uiso 1 1 calc R . . C11 C 0.62737(12) 0.2906(3) 0.1344(2) 0.0491(11) Uani 1 1 d . . . H11 H 0.6303 0.3417 0.1457 0.059 Uiso 1 1 calc R . . C12 C 0.69976(13) 0.2492(3) 0.1770(2) 0.0427(10) Uani 1 1 d . . . C13 C 0.71576(13) 0.3205(3) 0.1988(2) 0.0449(10) Uani 1 1 d . . . H13 H 0.6992 0.3631 0.1866 0.054 Uiso 1 1 calc R . . C14 C 0.75625(13) 0.3284(3) 0.2386(2) 0.0439(10) Uani 1 1 d . . . H14 H 0.7668 0.3761 0.2534 0.053 Uiso 1 1 calc R . . C15 C 0.78104(12) 0.2646(3) 0.2562(2) 0.0508(11) Uani 1 1 d . . . C16 C 0.76505(14) 0.1928(3) 0.2350(3) 0.0528(11) Uani 1 1 d . . . H16 H 0.7816 0.1502 0.2470 0.063 Uiso 1 1 calc R . . C17 C 0.72445(15) 0.1851(3) 0.1958(2) 0.0567(13) Uani 1 1 d . . . H17 H 0.7137 0.1373 0.1821 0.068 Uiso 1 1 calc R . . C18 C 0.82465(12) 0.2744(2) 0.2949(2) 0.0437(10) Uani 1 1 d . . . C19 C 0.84821(12) 0.3406(2) 0.3021(2) 0.0406(9) Uani 1 1 d . . . H19 H 0.8370 0.3841 0.2778 0.049 Uiso 1 1 calc R . . C20 C 0.88840(12) 0.3411(3) 0.3459(2) 0.0449(10) Uani 1 1 d . . . H20 H 0.9039 0.3852 0.3521 0.054 Uiso 1 1 calc R . . C21 C 0.90499(14) 0.2751(3) 0.3800(2) 0.0510(11) Uani 1 1 d . . . C22 C 0.88404(14) 0.2079(3) 0.3710(2) 0.0514(12) Uani 1 1 d . . . H22 H 0.8964 0.1627 0.3898 0.062 Uiso 1 1 calc R . . C23 C 0.84460(13) 0.2113(2) 0.3333(2) 0.0454(10) Uani 1 1 d . . . H23 H 0.8290 0.1682 0.3324 0.055 Uiso 1 1 calc R . . C24 C 0.96766(14) 0.3425(3) 0.4542(3) 0.0553(12) Uani 1 1 d . . . H24 H 0.9569 0.3912 0.4508 0.066 Uiso 1 1 calc R . . C25 C 0.97464(14) 0.2190(3) 0.4407(2) 0.0491(11) Uani 1 1 d . . . H25 H 0.9686 0.1688 0.4279 0.059 Uiso 1 1 calc R . . C26 C 1.01100(14) 0.2441(3) 0.4769(2) 0.0500(11) Uani 1 1 d . . . H26 H 1.0346 0.2150 0.4911 0.060 Uiso 1 1 calc R . . C27 C 0.41903(13) 0.4906(2) -0.1002(2) 0.0406(10) Uani 1 1 d . . . C28 C 0.38277(13) 0.5086(3) -0.1541(2) 0.0464(11) Uani 1 1 d . . . C29 C 0.38449(12) 0.5246(2) -0.2188(2) 0.0381(9) Uani 1 1 d . . . H29 H 0.3605 0.5354 -0.2539 0.046 Uiso 1 1 calc R . . C30 C 0.42117(12) 0.5250(2) -0.23303(19) 0.0331(8) Uani 1 1 d . . . C31 C 0.45714(13) 0.5084(2) -0.17974(19) 0.0391(9) Uani 1 1 d . . . H31 H 0.4820 0.5086 -0.1885 0.047 Uiso 1 1 calc R . . C32 C 0.45609(12) 0.4917(2) -0.11361(19) 0.0387(9) Uani 1 1 d . . . H32 H 0.4801 0.4813 -0.0786 0.046 Uiso 1 1 calc R . . C33 C 0.41873(13) 0.4665(3) -0.0335(2) 0.0474(11) Uani 1 1 d . . . C34 C 0.42296(12) 0.5407(3) -0.3031(2) 0.0424(10) Uani 1 1 d . . . C35 C 0.50550(15) 0.3395(3) 0.1562(2) 0.0544(13) Uani 1 1 d . . . H35 H 0.5152 0.3877 0.1710 0.065 Uiso 1 1 calc R . . C36 C 0.46308(15) 0.2416(3) 0.1037(2) 0.0479(11) Uani 1 1 d . . . H36 H 0.4406 0.2137 0.0783 0.058 Uiso 1 1 calc R . . C37 C 0.50362(13) 0.2133(2) 0.13522(19) 0.0417(10) Uani 1 1 d . . . H37 H 0.5116 0.1631 0.1346 0.050 Uiso 1 1 calc R . . C38 C 0.57104(14) 0.2743(3) 0.2075(2) 0.0453(10) Uani 1 1 d . . . C39 C 0.59350(14) 0.2103(3) 0.2043(2) 0.0536(12) Uani 1 1 d . . . H39 H 0.5803 0.1667 0.1832 0.064 Uiso 1 1 calc R . . C40 C 0.63318(14) 0.2109(3) 0.2309(3) 0.0603(14) Uani 1 1 d . . . H40 H 0.6472 0.1682 0.2239 0.072 Uiso 1 1 calc R . . C41 C 0.65672(11) 0.2712(2) 0.2696(2) 0.0415(10) Uani 1 1 d . . . C42 C 0.63429(13) 0.3383(3) 0.2697(2) 0.0485(11) Uani 1 1 d . . . H42 H 0.6477 0.3820 0.2901 0.058 Uiso 1 1 calc R . . C43 C 0.59313(13) 0.3390(3) 0.2400(2) 0.0523(13) Uani 1 1 d . . . H43 H 0.5790 0.3835 0.2411 0.063 Uiso 1 1 calc R . . C44 C 0.69784(13) 0.2547(3) 0.3110(2) 0.0511(11) Uani 1 1 d . . . C45 C 0.70947(14) 0.1798(3) 0.3295(3) 0.0547(12) Uani 1 1 d . . . H45 H 0.6928 0.1397 0.3081 0.066 Uiso 1 1 calc R . . C46 C 0.74605(13) 0.1665(3) 0.3801(2) 0.0463(11) Uani 1 1 d . . . H46 H 0.7541 0.1169 0.3926 0.056 Uiso 1 1 calc R . . C47 C 0.77093(14) 0.2255(3) 0.4124(2) 0.0479(11) Uani 1 1 d . . . C48 C 0.75941(13) 0.2993(3) 0.3929(2) 0.0484(11) Uani 1 1 d . . . H48 H 0.7763 0.3391 0.4140 0.058 Uiso 1 1 calc R . . C49 C 0.72291(14) 0.3143(3) 0.3420(2) 0.0529(12) Uani 1 1 d . . . H49 H 0.7153 0.3639 0.3289 0.063 Uiso 1 1 calc R . . C50 C 0.82668(14) 0.1540(3) 0.4889(2) 0.0488(11) Uani 1 1 d . . . H50 H 0.8182 0.1087 0.4657 0.059 Uiso 1 1 calc R . . C51 C 0.82904(12) 0.2779(2) 0.51823(18) 0.0373(9) Uani 1 1 d . . . H51 H 0.8231 0.3292 0.5180 0.045 Uiso 1 1 calc R . . C52 C 0.86332(14) 0.2417(2) 0.5657(2) 0.0462(10) Uani 1 1 d . . . H52 H 0.8829 0.2639 0.6028 0.055 Uiso 1 1 calc R . . C53 C 0.38287(13) 0.0184(2) 0.0660(2) 0.0384(9) Uani 1 1 d . . . C54 C 0.34741(13) 0.0044(2) 0.01517(19) 0.0378(9) Uani 1 1 d . . . C55 C 0.34740(14) -0.0105(2) -0.0524(2) 0.0412(10) Uani 1 1 d . . . H55 H 0.3231 -0.0203 -0.0870 0.049 Uiso 1 1 calc R . . C56 C 0.38351(13) -0.0105(2) -0.0665(2) 0.0386(9) Uani 1 1 d . . . C57 C 0.42019(13) -0.0009(2) -0.0135(2) 0.0411(10) Uani 1 1 d . . . H57 H 0.4447 -0.0060 -0.0227 0.049 Uiso 1 1 calc R . . C58 C 0.42051(13) 0.0161(2) 0.0525(2) 0.0390(9) Uani 1 1 d . . . H58 H 0.4449 0.0257 0.0871 0.047 Uiso 1 1 calc R . . C59 C 0.38304(13) 0.0430(2) 0.1369(2) 0.0407(9) Uani 1 1 d . . . C60 C 0.38530(13) -0.0314(3) -0.1364(2) 0.0432(10) Uani 1 1 d . . . C61 C 0.47247(12) 0.1639(2) 0.3512(2) 0.0367(9) Uani 1 1 d . . . H61 H 0.4770 0.1227 0.3809 0.044 Uiso 1 1 calc R . . C62 C 0.44353(13) 0.2491(2) 0.2658(2) 0.0391(9) Uani 1 1 d . . . H62 H 0.4246 0.2731 0.2291 0.047 Uiso 1 1 calc R . . C63 C 0.48140(12) 0.2757(2) 0.2993(2) 0.0424(10) Uani 1 1 d . . . H63 H 0.4931 0.3196 0.2888 0.051 Uiso 1 1 calc R . . C64 C 0.54314(13) 0.2288(2) 0.3997(2) 0.0420(10) Uani 1 1 d . . . C65 C 0.56109(13) 0.1676(2) 0.4408(2) 0.0420(10) Uani 1 1 d . . . H65 H 0.5465 0.1230 0.4389 0.050 Uiso 1 1 calc R . . C66 C 0.60087(14) 0.1731(2) 0.4847(2) 0.0501(12) Uani 1 1 d . . . H66 H 0.6129 0.1322 0.5121 0.060 Uiso 1 1 calc R . . C67 C 0.62271(14) 0.2398(2) 0.4875(2) 0.0498(12) Uani 1 1 d . . . C68 C 0.60477(15) 0.3010(3) 0.4464(2) 0.0549(13) Uani 1 1 d . . . H68 H 0.6194 0.3456 0.4483 0.066 Uiso 1 1 calc R . . C69 C 0.56498(12) 0.2955(2) 0.4026(2) 0.0405(9) Uani 1 1 d . . . H69 H 0.5530 0.3364 0.3751 0.049 Uiso 1 1 calc R . . C70 C 0.66526(15) 0.2552(3) 0.5303(2) 0.0510(11) Uani 1 1 d . . . C71 C 0.68797(14) 0.1915(3) 0.5414(2) 0.0487(11) Uani 1 1 d . . . H71 H 0.6767 0.1479 0.5175 0.058 Uiso 1 1 calc R . . C72 C 0.72747(14) 0.1877(3) 0.5869(2) 0.0504(11) Uani 1 1 d . . . H72 H 0.7418 0.1424 0.5964 0.060 Uiso 1 1 calc R . . C73 C 0.74439(13) 0.2562(2) 0.6174(2) 0.0464(10) Uani 1 1 d . . . C74 C 0.72288(12) 0.3219(2) 0.6048(2) 0.0432(10) Uani 1 1 d . . . H74 H 0.7353 0.3663 0.6255 0.052 Uiso 1 1 calc R . . C75 C 0.68306(12) 0.3244(3) 0.5623(2) 0.0459(10) Uani 1 1 d . . . H75 H 0.6683 0.3694 0.5547 0.055 Uiso 1 1 calc R . . C76 C 0.81113(12) 0.3160(2) 0.6835(2) 0.0408(9) Uani 1 1 d . . . H76 H 0.8023 0.3647 0.6687 0.049 Uiso 1 1 calc R . . C77 C 0.81284(12) 0.1899(2) 0.6996(2) 0.0394(9) Uani 1 1 d . . . H77 H 0.8052 0.1393 0.6981 0.047 Uiso 1 1 calc R . . C78 C 0.85079(11) 0.2183(2) 0.73672(19) 0.0349(8) Uani 1 1 d . . . H78 H 0.8728 0.1897 0.7628 0.042 Uiso 1 1 calc R . . C79 C 0.09848(13) 0.0139(2) 0.17730(19) 0.0381(9) Uani 1 1 d . . . C80 C 0.06335(11) -0.0030(2) 0.12494(19) 0.0322(8) Uani 1 1 d . . . C81 C 0.06471(11) -0.0179(2) 0.05660(19) 0.0339(8) Uani 1 1 d . . . H81 H 0.0407 -0.0267 0.0210 0.041 Uiso 1 1 calc R . . C82 C 0.10137(12) -0.0189(3) 0.0443(2) 0.0405(10) Uani 1 1 d . . . C83 C 0.13672(12) -0.0044(2) 0.09731(19) 0.0404(10) Uani 1 1 d . . . H83 H 0.1616 -0.0059 0.0889 0.049 Uiso 1 1 calc R . . C84 C 0.13587(12) 0.0125(2) 0.1634(2) 0.0417(10) Uani 1 1 d . . . H84 H 0.1600 0.0229 0.1983 0.050 Uiso 1 1 calc R . . C85 C 0.09710(12) 0.0327(2) 0.2434(2) 0.0381(9) Uani 1 1 d . . . C86 C 0.10181(13) -0.0342(2) -0.02683(19) 0.0402(10) Uani 1 1 d . . . C87 C 0.18532(12) 0.1546(2) 0.4327(2) 0.0407(9) Uani 1 1 d . . . H87 H 0.1969 0.1110 0.4214 0.049 Uiso 1 1 calc R . . C88 C 0.13809(14) 0.2431(3) 0.4377(2) 0.0476(10) Uani 1 1 d . . . H88 H 0.1136 0.2685 0.4311 0.057 Uiso 1 1 calc R . . C89 C 0.17750(13) 0.2694(3) 0.4765(2) 0.0452(10) Uani 1 1 d . . . H89 H 0.1833 0.3152 0.4999 0.054 Uiso 1 1 calc R . . C90 C 0.24886(14) 0.2209(3) 0.5162(2) 0.0492(11) Uani 1 1 d . . . C91 C 0.26521(15) 0.2913(3) 0.5414(2) 0.0538(12) Uani 1 1 d . . . H91 H 0.2485 0.3338 0.5342 0.065 Uiso 1 1 calc R . . C92 C 0.30612(14) 0.2978(3) 0.5768(2) 0.0499(11) Uani 1 1 d . . . H92 H 0.3168 0.3448 0.5937 0.060 Uiso 1 1 calc R . . C93 C 0.33165(12) 0.2349(2) 0.5877(2) 0.0423(10) Uani 1 1 d . . . C94 C 0.31537(14) 0.1647(2) 0.5623(2) 0.0468(11) Uani 1 1 d . . . H94 H 0.3322 0.1223 0.5692 0.056 Uiso 1 1 calc R . . C95 C 0.27406(13) 0.1580(2) 0.5268(2) 0.0437(10) Uani 1 1 d . . . H95 H 0.2633 0.1110 0.5100 0.052 Uiso 1 1 calc R . . C96 C 0.37609(13) 0.2435(2) 0.6273(2) 0.0428(10) Uani 1 1 d . . . C97 C 0.39702(13) 0.3135(2) 0.6356(2) 0.0431(10) Uani 1 1 d . . . H97 H 0.3835 0.3572 0.6154 0.052 Uiso 1 1 calc R . . C98 C 0.43793(14) 0.3162(3) 0.6742(2) 0.0549(12) Uani 1 1 d . . . H98 H 0.4516 0.3624 0.6804 0.066 Uiso 1 1 calc R . . C99 C 0.45848(14) 0.2526(3) 0.7031(2) 0.0523(11) Uani 1 1 d . . . C100 C 0.43823(12) 0.1838(2) 0.6973(2) 0.0417(10) Uani 1 1 d . . . H100 H 0.4521 0.1407 0.7185 0.050 Uiso 1 1 calc R . . C101 C 0.39744(13) 0.1798(2) 0.6601(2) 0.0404(10) Uani 1 1 d . . . H101 H 0.3839 0.1338 0.6567 0.048 Uiso 1 1 calc R . . C102 C 0.52109(14) 0.3178(2) 0.7678(2) 0.0415(10) Uani 1 1 d . . . H102 H 0.5096 0.3659 0.7633 0.050 Uiso 1 1 calc R . . C103 C 0.52878(12) 0.1896(2) 0.75692(18) 0.0353(9) Uani 1 1 d . . . H103 H 0.5233 0.1392 0.7441 0.042 Uiso 1 1 calc R . . C104 C 0.56666(14) 0.2208(3) 0.7985(2) 0.0457(10) Uani 1 1 d . . . H104 H 0.5905 0.1935 0.8180 0.055 Uiso 1 1 calc R . . C105 C 0.24267(12) 0.5121(3) 0.6203(2) 0.0425(10) Uani 1 1 d . . . C106 C 0.20469(13) 0.5005(3) 0.5690(2) 0.0439(10) Uani 1 1 d . . . C107 C 0.20518(13) 0.4890(2) 0.5027(2) 0.0406(10) Uani 1 1 d . . . H107 H 0.1808 0.4803 0.4678 0.049 Uiso 1 1 calc R . . C108 C 0.24124(12) 0.4902(2) 0.4876(2) 0.0372(9) Uani 1 1 d . . . C109 C 0.27746(14) 0.5021(3) 0.5374(2) 0.0434(10) Uani 1 1 d . . . H109 H 0.3015 0.5035 0.5262 0.052 Uiso 1 1 calc R . . C110 C 0.27840(13) 0.5120(3) 0.6050(2) 0.0421(10) Uani 1 1 d . . . H110 H 0.3031 0.5186 0.6396 0.051 Uiso 1 1 calc R . . C111 C 0.24190(12) 0.5274(2) 0.6922(2) 0.0382(9) Uani 1 1 d . . . C112 C 0.24115(14) 0.4753(3) 0.4165(2) 0.0473(11) Uani 1 1 d . . . C113 C 0.32852(12) 0.6522(3) 0.90498(19) 0.0415(10) Uani 1 1 d . . . H113 H 0.3344 0.6059 0.9276 0.050 Uiso 1 1 calc R . . C114 C 0.29503(13) 0.7453(3) 0.8321(2) 0.0453(11) Uani 1 1 d . . . H114 H 0.2756 0.7713 0.7975 0.054 Uiso 1 1 calc R . . C115 C 0.33244(13) 0.7763(2) 0.8779(2) 0.0396(9) Uani 1 1 d . . . H115 H 0.3412 0.8262 0.8789 0.048 Uiso 1 1 calc R . . C116 C 0.39349(11) 0.7225(2) 0.9646(2) 0.0412(10) Uani 1 1 d . . . C117 C 0.40615(11) 0.7920(2) 1.0002(2) 0.0409(10) Uani 1 1 d . . . H117 H 0.3885 0.8330 0.9941 0.049 Uiso 1 1 calc R . . C118 C 0.44430(12) 0.7960(2) 1.0425(2) 0.0439(10) Uani 1 1 d . . . H118 H 0.4529 0.8410 1.0662 0.053 Uiso 1 1 calc R . . C119 C 0.47255(13) 0.7350(3) 1.0534(2) 0.0439(10) Uani 1 1 d . . . C120 C 0.45974(13) 0.6666(3) 1.0189(2) 0.0457(11) Uani 1 1 d . . . H120 H 0.4775 0.6259 1.0243 0.055 Uiso 1 1 calc R . . C121 C 0.41970(13) 0.6615(2) 0.9764(2) 0.0406(9) Uani 1 1 d . . . H121 H 0.4103 0.6155 0.9552 0.049 Uiso 1 1 calc R . . C122 C 0.51517(12) 0.7438(2) 1.10043(19) 0.0396(9) Uani 1 1 d . . . C123 C 0.52968(13) 0.8154(3) 1.1251(2) 0.0446(11) Uani 1 1 d . . . H123 H 0.5124 0.8571 1.1138 0.053 Uiso 1 1 calc R . . C124 C 0.57005(12) 0.8245(2) 1.1667(2) 0.0391(9) Uani 1 1 d . . . H124 H 0.5798 0.8723 1.1827 0.047 Uiso 1 1 calc R . . C125 C 0.59566(12) 0.7620(2) 1.1843(2) 0.0388(9) Uani 1 1 d . . . C126 C 0.58116(14) 0.6911(3) 1.1600(2) 0.0574(13) Uani 1 1 d . . . H126 H 0.5983 0.6493 1.1718 0.069 Uiso 1 1 calc R . . C127 C 0.54124(13) 0.6817(3) 1.1183(2) 0.0454(10) Uani 1 1 d . . . H127 H 0.5318 0.6337 1.1022 0.054 Uiso 1 1 calc R . . C128 C 0.65794(13) 0.8392(3) 1.2360(2) 0.0475(11) Uani 1 1 d . . . H128 H 0.6489 0.8855 1.2152 0.057 Uiso 1 1 calc R . . C129 C 0.66001(14) 0.7130(3) 1.2650(3) 0.0570(13) Uani 1 1 d . . . H129 H 0.6528 0.6623 1.2651 0.068 Uiso 1 1 calc R . . C130 C 0.69803(14) 0.7469(3) 1.3060(2) 0.0497(11) Uani 1 1 d . . . H130 H 0.7191 0.7228 1.3392 0.060 Uiso 1 1 calc R . . Mn1 Mn 0.55735(3) 0.10402(4) 0.02374(4) 0.04342(18) Uani 1 1 d . . . Mn2 Mn 0.41581(3) 0.39911(4) 0.07705(4) 0.04003(16) Uani 1 1 d . . . Mn3 Mn 0.38421(3) 0.10253(4) 0.24978(4) 0.03899(16) Uani 1 1 d . . . Mn4 Mn 0.09279(2) 0.10245(4) 0.35211(4) 0.03360(14) Uani 1 1 d . . . Mn5 Mn 0.24454(2) 0.59183(3) 0.80604(4) 0.03630(14) Uani 1 1 d . . . N1 N 0.48616(11) 0.0085(2) -0.2006(2) 0.0471(9) Uani 1 1 d . . . H1A H 0.4648 0.0012 -0.2354 0.057 Uiso 1 1 calc R . . H1B H 0.4838 0.0168 -0.1607 0.057 Uiso 1 1 calc R . . N2 N 0.59916(12) 0.1740(2) 0.0931(2) 0.0528(10) Uani 1 1 d . . . N3 N 0.65973(11) 0.2357(2) 0.14250(18) 0.0391(8) Uani 1 1 d . . . N4 N 0.94610(13) 0.2792(2) 0.4241(2) 0.0538(10) Uani 1 1 d . . . N5 N 1.00839(13) 0.3234(3) 0.4908(2) 0.0560(11) Uani 1 1 d . . . N6 N 0.34418(11) 0.50283(19) -0.14757(17) 0.0412(8) Uani 1 1 d . . . H6A H 0.3230 0.5091 -0.1829 0.049 Uiso 1 1 calc R . . H6B H 0.3414 0.4929 -0.1082 0.049 Uiso 1 1 calc R . . N7 N 0.46381(11) 0.3198(2) 0.11865(17) 0.0391(8) Uani 1 1 d . . . N8 N 0.52872(13) 0.2721(2) 0.1664(2) 0.0537(10) Uani 1 1 d . . . N9 N 0.80595(12) 0.2250(2) 0.47245(19) 0.0462(9) Uani 1 1 d . . . N10 N 0.86142(12) 0.1636(2) 0.54461(19) 0.0473(9) Uani 1 1 d . . . N11 N 0.30827(11) 0.0064(2) 0.01562(19) 0.0466(9) Uani 1 1 d . . . H11B H 0.3042 0.0182 0.0556 0.056 Uiso 1 1 d R . . H11A H 0.2861 -0.0035 -0.0206 0.056 Uiso 1 1 d R . . N12 N 0.43687(12) 0.1768(2) 0.29579(18) 0.0443(9) Uani 1 1 d . . . N13 N 0.50015(12) 0.22375(18) 0.35424(17) 0.0398(8) Uani 1 1 d . . . N14 N 0.78772(10) 0.2488(2) 0.66492(19) 0.0428(9) Uani 1 1 d . . . N15 N 0.85038(11) 0.2966(2) 0.72845(18) 0.0426(8) Uani 1 1 d . . . N16 N 0.02510(10) 0.00057(16) 0.13207(18) 0.0354(8) Uani 1 1 d . . . H16A H 0.0223 0.0139 0.1707 0.042 Uiso 1 1 calc R . . H16B H 0.0040 -0.0105 0.0979 0.042 Uiso 1 1 calc R . . N17 N 0.14319(10) 0.1717(2) 0.41125(18) 0.0377(8) Uani 1 1 d . . . N18 N 0.20673(12) 0.2135(2) 0.47337(19) 0.0448(9) Uani 1 1 d . . . N19 N 0.50152(12) 0.2511(2) 0.73954(17) 0.0513(10) Uani 1 1 d . . . N20 N 0.56210(11) 0.29832(19) 0.80487(17) 0.0360(7) Uani 1 1 d . . . N21 N 0.16767(11) 0.4954(2) 0.5779(2) 0.0447(8) Uani 1 1 d . . . H21A H 0.1465 0.4855 0.5435 0.054 Uiso 1 1 calc R . . H21B H 0.1653 0.5020 0.6180 0.054 Uiso 1 1 calc R . . N22 N 0.29348(11) 0.6687(2) 0.84959(19) 0.0391(8) Uani 1 1 d . . . N23 N 0.35307(10) 0.7172(2) 0.92047(19) 0.0406(8) Uani 1 1 d . . . N24 N 0.63592(12) 0.7714(2) 1.2247(2) 0.0506(10) Uani 1 1 d . . . N25 N 0.69683(12) 0.8247(2) 1.2854(2) 0.0544(11) Uani 1 1 d . . . O1 O 0.59162(10) 0.08098(19) -0.04865(16) 0.0488(8) Uani 1 1 d . . . O2 O 0.53016(9) 0.02999(17) -0.07318(16) 0.0400(7) Uani 1 1 d . . . O3 O 0.52891(9) -0.05785(18) -0.40223(16) 0.0432(7) Uani 1 1 d . . . O4 O 0.59078(10) -0.02770(18) -0.38105(16) 0.0442(7) Uani 1 1 d . . . O5 O 0.45043(9) 0.44504(19) 0.01087(15) 0.0420(7) Uani 1 1 d . . . O6 O 0.38757(9) 0.46876(17) -0.01711(15) 0.0405(7) Uani 1 1 d . . . O7 O 0.39133(9) 0.56813(17) -0.34252(14) 0.0368(7) Uani 1 1 d . . . O8 O 0.45057(10) 0.52591(19) -0.32602(17) 0.0464(8) Uani 1 1 d . . . O9 O 0.41454(9) 0.07034(17) 0.18058(15) 0.0401(7) Uani 1 1 d . . . O10 O 0.35187(9) 0.03243(17) 0.15094(14) 0.0403(7) Uani 1 1 d . . . O11 O 0.35299(9) -0.05636(17) -0.17642(15) 0.0393(7) Uani 1 1 d . . . O12 O 0.41440(9) -0.02951(16) -0.16039(15) 0.0387(7) Uani 1 1 d . . . O13 O 0.12918(8) 0.05584(16) 0.28935(13) 0.0318(6) Uani 1 1 d . . . O14 O 0.06629(9) 0.02997(18) 0.26165(15) 0.0431(7) Uani 1 1 d . . . O15 O 0.06995(9) -0.06283(17) -0.06647(14) 0.0367(6) Uani 1 1 d . . . O16 O 0.13017(9) -0.02166(17) -0.04928(14) 0.0408(7) Uani 1 1 d . . . O17 O 0.27355(9) 0.54658(18) 0.73514(15) 0.0423(7) Uani 1 1 d . . . O18 O 0.21058(9) 0.51694(18) 0.70964(16) 0.0429(7) Uani 1 1 d . . . O19 O 0.20791(9) 0.45102(17) 0.37581(14) 0.0379(7) Uani 1 1 d . . . O20 O 0.26940(11) 0.4822(2) 0.39249(18) 0.0547(9) Uani 1 1 d . . . O1W O 0.7194(3) 0.4941(5) 0.4848(5) 0.039(2) Uani 0.30 1 d P . . H1X H 0.7070 0.4708 0.4479 0.047 Uiso 0.30 1 d PR . . H1Y H 0.7046 0.4948 0.5109 0.047 Uiso 0.30 1 d PR . . O2W O 0.2711(4) 0.9698(8) 0.7600(7) 0.044(3) Uani 0.20 1 d P . . H2X H 0.2578 0.9997 0.7284 0.052 Uiso 0.20 1 d PR . . H2Y H 0.2553 0.9356 0.7661 0.052 Uiso 0.20 1 d 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 C1 0.040(2) 0.038(2) 0.0287(19) 0.0127(16) 0.0081(16) 0.0142(17) C2 0.041(2) 0.042(2) 0.048(2) -0.0174(19) 0.0121(18) 0.0210(19) C3 0.049(2) 0.025(2) 0.040(2) -0.0160(16) 0.0123(18) -0.0053(17) C4 0.047(3) 0.059(3) 0.034(2) 0.0148(19) 0.0089(18) 0.018(2) C5 0.050(2) 0.0244(19) 0.042(2) 0.0087(17) 0.0167(18) 0.0111(17) C6 0.042(2) 0.042(2) 0.041(2) 0.0038(18) 0.0103(18) 0.0303(19) C7 0.040(2) 0.0228(18) 0.044(2) -0.0104(16) 0.0151(17) -0.0095(16) C8 0.051(2) 0.036(2) 0.030(2) 0.0128(16) 0.0119(17) -0.0086(18) C9 0.059(3) 0.043(2) 0.044(2) 0.0106(18) 0.034(2) -0.0077(19) C10 0.042(2) 0.079(4) 0.048(3) -0.023(2) 0.006(2) -0.012(2) C11 0.036(2) 0.055(3) 0.055(3) -0.007(2) 0.012(2) -0.0087(19) C12 0.043(2) 0.056(3) 0.0278(19) 0.0134(18) 0.0087(17) 0.008(2) C13 0.036(2) 0.041(2) 0.059(3) 0.013(2) 0.016(2) 0.0061(18) C14 0.044(2) 0.051(3) 0.033(2) -0.0098(18) 0.0078(18) 0.0095(19) C15 0.028(2) 0.060(3) 0.062(3) -0.012(2) 0.010(2) 0.0036(19) C16 0.050(3) 0.041(2) 0.060(3) 0.007(2) 0.006(2) 0.003(2) C17 0.066(3) 0.045(3) 0.035(2) -0.0160(19) -0.019(2) 0.012(2) C18 0.033(2) 0.048(2) 0.050(2) 0.027(2) 0.0131(18) -0.0121(18) C19 0.039(2) 0.034(2) 0.054(2) -0.0099(18) 0.0232(19) 0.0025(17) C20 0.035(2) 0.050(3) 0.061(3) -0.012(2) 0.031(2) -0.0110(19) C21 0.046(3) 0.057(3) 0.053(3) -0.006(2) 0.021(2) -0.002(2) C22 0.049(3) 0.045(3) 0.046(3) -0.002(2) -0.005(2) 0.009(2) C23 0.042(2) 0.040(2) 0.057(3) 0.008(2) 0.019(2) 0.0090(18) C24 0.045(2) 0.044(3) 0.090(4) -0.008(2) 0.040(3) -0.007(2) C25 0.063(3) 0.056(3) 0.032(2) 0.002(2) 0.019(2) 0.007(2) C26 0.054(3) 0.059(3) 0.042(2) 0.011(2) 0.022(2) 0.016(2) C27 0.052(3) 0.029(2) 0.047(2) 0.0051(17) 0.023(2) 0.0169(18) C28 0.044(2) 0.064(3) 0.036(2) 0.003(2) 0.0187(19) 0.007(2) C29 0.043(2) 0.043(2) 0.031(2) -0.0217(17) 0.0151(17) -0.0012(18) C30 0.043(2) 0.0260(19) 0.0310(19) -0.0101(15) 0.0123(17) 0.0077(16) C31 0.043(2) 0.044(2) 0.029(2) -0.0145(17) 0.0100(16) 0.0029(18) C32 0.036(2) 0.051(3) 0.0258(19) -0.0009(17) 0.0046(16) 0.0030(18) C33 0.038(2) 0.057(3) 0.043(2) -0.002(2) 0.0066(19) -0.028(2) C34 0.036(2) 0.048(3) 0.043(2) 0.0041(19) 0.0129(18) 0.0022(18) C35 0.060(3) 0.042(3) 0.037(2) 0.0040(19) -0.019(2) 0.005(2) C36 0.062(3) 0.047(3) 0.0262(19) -0.0073(17) 0.0019(18) -0.007(2) C37 0.053(2) 0.038(2) 0.031(2) 0.0170(17) 0.0089(18) 0.0008(19) C38 0.048(2) 0.044(2) 0.034(2) 0.0011(18) 0.0004(18) 0.007(2) C39 0.054(3) 0.051(3) 0.047(3) -0.026(2) 0.002(2) -0.006(2) C40 0.044(2) 0.079(4) 0.074(3) -0.037(3) 0.041(2) -0.020(2) C41 0.0298(19) 0.051(3) 0.049(2) -0.0152(19) 0.0197(18) -0.0061(18) C42 0.037(2) 0.060(3) 0.053(3) -0.001(2) 0.020(2) 0.004(2) C43 0.048(3) 0.036(2) 0.049(3) 0.0027(19) -0.018(2) 0.0168(19) C44 0.035(2) 0.068(3) 0.053(3) -0.018(2) 0.017(2) 0.004(2) C45 0.043(2) 0.056(3) 0.061(3) -0.025(2) 0.011(2) 0.006(2) C46 0.050(3) 0.051(3) 0.038(2) -0.0219(19) 0.013(2) 0.001(2) C47 0.052(3) 0.050(3) 0.045(2) -0.018(2) 0.019(2) -0.012(2) C48 0.044(2) 0.056(3) 0.047(2) -0.012(2) 0.016(2) 0.004(2) C49 0.050(3) 0.068(3) 0.038(2) 0.016(2) 0.0096(19) -0.025(2) C50 0.048(2) 0.056(3) 0.042(2) -0.008(2) 0.013(2) -0.009(2) C51 0.046(2) 0.044(2) 0.0260(18) -0.0005(16) 0.0168(17) -0.0088(18) C52 0.054(3) 0.044(2) 0.031(2) 0.0012(17) 0.0003(18) -0.016(2) C53 0.051(2) 0.026(2) 0.041(2) -0.0063(16) 0.0185(19) 0.0039(17) C54 0.050(2) 0.043(2) 0.0241(18) 0.0135(16) 0.0171(16) -0.0154(19) C55 0.055(3) 0.047(2) 0.028(2) 0.0017(17) 0.0228(18) 0.017(2) C56 0.048(2) 0.036(2) 0.031(2) 0.0141(17) 0.0110(17) 0.0190(18) C57 0.046(2) 0.043(2) 0.037(2) -0.0091(18) 0.0170(18) -0.0106(19) C58 0.046(2) 0.033(2) 0.039(2) 0.0006(17) 0.0154(18) -0.0051(18) C59 0.050(2) 0.041(2) 0.032(2) 0.0082(17) 0.0143(17) -0.0124(19) C60 0.050(2) 0.046(3) 0.039(2) -0.0122(19) 0.0221(19) -0.0087(19) C61 0.046(2) 0.0175(17) 0.048(2) -0.0087(15) 0.0163(19) 0.0071(15) C62 0.043(2) 0.029(2) 0.048(2) -0.0010(17) 0.0184(19) 0.0094(17) C63 0.043(2) 0.045(2) 0.042(2) 0.0220(19) 0.0170(18) 0.0126(19) C64 0.055(3) 0.038(2) 0.032(2) 0.0231(17) 0.0112(18) -0.0002(19) C65 0.053(3) 0.030(2) 0.034(2) 0.0014(16) 0.0010(18) 0.0096(18) C66 0.059(3) 0.027(2) 0.043(2) -0.0089(17) -0.016(2) 0.0085(19) C67 0.062(3) 0.035(2) 0.031(2) -0.0047(17) -0.017(2) 0.004(2) C68 0.061(3) 0.037(2) 0.043(2) -0.0026(19) -0.017(2) -0.007(2) C69 0.042(2) 0.039(2) 0.039(2) 0.0112(17) 0.0111(18) 0.0056(18) C70 0.060(3) 0.038(2) 0.046(2) -0.0154(19) 0.004(2) -0.003(2) C71 0.049(3) 0.049(3) 0.037(2) 0.0017(19) -0.0034(19) -0.001(2) C72 0.052(3) 0.050(3) 0.044(2) -0.002(2) 0.007(2) -0.005(2) C73 0.042(2) 0.037(2) 0.061(3) -0.005(2) 0.018(2) 0.0063(19) C74 0.038(2) 0.039(2) 0.051(2) 0.0156(19) 0.0115(19) 0.0027(18) C75 0.032(2) 0.055(3) 0.045(2) -0.017(2) 0.0034(18) -0.0023(19) C76 0.046(2) 0.0219(18) 0.063(3) -0.0023(18) 0.028(2) 0.0062(16) C77 0.036(2) 0.038(2) 0.041(2) -0.0055(17) 0.0080(17) 0.0026(17) C78 0.0239(17) 0.050(2) 0.0362(19) 0.0045(17) 0.0167(15) 0.0067(16) C79 0.051(2) 0.034(2) 0.0281(19) 0.0062(16) 0.0106(17) -0.0075(18) C80 0.0301(19) 0.033(2) 0.0301(19) 0.0062(16) 0.0041(15) 0.0074(16) C81 0.031(2) 0.037(2) 0.0285(19) 0.0058(15) 0.0027(15) 0.0106(16) C82 0.042(2) 0.051(3) 0.028(2) -0.0065(17) 0.0101(17) -0.0059(19) C83 0.035(2) 0.052(3) 0.026(2) 0.0109(17) -0.0024(16) 0.0066(18) C84 0.038(2) 0.047(3) 0.036(2) -0.0091(18) 0.0048(17) -0.0085(18) C85 0.041(2) 0.036(2) 0.036(2) 0.0072(16) 0.0104(17) -0.0092(17) C86 0.048(2) 0.048(2) 0.0237(19) 0.0095(16) 0.0095(17) 0.0067(19) C87 0.043(2) 0.045(2) 0.037(2) 0.0047(18) 0.0171(18) -0.0025(18) C88 0.050(2) 0.058(3) 0.045(2) -0.008(2) 0.030(2) 0.003(2) C89 0.043(2) 0.047(3) 0.052(3) 0.003(2) 0.025(2) 0.0011(19) C90 0.050(3) 0.040(2) 0.059(3) -0.018(2) 0.019(2) 0.005(2) C91 0.060(3) 0.039(2) 0.043(2) -0.0094(19) -0.012(2) -0.002(2) C92 0.057(3) 0.046(3) 0.038(2) -0.0197(19) 0.004(2) 0.010(2) C93 0.039(2) 0.043(2) 0.048(2) -0.0177(19) 0.0180(19) -0.0066(18) C94 0.054(3) 0.038(2) 0.046(2) -0.0182(18) 0.011(2) 0.0068(19) C95 0.051(2) 0.036(2) 0.036(2) -0.0115(17) 0.0022(19) -0.0044(19) C96 0.049(2) 0.038(2) 0.037(2) 0.0057(17) 0.0070(18) 0.0001(19) C97 0.055(3) 0.041(2) 0.0271(19) -0.0115(17) 0.0040(18) -0.007(2) C98 0.050(3) 0.041(3) 0.059(3) 0.003(2) -0.004(2) -0.010(2) C99 0.051(3) 0.053(3) 0.049(3) -0.014(2) 0.009(2) 0.008(2) C100 0.043(2) 0.045(2) 0.055(2) 0.0085(19) 0.040(2) 0.0153(19) C101 0.050(2) 0.029(2) 0.050(2) -0.0106(18) 0.027(2) 0.0112(18) C102 0.056(3) 0.039(2) 0.034(2) 0.0115(17) 0.020(2) 0.002(2) C103 0.041(2) 0.046(2) 0.0235(18) 0.0097(16) 0.0157(16) -0.0109(18) C104 0.045(2) 0.047(3) 0.035(2) -0.0084(18) -0.0009(18) 0.002(2) C105 0.033(2) 0.051(3) 0.042(2) -0.0143(19) 0.0083(18) 0.0107(19) C106 0.039(2) 0.058(3) 0.028(2) 0.0147(19) -0.0001(17) 0.022(2) C107 0.042(2) 0.035(2) 0.043(2) -0.0076(18) 0.0121(19) -0.0060(18) C108 0.036(2) 0.038(2) 0.034(2) 0.0154(17) 0.0048(17) 0.0093(17) C109 0.045(2) 0.045(3) 0.040(2) -0.0142(19) 0.0126(19) -0.007(2) C110 0.038(2) 0.053(3) 0.033(2) 0.0093(19) 0.0066(17) 0.003(2) C111 0.031(2) 0.043(2) 0.039(2) -0.0069(18) 0.0070(18) -0.0053(17) C112 0.036(2) 0.058(3) 0.034(2) -0.015(2) -0.0098(19) 0.009(2) C113 0.033(2) 0.060(3) 0.0277(19) 0.0125(18) 0.0042(16) -0.028(2) C114 0.048(2) 0.057(3) 0.0247(19) 0.0165(18) 0.0028(17) -0.028(2) C115 0.047(2) 0.041(2) 0.032(2) -0.0108(17) 0.0131(18) -0.0095(19) C116 0.0244(19) 0.047(2) 0.053(2) -0.026(2) 0.0129(17) 0.0012(17) C117 0.028(2) 0.043(2) 0.048(2) -0.0236(19) 0.0071(18) 0.0107(17) C118 0.037(2) 0.023(2) 0.063(3) -0.0082(18) 0.003(2) -0.0065(17) C119 0.039(2) 0.054(3) 0.038(2) -0.0165(19) 0.0126(18) 0.014(2) C120 0.035(2) 0.047(3) 0.061(3) -0.022(2) 0.022(2) 0.0025(18) C121 0.045(2) 0.036(2) 0.042(2) -0.0090(17) 0.0154(19) -0.0008(18) C122 0.039(2) 0.048(3) 0.0261(19) 0.0049(17) 0.0012(17) 0.0031(19) C123 0.039(2) 0.057(3) 0.039(2) -0.014(2) 0.0140(19) 0.015(2) C124 0.042(2) 0.039(2) 0.040(2) -0.0062(17) 0.0184(19) -0.0084(18) C125 0.038(2) 0.044(2) 0.0264(19) 0.0063(17) -0.0015(16) -0.0002(18) C126 0.050(3) 0.060(3) 0.043(3) -0.020(2) -0.013(2) 0.010(2) C127 0.034(2) 0.049(3) 0.049(3) 0.003(2) 0.0073(19) 0.0054(19) C128 0.036(2) 0.060(3) 0.043(2) 0.012(2) 0.0068(19) -0.007(2) C129 0.038(2) 0.051(3) 0.069(3) -0.016(2) -0.001(2) -0.002(2) C130 0.041(2) 0.050(3) 0.051(3) 0.000(2) 0.004(2) -0.014(2) Mn1 0.0512(5) 0.0422(4) 0.0411(4) 0.0012(3) 0.0206(3) -0.0040(3) Mn2 0.0403(4) 0.0473(4) 0.0352(3) -0.0073(3) 0.0157(3) -0.0139(3) Mn3 0.0455(4) 0.0388(4) 0.0386(4) 0.0077(3) 0.0217(3) 0.0025(3) Mn4 0.0308(3) 0.0431(4) 0.0317(3) 0.0076(3) 0.0168(2) 0.0078(3) Mn5 0.0305(4) 0.0454(3) 0.0317(3) -0.0014(3) 0.0078(3) -0.0071(3) N1 0.049(2) 0.050(2) 0.048(2) -0.0168(17) 0.0227(17) -0.0137(18) N2 0.054(2) 0.068(3) 0.045(2) -0.0213(19) 0.0278(18) -0.020(2) N3 0.0387(18) 0.041(2) 0.0435(19) 0.0071(15) 0.0220(16) -0.0021(15) N4 0.051(2) 0.048(2) 0.065(3) -0.009(2) 0.022(2) -0.0054(19) N5 0.054(3) 0.054(3) 0.061(3) 0.003(2) 0.020(2) -0.010(2) N6 0.049(2) 0.048(2) 0.0272(16) 0.0101(14) 0.0121(15) -0.0096(16) N7 0.049(2) 0.046(2) 0.0317(18) -0.0120(14) 0.0254(17) 0.0001(16) N8 0.052(2) 0.050(2) 0.050(2) -0.0007(19) 0.0026(19) 0.0007(19) N9 0.041(2) 0.054(2) 0.044(2) -0.0153(18) 0.0133(17) -0.0095(17) N10 0.044(2) 0.057(2) 0.042(2) 0.0009(17) 0.0155(17) 0.0087(18) N11 0.050(2) 0.052(2) 0.0383(19) -0.0126(16) 0.0149(16) 0.0203(17) N12 0.056(2) 0.043(2) 0.0321(18) 0.0052(15) 0.0117(17) 0.0010(18) N13 0.056(2) 0.0295(17) 0.0285(16) 0.0106(14) 0.0061(15) -0.0022(16) N14 0.0300(17) 0.043(2) 0.057(2) 0.0263(17) 0.0159(16) -0.0020(15) N15 0.051(2) 0.048(2) 0.0316(18) 0.0052(15) 0.0159(16) -0.0079(17) N16 0.0407(18) 0.0211(15) 0.048(2) 0.0127(13) 0.0192(15) -0.0126(13) N17 0.036(2) 0.048(2) 0.0335(17) 0.0000(15) 0.0166(16) 0.0051(15) N18 0.046(2) 0.050(2) 0.043(2) -0.0071(17) 0.0211(17) -0.0039(17) N19 0.064(3) 0.053(2) 0.0255(17) -0.0136(16) -0.0032(17) 0.006(2) N20 0.0435(19) 0.0368(19) 0.0312(16) 0.0091(14) 0.0169(15) -0.0048(15) N21 0.040(2) 0.046(2) 0.048(2) -0.0138(16) 0.0136(16) 0.0009(16) N22 0.0354(19) 0.042(2) 0.0377(19) 0.0005(15) 0.0082(15) 0.0009(15) N23 0.0296(17) 0.043(2) 0.049(2) -0.0006(17) 0.0123(16) -0.0128(15) N24 0.041(2) 0.050(2) 0.055(2) -0.0193(19) 0.0063(18) -0.0048(18) N25 0.049(2) 0.035(2) 0.063(3) -0.0245(18) -0.0057(19) 0.0073(17) O1 0.059(2) 0.0477(18) 0.0466(18) -0.0200(14) 0.0261(16) -0.0255(15) O2 0.0430(17) 0.0368(17) 0.0408(16) 0.0030(13) 0.0140(13) -0.0112(13) O3 0.0459(18) 0.0464(19) 0.0404(16) 0.0017(14) 0.0178(14) -0.0022(14) O4 0.0504(18) 0.0431(18) 0.0451(17) -0.0021(14) 0.0238(15) -0.0102(14) O5 0.0417(16) 0.0548(19) 0.0297(14) -0.0023(13) 0.0115(12) -0.0170(14) O6 0.0458(17) 0.0348(16) 0.0366(15) -0.0108(12) 0.0068(13) -0.0149(13) O7 0.0356(15) 0.0388(16) 0.0344(15) -0.0098(12) 0.0085(12) -0.0106(12) O8 0.0478(18) 0.051(2) 0.0459(18) 0.0207(15) 0.0218(15) 0.0121(15) O9 0.0434(16) 0.0369(16) 0.0439(16) -0.0029(13) 0.0196(13) -0.0108(13) O10 0.0440(17) 0.0446(17) 0.0296(14) 0.0155(12) 0.0078(12) -0.0023(13) O11 0.0458(16) 0.0391(17) 0.0385(15) 0.0074(13) 0.0211(13) 0.0038(13) O12 0.0436(17) 0.0369(16) 0.0417(16) -0.0074(12) 0.0220(13) 0.0051(13) O13 0.0312(14) 0.0433(16) 0.0312(14) 0.0078(12) 0.0246(11) 0.0023(12) O14 0.0485(18) 0.0466(19) 0.0323(15) 0.0037(13) 0.0101(13) -0.0055(14) O15 0.0410(16) 0.0438(16) 0.0276(14) -0.0064(12) 0.0138(12) 0.0035(13) O16 0.0500(18) 0.0461(18) 0.0286(14) -0.0007(12) 0.0157(13) -0.0047(14) O17 0.0338(15) 0.0535(19) 0.0334(15) -0.0016(14) 0.0014(12) 0.0017(14) O18 0.0381(17) 0.053(2) 0.0360(16) -0.0121(14) 0.0094(13) -0.0101(14) O19 0.0371(16) 0.0423(17) 0.0318(15) 0.0016(12) 0.0073(12) 0.0072(13) O20 0.043(2) 0.055(2) 0.049(2) 0.0023(16) -0.0109(16) 0.0073(16) O1W 0.044(5) 0.038(5) 0.039(5) 0.008(4) 0.016(4) 0.004(4) O2W 0.052(9) 0.048(9) 0.036(7) 0.002(6) 0.021(7) -0.001(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 1.360(6) . ? C1 C2 1.411(6) . ? C1 C7 1.511(5) . ? C2 N1 1.369(4) . ? C2 C3 1.383(6) . ? C3 C4 1.413(6) . ? C3 H3 0.9300 . ? C4 C5 1.425(6) . ? C4 C8 1.482(6) . ? C5 C6 1.379(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.236(4) . ? C7 O2 1.251(4) . ? C7 Mn1 2.533(4) . ? C8 O3 1.220(4) . ? C8 O4 1.255(4) . ? C9 N2 1.413(5) . ? C9 N3 1.414(4) . ? C9 H9 0.9300 . ? C10 C11 1.362(6) . ? C10 N2 1.443(5) . ? C10 H10 0.9300 . ? C11 N3 1.449(5) . ? C11 H11 0.9300 . ? C12 N3 1.362(4) . ? C12 C13 1.390(6) . ? C12 C17 1.397(6) . ? C13 C14 1.388(6) . ? C13 H13 0.9300 . ? C14 C15 1.393(6) . ? C14 H14 0.9300 . ? C15 C16 1.397(6) . ? C15 C18 1.476(5) . ? C16 C17 1.387(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.406(6) . ? C18 C23 1.413(6) . ? C19 C20 1.397(6) . ? C19 H19 0.9300 . ? C20 C21 1.388(7) . ? C20 H20 0.9300 . ? C21 C22 1.372(7) . ? C21 N4 1.426(5) . ? C22 C23 1.340(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 N4 1.377(5) . ? C24 N5 1.413(5) . ? C24 H24 0.9300 . ? C25 C26 1.319(6) . ? C25 N4 1.417(5) . ? C25 H25 0.9300 . ? C26 N5 1.438(5) . ? C26 H26 0.9300 . ? C27 C32 1.392(6) . ? C27 C28 1.422(6) . ? C27 C33 1.436(6) . ? C28 C29 1.376(6) . ? C28 N6 1.386(4) . ? C29 C30 1.387(5) . ? C29 H29 0.9300 . ? C30 C31 1.404(5) . ? C30 C34 1.484(6) . ? C31 C32 1.399(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O6 1.226(4) . ? C33 O5 1.243(4) . ? C33 Mn2 2.590(4) . ? C34 O8 1.217(4) . ? C34 O7 1.236(4) . ? C34 Mn2 2.617(4) 2_564 ? C35 N8 1.413(5) . ? C35 N7 1.447(5) . ? C35 H35 0.9300 . ? C36 N7 1.413(4) . ? C36 C37 1.436(6) . ? C36 H36 0.9300 . ? C37 N8 1.376(4) . ? C37 H37 0.9300 . ? C38 C39 1.384(6) . ? C38 C43 1.418(6) . ? C38 N8 1.441(4) . ? C39 C40 1.307(6) . ? C39 H39 0.9300 . ? C40 C41 1.421(6) . ? C40 H40 0.9300 . ? C41 C42 1.417(6) . ? C41 C44 1.438(6) . ? C42 C43 1.360(6) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C49 1.384(6) . ? C44 C45 1.399(7) . ? C45 C46 1.380(6) . ? C45 H45 0.9300 . ? C46 C47 1.380(6) . ? C46 H46 0.9300 . ? C47 C48 1.385(7) . ? C47 N9 1.430(4) . ? C48 C49 1.386(6) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 N10 1.384(4) . ? C50 N9 1.430(5) . ? C50 H50 0.9300 . ? C51 N9 1.385(4) . ? C51 C52 1.427(6) . ? C51 H51 0.9300 . ? C52 N10 1.441(4) . ? C52 H52 0.9300 . ? C53 C54 1.359(6) . ? C53 C58 1.413(6) . ? C53 C59 1.514(6) . ? C54 N11 1.356(4) . ? C54 C55 1.410(5) . ? C55 C56 1.367(6) . ? C55 H55 0.9300 . ? C56 C57 1.397(6) . ? C56 C60 1.500(6) . ? C57 C58 1.383(6) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 O10 1.214(4) . ? C59 O9 1.268(4) . ? C59 Mn3 2.532(4) . ? C60 O11 1.241(4) . ? C60 O12 1.251(4) . ? C61 N12 1.406(4) . ? C61 N13 1.414(4) . ? C61 H61 0.9300 . ? C62 C63 1.358(6) . ? C62 N12 1.466(4) . ? C62 H62 0.9300 . ? C63 N13 1.439(4) . ? C63 H63 0.9300 . ? C64 C65 1.390(5) . ? C64 C69 1.390(6) . ? C64 N13 1.488(4) . ? C65 C66 1.390(6) . ? C65 H65 0.9300 . ? C66 C67 1.390(7) . ? C66 H66 0.9300 . ? C67 C68 1.390(6) . ? C67 C70 1.482(6) . ? C68 C69 1.390(6) . ? C68 H68 0.9300 . ? C69 H69 0.9300 . ? C70 C71 1.350(6) . ? C70 C75 1.430(6) . ? C71 C72 1.392(6) . ? C71 H71 0.9300 . ? C72 C73 1.402(6) . ? C72 H72 0.9300 . ? C73 C74 1.357(6) . ? C73 N14 1.514(4) . ? C74 C75 1.380(6) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C76 N14 1.419(4) . ? C76 N15 1.422(4) . ? C76 H76 0.9300 . ? C77 C78 1.387(5) . ? C77 N14 1.398(4) . ? C77 H77 0.9300 . ? C78 N15 1.393(4) . ? C78 H78 0.9300 . ? C79 C80 1.377(5) . ? C79 C84 1.408(6) . ? C79 C85 1.410(6) . ? C80 N16 1.377(4) . ? C80 C81 1.441(5) . ? C81 C82 1.368(6) . ? C81 H81 0.9300 . ? C82 C83 1.380(5) . ? C82 C86 1.488(5) . ? C83 C84 1.398(6) . ? C83 H83 0.9300 . ? C84 H84 0.9300 . ? C85 O14 1.237(4) . ? C85 O13 1.276(4) . ? C85 Mn4 2.592(4) . ? C86 O16 1.227(4) . ? C86 O15 1.252(4) . ? C87 N18 1.391(4) . ? C87 N17 1.415(4) . ? C87 H87 0.9300 . ? C88 N17 1.407(4) . ? C88 C89 1.422(6) . ? C88 H88 0.9300 . ? C89 N18 1.429(4) . ? C89 H89 0.9300 . ? C90 C95 1.387(6) . ? C90 C91 1.395(6) . ? C90 N18 1.451(5) . ? C91 C92 1.376(6) . ? C91 H91 0.9300 . ? C92 C93 1.391(6) . ? C92 H92 0.9300 . ? C93 C94 1.393(6) . ? C93 C96 1.503(6) . ? C94 C95 1.389(6) . ? C94 H94 0.9300 . ? C95 H95 0.9300 . ? C96 C101 1.397(4) . ? C96 C97 1.414(6) . ? C97 C98 1.387(6) . ? C97 H97 0.9300 . ? C98 C99 1.361(7) . ? C98 H98 0.9300 . ? C99 C100 1.389(6) . ? C99 N19 1.440(5) . ? C100 C101 1.378(4) . ? C100 H100 0.9300 . ? C101 H101 0.9300 . ? C102 N19 1.390(6) . ? C102 N20 1.424(6) . ? C102 H102 0.9300 . ? C103 N19 1.408(6) . ? C103 C104 1.429(6) . ? C103 H103 0.9300 . ? C104 N20 1.389(6) . ? C104 H104 0.9300 . ? C105 C110 1.366(6) . ? C105 C106 1.416(6) . ? C105 C111 1.506(6) . ? C106 N21 1.352(6) . ? C106 C107 1.380(6) . ? C107 C108 1.376(6) . ? C107 H107 0.9300 . ? C108 C109 1.360(6) . ? C108 C112 1.481(6) . ? C109 C110 1.387(6) . ? C109 H109 0.9300 . ? C110 H110 0.9300 . ? C111 O17 1.217(5) . ? C111 O18 1.257(5) . ? C111 Mn5 2.573(4) . ? C112 O20 1.230(6) . ? C112 O19 1.264(5) . ? C112 Mn5 2.591(4) 2_564 ? C113 N23 1.403(5) . ? C113 N22 1.406(5) . ? C113 H113 0.9300 . ? C114 N22 1.404(6) . ? C114 C115 1.445(5) . ? C114 H114 0.9300 . ? C115 N23 1.403(6) . ? C115 H115 0.9300 . ? C116 C121 1.380(6) . ? C116 N23 1.409(5) . ? C116 C117 1.423(5) . ? C117 C118 1.333(5) . ? C117 H117 0.9300 . ? C118 C119 1.423(6) . ? C118 H118 0.9300 . ? C119 C120 1.399(6) . ? C119 C122 1.493(6) . ? C120 C121 1.387(6) . ? C120 H120 0.9300 . ? C121 H121 0.9300 . ? C122 C127 1.393(6) . ? C122 C123 1.394(6) . ? C123 C124 1.397(6) . ? C123 H123 0.9300 . ? C124 C125 1.389(6) . ? C124 H124 0.9300 . ? C125 C126 1.381(6) . ? C125 N24 1.388(5) . ? C126 C127 1.386(6) . ? C126 H126 0.9300 . ? C127 H127 0.9300 . ? C128 N24 1.399(6) . ? C128 N25 1.429(6) . ? C128 H128 0.9300 . ? C129 N24 1.417(6) . ? C129 C130 1.448(6) . ? C129 H129 0.9300 . ? C130 N25 1.434(6) . ? C130 H130 0.9300 . ? Mn1 N5 2.060(4) 4_454 ? Mn1 N2 2.084(4) . ? Mn1 O3 2.207(3) 2 ? Mn1 O1 2.209(3) . ? Mn1 O2 2.317(3) . ? Mn1 O4 2.354(3) 2 ? Mn2 N10 2.102(4) 4_454 ? Mn2 N7 2.133(4) . ? Mn2 O7 2.156(3) 2_565 ? Mn2 O5 2.225(3) . ? Mn2 O6 2.238(3) . ? Mn2 O8 2.376(3) 2_565 ? Mn2 C34 2.617(4) 2_565 ? Mn3 O9 2.091(3) . ? Mn3 N15 2.099(4) 4_454 ? Mn3 N12 2.201(4) . ? Mn3 O12 2.222(3) 2 ? Mn3 O11 2.268(3) 2 ? Mn3 O10 2.338(3) . ? Mn4 N20 2.118(3) 4_454 ? Mn4 N17 2.161(4) . ? Mn4 O15 2.175(3) 2 ? Mn4 O14 2.202(3) . ? Mn4 O13 2.221(2) . ? Mn4 O16 2.480(3) 2 ? Mn5 N22 2.134(4) . ? Mn5 O20 2.152(3) 2_565 ? Mn5 N25 2.152(4) 4_464 ? Mn5 O17 2.162(3) . ? Mn5 O19 2.315(3) 2_565 ? Mn5 O18 2.361(3) . ? Mn5 C112 2.591(4) 2_565 ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? N5 Mn1 2.060(4) 4 ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? N10 Mn2 2.102(4) 4 ? N11 H11B 0.8999 . ? N11 H11A 0.9000 . ? N15 Mn3 2.099(4) 4 ? N16 H16A 0.8600 . ? N16 H16B 0.8600 . ? N20 Mn4 2.118(3) 4 ? N21 H21A 0.8600 . ? N21 H21B 0.8600 . ? N25 Mn5 2.152(4) 4_565 ? O3 Mn1 2.207(3) 2_554 ? O4 Mn1 2.354(3) 2_554 ? O7 Mn2 2.156(3) 2_564 ? O8 Mn2 2.376(3) 2_564 ? O11 Mn3 2.268(3) 2_554 ? O12 Mn3 2.222(3) 2_554 ? O15 Mn4 2.175(3) 2_554 ? O16 Mn4 2.480(3) 2_554 ? O19 Mn5 2.315(3) 2_564 ? O20 Mn5 2.152(3) 2_564 ? O1W H1X 0.8501 . ? O1W H1Y 0.8501 . ? O2W H2X 0.8500 . ? O2W H2Y 0.8502 . ? 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(4) . . ? C6 C1 C7 119.8(4) . . ? C2 C1 C7 119.8(3) . . ? N1 C2 C3 114.3(3) . . ? N1 C2 C1 126.4(3) . . ? C3 C2 C1 119.2(4) . . ? C2 C3 C4 120.8(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 118.9(4) . . ? C3 C4 C8 120.0(4) . . ? C5 C4 C8 120.8(4) . . ? C6 C5 C4 118.4(4) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C1 C6 C5 122.7(4) . . ? C1 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? O1 C7 O2 125.8(3) . . ? O1 C7 C1 120.5(3) . . ? O2 C7 C1 113.6(3) . . ? O1 C7 Mn1 60.70(16) . . ? O2 C7 Mn1 65.66(16) . . ? C1 C7 Mn1 172.6(3) . . ? O3 C8 O4 117.2(3) . . ? O3 C8 C4 120.3(4) . . ? O4 C8 C4 122.5(4) . . ? N2 C9 N3 108.5(3) . . ? N2 C9 H9 125.8 . . ? N3 C9 H9 125.8 . . ? C11 C10 N2 111.7(4) . . ? C11 C10 H10 124.2 . . ? N2 C10 H10 124.2 . . ? C10 C11 N3 106.0(4) . . ? C10 C11 H11 127.0 . . ? N3 C11 H11 127.0 . . ? N3 C12 C13 124.2(4) . . ? N3 C12 C17 115.8(4) . . ? C13 C12 C17 119.8(4) . . ? C14 C13 C12 120.4(4) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 C18 119.1(4) . . ? C16 C15 C18 120.7(4) . . ? C17 C16 C15 119.8(4) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C12 120.1(4) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C19 C18 C23 115.6(4) . . ? C19 C18 C15 127.9(4) . . ? C23 C18 C15 116.3(4) . . ? C20 C19 C18 119.9(4) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 119.2(4) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 122.8(4) . . ? C22 C21 N4 120.5(4) . . ? C20 C21 N4 116.6(4) . . ? C23 C22 C21 115.9(4) . . ? C23 C22 H22 122.1 . . ? C21 C22 H22 122.1 . . ? C22 C23 C18 125.9(4) . . ? C22 C23 H23 117.0 . . ? C18 C23 H23 117.0 . . ? N4 C24 N5 110.7(3) . . ? N4 C24 H24 124.7 . . ? N5 C24 H24 124.7 . . ? C26 C25 N4 110.6(4) . . ? C26 C25 H25 124.7 . . ? N4 C25 H25 124.7 . . ? C25 C26 N5 109.3(4) . . ? C25 C26 H26 125.4 . . ? N5 C26 H26 125.4 . . ? C32 C27 C28 119.0(4) . . ? C32 C27 C33 118.3(4) . . ? C28 C27 C33 122.5(4) . . ? C29 C28 N6 116.3(4) . . ? C29 C28 C27 120.0(4) . . ? N6 C28 C27 123.3(3) . . ? C28 C29 C30 121.5(4) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C29 C30 C31 118.7(4) . . ? C29 C30 C34 121.5(4) . . ? C31 C30 C34 119.7(4) . . ? C32 C31 C30 120.8(4) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C27 C32 C31 120.0(4) . . ? C27 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? O6 C33 O5 117.2(3) . . ? O6 C33 C27 121.5(4) . . ? O5 C33 C27 121.3(4) . . ? O6 C33 Mn2 59.69(17) . . ? O5 C33 Mn2 59.14(17) . . ? C27 C33 Mn2 169.7(3) . . ? O8 C34 O7 118.1(3) . . ? O8 C34 C30 127.6(3) . . ? O7 C34 C30 114.1(3) . . ? O8 C34 Mn2 65.09(18) . 2_564 ? O7 C34 Mn2 54.82(16) . 2_564 ? C30 C34 Mn2 164.8(3) . 2_564 ? N8 C35 N7 107.5(3) . . ? N8 C35 H35 126.2 . . ? N7 C35 H35 126.2 . . ? N7 C36 C37 107.1(3) . . ? N7 C36 H36 126.4 . . ? C37 C36 H36 126.4 . . ? N8 C37 C36 109.2(3) . . ? N8 C37 H37 125.4 . . ? C36 C37 H37 125.4 . . ? C39 C38 C43 116.9(4) . . ? C39 C38 N8 115.6(4) . . ? C43 C38 N8 126.4(3) . . ? C40 C39 C38 120.3(4) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 125.5(5) . . ? C39 C40 H40 117.3 . . ? C41 C40 H40 117.3 . . ? C42 C41 C40 114.2(4) . . ? C42 C41 C44 127.5(4) . . ? C40 C41 C44 117.6(4) . . ? C43 C42 C41 120.1(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C38 122.4(4) . . ? C42 C43 H43 118.8 . . ? C38 C43 H43 118.8 . . ? C49 C44 C45 120.6(4) . . ? C49 C44 C41 118.5(4) . . ? C45 C44 C41 119.9(4) . . ? C46 C45 C44 118.8(4) . . ? C46 C45 H45 120.6 . . ? C44 C45 H45 120.6 . . ? C47 C46 C45 121.2(5) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 119.5(4) . . ? C46 C47 N9 129.8(4) . . ? C48 C47 N9 110.1(3) . . ? C47 C48 C49 120.5(4) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C44 C49 C48 119.4(5) . . ? C44 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? N10 C50 N9 109.2(3) . . ? N10 C50 H50 125.4 . . ? N9 C50 H50 125.4 . . ? N9 C51 C52 109.8(3) . . ? N9 C51 H51 125.1 . . ? C52 C51 H51 125.1 . . ? C51 C52 N10 105.9(3) . . ? C51 C52 H52 127.1 . . ? N10 C52 H52 127.1 . . ? C54 C53 C58 120.6(4) . . ? C54 C53 C59 121.2(4) . . ? C58 C53 C59 118.0(4) . . ? N11 C54 C53 130.6(3) . . ? N11 C54 C55 108.6(3) . . ? C53 C54 C55 120.6(4) . . ? C56 C55 C54 119.3(4) . . ? C56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C55 C56 C57 120.0(4) . . ? C55 C56 C60 121.1(4) . . ? C57 C56 C60 118.3(4) . . ? C58 C57 C56 120.9(4) . . ? C58 C57 H57 119.5 . . ? C56 C57 H57 119.5 . . ? C57 C58 C53 118.2(4) . . ? C57 C58 H58 120.9 . . ? C53 C58 H58 120.9 . . ? O10 C59 O9 121.3(3) . . ? O10 C59 C53 116.6(3) . . ? O9 C59 C53 122.0(3) . . ? O10 C59 Mn3 66.84(19) . . ? O9 C59 Mn3 55.41(16) . . ? C53 C59 Mn3 172.1(3) . . ? O11 C60 O12 114.7(3) . . ? O11 C60 C56 114.9(3) . . ? O12 C60 C56 130.4(4) . . ? N12 C61 N13 108.8(3) . . ? N12 C61 H61 125.6 . . ? N13 C61 H61 125.6 . . ? C63 C62 N12 110.0(3) . . ? C63 C62 H62 125.0 . . ? N12 C62 H62 125.0 . . ? C62 C63 N13 107.5(3) . . ? C62 C63 H63 126.2 . . ? N13 C63 H63 126.2 . . ? C65 C64 C69 120.0(4) . . ? C65 C64 N13 120.0(3) . . ? C69 C64 N13 119.9(3) . . ? C66 C65 C64 120.0(4) . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C67 120.0(4) . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C68 C67 C66 120.0(4) . . ? C68 C67 C70 112.8(4) . . ? C66 C67 C70 127.2(4) . . ? C67 C68 C69 120.0(4) . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C68 C69 C64 120.0(4) . . ? C68 C69 H69 120.0 . . ? C64 C69 H69 120.0 . . ? C71 C70 C75 119.4(4) . . ? C71 C70 C67 111.3(4) . . ? C75 C70 C67 129.2(4) . . ? C70 C71 C72 123.3(4) . . ? C70 C71 H71 118.3 . . ? C72 C71 H71 118.3 . . ? C71 C72 C73 116.2(4) . . ? C71 C72 H72 121.9 . . ? C73 C72 H72 121.9 . . ? C74 C73 C72 121.7(4) . . ? C74 C73 N14 124.6(4) . . ? C72 C73 N14 113.7(3) . . ? C73 C74 C75 121.7(4) . . ? C73 C74 H74 119.1 . . ? C75 C74 H74 119.1 . . ? C74 C75 C70 117.5(4) . . ? C74 C75 H75 121.2 . . ? C70 C75 H75 121.2 . . ? N14 C76 N15 108.7(3) . . ? N14 C76 H76 125.7 . . ? N15 C76 H76 125.7 . . ? C78 C77 N14 109.9(3) . . ? C78 C77 H77 125.1 . . ? N14 C77 H77 125.1 . . ? C77 C78 N15 108.7(3) . . ? C77 C78 H78 125.7 . . ? N15 C78 H78 125.7 . . ? C80 C79 C84 118.6(4) . . ? C80 C79 C85 120.8(4) . . ? C84 C79 C85 120.6(4) . . ? N16 C80 C79 123.2(3) . . ? N16 C80 C81 116.0(3) . . ? C79 C80 C81 120.5(4) . . ? C82 C81 C80 119.8(3) . . ? C82 C81 H81 120.1 . . ? C80 C81 H81 120.1 . . ? C81 C82 C83 119.6(4) . . ? C81 C82 C86 118.6(3) . . ? C83 C82 C86 121.7(4) . . ? C82 C83 C84 121.3(4) . . ? C82 C83 H83 119.3 . . ? C84 C83 H83 119.3 . . ? C83 C84 C79 120.0(4) . . ? C83 C84 H84 120.0 . . ? C79 C84 H84 120.0 . . ? O14 C85 O13 114.8(3) . . ? O14 C85 C79 125.1(3) . . ? O13 C85 C79 120.1(4) . . ? O14 C85 Mn4 57.98(17) . . ? O13 C85 Mn4 58.94(16) . . ? C79 C85 Mn4 165.2(3) . . ? O16 C86 O15 118.2(3) . . ? O16 C86 C82 126.2(4) . . ? O15 C86 C82 115.6(3) . . ? N18 C87 N17 109.2(3) . . ? N18 C87 H87 125.4 . . ? N17 C87 H87 125.4 . . ? N17 C88 C89 107.1(3) . . ? N17 C88 H88 126.5 . . ? C89 C88 H88 126.5 . . ? C88 C89 N18 108.5(4) . . ? C88 C89 H89 125.8 . . ? N18 C89 H89 125.8 . . ? C95 C90 C91 119.7(4) . . ? C95 C90 N18 118.9(3) . . ? C91 C90 N18 121.2(4) . . ? C92 C91 C90 119.9(4) . . ? C92 C91 H91 120.1 . . ? C90 C91 H91 120.1 . . ? C91 C92 C93 120.9(4) . . ? C91 C92 H92 119.6 . . ? C93 C92 H92 119.6 . . ? C92 C93 C94 119.2(4) . . ? C92 C93 C96 119.7(4) . . ? C94 C93 C96 121.1(4) . . ? C95 C94 C93 120.0(4) . . ? C95 C94 H94 120.0 . . ? C93 C94 H94 120.0 . . ? C90 C95 C94 120.3(4) . . ? C90 C95 H95 119.8 . . ? C94 C95 H95 119.8 . . ? C101 C96 C97 118.2(3) . . ? C101 C96 C93 118.3(3) . . ? C97 C96 C93 123.4(4) . . ? C98 C97 C96 119.3(4) . . ? C98 C97 H97 120.3 . . ? C96 C97 H97 120.3 . . ? C99 C98 C97 121.2(4) . . ? C99 C98 H98 119.4 . . ? C97 C98 H98 119.4 . . ? C98 C99 C100 120.3(4) . . ? C98 C99 N19 123.6(4) . . ? C100 C99 N19 116.1(4) . . ? C101 C100 C99 119.5(4) . . ? C101 C100 H100 120.2 . . ? C99 C100 H100 120.2 . . ? C100 C101 C96 121.3(3) . . ? C100 C101 H101 119.4 . . ? C96 C101 H101 119.4 . . ? N19 C102 N20 106.9(4) . . ? N19 C102 H102 126.6 . . ? N20 C102 H102 126.6 . . ? N19 C103 C104 105.6(4) . . ? N19 C103 H103 127.2 . . ? C104 C103 H103 127.2 . . ? N20 C104 C103 109.0(4) . . ? N20 C104 H104 125.5 . . ? C103 C104 H104 125.5 . . ? C110 C105 C106 121.6(4) . . ? C110 C105 C111 121.3(4) . . ? C106 C105 C111 117.1(4) . . ? N21 C106 C107 115.4(4) . . ? N21 C106 C105 127.3(4) . . ? C107 C106 C105 117.2(4) . . ? C108 C107 C106 120.8(4) . . ? C108 C107 H107 119.6 . . ? C106 C107 H107 119.6 . . ? C109 C108 C107 121.3(4) . . ? C109 C108 C112 118.9(4) . . ? C107 C108 C112 119.8(4) . . ? C108 C109 C110 119.8(4) . . ? C108 C109 H109 120.1 . . ? C110 C109 H109 120.1 . . ? C105 C110 C109 119.4(4) . . ? C105 C110 H110 120.3 . . ? C109 C110 H110 120.3 . . ? O17 C111 O18 119.6(4) . . ? O17 C111 C105 118.0(4) . . ? O18 C111 C105 122.3(4) . . ? O17 C111 Mn5 56.8(2) . . ? O18 C111 Mn5 66.1(2) . . ? C105 C111 Mn5 163.8(3) . . ? O20 C112 O19 116.2(4) . . ? O20 C112 C108 128.4(4) . . ? O19 C112 C108 115.5(4) . . ? O20 C112 Mn5 55.6(2) . 2_564 ? O19 C112 Mn5 63.2(2) . 2_564 ? C108 C112 Mn5 162.8(3) . 2_564 ? N23 C113 N22 108.6(4) . . ? N23 C113 H113 125.7 . . ? N22 C113 H113 125.7 . . ? N22 C114 C115 107.3(4) . . ? N22 C114 H114 126.4 . . ? C115 C114 H114 126.4 . . ? N23 C115 C114 107.4(4) . . ? N23 C115 H115 126.3 . . ? C114 C115 H115 126.3 . . ? C121 C116 N23 121.6(4) . . ? C121 C116 C117 120.3(4) . . ? N23 C116 C117 118.0(3) . . ? C118 C117 C116 117.4(4) . . ? C118 C117 H117 121.3 . . ? C116 C117 H117 121.3 . . ? C117 C118 C119 123.5(4) . . ? C117 C118 H118 118.3 . . ? C119 C118 H118 118.3 . . ? C120 C119 C118 118.7(4) . . ? C120 C119 C122 120.5(4) . . ? C118 C119 C122 120.8(4) . . ? C121 C120 C119 118.0(4) . . ? C121 C120 H120 121.0 . . ? C119 C120 H120 121.0 . . ? C116 C121 C120 121.9(4) . . ? C116 C121 H121 119.0 . . ? C120 C121 H121 119.0 . . ? C127 C122 C123 119.3(4) . . ? C127 C122 C119 120.9(4) . . ? C123 C122 C119 119.8(4) . . ? C122 C123 C124 120.1(4) . . ? C122 C123 H123 119.9 . . ? C124 C123 H123 119.9 . . ? C125 C124 C123 120.0(4) . . ? C125 C124 H124 120.0 . . ? C123 C124 H124 120.0 . . ? C126 C125 N24 120.4(4) . . ? C126 C125 C124 119.8(4) . . ? N24 C125 C124 119.8(4) . . ? C125 C126 C127 120.6(4) . . ? C125 C126 H126 119.7 . . ? C127 C126 H126 119.7 . . ? C126 C127 C122 120.3(4) . . ? C126 C127 H127 119.9 . . ? C122 C127 H127 119.9 . . ? N24 C128 N25 107.8(4) . . ? N24 C128 H128 126.1 . . ? N25 C128 H128 126.1 . . ? N24 C129 C130 107.3(4) . . ? N24 C129 H129 126.3 . . ? C130 C129 H129 126.3 . . ? N25 C130 C129 106.7(4) . . ? N25 C130 H130 126.6 . . ? C129 C130 H130 126.6 . . ? N5 Mn1 N2 100.20(18) 4_454 . ? N5 Mn1 O3 87.54(15) 4_454 2 ? N2 Mn1 O3 96.47(13) . 2 ? N5 Mn1 O1 116.98(16) 4_454 . ? N2 Mn1 O1 99.46(13) . . ? O3 Mn1 O1 147.46(13) 2 . ? N5 Mn1 O2 90.00(15) 4_454 . ? N2 Mn1 O2 157.97(13) . . ? O3 Mn1 O2 103.49(11) 2 . ? O1 Mn1 O2 58.55(11) . . ? N5 Mn1 O4 140.00(15) 4_454 2 ? N2 Mn1 O4 73.68(15) . 2 ? O3 Mn1 O4 55.05(11) 2 2 ? O1 Mn1 O4 102.98(12) . 2 ? O2 Mn1 O4 110.45(11) . 2 ? N5 Mn1 C7 103.22(13) 4_454 . ? N2 Mn1 C7 128.49(11) . . ? O3 Mn1 C7 129.51(9) 2 . ? O1 Mn1 C7 29.22(8) . . ? O2 Mn1 C7 29.48(8) . . ? O4 Mn1 C7 111.35(9) 2 . ? N10 Mn2 N7 106.67(16) 4_454 . ? N10 Mn2 O7 81.73(13) 4_454 2_565 ? N7 Mn2 O7 108.25(11) . 2_565 ? N10 Mn2 O5 126.73(13) 4_454 . ? N7 Mn2 O5 89.04(13) . . ? O7 Mn2 O5 141.66(12) 2_565 . ? N10 Mn2 O6 84.96(13) 4_454 . ? N7 Mn2 O6 141.18(12) . . ? O7 Mn2 O6 110.05(11) 2_565 . ? O5 Mn2 O6 56.36(11) . . ? N10 Mn2 O8 136.48(13) 4_454 2_565 ? N7 Mn2 O8 84.60(13) . 2_565 ? O7 Mn2 O8 55.08(11) 2_565 2_565 ? O5 Mn2 O8 94.56(11) . 2_565 ? O6 Mn2 O8 112.60(11) . 2_565 ? N10 Mn2 C33 104.01(11) 4_454 . ? N7 Mn2 C33 114.33(11) . . ? O7 Mn2 C33 132.76(12) 2_565 . ? O5 Mn2 C33 28.65(9) . . ? O6 Mn2 C33 28.23(10) . . ? O8 Mn2 C33 109.12(9) 2_565 . ? N10 Mn2 C34 108.79(11) 4_454 2_565 ? N7 Mn2 C34 93.39(9) . 2_565 ? O7 Mn2 C34 27.94(9) 2_565 2_565 ? O5 Mn2 C34 120.97(9) . 2_565 ? O6 Mn2 C34 118.28(10) . 2_565 ? O8 Mn2 C34 27.69(9) 2_565 2_565 ? C33 Mn2 C34 128.11(14) . 2_565 ? O9 Mn3 N15 117.03(13) . 4_454 ? O9 Mn3 N12 85.94(13) . . ? N15 Mn3 N12 85.15(15) 4_454 . ? O9 Mn3 O12 101.52(11) . 2 ? N15 Mn3 O12 138.65(12) 4_454 2 ? N12 Mn3 O12 83.15(12) . 2 ? O9 Mn3 O11 143.16(11) . 2 ? N15 Mn3 O11 95.34(13) 4_454 2 ? N12 Mn3 O11 115.54(12) . 2 ? O12 Mn3 O11 55.70(11) 2 2 ? O9 Mn3 O10 58.18(11) . . ? N15 Mn3 O10 100.67(12) 4_454 . ? N12 Mn3 O10 142.45(12) . . ? O12 Mn3 O10 112.55(11) 2 . ? O11 Mn3 O10 100.95(10) 2 . ? O9 Mn3 C59 29.96(9) . . ? N15 Mn3 C59 108.29(10) 4_454 . ? N12 Mn3 C59 114.38(10) . . ? O12 Mn3 C59 112.68(10) 2 . ? O11 Mn3 C59 125.92(9) 2 . ? O10 Mn3 C59 28.53(9) . . ? N20 Mn4 N17 89.34(13) 4_454 . ? N20 Mn4 O15 111.50(12) 4_454 2 ? N17 Mn4 O15 100.05(12) . 2 ? N20 Mn4 O14 94.57(12) 4_454 . ? N17 Mn4 O14 148.18(12) . . ? O15 Mn4 O14 107.72(11) 2 . ? N20 Mn4 O13 109.57(11) 4_454 . ? N17 Mn4 O13 91.77(11) . . ? O15 Mn4 O13 137.23(11) 2 . ? O14 Mn4 O13 57.19(11) . . ? N20 Mn4 O16 154.99(11) 4_454 2 ? N17 Mn4 O16 75.30(12) . 2 ? O15 Mn4 O16 53.91(10) 2 2 ? O14 Mn4 O16 108.94(11) . 2 ? O13 Mn4 O16 90.83(10) . 2 ? N20 Mn4 C85 98.94(9) 4_454 . ? N17 Mn4 C85 119.79(9) . . ? O15 Mn4 C85 129.84(8) 2 . ? O14 Mn4 C85 28.43(9) . . ? O13 Mn4 C85 29.47(9) . . ? O16 Mn4 C85 105.79(9) 2 . ? N22 Mn5 O20 89.02(13) . 2_565 ? N22 Mn5 N25 95.99(14) . 4_464 ? O20 Mn5 N25 131.35(16) 2_565 4_464 ? N22 Mn5 O17 92.42(13) . . ? O20 Mn5 O17 100.37(14) 2_565 . ? N25 Mn5 O17 127.56(14) 4_464 . ? N22 Mn5 O19 117.71(12) . 2_565 ? O20 Mn5 O19 56.43(13) 2_565 2_565 ? N25 Mn5 O19 79.11(14) 4_464 2_565 ? O17 Mn5 O19 138.95(10) . 2_565 ? N22 Mn5 O18 145.78(12) . . ? O20 Mn5 O18 108.32(11) 2_565 . ? N25 Mn5 O18 94.02(14) 4_464 . ? O17 Mn5 O18 56.21(11) . . ? O19 Mn5 O18 96.29(10) 2_565 . ? N22 Mn5 C111 117.28(13) . . ? O20 Mn5 C111 111.73(14) 2_565 . ? N25 Mn5 C111 108.53(15) 4_464 . ? O17 Mn5 C111 28.12(11) . . ? O19 Mn5 C111 123.09(12) 2_565 . ? O18 Mn5 C111 29.10(11) . . ? N22 Mn5 C112 99.98(14) . 2_565 ? O20 Mn5 C112 28.15(14) 2_565 2_565 ? N25 Mn5 C112 104.06(17) 4_464 2_565 ? O17 Mn5 C112 125.20(15) . 2_565 ? O19 Mn5 C112 29.17(12) 2_565 2_565 ? O18 Mn5 C112 109.15(13) . 2_565 ? C111 Mn5 C112 126.32(14) . 2_565 ? C2 N1 H1A 120.0 . . ? C2 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C9 N2 C10 105.4(3) . . ? C9 N2 Mn1 126.8(2) . . ? C10 N2 Mn1 124.9(3) . . ? C12 N3 C9 126.7(3) . . ? C12 N3 C11 124.3(3) . . ? C9 N3 C11 108.4(3) . . ? C24 N4 C25 105.3(3) . . ? C24 N4 C21 128.1(3) . . ? C25 N4 C21 126.4(3) . . ? C24 N5 C26 103.9(3) . . ? C24 N5 Mn1 127.2(3) . 4 ? C26 N5 Mn1 125.1(3) . 4 ? C28 N6 H6A 120.0 . . ? C28 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C36 N7 C35 107.3(3) . . ? C36 N7 Mn2 126.6(2) . . ? C35 N7 Mn2 125.1(2) . . ? C37 N8 C35 108.7(3) . . ? C37 N8 C38 131.9(3) . . ? C35 N8 C38 119.3(3) . . ? C51 N9 C50 107.0(3) . . ? C51 N9 C47 137.0(3) . . ? C50 N9 C47 115.7(3) . . ? C50 N10 C52 108.1(3) . . ? C50 N10 Mn2 130.9(2) . 4 ? C52 N10 Mn2 117.2(2) . 4 ? C54 N11 H11B 117.1 . . ? C54 N11 H11A 125.5 . . ? H11B N11 H11A 117.4 . . ? C61 N12 C62 105.5(2) . . ? C61 N12 Mn3 130.2(2) . . ? C62 N12 Mn3 123.8(2) . . ? C61 N13 C63 108.1(2) . . ? C61 N13 C64 127.0(2) . . ? C63 N13 C64 124.6(2) . . ? C77 N14 C76 106.0(2) . . ? C77 N14 C73 136.2(3) . . ? C76 N14 C73 117.8(2) . . ? C78 N15 C76 106.8(2) . . ? C78 N15 Mn3 146.4(2) . 4 ? C76 N15 Mn3 106.7(2) . 4 ? C80 N16 H16A 120.0 . . ? C80 N16 H16B 120.0 . . ? H16A N16 H16B 120.0 . . ? C88 N17 C87 108.2(3) . . ? C88 N17 Mn4 123.16(19) . . ? C87 N17 Mn4 128.6(2) . . ? C87 N18 C89 107.0(3) . . ? C87 N18 C90 132.4(3) . . ? C89 N18 C90 120.0(2) . . ? C102 N19 C103 110.4(4) . . ? C102 N19 C99 119.3(3) . . ? C103 N19 C99 130.2(3) . . ? C104 N20 C102 108.1(3) . . ? C104 N20 Mn4 143.4(3) . 4 ? C102 N20 Mn4 108.4(3) . 4 ? C106 N21 H21A 120.0 . . ? C106 N21 H21B 120.0 . . ? H21A N21 H21B 120.0 . . ? C114 N22 C113 108.3(3) . . ? C114 N22 Mn5 126.5(3) . . ? C113 N22 Mn5 125.0(3) . . ? C113 N23 C115 108.4(3) . . ? C113 N23 C116 127.4(4) . . ? C115 N23 C116 123.8(4) . . ? C125 N24 C128 126.4(4) . . ? C125 N24 C129 123.8(4) . . ? C128 N24 C129 109.7(4) . . ? C128 N25 C130 108.3(4) . . ? C128 N25 Mn5 120.6(3) . 4_565 ? C130 N25 Mn5 130.4(3) . 4_565 ? C7 O1 Mn1 90.08(19) . . ? C7 O2 Mn1 84.86(17) . . ? C8 O3 Mn1 97.1(2) . 2_554 ? C8 O4 Mn1 89.14(19) . 2_554 ? C33 O5 Mn2 92.20(19) . . ? C33 O6 Mn2 92.1(2) . . ? C34 O7 Mn2 97.2(2) . 2_564 ? C34 O8 Mn2 87.2(2) . 2_564 ? C59 O9 Mn3 94.6(2) . . ? C59 O10 Mn3 84.6(2) . . ? C60 O11 Mn3 92.91(19) . 2_554 ? C60 O12 Mn3 94.83(19) . 2_554 ? C85 O13 Mn4 91.59(19) . . ? C85 O14 Mn4 93.59(19) . . ? C86 O15 Mn4 99.82(19) . 2_554 ? C86 O16 Mn4 85.94(19) . 2_554 ? C111 O17 Mn5 95.0(3) . . ? C111 O18 Mn5 84.8(2) . . ? C112 O19 Mn5 87.6(3) . 2_564 ? C112 O20 Mn5 96.2(3) . 2_564 ? H1X O1W H1Y 109.5 . . ? H2X O2W H2Y 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 C6 C1 C2 N1 -176.9(4) . . . . ? C7 C1 C2 N1 -4.4(6) . . . . ? C6 C1 C2 C3 -0.4(6) . . . . ? C7 C1 C2 C3 172.0(4) . . . . ? N1 C2 C3 C4 178.3(3) . . . . ? C1 C2 C3 C4 1.5(6) . . . . ? C2 C3 C4 C5 -1.9(6) . . . . ? C2 C3 C4 C8 172.6(4) . . . . ? C3 C4 C5 C6 1.2(6) . . . . ? C8 C4 C5 C6 -173.2(4) . . . . ? C2 C1 C6 C5 -0.2(6) . . . . ? C7 C1 C6 C5 -172.6(4) . . . . ? C4 C5 C6 C1 -0.2(6) . . . . ? C6 C1 C7 O1 13.7(6) . . . . ? C2 C1 C7 O1 -158.7(4) . . . . ? C6 C1 C7 O2 -166.0(3) . . . . ? C2 C1 C7 O2 21.6(5) . . . . ? C3 C4 C8 O3 -7.4(6) . . . . ? C5 C4 C8 O3 166.9(4) . . . . ? C3 C4 C8 O4 173.7(3) . . . . ? C5 C4 C8 O4 -11.9(6) . . . . ? N2 C10 C11 N3 -2.5(5) . . . . ? N3 C12 C13 C14 174.6(3) . . . . ? C17 C12 C13 C14 0.7(6) . . . . ? C12 C13 C14 C15 0.6(7) . . . . ? C13 C14 C15 C16 -1.1(7) . . . . ? C13 C14 C15 C18 176.2(4) . . . . ? C14 C15 C16 C17 0.4(8) . . . . ? C18 C15 C16 C17 -176.8(5) . . . . ? C15 C16 C17 C12 0.9(8) . . . . ? N3 C12 C17 C16 -175.8(4) . . . . ? C13 C12 C17 C16 -1.4(7) . . . . ? C14 C15 C18 C19 -18.3(7) . . . . ? C16 C15 C18 C19 159.0(5) . . . . ? C14 C15 C18 C23 156.8(4) . . . . ? C16 C15 C18 C23 -26.0(7) . . . . ? C23 C18 C19 C20 -0.8(6) . . . . ? C15 C18 C19 C20 174.3(4) . . . . ? C18 C19 C20 C21 2.1(6) . . . . ? C19 C20 C21 C22 2.2(7) . . . . ? C19 C20 C21 N4 -179.8(3) . . . . ? C20 C21 C22 C23 -7.7(7) . . . . ? N4 C21 C22 C23 174.5(4) . . . . ? C21 C22 C23 C18 9.4(7) . . . . ? C19 C18 C23 C22 -5.4(7) . . . . ? C15 C18 C23 C22 179.0(4) . . . . ? N4 C25 C26 N5 3.8(4) . . . . ? C32 C27 C28 C29 1.9(7) . . . . ? C33 C27 C28 C29 -174.0(4) . . . . ? C32 C27 C28 N6 174.3(4) . . . . ? C33 C27 C28 N6 -1.6(7) . . . . ? N6 C28 C29 C30 -174.1(3) . . . . ? C27 C28 C29 C30 -1.2(7) . . . . ? C28 C29 C30 C31 0.1(6) . . . . ? C28 C29 C30 C34 178.8(4) . . . . ? C29 C30 C31 C32 0.2(6) . . . . ? C34 C30 C31 C32 -178.5(4) . . . . ? C28 C27 C32 C31 -1.6(6) . . . . ? C33 C27 C32 C31 174.4(4) . . . . ? C30 C31 C32 C27 0.6(6) . . . . ? C32 C27 C33 O6 175.4(4) . . . . ? C28 C27 C33 O6 -8.7(7) . . . . ? C32 C27 C33 O5 -2.0(6) . . . . ? C28 C27 C33 O5 173.9(4) . . . . ? C32 C27 C33 Mn2 -91.3(18) . . . . ? C28 C27 C33 Mn2 84.6(19) . . . . ? C29 C30 C34 O8 -161.4(4) . . . . ? C31 C30 C34 O8 17.2(6) . . . . ? C29 C30 C34 O7 14.2(6) . . . . ? C31 C30 C34 O7 -167.2(3) . . . . ? C29 C30 C34 Mn2 54.9(13) . . . 2_564 ? C31 C30 C34 Mn2 -126.5(10) . . . 2_564 ? N7 C36 C37 N8 -1.9(4) . . . . ? C43 C38 C39 C40 0.4(7) . . . . ? N8 C38 C39 C40 169.4(4) . . . . ? C38 C39 C40 C41 5.8(8) . . . . ? C39 C40 C41 C42 -8.9(7) . . . . ? C39 C40 C41 C44 162.6(5) . . . . ? C40 C41 C42 C43 6.0(6) . . . . ? C44 C41 C42 C43 -164.5(5) . . . . ? C41 C42 C43 C38 -0.7(7) . . . . ? C39 C38 C43 C42 -2.8(7) . . . . ? N8 C38 C43 C42 -170.5(4) . . . . ? C42 C41 C44 C49 -18.0(7) . . . . ? C40 C41 C44 C49 171.8(4) . . . . ? C42 C41 C44 C45 150.3(5) . . . . ? C40 C41 C44 C45 -19.9(6) . . . . ? C49 C44 C45 C46 1.1(7) . . . . ? C41 C44 C45 C46 -167.0(4) . . . . ? C44 C45 C46 C47 0.2(7) . . . . ? C45 C46 C47 C48 -1.2(7) . . . . ? C45 C46 C47 N9 168.5(4) . . . . ? C46 C47 C48 C49 1.0(7) . . . . ? N9 C47 C48 C49 -170.7(4) . . . . ? C45 C44 C49 C48 -1.4(7) . . . . ? C41 C44 C49 C48 166.9(4) . . . . ? C47 C48 C49 C44 0.4(7) . . . . ? N9 C51 C52 N10 3.0(4) . . . . ? C58 C53 C54 N11 -177.1(4) . . . . ? C59 C53 C54 N11 -2.1(7) . . . . ? C58 C53 C54 C55 -1.9(6) . . . . ? C59 C53 C54 C55 173.1(4) . . . . ? N11 C54 C55 C56 175.9(3) . . . . ? C53 C54 C55 C56 -0.3(6) . . . . ? C54 C55 C56 C57 4.4(6) . . . . ? C54 C55 C56 C60 175.6(4) . . . . ? C55 C56 C57 C58 -6.4(6) . . . . ? C60 C56 C57 C58 -178.0(4) . . . . ? C56 C57 C58 C53 4.2(6) . . . . ? C54 C53 C58 C57 -0.1(6) . . . . ? C59 C53 C58 C57 -175.3(4) . . . . ? C54 C53 C59 O10 16.9(6) . . . . ? C58 C53 C59 O10 -168.0(3) . . . . ? C54 C53 C59 O9 -166.0(4) . . . . ? C58 C53 C59 O9 9.1(6) . . . . ? C55 C56 C60 O11 -7.8(6) . . . . ? C57 C56 C60 O11 163.6(4) . . . . ? C55 C56 C60 O12 174.3(4) . . . . ? C57 C56 C60 O12 -14.3(7) . . . . ? N12 C62 C63 N13 -2.5(4) . . . . ? C69 C64 C65 C66 0.0(7) . . . . ? N13 C64 C65 C66 -178.2(4) . . . . ? C64 C65 C66 C67 0.0(7) . . . . ? C65 C66 C67 C68 0.0(7) . . . . ? C65 C66 C67 C70 -179.2(5) . . . . ? C66 C67 C68 C69 0.0(8) . . . . ? C70 C67 C68 C69 179.3(4) . . . . ? C67 C68 C69 C64 0.0(7) . . . . ? C65 C64 C69 C68 0.0(7) . . . . ? N13 C64 C69 C68 178.2(4) . . . . ? C68 C67 C70 C71 -148.8(5) . . . . ? C66 C67 C70 C71 30.4(7) . . . . ? C68 C67 C70 C75 35.2(7) . . . . ? C66 C67 C70 C75 -145.6(5) . . . . ? C75 C70 C71 C72 4.9(8) . . . . ? C67 C70 C71 C72 -171.6(4) . . . . ? C70 C71 C72 C73 -5.1(7) . . . . ? C71 C72 C73 C74 2.0(7) . . . . ? C71 C72 C73 N14 -178.6(4) . . . . ? C72 C73 C74 C75 1.0(7) . . . . ? N14 C73 C74 C75 -178.3(4) . . . . ? C73 C74 C75 C70 -1.3(7) . . . . ? C71 C70 C75 C74 -1.5(7) . . . . ? C67 C70 C75 C74 174.2(5) . . . . ? N14 C77 C78 N15 2.0(4) . . . . ? C84 C79 C80 N16 -176.5(3) . . . . ? C85 C79 C80 N16 3.2(6) . . . . ? C84 C79 C80 C81 -3.3(6) . . . . ? C85 C79 C80 C81 176.3(4) . . . . ? N16 C80 C81 C82 177.0(3) . . . . ? C79 C80 C81 C82 3.3(6) . . . . ? C80 C81 C82 C83 -1.1(6) . . . . ? C80 C81 C82 C86 -179.8(4) . . . . ? C81 C82 C83 C84 -1.0(7) . . . . ? C86 C82 C83 C84 177.7(4) . . . . ? C82 C83 C84 C79 0.9(7) . . . . ? C80 C79 C84 C83 1.2(6) . . . . ? C85 C79 C84 C83 -178.4(4) . . . . ? C80 C79 C85 O14 6.1(6) . . . . ? C84 C79 C85 O14 -174.3(4) . . . . ? C80 C79 C85 O13 -172.8(3) . . . . ? C84 C79 C85 O13 6.8(6) . . . . ? C80 C79 C85 Mn4 -90.9(12) . . . . ? C84 C79 C85 Mn4 88.7(12) . . . . ? C81 C82 C86 O16 163.7(4) . . . . ? C83 C82 C86 O16 -15.0(7) . . . . ? C81 C82 C86 O15 -16.7(6) . . . . ? C83 C82 C86 O15 164.6(4) . . . . ? N17 C88 C89 N18 0.1(4) . . . . ? C95 C90 C91 C92 -0.4(8) . . . . ? N18 C90 C91 C92 -174.3(4) . . . . ? C90 C91 C92 C93 0.3(8) . . . . ? C91 C92 C93 C94 -0.1(7) . . . . ? C91 C92 C93 C96 -179.2(4) . . . . ? C92 C93 C94 C95 -0.1(7) . . . . ? C96 C93 C94 C95 179.0(4) . . . . ? C91 C90 C95 C94 0.1(7) . . . . ? N18 C90 C95 C94 174.2(4) . . . . ? C93 C94 C95 C90 0.1(7) . . . . ? C92 C93 C96 C101 155.8(4) . . . . ? C94 C93 C96 C101 -23.4(6) . . . . ? C92 C93 C96 C97 -21.4(6) . . . . ? C94 C93 C96 C97 159.4(4) . . . . ? C101 C96 C97 C98 1.6(6) . . . . ? C93 C96 C97 C98 178.8(4) . . . . ? C96 C97 C98 C99 1.3(7) . . . . ? C97 C98 C99 C100 -3.3(8) . . . . ? C97 C98 C99 N19 175.5(4) . . . . ? C98 C99 C100 C101 2.3(6) . . . . ? N19 C99 C100 C101 -176.6(3) . . . . ? C99 C100 C101 C96 0.7(5) . . . . ? C97 C96 C101 C100 -2.6(5) . . . . ? C93 C96 C101 C100 -179.9(3) . . . . ? N19 C103 C104 N20 -0.6(5) . . . . ? C110 C105 C106 N21 176.3(4) . . . . ? C111 C105 C106 N21 -5.8(7) . . . . ? C110 C105 C106 C107 0.0(7) . . . . ? C111 C105 C106 C107 177.9(4) . . . . ? N21 C106 C107 C108 -177.8(4) . . . . ? C105 C106 C107 C108 -1.1(6) . . . . ? C106 C107 C108 C109 0.6(7) . . . . ? C106 C107 C108 C112 178.1(4) . . . . ? C107 C108 C109 C110 1.0(7) . . . . ? C112 C108 C109 C110 -176.5(4) . . . . ? C106 C105 C110 C109 1.5(7) . . . . ? C111 C105 C110 C109 -176.3(4) . . . . ? C108 C109 C110 C105 -2.0(7) . . . . ? C110 C105 C111 O17 6.6(7) . . . . ? C106 C105 C111 O17 -171.3(4) . . . . ? C110 C105 C111 O18 -169.3(4) . . . . ? C106 C105 C111 O18 12.8(7) . . . . ? C110 C105 C111 Mn5 73.6(11) . . . . ? C106 C105 C111 Mn5 -104.3(10) . . . . ? C109 C108 C112 O20 -11.1(8) . . . . ? C107 C108 C112 O20 171.4(5) . . . . ? C109 C108 C112 O19 167.3(4) . . . . ? C107 C108 C112 O19 -10.3(6) . . . . ? C109 C108 C112 Mn5 85.9(12) . . . 2_564 ? C107 C108 C112 Mn5 -91.7(11) . . . 2_564 ? N22 C114 C115 N23 1.7(5) . . . . ? C121 C116 C117 C118 2.5(7) . . . . ? N23 C116 C117 C118 179.1(4) . . . . ? C116 C117 C118 C119 0.2(7) . . . . ? C117 C118 C119 C120 -1.0(7) . . . . ? C117 C118 C119 C122 178.6(4) . . . . ? C118 C119 C120 C121 -1.0(7) . . . . ? C122 C119 C120 C121 179.4(4) . . . . ? N23 C116 C121 C120 178.9(4) . . . . ? C117 C116 C121 C120 -4.6(7) . . . . ? C119 C120 C121 C116 3.7(7) . . . . ? C120 C119 C122 C127 -8.9(6) . . . . ? C118 C119 C122 C127 171.5(4) . . . . ? C120 C119 C122 C123 168.9(4) . . . . ? C118 C119 C122 C123 -10.7(6) . . . . ? C127 C122 C123 C124 0.6(6) . . . . ? C119 C122 C123 C124 -177.3(4) . . . . ? C122 C123 C124 C125 -0.8(6) . . . . ? C123 C124 C125 C126 0.5(6) . . . . ? C123 C124 C125 N24 179.0(4) . . . . ? N24 C125 C126 C127 -178.5(4) . . . . ? C124 C125 C126 C127 0.0(7) . . . . ? C125 C126 C127 C122 -0.2(7) . . . . ? C123 C122 C127 C126 -0.1(7) . . . . ? C119 C122 C127 C126 177.7(4) . . . . ? N24 C129 C130 N25 -4.0(6) . . . . ? O1 C7 Mn1 N5 122.3(2) . . . 4_454 ? O2 C7 Mn1 N5 -65.4(2) . . . 4_454 ? O1 C7 Mn1 N2 7.5(2) . . . . ? O2 C7 Mn1 N2 179.8(2) . . . . ? O1 C7 Mn1 O3 -139.8(2) . . . 2 ? O2 C7 Mn1 O3 32.4(2) . . . 2 ? O2 C7 Mn1 O1 172.2(3) . . . . ? O1 C7 Mn1 O2 -172.2(3) . . . . ? O1 C7 Mn1 O4 -78.2(2) . . . 2 ? O2 C7 Mn1 O4 94.06(18) . . . 2 ? O5 C33 Mn2 N10 -146.0(2) . . . 4_454 ? C27 C33 Mn2 N10 -50.5(18) . . . 4_454 ? O6 C33 Mn2 N7 164.93(18) . . . . ? O5 C33 Mn2 N7 -30.0(2) . . . . ? C27 C33 Mn2 N7 65.5(18) . . . . ? O6 C33 Mn2 O7 -42.7(2) . . . 2_565 ? O5 C33 Mn2 O7 122.4(2) . . . 2_565 ? C27 C33 Mn2 O7 -142.1(18) . . . 2_565 ? O6 C33 Mn2 O5 -165.1(4) . . . . ? C27 C33 Mn2 O5 95.5(19) . . . . ? O5 C33 Mn2 O6 165.1(4) . . . . ? C27 C33 Mn2 O6 -99.5(18) . . . . ? O6 C33 Mn2 O8 -102.36(17) . . . 2_565 ? O5 C33 Mn2 O8 62.7(2) . . . 2_565 ? C27 C33 Mn2 O8 158.2(18) . . . 2_565 ? O6 C33 Mn2 C34 -79.2(2) . . . 2_565 ? O5 C33 Mn2 C34 85.9(3) . . . 2_565 ? O10 C59 Mn3 O9 168.9(3) . . . . ? O10 C59 Mn3 N15 -78.47(18) . . . 4_454 ? O9 C59 Mn3 N15 112.6(2) . . . 4_454 ? O10 C59 Mn3 N12 -171.46(18) . . . . ? O9 C59 Mn3 N12 19.7(2) . . . . ? O10 C59 Mn3 O12 95.82(18) . . . 2 ? O9 C59 Mn3 O12 -73.06(18) . . . 2 ? O10 C59 Mn3 O11 32.7(2) . . . 2 ? O9 C59 Mn3 O11 -136.22(19) . . . 2 ? O9 C59 Mn3 O10 -168.9(3) . . . . ? O14 C85 Mn4 N20 -83.04(19) . . . 4_454 ? O13 C85 Mn4 N20 114.26(17) . . . 4_454 ? C79 C85 Mn4 N20 23.6(12) . . . 4_454 ? O14 C85 Mn4 N17 -177.4(2) . . . . ? O13 C85 Mn4 N17 19.9(2) . . . . ? C79 C85 Mn4 N17 -70.8(12) . . . . ? O14 C85 Mn4 O15 44.9(2) . . . 2 ? O13 C85 Mn4 O15 -117.82(17) . . . 2 ? C79 C85 Mn4 O15 151.5(11) . . . 2 ? O13 C85 Mn4 O14 -162.7(3) . . . . ? C79 C85 Mn4 O14 106.6(12) . . . . ? O14 C85 Mn4 O13 162.7(3) . . . . ? C79 C85 Mn4 O13 -90.7(12) . . . . ? O14 C85 Mn4 O16 100.73(18) . . . 2 ? O13 C85 Mn4 O16 -61.97(16) . . . 2 ? C79 C85 Mn4 O16 -152.6(12) . . . 2 ? O17 C111 Mn5 N22 30.2(3) . . . . ? O18 C111 Mn5 N22 -170.5(2) . . . . ? C105 C111 Mn5 N22 -45.9(10) . . . . ? O17 C111 Mn5 O20 -70.4(3) . . . 2_565 ? O18 C111 Mn5 O20 88.8(3) . . . 2_565 ? C105 C111 Mn5 O20 -146.6(10) . . . 2_565 ? O17 C111 Mn5 N25 137.5(3) . . . 4_464 ? O18 C111 Mn5 N25 -63.3(3) . . . 4_464 ? C105 C111 Mn5 N25 61.3(10) . . . 4_464 ? O18 C111 Mn5 O17 159.3(4) . . . . ? C105 C111 Mn5 O17 -76.1(10) . . . . ? O17 C111 Mn5 O19 -133.6(2) . . . 2_565 ? O18 C111 Mn5 O19 25.6(3) . . . 2_565 ? C105 C111 Mn5 O19 150.2(10) . . . 2_565 ? O17 C111 Mn5 O18 -159.3(4) . . . . ? C105 C111 Mn5 O18 124.6(11) . . . . ? O17 C111 Mn5 C112 -98.2(3) . . . 2_565 ? O18 C111 Mn5 C112 61.1(3) . . . 2_565 ? C105 C111 Mn5 C112 -174.3(10) . . . 2_565 ? N3 C9 N2 C10 -2.1(3) . . . . ? N3 C9 N2 Mn1 159.1(3) . . . . ? C11 C10 N2 C9 2.9(4) . . . . ? C11 C10 N2 Mn1 -158.7(3) . . . . ? N5 Mn1 N2 C9 -159.9(3) 4_454 . . . ? O3 Mn1 N2 C9 111.4(3) 2 . . . ? O1 Mn1 N2 C9 -40.1(3) . . . . ? O2 Mn1 N2 C9 -43.6(6) . . . . ? O4 Mn1 N2 C9 60.7(3) 2 . . . ? C7 Mn1 N2 C9 -43.8(4) . . . . ? N5 Mn1 N2 C10 -2.3(3) 4_454 . . . ? O3 Mn1 N2 C10 -90.9(3) 2 . . . ? O1 Mn1 N2 C10 117.6(3) . . . . ? O2 Mn1 N2 C10 114.1(4) . . . . ? O4 Mn1 N2 C10 -141.6(3) 2 . . . ? C7 Mn1 N2 C10 113.8(3) . . . . ? C13 C12 N3 C9 178.2(3) . . . . ? C17 C12 N3 C9 -7.6(5) . . . . ? C13 C12 N3 C11 -11.3(5) . . . . ? C17 C12 N3 C11 162.8(4) . . . . ? N2 C9 N3 C12 172.4(3) . . . . ? N2 C9 N3 C11 0.7(3) . . . . ? C10 C11 N3 C12 -170.8(3) . . . . ? C10 C11 N3 C9 1.1(4) . . . . ? N5 C24 N4 C25 -1.9(4) . . . . ? N5 C24 N4 C21 -176.3(3) . . . . ? C26 C25 N4 C24 -1.3(4) . . . . ? C26 C25 N4 C21 173.3(3) . . . . ? C22 C21 N4 C24 -160.0(4) . . . . ? C20 C21 N4 C24 22.0(5) . . . . ? C22 C21 N4 C25 26.6(6) . . . . ? C20 C21 N4 C25 -151.4(3) . . . . ? N4 C24 N5 C26 4.0(4) . . . . ? N4 C24 N5 Mn1 162.6(3) . . . 4 ? C25 C26 N5 C24 -4.7(4) . . . . ? C25 C26 N5 Mn1 -164.0(2) . . . 4 ? C37 C36 N7 C35 3.0(4) . . . . ? C37 C36 N7 Mn2 171.68(19) . . . . ? N8 C35 N7 C36 -3.0(4) . . . . ? N8 C35 N7 Mn2 -171.9(2) . . . . ? N10 Mn2 N7 C36 23.1(3) 4_454 . . . ? O7 Mn2 N7 C36 109.7(2) 2_565 . . . ? O5 Mn2 N7 C36 -105.2(2) . . . . ? O6 Mn2 N7 C36 -80.0(3) . . . . ? O8 Mn2 N7 C36 160.1(3) 2_565 . . . ? C33 Mn2 N7 C36 -91.3(2) . . . . ? C34 Mn2 N7 C36 133.8(2) 2_565 . . . ? N10 Mn2 N7 C35 -170.2(3) 4_454 . . . ? O7 Mn2 N7 C35 -83.6(3) 2_565 . . . ? O5 Mn2 N7 C35 61.5(3) . . . . ? O6 Mn2 N7 C35 86.8(3) . . . . ? O8 Mn2 N7 C35 -33.1(3) 2_565 . . . ? C33 Mn2 N7 C35 75.4(3) . . . . ? C34 Mn2 N7 C35 -59.4(3) 2_565 . . . ? C36 C37 N8 C35 0.0(4) . . . . ? C36 C37 N8 C38 176.5(3) . . . . ? N7 C35 N8 C37 1.8(4) . . . . ? N7 C35 N8 C38 -175.1(3) . . . . ? C39 C38 N8 C37 15.7(6) . . . . ? C43 C38 N8 C37 -176.5(4) . . . . ? C39 C38 N8 C35 -168.2(4) . . . . ? C43 C38 N8 C35 -0.4(6) . . . . ? C52 C51 N9 C50 -2.5(3) . . . . ? C52 C51 N9 C47 -175.0(3) . . . . ? N10 C50 N9 C51 1.1(3) . . . . ? N10 C50 N9 C47 175.4(3) . . . . ? C46 C47 N9 C51 -164.5(3) . . . . ? C48 C47 N9 C51 6.0(5) . . . . ? C46 C47 N9 C50 23.5(5) . . . . ? C48 C47 N9 C50 -166.0(3) . . . . ? N9 C50 N10 C52 0.7(3) . . . . ? N9 C50 N10 Mn2 -156.3(3) . . . 4 ? C51 C52 N10 C50 -2.2(3) . . . . ? C51 C52 N10 Mn2 158.4(2) . . . 4 ? N13 C61 N12 C62 -1.5(3) . . . . ? N13 C61 N12 Mn3 170.6(3) . . . . ? C63 C62 N12 C61 2.5(4) . . . . ? C63 C62 N12 Mn3 -170.2(2) . . . . ? O9 Mn3 N12 C61 -93.9(3) . . . . ? N15 Mn3 N12 C61 148.5(3) 4_454 . . . ? O12 Mn3 N12 C61 8.3(3) 2 . . . ? O11 Mn3 N12 C61 54.9(3) 2 . . . ? O10 Mn3 N12 C61 -110.3(3) . . . . ? C59 Mn3 N12 C61 -103.6(3) . . . . ? O9 Mn3 N12 C62 76.9(3) . . . . ? N15 Mn3 N12 C62 -40.7(3) 4_454 . . . ? O12 Mn3 N12 C62 179.1(3) 2 . . . ? O11 Mn3 N12 C62 -134.3(2) 2 . . . ? O10 Mn3 N12 C62 60.5(4) . . . . ? C59 Mn3 N12 C62 67.2(3) . . . . ? N12 C61 N13 C63 0.1(3) . . . . ? N12 C61 N13 C64 -172.7(3) . . . . ? C62 C63 N13 C61 1.5(4) . . . . ? C62 C63 N13 C64 174.5(3) . . . . ? C65 C64 N13 C61 6.0(5) . . . . ? C69 C64 N13 C61 -172.3(3) . . . . ? C65 C64 N13 C63 -165.8(4) . . . . ? C69 C64 N13 C63 16.0(5) . . . . ? C78 C77 N14 C76 -1.8(4) . . . . ? C78 C77 N14 C73 -180.0(3) . . . . ? N15 C76 N14 C77 0.9(3) . . . . ? N15 C76 N14 C73 179.5(2) . . . . ? C74 C73 N14 C77 160.7(4) . . . . ? C72 C73 N14 C77 -18.6(6) . . . . ? C74 C73 N14 C76 -17.3(5) . . . . ? C72 C73 N14 C76 163.3(3) . . . . ? C77 C78 N15 C76 -1.4(4) . . . . ? C77 C78 N15 Mn3 -176.0(3) . . . 4 ? N14 C76 N15 C78 0.3(3) . . . . ? N14 C76 N15 Mn3 177.20(18) . . . 4 ? C89 C88 N17 C87 -0.8(4) . . . . ? C89 C88 N17 Mn4 176.8(2) . . . . ? N18 C87 N17 C88 1.2(3) . . . . ? N18 C87 N17 Mn4 -176.3(2) . . . . ? N20 Mn4 N17 C88 37.4(2) 4_454 . . . ? O15 Mn4 N17 C88 -74.3(2) 2 . . . ? O14 Mn4 N17 C88 135.0(2) . . . . ? O13 Mn4 N17 C88 147.0(2) . . . . ? O16 Mn4 N17 C88 -122.6(2) 2 . . . ? C85 Mn4 N17 C88 137.3(2) . . . . ? N20 Mn4 N17 C87 -145.4(3) 4_454 . . . ? O15 Mn4 N17 C87 102.8(3) 2 . . . ? O14 Mn4 N17 C87 -47.8(4) . . . . ? O13 Mn4 N17 C87 -35.9(3) . . . . ? O16 Mn4 N17 C87 54.5(2) 2 . . . ? C85 Mn4 N17 C87 -45.5(3) . . . . ? N17 C87 N18 C89 -1.1(3) . . . . ? N17 C87 N18 C90 169.6(3) . . . . ? C88 C89 N18 C87 0.6(4) . . . . ? C88 C89 N18 C90 -171.5(3) . . . . ? C95 C90 N18 C87 -7.1(6) . . . . ? C91 C90 N18 C87 166.9(4) . . . . ? C95 C90 N18 C89 162.7(4) . . . . ? C91 C90 N18 C89 -23.3(6) . . . . ? N20 C102 N19 C103 -0.4(4) . . . . ? N20 C102 N19 C99 175.5(3) . . . . ? C104 C103 N19 C102 0.6(4) . . . . ? C104 C103 N19 C99 -174.7(4) . . . . ? C98 C99 N19 C102 22.9(5) . . . . ? C100 C99 N19 C102 -158.2(3) . . . . ? C98 C99 N19 C103 -162.1(3) . . . . ? C100 C99 N19 C103 16.7(5) . . . . ? C103 C104 N20 C102 0.4(5) . . . . ? C103 C104 N20 Mn4 177.2(3) . . . 4 ? N19 C102 N20 C104 0.0(4) . . . . ? N19 C102 N20 Mn4 -178.0(3) . . . 4 ? C115 C114 N22 C113 0.6(5) . . . . ? C115 C114 N22 Mn5 176.0(3) . . . . ? N23 C113 N22 C114 -2.6(5) . . . . ? N23 C113 N22 Mn5 -178.1(3) . . . . ? O20 Mn5 N22 C114 -162.8(4) 2_565 . . . ? N25 Mn5 N22 C114 -31.3(4) 4_464 . . . ? O17 Mn5 N22 C114 96.9(4) . . . . ? O19 Mn5 N22 C114 -112.1(3) 2_565 . . . ? O18 Mn5 N22 C114 74.9(4) . . . . ? C111 Mn5 N22 C114 83.1(4) . . . . ? C112 Mn5 N22 C114 -136.7(4) 2_565 . . . ? O20 Mn5 N22 C113 11.9(3) 2_565 . . . ? N25 Mn5 N22 C113 143.4(3) 4_464 . . . ? O17 Mn5 N22 C113 -88.5(3) . . . . ? O19 Mn5 N22 C113 62.6(4) 2_565 . . . ? O18 Mn5 N22 C113 -110.4(4) . . . . ? C111 Mn5 N22 C113 -102.2(3) . . . . ? C112 Mn5 N22 C113 37.9(4) 2_565 . . . ? N22 C113 N23 C115 3.7(5) . . . . ? N22 C113 N23 C116 -169.2(4) . . . . ? C114 C115 N23 C113 -3.3(5) . . . . ? C114 C115 N23 C116 169.9(4) . . . . ? C121 C116 N23 C113 27.5(7) . . . . ? C117 C116 N23 C113 -149.1(4) . . . . ? C121 C116 N23 C115 -144.5(4) . . . . ? C117 C116 N23 C115 38.9(6) . . . . ? C126 C125 N24 C128 160.0(5) . . . . ? C124 C125 N24 C128 -18.5(7) . . . . ? C126 C125 N24 C129 -24.8(7) . . . . ? C124 C125 N24 C129 156.7(4) . . . . ? N25 C128 N24 C125 175.0(4) . . . . ? N25 C128 N24 C129 -0.8(5) . . . . ? C130 C129 N24 C125 -172.9(4) . . . . ? C130 C129 N24 C128 3.0(6) . . . . ? N24 C128 N25 C130 -1.7(5) . . . . ? N24 C128 N25 Mn5 169.8(3) . . . 4_565 ? C129 C130 N25 C128 3.5(5) . . . . ? C129 C130 N25 Mn5 -166.9(3) . . . 4_565 ? O2 C7 O1 Mn1 -8.7(4) . . . . ? C1 C7 O1 Mn1 171.6(3) . . . . ? N5 Mn1 O1 C7 -67.4(2) 4_454 . . . ? N2 Mn1 O1 C7 -174.0(2) . . . . ? O3 Mn1 O1 C7 67.7(3) 2 . . . ? O2 Mn1 O1 C7 4.47(18) . . . . ? O4 Mn1 O1 C7 110.69(19) 2 . . . ? O1 C7 O2 Mn1 8.4(3) . . . . ? C1 C7 O2 Mn1 -172.0(3) . . . . ? N5 Mn1 O2 C7 117.69(19) 4_454 . . . ? N2 Mn1 O2 C7 -0.5(5) . . . . ? O3 Mn1 O2 C7 -154.84(18) 2 . . . ? O1 Mn1 O2 C7 -4.44(18) . . . . ? O4 Mn1 O2 C7 -97.47(18) 2 . . . ? O4 C8 O3 Mn1 12.6(3) . . . 2_554 ? C4 C8 O3 Mn1 -166.3(3) . . . 2_554 ? O3 C8 O4 Mn1 -11.7(3) . . . 2_554 ? C4 C8 O4 Mn1 167.2(4) . . . 2_554 ? O6 C33 O5 Mn2 14.5(4) . . . . ? C27 C33 O5 Mn2 -168.0(4) . . . . ? N10 Mn2 O5 C33 42.7(3) 4_454 . . . ? N7 Mn2 O5 C33 152.9(2) . . . . ? O7 Mn2 O5 C33 -88.2(2) 2_565 . . . ? O6 Mn2 O5 C33 -8.4(2) . . . . ? O8 Mn2 O5 C33 -122.6(2) 2_565 . . . ? C34 Mn2 O5 C33 -113.8(2) 2_565 . . . ? O5 C33 O6 Mn2 -14.4(4) . . . . ? C27 C33 O6 Mn2 168.1(4) . . . . ? N10 Mn2 O6 C33 -132.7(2) 4_454 . . . ? N7 Mn2 O6 C33 -22.2(3) . . . . ? O7 Mn2 O6 C33 148.0(2) 2_565 . . . ? O5 Mn2 O6 C33 8.5(2) . . . . ? O8 Mn2 O6 C33 88.6(2) 2_565 . . . ? C34 Mn2 O6 C33 118.7(2) 2_565 . . . ? O8 C34 O7 Mn2 -16.0(4) . . . 2_564 ? C30 C34 O7 Mn2 167.9(3) . . . 2_564 ? O7 C34 O8 Mn2 14.3(3) . . . 2_564 ? C30 C34 O8 Mn2 -170.2(4) . . . 2_564 ? O10 C59 O9 Mn3 -12.0(4) . . . . ? C53 C59 O9 Mn3 171.1(3) . . . . ? N15 Mn3 O9 C59 -79.65(19) 4_454 . . . ? N12 Mn3 O9 C59 -162.11(19) . . . . ? O12 Mn3 O9 C59 115.74(19) 2 . . . ? O11 Mn3 O9 C59 69.1(2) 2 . . . ? O10 Mn3 O9 C59 6.22(19) . . . . ? O9 C59 O10 Mn3 10.7(3) . . . . ? C53 C59 O10 Mn3 -172.2(3) . . . . ? O9 Mn3 O10 C59 -6.5(2) . . . . ? N15 Mn3 O10 C59 108.8(2) 4_454 . . . ? N12 Mn3 O10 C59 12.8(3) . . . . ? O12 Mn3 O10 C59 -96.3(2) 2 . . . ? O11 Mn3 O10 C59 -153.6(2) 2 . . . ? O12 C60 O11 Mn3 13.2(3) . . . 2_554 ? C56 C60 O11 Mn3 -165.1(3) . . . 2_554 ? O11 C60 O12 Mn3 -13.5(4) . . . 2_554 ? C56 C60 O12 Mn3 164.5(4) . . . 2_554 ? O14 C85 O13 Mn4 -16.1(3) . . . . ? C79 C85 O13 Mn4 162.8(3) . . . . ? N20 Mn4 O13 C85 -72.91(17) 4_454 . . . ? N17 Mn4 O13 C85 -162.83(17) . . . . ? O15 Mn4 O13 C85 90.27(18) 2 . . . ? O14 Mn4 O13 C85 9.70(17) . . . . ? O16 Mn4 O13 C85 121.84(17) 2 . . . ? O13 C85 O14 Mn4 16.3(3) . . . . ? C79 C85 O14 Mn4 -162.6(4) . . . . ? N20 Mn4 O14 C85 100.36(18) 4_454 . . . ? N17 Mn4 O14 C85 4.2(3) . . . . ? O15 Mn4 O14 C85 -145.34(18) 2 . . . ? O13 Mn4 O14 C85 -10.03(18) . . . . ? O16 Mn4 O14 C85 -88.30(18) 2 . . . ? O16 C86 O15 Mn4 15.5(4) . . . 2_554 ? C82 C86 O15 Mn4 -164.2(3) . . . 2_554 ? O15 C86 O16 Mn4 -13.4(3) . . . 2_554 ? C82 C86 O16 Mn4 166.3(4) . . . 2_554 ? O18 C111 O17 Mn5 -21.8(4) . . . . ? C105 C111 O17 Mn5 162.1(4) . . . . ? N22 Mn5 O17 C111 -153.4(3) . . . . ? O20 Mn5 O17 C111 117.1(3) 2_565 . . . ? N25 Mn5 O17 C111 -54.0(3) 4_464 . . . ? O19 Mn5 O17 C111 67.4(3) 2_565 . . . ? O18 Mn5 O17 C111 11.9(3) . . . . ? C112 Mn5 O17 C111 102.6(3) 2_565 . . . ? O17 C111 O18 Mn5 19.9(4) . . . . ? C105 C111 O18 Mn5 -164.2(4) . . . . ? N22 Mn5 O18 C111 15.1(4) . . . . ? O20 Mn5 O18 C111 -101.9(3) 2_565 . . . ? N25 Mn5 O18 C111 121.9(3) 4_464 . . . ? O17 Mn5 O18 C111 -11.6(2) . . . . ? O19 Mn5 O18 C111 -158.6(3) 2_565 . . . ? C112 Mn5 O18 C111 -131.7(3) 2_565 . . . ? O20 C112 O19 Mn5 17.7(4) . . . 2_564 ? C108 C112 O19 Mn5 -160.8(4) . . . 2_564 ? O19 C112 O20 Mn5 -19.3(5) . . . 2_564 ? C108 C112 O20 Mn5 159.1(4) . . . 2_564 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.550 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.059 ########################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 866678' #TrackingRef '- new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H19 N5 O4 Zn, 2(C3 H7 N O)' _chemical_formula_sum 'C28 H33 N7 O6 Zn' _chemical_formula_weight 628.98 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' 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 'Cc ' _symmetry_space_group_name_Hall 'C -2yc ' 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' _cell_length_a 20.661(4) _cell_length_b 11.567(2) _cell_length_c 14.227(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.01(3) _cell_angle_gamma 90.00 _cell_volume 3055.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2715 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 23.52 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7957 _exptl_absorpt_correction_T_max 0.8341 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 8464 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.36 _reflns_number_total 4519 _reflns_number_gt 3832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.07P)^2^+1.99P] 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 0.02(2) _refine_ls_number_reflns 4519 _refine_ls_number_parameters 372 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1331 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 0.0083(5) 0.4124(6) 0.1180(7) 0.052(2) Uani 1 1 d . . . C2 C -0.0550(4) 0.3346(7) 0.0540(6) 0.0413(18) Uani 1 1 d . . . C3 C -0.1164(4) 0.3798(6) -0.0279(6) 0.0403(19) Uani 1 1 d . . . C4 C -0.1695(4) 0.2948(8) -0.0891(6) 0.051(2) Uani 1 1 d . . . H4 H -0.2109 0.3199 -0.1461 0.061 Uiso 1 1 calc R . . C5 C -0.1615(4) 0.1783(7) -0.0670(5) 0.0405(19) Uani 1 1 d . . . C6 C -0.0989(4) 0.1460(6) 0.0158(6) 0.045(2) Uani 1 1 d . . . H6 H -0.0932 0.0676 0.0317 0.054 Uiso 1 1 calc R . . C7 C -0.0452(5) 0.2151(6) 0.0760(7) 0.046(2) Uani 1 1 d . . . H7 H -0.0034 0.1863 0.1299 0.055 Uiso 1 1 calc R . . C8 C -0.2158(4) 0.0891(8) -0.1298(6) 0.042(2) Uani 1 1 d . . . C9 C 0.1742(4) 0.6346(7) 0.4337(5) 0.043(2) Uani 1 1 d . . . H9 H 0.2231 0.6416 0.4523 0.051 Uiso 1 1 calc R . . C10 C 0.0564(4) 0.5912(7) 0.3429(6) 0.046(2) Uani 1 1 d . . . H10 H 0.0131 0.5631 0.2917 0.055 Uiso 1 1 calc R . . C11 C 0.0656(5) 0.6603(7) 0.4298(6) 0.046(2) Uani 1 1 d . . . H11 H 0.0292 0.6859 0.4465 0.055 Uiso 1 1 calc R . . C12 C 0.1699(4) 0.7710(7) 0.5704(6) 0.0414(18) Uani 1 1 d . . . H12A H 0.1484 0.7619 0.6185 0.050 Uiso 1 1 calc R . . H12B H 0.2213 0.7582 0.6092 0.050 Uiso 1 1 calc R . . C13 C 0.1570(3) 0.8904(4) 0.5284(4) 0.054(2) Uani 1 1 d G . . C14 C 0.1980(3) 0.9421(4) 0.4844(4) 0.061(3) Uani 1 1 d G . . H14 H 0.2357 0.9016 0.4807 0.073 Uiso 1 1 calc R . . C15 C 0.1825(3) 1.0542(4) 0.4457(4) 0.050(2) Uani 1 1 d G . . H15 H 0.2099 1.0887 0.4162 0.060 Uiso 1 1 calc R . . C16 C 0.1261(3) 1.1146(4) 0.4511(3) 0.0369(16) Uani 1 1 d G . . C17 C 0.0851(2) 1.0629(4) 0.4952(3) 0.0379(18) Uani 1 1 d G . . H17 H 0.0474 1.1033 0.4988 0.046 Uiso 1 1 calc R . . C18 C 0.1006(3) 0.9508(4) 0.5338(3) 0.0418(19) Uani 1 1 d G . . H18 H 0.0732 0.9162 0.5633 0.050 Uiso 1 1 calc R . . C19 C 0.1034(5) 1.2370(6) 0.4075(5) 0.0425(19) Uani 1 1 d . . . H19A H 0.1185 1.2544 0.3534 0.051 Uiso 1 1 calc R . . H19B H 0.0517 1.2472 0.3796 0.051 Uiso 1 1 calc R . . C20 C 0.1063(5) 1.3718(7) 0.5566(6) 0.049(2) Uani 1 1 d . . . H20 H 0.0571 1.3721 0.5378 0.059 Uiso 1 1 calc R . . C21 C 0.2278(4) 1.4147(7) 0.6361(7) 0.047(2) Uani 1 1 d . . . H21 H 0.2717 1.4465 0.6822 0.056 Uiso 1 1 calc R . . C22 C 0.2170(4) 1.3434(7) 0.5489(6) 0.0406(19) Uani 1 1 d . . . H22 H 0.2513 1.3225 0.5264 0.049 Uiso 1 1 calc R . . C23 C 0.3148(3) 0.2222(5) 0.8389(5) 0.0423(14) Uani 1 1 d . . . H23 H 0.2924 0.2684 0.8695 0.051 Uiso 1 1 calc R . . C24 C 0.2025(4) 0.1160(7) 0.7351(6) 0.0578(19) Uani 1 1 d . . . H24A H 0.1979 0.0423 0.7625 0.087 Uiso 1 1 calc R . . H24B H 0.1738 0.1169 0.6607 0.087 Uiso 1 1 calc R . . H24C H 0.1862 0.1758 0.7665 0.087 Uiso 1 1 calc R . . C25 C 0.3129(4) 0.0634(5) 0.7013(5) 0.0452(15) Uani 1 1 d . . . H25A H 0.3498 0.1076 0.6942 0.068 Uiso 1 1 calc R . . H25B H 0.2765 0.0428 0.6333 0.068 Uiso 1 1 calc R . . H25C H 0.3336 -0.0055 0.7407 0.068 Uiso 1 1 calc R . . C26 C 0.4110(4) 0.2715(7) 0.1014(5) 0.048(2) Uani 1 1 d . . . H26 H 0.4315 0.2287 0.0661 0.057 Uiso 1 1 calc R . . C27 C 0.4139(3) 0.4156(5) 0.2351(5) 0.0392(14) Uani 1 1 d . . . H27A H 0.3629 0.4055 0.1960 0.059 Uiso 1 1 calc R . . H27B H 0.4251 0.4966 0.2433 0.059 Uiso 1 1 calc R . . H27C H 0.4298 0.3804 0.3027 0.059 Uiso 1 1 calc R . . C28 C 0.5259(4) 0.3796(7) 0.1838(5) 0.0494(16) Uani 1 1 d . . . H28A H 0.5393 0.3148 0.1540 0.074 Uiso 1 1 calc R . . H28B H 0.5600 0.3884 0.2557 0.074 Uiso 1 1 calc R . . H28C H 0.5254 0.4485 0.1458 0.074 Uiso 1 1 calc R . . N1 N 0.1251(4) 0.5733(6) 0.3488(5) 0.0412(17) Uani 1 1 d . . . N2 N 0.1390(4) 0.6832(6) 0.4860(6) 0.0450(17) Uani 1 1 d . . . N3 N 0.1602(3) 1.4303(6) 0.6421(5) 0.0379(15) Uani 1 1 d . . . N4 N 0.1427(4) 1.3102(5) 0.5026(5) 0.0402(15) Uani 1 1 d . . . N5 N -0.1325(3) 0.4851(5) -0.0400(5) 0.0600(18) Uani 1 1 d . . . H5A H -0.1047 0.5350 0.0040 0.072 Uiso 1 1 calc R . . H5B H -0.1713 0.5074 -0.0923 0.072 Uiso 1 1 calc R . . N6 N 0.2788(3) 0.1364(5) 0.7592(4) 0.0510(15) Uani 1 1 d . . . N7 N 0.4517(3) 0.3595(5) 0.1773(4) 0.0454(13) Uani 1 1 d . . . O1 O -0.0057(3) 0.5197(4) 0.1039(5) 0.0456(15) Uani 1 1 d . . . O2 O 0.0669(3) 0.3689(4) 0.1780(4) 0.0383(12) Uani 1 1 d . . . O3 O -0.2740(3) 0.1327(6) -0.1907(4) 0.0489(15) Uani 1 1 d . . . O4 O -0.2088(3) -0.0208(5) -0.1206(5) 0.0491(17) Uani 1 1 d . . . O5 O 0.3796(3) 0.2256(4) 0.8607(4) 0.0462(13) Uani 1 1 d . . . O6 O 0.3458(2) 0.2557(4) 0.0854(3) 0.0459(11) Uani 1 1 d . . . Zn1 Zn 0.14187(6) 0.48701(5) 0.24376(7) 0.03581(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(6) 0.033(4) 0.049(5) -0.012(4) 0.008(4) -0.002(4) C2 0.039(4) 0.035(4) 0.048(4) -0.005(3) 0.017(4) -0.010(3) C3 0.034(4) 0.029(4) 0.045(4) 0.020(3) 0.006(3) -0.013(3) C4 0.036(4) 0.059(5) 0.035(4) 0.013(4) -0.005(3) -0.011(4) C5 0.052(5) 0.044(5) 0.032(4) -0.014(3) 0.024(4) -0.014(4) C6 0.048(4) 0.030(4) 0.041(4) 0.005(3) 0.006(4) -0.014(3) C7 0.059(5) 0.021(3) 0.074(6) -0.002(3) 0.044(5) -0.013(3) C8 0.024(4) 0.051(5) 0.035(4) 0.010(3) -0.002(3) -0.008(3) C9 0.031(4) 0.069(5) 0.026(3) -0.002(3) 0.010(3) -0.012(4) C10 0.047(5) 0.049(5) 0.042(4) -0.009(3) 0.019(4) -0.027(4) C11 0.055(5) 0.035(4) 0.042(4) 0.001(4) 0.018(4) -0.001(4) C12 0.025(3) 0.048(4) 0.052(4) 0.000(3) 0.017(3) -0.005(3) C13 0.071(7) 0.034(4) 0.058(5) 0.006(4) 0.030(5) 0.009(4) C14 0.051(6) 0.043(5) 0.077(6) 0.022(5) 0.019(5) 0.004(4) C15 0.030(4) 0.038(4) 0.059(5) 0.017(4) 0.000(4) 0.006(3) C16 0.029(4) 0.035(4) 0.032(3) -0.012(3) 0.000(3) -0.007(3) C17 0.036(4) 0.051(4) 0.019(3) 0.003(3) 0.004(3) 0.015(3) C18 0.057(5) 0.033(4) 0.031(3) -0.007(3) 0.015(4) 0.001(4) C19 0.053(4) 0.041(4) 0.027(3) -0.003(3) 0.011(3) 0.007(3) C20 0.053(5) 0.032(4) 0.049(4) 0.013(3) 0.009(4) 0.016(4) C21 0.036(4) 0.039(4) 0.052(4) 0.015(4) 0.009(3) 0.013(3) C22 0.040(4) 0.047(5) 0.034(4) 0.023(3) 0.015(3) 0.012(4) C23 0.034(3) 0.039(3) 0.054(4) -0.005(3) 0.020(3) -0.010(3) C24 0.066(5) 0.053(4) 0.053(4) 0.016(3) 0.024(4) 0.021(4) C25 0.049(4) 0.037(3) 0.039(3) 0.009(3) 0.009(3) 0.002(3) C26 0.045(4) 0.060(5) 0.033(3) 0.008(3) 0.013(3) 0.028(3) C27 0.035(3) 0.038(3) 0.050(3) -0.008(3) 0.023(3) -0.011(3) C28 0.050(4) 0.063(4) 0.033(3) -0.002(3) 0.016(3) -0.011(3) N1 0.058(5) 0.031(3) 0.026(3) -0.002(3) 0.010(3) -0.004(3) N2 0.054(4) 0.036(4) 0.048(4) -0.007(3) 0.024(3) -0.022(3) N3 0.039(4) 0.043(4) 0.035(3) 0.005(3) 0.019(3) -0.007(3) N4 0.045(4) 0.036(4) 0.030(3) -0.014(3) 0.008(3) -0.008(3) N5 0.052(3) 0.052(4) 0.049(3) 0.021(3) -0.003(3) -0.017(3) N6 0.060(4) 0.043(3) 0.037(3) 0.015(2) 0.010(3) -0.012(3) N7 0.039(3) 0.042(3) 0.045(3) 0.017(2) 0.008(2) 0.017(2) O1 0.046(4) 0.033(3) 0.051(3) -0.011(3) 0.015(3) -0.014(3) O2 0.043(3) 0.024(2) 0.038(3) -0.0066(19) 0.008(2) -0.010(2) O3 0.023(2) 0.069(4) 0.043(3) -0.014(3) 0.004(2) 0.006(2) O4 0.050(4) 0.055(4) 0.045(3) -0.017(3) 0.023(3) 0.001(3) O5 0.051(3) 0.044(3) 0.041(3) -0.012(2) 0.017(2) -0.014(2) O6 0.039(2) 0.050(3) 0.050(3) -0.020(2) 0.021(2) -0.008(2) Zn1 0.0352(3) 0.0364(3) 0.0345(3) 0.0007(5) 0.0140(2) -0.0091(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.242(10) . ? C1 O1 1.270(9) . ? C1 C2 1.518(11) . ? C2 C3 1.395(10) . ? C2 C7 1.411(10) . ? C3 N5 1.254(9) . ? C3 C4 1.445(10) . ? C4 C5 1.377(11) . ? C4 H4 0.9300 . ? C5 C6 1.364(11) . ? C5 C8 1.498(10) . ? C6 C7 1.331(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.240(9) . ? C8 O4 1.279(10) . ? C9 N2 1.367(11) . ? C9 N1 1.384(9) . ? C9 H9 0.9300 . ? C10 N1 1.399(11) . ? C10 C11 1.413(12) . ? C10 H10 0.9300 . ? C11 N2 1.395(12) . ? C11 H11 0.9300 . ? C12 C13 1.481(9) . ? C12 N2 1.487(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 C19 1.534(8) . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 N4 1.497(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N3 1.411(10) . ? C20 N4 1.473(12) . ? C20 H20 0.9300 . ? C21 C22 1.424(12) . ? C21 N3 1.448(10) . ? C21 H21 0.9300 . ? C22 N4 1.432(11) . ? C22 H22 0.9300 . ? C23 O5 1.234(8) . ? C23 N6 1.445(8) . ? C23 H23 0.9300 . ? C24 N6 1.479(10) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N6 1.548(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O6 1.277(9) . ? C26 N7 1.453(10) . ? C26 H26 0.9300 . ? C27 N7 1.506(8) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N7 1.512(9) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? N1 Zn1 1.951(7) . ? N3 Zn1 1.905(7) 2_575 ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? O2 Zn1 1.967(5) . ? O3 Zn1 2.095(6) 4_454 ? Zn1 N3 1.905(7) 2_574 ? Zn1 O3 2.095(6) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 126.2(8) . . ? O2 C1 C2 119.7(7) . . ? O1 C1 C2 114.1(8) . . ? C3 C2 C7 122.8(7) . . ? C3 C2 C1 120.5(7) . . ? C7 C2 C1 116.4(7) . . ? N5 C3 C2 124.6(7) . . ? N5 C3 C4 119.5(7) . . ? C2 C3 C4 114.8(7) . . ? C5 C4 C3 123.0(7) . . ? C5 C4 H4 118.5 . . ? C3 C4 H4 118.5 . . ? C6 C5 C4 116.0(7) . . ? C6 C5 C8 120.3(7) . . ? C4 C5 C8 123.6(7) . . ? C7 C6 C5 126.7(8) . . ? C7 C6 H6 116.6 . . ? C5 C6 H6 116.6 . . ? C6 C7 C2 116.6(8) . . ? C6 C7 H7 121.7 . . ? C2 C7 H7 121.7 . . ? O3 C8 O4 120.5(7) . . ? O3 C8 C5 112.3(8) . . ? O4 C8 C5 127.0(7) . . ? N2 C9 N1 108.9(7) . . ? N2 C9 H9 125.5 . . ? N1 C9 H9 125.5 . . ? N1 C10 C11 106.7(7) . . ? N1 C10 H10 126.7 . . ? C11 C10 H10 126.7 . . ? N2 C11 C10 107.7(8) . . ? N2 C11 H11 126.1 . . ? C10 C11 H11 126.1 . . ? C13 C12 N2 111.9(6) . . ? C13 C12 H12A 109.2 . . ? N2 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? N2 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C18 120.0 . . ? C14 C13 C12 123.1(4) . . ? C18 C13 C12 116.9(4) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 C19 123.8(4) . . ? C17 C16 C19 116.1(4) . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? N4 C19 C16 102.0(5) . . ? N4 C19 H19A 111.4 . . ? C16 C19 H19A 111.4 . . ? N4 C19 H19B 111.4 . . ? C16 C19 H19B 111.4 . . ? H19A C19 H19B 109.2 . . ? N3 C20 N4 106.9(7) . . ? N3 C20 H20 126.5 . . ? N4 C20 H20 126.5 . . ? C22 C21 N3 109.6(7) . . ? C22 C21 H21 125.2 . . ? N3 C21 H21 125.2 . . ? C21 C22 N4 106.5(7) . . ? C21 C22 H22 126.7 . . ? N4 C22 H22 126.7 . . ? O5 C23 N6 110.3(6) . . ? O5 C23 H23 124.8 . . ? N6 C23 H23 124.8 . . ? N6 C24 H24A 109.5 . . ? N6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C25 H25A 109.5 . . ? N6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 N7 117.1(6) . . ? O6 C26 H26 121.5 . . ? N7 C26 H26 121.5 . . ? N7 C27 H27A 109.5 . . ? N7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N7 C28 H28A 109.5 . . ? N7 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N7 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C9 N1 C10 108.2(7) . . ? C9 N1 Zn1 128.5(6) . . ? C10 N1 Zn1 123.1(5) . . ? C9 N2 C11 108.3(7) . . ? C9 N2 C12 125.3(7) . . ? C11 N2 C12 124.5(8) . . ? C20 N3 C21 107.9(7) . . ? C20 N3 Zn1 123.4(5) . 2_575 ? C21 N3 Zn1 128.7(5) . 2_575 ? C22 N4 C20 108.6(6) . . ? C22 N4 C19 127.9(8) . . ? C20 N4 C19 123.1(7) . . ? C3 N5 H5A 120.0 . . ? C3 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C23 N6 C24 114.9(6) . . ? C23 N6 C25 126.5(6) . . ? C24 N6 C25 118.6(5) . . ? C26 N7 C27 115.9(5) . . ? C26 N7 C28 113.2(6) . . ? C27 N7 C28 130.8(5) . . ? C1 O2 Zn1 111.9(5) . . ? C8 O3 Zn1 113.8(6) . 4_454 ? N3 Zn1 N1 119.07(16) 2_574 . ? N3 Zn1 O2 111.4(3) 2_574 . ? N1 Zn1 O2 110.6(3) . . ? N3 Zn1 O3 105.5(3) 2_574 4 ? N1 Zn1 O3 112.9(3) . 4 ? O2 Zn1 O3 94.53(15) . 4 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -167.6(8) . . . . ? O1 C1 C2 C3 13.0(13) . . . . ? O2 C1 C2 C7 7.1(13) . . . . ? O1 C1 C2 C7 -172.4(8) . . . . ? C7 C2 C3 N5 168.0(8) . . . . ? C1 C2 C3 N5 -17.7(13) . . . . ? C7 C2 C3 C4 -0.3(12) . . . . ? C1 C2 C3 C4 174.0(8) . . . . ? N5 C3 C4 C5 -167.0(9) . . . . ? C2 C3 C4 C5 1.9(12) . . . . ? C3 C4 C5 C6 -1.6(13) . . . . ? C3 C4 C5 C8 -179.9(8) . . . . ? C4 C5 C6 C7 -0.5(13) . . . . ? C8 C5 C6 C7 177.8(9) . . . . ? C5 C6 C7 C2 2.0(12) . . . . ? C3 C2 C7 C6 -1.6(13) . . . . ? C1 C2 C7 C6 -176.0(8) . . . . ? C6 C5 C8 O3 169.1(7) . . . . ? C4 C5 C8 O3 -12.7(12) . . . . ? C6 C5 C8 O4 -6.0(13) . . . . ? C4 C5 C8 O4 172.2(9) . . . . ? N1 C10 C11 N2 0.3(9) . . . . ? N2 C12 C13 C14 -79.3(7) . . . . ? N2 C12 C13 C18 100.2(7) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C12 C13 C14 C15 179.5(5) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C14 C15 C16 C19 -178.0(4) . . . . ? C15 C16 C17 C18 0.0 . . . . ? C19 C16 C17 C18 178.2(4) . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? C12 C13 C18 C17 -179.5(5) . . . . ? C15 C16 C19 N4 -95.8(6) . . . . ? C17 C16 C19 N4 86.1(6) . . . . ? N3 C21 C22 N4 -2.3(8) . . . . ? N2 C9 N1 C10 4.6(9) . . . . ? N2 C9 N1 Zn1 179.1(5) . . . . ? C11 C10 N1 C9 -2.9(9) . . . . ? C11 C10 N1 Zn1 -177.8(5) . . . . ? N1 C9 N2 C11 -4.4(9) . . . . ? N1 C9 N2 C12 -169.3(7) . . . . ? C10 C11 N2 C9 2.5(9) . . . . ? C10 C11 N2 C12 167.6(7) . . . . ? C13 C12 N2 C9 89.4(9) . . . . ? C13 C12 N2 C11 -73.1(10) . . . . ? N4 C20 N3 C21 5.3(8) . . . . ? N4 C20 N3 Zn1 -174.8(5) . . . 2_575 ? C22 C21 N3 C20 -1.9(9) . . . . ? C22 C21 N3 Zn1 178.1(5) . . . 2_575 ? C21 C22 N4 C20 5.6(8) . . . . ? C21 C22 N4 C19 178.8(7) . . . . ? N3 C20 N4 C22 -6.8(8) . . . . ? N3 C20 N4 C19 179.6(7) . . . . ? C16 C19 N4 C22 79.4(9) . . . . ? C16 C19 N4 C20 -108.3(7) . . . . ? O5 C23 N6 C24 173.7(6) . . . . ? O5 C23 N6 C25 -4.1(8) . . . . ? O6 C26 N7 C27 4.8(9) . . . . ? O6 C26 N7 C28 -174.8(6) . . . . ? O1 C1 O2 Zn1 -4.9(12) . . . . ? C2 C1 O2 Zn1 175.7(6) . . . . ? O4 C8 O3 Zn1 7.9(10) . . . 4_454 ? C5 C8 O3 Zn1 -167.5(5) . . . 4_454 ? C9 N1 Zn1 N3 -72.1(8) . . . 2_574 ? C10 N1 Zn1 N3 101.7(7) . . . 2_574 ? C9 N1 Zn1 O2 157.0(6) . . . . ? C10 N1 Zn1 O2 -29.3(7) . . . . ? C9 N1 Zn1 O3 52.5(7) . . . 4 ? C10 N1 Zn1 O3 -133.8(6) . . . 4 ? C1 O2 Zn1 N3 -62.2(6) . . . 2_574 ? C1 O2 Zn1 N1 72.6(6) . . . . ? C1 O2 Zn1 O3 -170.8(6) . . . 4 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.272 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.067 ################################################ data_3 _database_code_depnum_ccdc_archive 'CCDC 866679' #TrackingRef '- new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 Co N6 O6' _chemical_formula_weight 581.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' 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' _cell_length_a 20.960(4) _cell_length_b 11.530(2) _cell_length_c 14.211(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.24(3) _cell_angle_gamma 90.00 _cell_volume 3080.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3917 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 25.12 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 0.603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9097 _exptl_absorpt_correction_T_max 0.9422 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12113 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5741 _reflns_number_gt 3903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.4400P] 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 0.03(2) _refine_ls_number_reflns 5741 _refine_ls_number_parameters 380 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.075 _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 0.8063(4) 0.5991(6) 0.7135(5) 0.0646(18) Uani 1 1 d . . . C2 C 0.8623(3) 0.6715(6) 0.7696(4) 0.0617(17) Uani 1 1 d . . . C3 C 0.8543(3) 0.7939(6) 0.7542(4) 0.0641(17) Uani 1 1 d . . . H3 H 0.8115 0.8233 0.7035 0.077 Uiso 1 1 calc R . . C4 C 0.9098(3) 0.8718(6) 0.8141(5) 0.0602(16) Uani 1 1 d . . . C5 C 0.9731(3) 0.8241(4) 0.8924(4) 0.0526(14) Uani 1 1 d . . . C6 C 1.0319(3) 0.9044(6) 0.9616(5) 0.0603(16) Uani 1 1 d . . . C7 C 0.9802(3) 0.7079(5) 0.9028(4) 0.0600(16) Uani 1 1 d . . . H7 H 1.0224 0.6779 0.9542 0.072 Uiso 1 1 calc R . . C8 C 0.9290(3) 0.6331(5) 0.8422(4) 0.0631(17) Uani 1 1 d . . . H8 H 0.9385 0.5539 0.8491 0.076 Uiso 1 1 calc R . . C9 C 0.7025(3) 0.3728(5) 0.7713(5) 0.0593(16) Uani 1 1 d . . . H9 H 0.7507 0.3661 0.7890 0.071 Uiso 1 1 calc R . . C10 C 0.5889(3) 0.4054(6) 0.6974(5) 0.0660(17) Uani 1 1 d . . . H10 H 0.5446 0.4338 0.6508 0.079 Uiso 1 1 calc R . . C11 C 0.6008(3) 0.3364(5) 0.7745(4) 0.0545(13) Uani 1 1 d . . . H11 H 0.5665 0.3043 0.7915 0.065 Uiso 1 1 calc R . . C12 C 0.7005(3) 0.2341(4) 0.9146(4) 0.0530(14) Uani 1 1 d . . . H12A H 0.7515 0.2467 0.9515 0.064 Uiso 1 1 calc R A 1 H12B H 0.6805 0.2467 0.9636 0.064 Uiso 1 1 calc R A 1 C13 C 0.6862(3) 0.1117(3) 0.8745(4) 0.058(12) Uani 0.574(11) 1 d PG B 1 C14 C 0.7269(4) 0.0605(4) 0.8308(7) 0.070(4) Uani 0.574(11) 1 d PG B 1 H14 H 0.7646 0.1010 0.8287 0.084 Uiso 0.574(11) 1 calc PR B 1 C15 C 0.7113(4) -0.0513(4) 0.7904(7) 0.073(4) Uani 0.574(11) 1 d PG B 1 H15 H 0.7386 -0.0855 0.7612 0.088 Uiso 0.574(11) 1 calc PR B 1 C16 C 0.6550(3) -0.1118(4) 0.7936(4) 0.053(4) Uani 0.574(11) 1 d PG B 1 C17 C 0.6142(3) -0.0606(4) 0.8373(7) 0.060(3) Uani 0.574(11) 1 d PG B 1 H17 H 0.5765 -0.1011 0.8394 0.072 Uiso 0.574(11) 1 calc PR B 1 C18 C 0.6298(3) 0.0512(4) 0.8777(7) 0.059(3) Uani 0.574(11) 1 d PG B 1 H18 H 0.6025 0.0854 0.9069 0.071 Uiso 0.574(11) 1 calc PR B 1 C13' C 0.6842(3) 0.1117(3) 0.8723(4) 0.064(17) Uani 0.426(11) 1 d PG B 2 C14' C 0.6892(5) 0.0702(4) 0.7839(5) 0.064(4) Uani 0.426(11) 1 d PG B 2 H14' H 0.7041 0.1192 0.7455 0.076 Uiso 0.426(11) 1 calc PR B 2 C15' C 0.6718(5) -0.0445(4) 0.7529(4) 0.056(4) Uani 0.426(11) 1 d PG B 2 H15' H 0.6752 -0.0722 0.6938 0.067 Uiso 0.426(11) 1 calc PR B 2 C16' C 0.6496(3) -0.1177(4) 0.8103(5) 0.053(5) Uani 0.426(11) 1 d PG B 2 C17' C 0.6446(5) -0.0762(4) 0.8987(6) 0.064(4) Uani 0.426(11) 1 d PG B 2 H17' H 0.6297 -0.1252 0.9371 0.077 Uiso 0.426(11) 1 calc PR B 2 C18' C 0.6619(5) 0.0385(4) 0.9297(5) 0.074(5) Uani 0.426(11) 1 d PG B 2 H18' H 0.6586 0.0662 0.9888 0.089 Uiso 0.426(11) 1 calc PR B 2 C19 C 0.6346(3) -0.2380(5) 0.7587(4) 0.0707(18) Uani 1 1 d . . . H19A H 0.5832 -0.2462 0.7278 0.085 Uiso 1 1 calc R B 1 H19B H 0.6501 -0.2579 0.7058 0.085 Uiso 1 1 calc R B 1 C20 C 0.7440(4) -0.3503(6) 0.8979(5) 0.0757(19) Uani 1 1 d . . . H20 H 0.7798 -0.3278 0.8799 0.091 Uiso 1 1 calc R B . C21 C 0.7507(3) -0.4219(5) 0.9770(5) 0.0637(17) Uani 1 1 d . . . H21 H 0.7926 -0.4582 1.0227 0.076 Uiso 1 1 calc R . . C22 C 0.6425(4) -0.3687(6) 0.8971(5) 0.0707(19) Uani 1 1 d . . . H22 H 0.5944 -0.3662 0.8807 0.085 Uiso 1 1 calc R B . C23 C 0.4640(3) 0.0937(4) 0.6228(4) 0.0687(13) Uani 1 1 d . . . H23A H 0.4689 0.1454 0.6785 0.103 Uiso 1 1 calc R . . H23B H 0.4985 0.0326 0.6502 0.103 Uiso 1 1 calc R . . H23C H 0.4170 0.0610 0.5921 0.103 Uiso 1 1 calc R . . C24 C 0.5447(3) 0.1503(4) 0.5368(4) 0.0750(13) Uani 1 1 d . . . H24A H 0.5412 0.0944 0.4846 0.112 Uiso 1 1 calc R . . H24B H 0.5806 0.1261 0.6041 0.112 Uiso 1 1 calc R . . H24C H 0.5573 0.2244 0.5192 0.112 Uiso 1 1 calc R . . C25 C 0.4178(3) 0.2265(4) 0.4635(4) 0.0758(14) Uani 1 1 d . . . H25 H 0.4262 0.2801 0.4213 0.091 Uiso 1 1 calc R . . Co1 Co 0.67055(5) 0.52565(4) 0.58687(7) 0.05607(15) Uani 1 1 d . . . N1 N 0.8988(2) 0.9827(4) 0.8278(3) 0.0764(12) Uani 1 1 d . . . H1X H 0.9343 1.0256 0.8283 0.092 Uiso 1 1 d R . . H1Y H 0.8584 0.9893 0.8337 0.092 Uiso 1 1 d R . . N2 N 0.6575(3) 0.4321(5) 0.6946(4) 0.0554(12) Uani 1 1 d . . . N3 N 0.6679(3) 0.3197(4) 0.8239(4) 0.0512(11) Uani 1 1 d . B . N4 N 0.6659(3) -0.3136(4) 0.8440(4) 0.0627(14) Uani 1 1 d . B . N5 N 0.6884(3) -0.4326(4) 0.9797(4) 0.0585(14) Uani 1 1 d . . . N6 N 0.4757(2) 0.1594(4) 0.5407(4) 0.0694(14) Uani 1 1 d . . . O1 O 0.8170(2) 0.4910(4) 0.7148(3) 0.0669(12) Uani 1 1 d . . . O2 O 0.7465(2) 0.6391(4) 0.6545(3) 0.0698(12) Uani 1 1 d . . . O3 O 1.09090(19) 0.8583(4) 1.0182(3) 0.0643(11) Uani 1 1 d . . . O4 O 1.0291(2) 1.0107(4) 0.9507(4) 0.0685(12) Uani 1 1 d . . . O5 O 0.3573(2) 0.2113(3) 0.4550(3) 0.0812(10) Uani 1 1 d . . . O6 O 0.83658(17) 0.7513(3) 0.1630(3) 0.0803(10) Uani 1 1 d . . . H6B H 0.8518 0.6823 0.1792 0.096 Uiso 1 1 d R . . C26 C 0.8798(3) 0.8367(6) 0.1451(5) 0.0694(18) Uani 1 1 d . . . H26C H 0.8700 0.9118 0.1649 0.104 Uiso 1 1 calc R . . H26D H 0.8692 0.8373 0.0721 0.104 Uiso 1 1 calc R . . H26A H 0.9291 0.8182 0.1864 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.066(4) 0.054(4) 0.059(4) 0.013(3) 0.014(3) 0.004(3) C2 0.055(3) 0.085(4) 0.041(3) 0.010(3) 0.017(2) 0.021(3) C3 0.038(3) 0.078(4) 0.055(3) 0.012(3) 0.001(2) -0.005(3) C4 0.034(3) 0.063(4) 0.064(3) 0.016(3) 0.004(2) 0.008(2) C5 0.042(3) 0.041(3) 0.052(3) -0.001(2) 0.000(2) -0.022(2) C6 0.039(3) 0.068(5) 0.061(3) -0.013(3) 0.011(2) -0.014(3) C7 0.038(3) 0.049(3) 0.052(3) -0.001(2) -0.017(2) 0.007(2) C8 0.052(3) 0.051(3) 0.061(3) 0.006(2) 0.002(3) -0.002(3) C9 0.059(4) 0.034(3) 0.071(4) 0.006(3) 0.016(3) -0.015(3) C10 0.068(4) 0.064(4) 0.056(4) 0.003(3) 0.018(3) -0.003(3) C11 0.064(3) 0.050(3) 0.051(3) -0.010(2) 0.026(3) 0.001(3) C12 0.073(4) 0.034(3) 0.041(3) 0.005(2) 0.016(3) 0.006(3) C13 0.072(15) 0.033(15) 0.041(15) 0.008(10) 0.000(10) 0.018(9) C14 0.091(9) 0.036(6) 0.066(8) -0.002(5) 0.021(7) 0.011(6) C15 0.065(8) 0.036(6) 0.105(10) -0.027(6) 0.025(7) -0.010(5) C16 0.052(8) 0.065(10) 0.032(6) 0.000(5) 0.010(6) -0.004(7) C17 0.063(7) 0.046(7) 0.067(8) 0.002(6) 0.025(6) -0.013(6) C18 0.088(9) 0.059(7) 0.038(6) 0.001(5) 0.035(6) 0.005(6) C13' 0.08(2) 0.029(19) 0.07(3) 0.012(15) 0.023(17) -0.022(13) C14' 0.061(9) 0.058(10) 0.078(10) -0.024(8) 0.036(8) -0.031(7) C15' 0.080(11) 0.046(8) 0.046(7) -0.013(6) 0.031(8) -0.004(7) C16' 0.045(9) 0.061(12) 0.046(8) -0.008(7) 0.014(7) -0.013(8) C17' 0.086(11) 0.041(7) 0.045(8) 0.003(6) 0.010(8) 0.011(7) C18' 0.062(9) 0.088(11) 0.041(7) 0.010(7) -0.007(7) -0.033(7) C19 0.063(4) 0.057(4) 0.069(4) -0.005(3) 0.008(3) -0.020(3) C20 0.068(4) 0.071(4) 0.067(4) 0.012(3) 0.011(3) 0.002(4) C21 0.064(4) 0.046(3) 0.071(4) -0.007(3) 0.021(3) 0.000(3) C22 0.073(4) 0.052(4) 0.059(4) 0.010(3) 0.004(3) 0.008(3) C23 0.065(3) 0.066(3) 0.075(3) 0.024(2) 0.031(2) 0.015(2) C24 0.068(3) 0.068(3) 0.069(3) -0.008(2) 0.012(2) 0.007(2) C25 0.092(4) 0.063(3) 0.058(3) -0.020(2) 0.019(3) -0.017(3) Co1 0.0569(3) 0.0393(2) 0.0588(3) -0.0023(5) 0.0136(2) -0.0017(5) N1 0.063(2) 0.066(3) 0.075(3) 0.013(2) 0.009(2) 0.0089(19) N2 0.064(3) 0.043(3) 0.053(3) -0.010(2) 0.020(2) -0.005(3) N3 0.067(3) 0.029(3) 0.054(3) -0.0008(18) 0.024(2) 0.0025(19) N4 0.073(3) 0.038(3) 0.056(3) -0.003(2) 0.009(2) -0.010(2) N5 0.061(3) 0.032(2) 0.059(3) 0.000(2) 0.005(2) -0.005(2) N6 0.055(3) 0.064(3) 0.065(3) -0.001(2) 0.004(2) -0.022(2) O1 0.067(3) 0.061(3) 0.061(3) -0.0167(19) 0.018(2) -0.017(2) O2 0.046(2) 0.069(3) 0.069(2) 0.022(2) 0.002(2) -0.016(2) O3 0.049(2) 0.071(3) 0.056(2) -0.015(2) 0.0072(19) 0.001(2) O4 0.056(2) 0.065(3) 0.069(3) -0.007(2) 0.013(2) -0.007(2) O5 0.067(2) 0.082(2) 0.073(2) -0.0087(18) 0.0111(18) 0.0096(18) O6 0.0538(18) 0.087(2) 0.074(2) -0.0187(18) 0.0041(15) -0.0055(18) C26 0.050(3) 0.080(4) 0.066(4) -0.036(3) 0.015(3) -0.021(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 O2 1.248(7) . ? C1 O1 1.265(7) . ? C1 C2 1.372(8) . ? C2 C8 1.393(7) . ? C2 C3 1.426(8) . ? C3 C4 1.418(8) . ? C3 H3 0.9300 . ? C4 N1 1.329(7) . ? C4 C5 1.413(7) . ? C5 C7 1.349(7) . ? C5 C6 1.508(7) . ? C6 O4 1.233(7) . ? C6 O3 1.257(7) . ? C7 C8 1.349(7) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 N2 1.279(8) . ? C9 N3 1.393(7) . ? C9 H9 0.9300 . ? C10 C11 1.286(8) . ? C10 N2 1.488(8) . ? C10 H10 0.9300 . ? C11 N3 1.280(7) . ? C11 H11 0.9300 . ? C12 C13 1.501(6) . ? C12 C13' 1.512(6) . ? C12 N3 1.524(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 C19 1.535(7) . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C13' C14' 1.3900 . ? C13' C18' 1.3901 . ? C14' C15' 1.3899 . ? C14' H14' 0.9300 . ? C15' C16' 1.3899 . ? C15' H15' 0.9300 . ? C16' C17' 1.3900 . ? C16' C19 1.535(7) . ? C17' C18' 1.3900 . ? C17' H17' 0.9300 . ? C18' H18' 0.9300 . ? C19 N4 1.399(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.351(9) . ? C20 N4 1.529(8) . ? C20 H20 0.9300 . ? C21 N5 1.329(7) . ? C21 H21 0.9300 . ? C22 N4 1.240(8) . ? C22 N5 1.359(7) . ? C22 H22 0.9300 . ? C23 N6 1.500(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N6 1.475(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O5 1.233(6) . ? C25 N6 1.448(7) . ? C25 H25 0.9300 . ? Co1 O2 1.953(4) . ? Co1 N2 1.988(5) . ? Co1 O3 2.022(4) 4_464 ? Co1 N5 2.028(5) 2_554 ? N1 H1X 0.8900 . ? N1 H1Y 0.8899 . ? N5 Co1 2.028(5) 2 ? O3 Co1 2.022(4) 4_565 ? O6 C26 1.435(7) . ? O6 H6B 0.8500 . ? C26 H26C 0.9600 . ? C26 H26D 0.9600 . ? C26 H26A 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 O2 C1 O1 119.6(6) . . ? O2 C1 C2 120.8(6) . . ? O1 C1 C2 119.3(6) . . ? C1 C2 C8 123.9(6) . . ? C1 C2 C3 120.0(5) . . ? C8 C2 C3 116.1(6) . . ? C4 C3 C2 121.7(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? N1 C4 C5 115.0(5) . . ? N1 C4 C3 123.3(5) . . ? C5 C4 C3 117.5(5) . . ? C7 C5 C4 119.6(5) . . ? C7 C5 C6 121.3(5) . . ? C4 C5 C6 119.1(5) . . ? O4 C6 O3 118.7(6) . . ? O4 C6 C5 123.2(6) . . ? O3 C6 C5 116.6(6) . . ? C5 C7 C8 123.2(5) . . ? C5 C7 H7 118.4 . . ? C8 C7 H7 118.4 . . ? C7 C8 C2 121.6(6) . . ? C7 C8 H8 119.2 . . ? C2 C8 H8 119.2 . . ? N2 C9 N3 109.2(6) . . ? N2 C9 H9 125.4 . . ? N3 C9 H9 125.4 . . ? C11 C10 N2 109.0(6) . . ? C11 C10 H10 125.5 . . ? N2 C10 H10 125.5 . . ? N3 C11 C10 108.2(6) . . ? N3 C11 H11 125.9 . . ? C10 C11 H11 125.9 . . ? C13 C12 C13' 1.4 . . ? C13 C12 N3 110.4(4) . . ? C13' C12 N3 109.3(4) . . ? C13 C12 H12A 109.6 . . ? C13' C12 H12A 110.9 . . ? N3 C12 H12A 109.6 . . ? C13 C12 H12B 109.6 . . ? C13' C12 H12B 109.4 . . ? N3 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C18 120.0 . . ? C14 C13 C12 120.6(4) . . ? C18 C13 C12 119.4(4) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 C19 125.8(4) . . ? C17 C16 C19 114.1(4) . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C14' C13' C18' 120.0 . . ? C14' C13' C12 125.9(3) . . ? C18' C13' C12 114.1(3) . . ? C15' C14' C13' 120.0 . . ? C15' C14' H14' 120.0 . . ? C13' C14' H14' 120.0 . . ? C16' C15' C14' 120.0 . . ? C16' C15' H15' 120.0 . . ? C14' C15' H15' 120.0 . . ? C15' C16' C17' 120.0 . . ? C15' C16' C19 108.6(4) . . ? C17' C16' C19 131.4(4) . . ? C18' C17' C16' 120.0 . . ? C18' C17' H17' 120.0 . . ? C16' C17' H17' 120.0 . . ? C17' C18' C13' 120.0 . . ? C17' C18' H18' 120.0 . . ? C13' C18' H18' 120.0 . . ? N4 C19 C16' 103.4(5) . . ? N4 C19 C16 110.7(5) . . ? C16' C19 C16 11.67(5) . . ? N4 C19 H19A 109.5 . . ? C16' C19 H19A 104.9 . . ? C16 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? C16' C19 H19B 121.1 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 N4 106.2(6) . . ? C21 C20 H20 126.9 . . ? N4 C20 H20 126.9 . . ? N5 C21 C20 109.9(6) . . ? N5 C21 H21 125.1 . . ? C20 C21 H21 125.1 . . ? N4 C22 N5 119.0(7) . . ? N4 C22 H22 120.5 . . ? N5 C22 H22 120.5 . . ? N6 C23 H23A 109.5 . . ? N6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 H24A 109.5 . . ? N6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 N6 118.7(5) . . ? O5 C25 H25 120.7 . . ? N6 C25 H25 120.7 . . ? O2 Co1 N2 110.14(18) . . ? O2 Co1 O3 96.52(10) . 4_464 ? N2 Co1 O3 111.40(19) . 4_464 ? O2 Co1 N5 110.0(2) . 2_554 ? N2 Co1 N5 115.19(11) . 2_554 ? O3 Co1 N5 111.99(18) 4_464 2_554 ? C4 N1 H1X 109.7 . . ? C4 N1 H1Y 109.2 . . ? H1X N1 H1Y 141.1 . . ? C9 N2 C10 103.0(6) . . ? C9 N2 Co1 130.1(5) . . ? C10 N2 Co1 126.6(4) . . ? C11 N3 C9 110.3(5) . . ? C11 N3 C12 122.4(5) . . ? C9 N3 C12 126.4(5) . . ? C22 N4 C19 133.3(6) . . ? C22 N4 C20 100.2(5) . . ? C19 N4 C20 126.5(6) . . ? C21 N5 C22 104.6(6) . . ? C21 N5 Co1 125.5(4) . 2 ? C22 N5 Co1 129.9(5) . 2 ? C25 N6 C24 121.2(4) . . ? C25 N6 C23 119.2(4) . . ? C24 N6 C23 119.6(4) . . ? C1 O2 Co1 116.2(4) . . ? C6 O3 Co1 113.4(4) . 4_565 ? C26 O6 H6B 119.9 . . ? O6 C26 H26C 109.5 . . ? O6 C26 H26D 109.5 . . ? H26C C26 H26D 109.5 . . ? O6 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? H26D C26 H26A 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 O2 C1 C2 C8 175.4(6) . . . . ? O1 C1 C2 C8 -10.6(10) . . . . ? O2 C1 C2 C3 -5.5(10) . . . . ? O1 C1 C2 C3 168.5(6) . . . . ? C1 C2 C3 C4 177.1(6) . . . . ? C8 C2 C3 C4 -3.7(9) . . . . ? C2 C3 C4 N1 -157.5(6) . . . . ? C2 C3 C4 C5 -1.9(8) . . . . ? N1 C4 C5 C7 161.8(6) . . . . ? C3 C4 C5 C7 4.2(8) . . . . ? N1 C4 C5 C6 -19.2(8) . . . . ? C3 C4 C5 C6 -176.8(6) . . . . ? C7 C5 C6 O4 175.8(7) . . . . ? C4 C5 C6 O4 -3.2(10) . . . . ? C7 C5 C6 O3 10.0(10) . . . . ? C4 C5 C6 O3 -169.0(5) . . . . ? C4 C5 C7 C8 -0.7(10) . . . . ? C6 C5 C7 C8 -179.7(6) . . . . ? C5 C7 C8 C2 -5.4(9) . . . . ? C1 C2 C8 C7 -173.5(6) . . . . ? C3 C2 C8 C7 7.3(8) . . . . ? N2 C10 C11 N3 2.7(7) . . . . ? C13' C12 C13 C14 119.3(3) . . . . ? N3 C12 C13 C14 79.7(6) . . . . ? C13' C12 C13 C18 -58.22(17) . . . . ? N3 C12 C13 C18 -97.9(6) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C12 C13 C14 C15 -177.5(4) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C14 C15 C16 C19 -175.8(5) . . . . ? C15 C16 C17 C18 0.0 . . . . ? C19 C16 C17 C18 176.2(4) . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? C12 C13 C18 C17 177.6(3) . . . . ? C13 C12 C13' C14' -96.6(3) . . . . ? N3 C12 C13' C14' 44.1(7) . . . . ? C13 C12 C13' C18' 84.0(2) . . . . ? N3 C12 C13' C18' -135.3(5) . . . . ? C18' C13' C14' C15' 0.0 . . . . ? C12 C13' C14' C15' -179.4(4) . . . . ? C13' C14' C15' C16' 0.0 . . . . ? C14' C15' C16' C17' 0.0 . . . . ? C14' C15' C16' C19 -179.8(4) . . . . ? C15' C16' C17' C18' 0.0 . . . . ? C19 C16' C17' C18' 179.7(5) . . . . ? C16' C17' C18' C13' 0.0 . . . . ? C14' C13' C18' C17' 0.0 . . . . ? C12 C13' C18' C17' 179.4(4) . . . . ? C15' C16' C19 N4 135.9(5) . . . . ? C17' C16' C19 N4 -43.8(8) . . . . ? C15' C16' C19 C16 5.51(16) . . . . ? C17' C16' C19 C16 -174.2(3) . . . . ? C15 C16 C19 N4 94.1(7) . . . . ? C17 C16 C19 N4 -81.9(7) . . . . ? C15 C16 C19 C16' 146.5(2) . . . . ? C17 C16 C19 C16' -29.5(2) . . . . ? N4 C20 C21 N5 -0.8(8) . . . . ? N3 C9 N2 C10 -4.2(7) . . . . ? N3 C9 N2 Co1 -178.5(4) . . . . ? C11 C10 N2 C9 1.1(7) . . . . ? C11 C10 N2 Co1 175.7(4) . . . . ? O2 Co1 N2 C9 -54.5(6) . . . . ? O3 Co1 N2 C9 -160.4(6) 4_464 . . . ? N5 Co1 N2 C9 70.6(6) 2_554 . . . ? O2 Co1 N2 C10 132.3(5) . . . . ? O3 Co1 N2 C10 26.5(5) 4_464 . . . ? N5 Co1 N2 C10 -102.5(5) 2_554 . . . ? C10 C11 N3 C9 -5.4(7) . . . . ? C10 C11 N3 C12 -174.7(5) . . . . ? N2 C9 N3 C11 6.3(7) . . . . ? N2 C9 N3 C12 175.0(5) . . . . ? C13 C12 N3 C11 72.3(7) . . . . ? C13' C12 N3 C11 71.4(7) . . . . ? C13 C12 N3 C9 -95.2(6) . . . . ? C13' C12 N3 C9 -96.1(6) . . . . ? N5 C22 N4 C19 -177.2(6) . . . . ? N5 C22 N4 C20 2.6(8) . . . . ? C16' C19 N4 C22 95.3(8) . . . . ? C16 C19 N4 C22 104.8(8) . . . . ? C16' C19 N4 C20 -84.5(7) . . . . ? C16 C19 N4 C20 -75.0(8) . . . . ? C21 C20 N4 C22 -1.0(7) . . . . ? C21 C20 N4 C19 178.9(6) . . . . ? C20 C21 N5 C22 2.2(7) . . . . ? C20 C21 N5 Co1 -177.6(4) . . . 2 ? N4 C22 N5 C21 -3.3(8) . . . . ? N4 C22 N5 Co1 176.5(5) . . . 2 ? O5 C25 N6 C24 163.9(4) . . . . ? O5 C25 N6 C23 -13.2(7) . . . . ? O1 C1 O2 Co1 9.9(8) . . . . ? C2 C1 O2 Co1 -176.1(5) . . . . ? N2 Co1 O2 C1 59.3(5) . . . . ? O3 Co1 O2 C1 175.0(4) 4_464 . . . ? N5 Co1 O2 C1 -68.7(5) 2_554 . . . ? O4 C6 O3 Co1 2.7(8) . . . 4_565 ? C5 C6 O3 Co1 169.1(4) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.505 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.043 ############################################### data_4 _database_code_depnum_ccdc_archive 'CCDC 866680' #TrackingRef '- new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H19 Co N3 O4' _chemical_formula_weight 436.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 11.7678(14) _cell_length_b 17.166(2) _cell_length_c 19.269(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3892.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.957 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26667 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.40 _reflns_number_total 3584 _reflns_number_gt 2176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^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 3584 _refine_ls_number_parameters 277 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.009 _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 O4 O 0.47860(19) 0.35173(13) 1.04094(11) 0.0680(6) Uani 1 1 d . . . C8 C 0.5514(3) 0.29916(18) 1.02668(16) 0.0586(8) Uani 1 1 d . . . C5 C 0.5469(2) 0.26181(16) 0.95684(14) 0.0499(7) Uani 1 1 d . C . C4 C 0.4540(3) 0.27409(17) 0.91418(15) 0.0625(8) Uani 1 1 d . C . H4 H 0.3928 0.3028 0.9308 0.075 Uiso 1 1 calc R . . Co1 Co 0.54330(3) 0.10930(2) 0.631919(18) 0.05057(15) Uani 1 1 d . . . C1 C 0.5361(3) 0.16921(19) 0.74995(17) 0.0653(9) Uani 1 1 d . . . C2 C 0.5397(3) 0.20200(16) 0.82154(15) 0.0540(7) Uani 1 1 d . B . C3 C 0.4500(3) 0.24465(19) 0.84747(16) 0.0632(8) Uani 1 1 d D . . H3 H 0.3865 0.2537 0.8199 0.076 Uiso 0.69 1 calc PR A 1 N1' N 0.7205(2) 0.14126(16) 0.85365(15) 0.088(3) Uani 0.31 1 d PD B 2 H1C H 0.7246 0.1138 0.8164 0.106 Uiso 0.31 1 calc PR B 2 H1D H 0.7734 0.1381 0.8844 0.106 Uiso 0.31 1 calc PR B 2 C6 C 0.6380(2) 0.21801(16) 0.93112(15) 0.0579(8) Uani 1 1 d RD . . H6 H 0.7015 0.2088 0.9587 0.070 Uiso 0.64 1 calc PR B 1 N1 N 0.7380(5) 0.2042(4) 0.9661(3) 0.072(2) Uani 0.36 1 d PD C 2 H1A H 0.7920 0.1788 0.9463 0.087 Uiso 0.36 1 calc PR C 2 H1B H 0.7465 0.2210 1.0079 0.087 Uiso 0.36 1 calc PR C 2 C7 C 0.6328(3) 0.18834(17) 0.86375(17) 0.0595(8) Uani 1 1 d D B . H7 H 0.6930 0.1588 0.8469 0.071 Uiso 0.67 1 calc PR D 1 N1'' N 0.3374(8) 0.2519(6) 0.8173(5) 0.108(3) Uani 0.33 1 d PD E 2 H1E H 0.3213 0.2281 0.7793 0.130 Uiso 0.33 1 calc PR E 2 H1F H 0.2867 0.2801 0.8374 0.130 Uiso 0.33 1 calc PR E 2 C9 C 0.7874(3) 0.08040(19) 0.60562(18) 0.0695(9) Uani 1 1 d . . . H9 H 0.7874 0.1342 0.6109 0.083 Uiso 1 1 calc R . . C10 C 0.8896(3) 0.0438(2) 0.59813(18) 0.0709(9) Uani 1 1 d . . . H10 H 0.9560 0.0731 0.5975 0.085 Uiso 1 1 calc R . . C11 C 0.8956(3) -0.03555(18) 0.59159(15) 0.0568(8) Uani 1 1 d . . . C12 C 0.7927(3) -0.07395(19) 0.59221(19) 0.0759(10) Uani 1 1 d . . . H12 H 0.7908 -0.1279 0.5878 0.091 Uiso 1 1 calc R . . C13 C 0.6932(3) -0.03317(19) 0.59932(19) 0.0694(9) Uani 1 1 d . . . H13 H 0.6255 -0.0610 0.5996 0.083 Uiso 1 1 calc R . . C14 C 1.0068(3) -0.0780(2) 0.58706(18) 0.0735(10) Uani 1 1 d . . . H14A H 1.0655 -0.0418 0.5726 0.088 Uiso 1 1 calc R . . H14B H 1.0011 -0.1183 0.5520 0.088 Uiso 1 1 calc R . . C15 C 1.0411(3) -0.1146(2) 0.65520(19) 0.0800(11) Uani 1 1 d . . . H15A H 0.9856 -0.1539 0.6677 0.096 Uiso 1 1 calc R . . H15B H 1.0406 -0.0750 0.6911 0.096 Uiso 1 1 calc R . . C16 C 1.1585(3) -0.1519(2) 0.6524(2) 0.0910(12) Uani 1 1 d . . . H16A H 1.1695 -0.1837 0.6935 0.109 Uiso 1 1 calc R . . H16B H 1.1628 -0.1859 0.6122 0.109 Uiso 1 1 calc R . . C17 C 1.2518(3) -0.09275(18) 0.64827(19) 0.0661(9) Uani 1 1 d . . . C18 C 1.3020(3) -0.07231(18) 0.58674(17) 0.0653(9) Uani 1 1 d . . . H18 H 1.2798 -0.0965 0.5458 0.078 Uiso 1 1 calc R . . C19 C 1.3848(3) -0.01636(19) 0.58540(16) 0.0635(9) Uani 1 1 d . . . H19 H 1.4168 -0.0037 0.5427 0.076 Uiso 1 1 calc R . . C20 C 1.3737(3) 0.0003(2) 0.70066(17) 0.0894(12) Uani 1 1 d . . . H20 H 1.3977 0.0246 0.7412 0.107 Uiso 1 1 calc R . . C21 C 1.2906(3) -0.0547(2) 0.7057(2) 0.0957(13) Uani 1 1 d . . . H21 H 1.2599 -0.0664 0.7490 0.115 Uiso 1 1 calc R . . N2 N 0.6878(2) 0.04400(14) 0.60579(12) 0.0518(6) Uani 1 1 d . . . N3 N 1.4224(2) 0.02121(15) 0.64147(12) 0.0552(6) Uani 1 1 d . . . O1 O 0.4568(2) 0.18533(14) 0.70982(12) 0.0913(8) Uani 1 1 d . . . O2 O 0.6118(2) 0.12396(17) 0.73020(12) 0.0996(9) Uani 1 1 d . . . O3 O 0.6279(2) 0.28192(13) 1.06878(11) 0.0748(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O4 0.0647(15) 0.0756(14) 0.0637(14) -0.0187(12) 0.0035(12) 0.0021(13) C8 0.062(2) 0.0593(19) 0.0550(19) -0.0005(16) 0.0009(18) -0.0156(18) C5 0.0515(18) 0.0479(15) 0.0504(16) -0.0030(14) -0.0042(15) -0.0036(15) C4 0.062(2) 0.0616(19) 0.064(2) -0.0100(16) -0.0028(17) 0.0157(17) Co1 0.0493(2) 0.0579(2) 0.0445(2) -0.0017(2) -0.00345(19) 0.0010(2) C1 0.072(2) 0.065(2) 0.059(2) -0.0079(18) 0.002(2) -0.007(2) C2 0.062(2) 0.0475(16) 0.0527(17) -0.0029(14) 0.0066(17) -0.0026(17) C3 0.074(2) 0.0614(19) 0.0544(18) -0.0037(15) -0.0145(18) 0.0102(18) N1' 0.073(7) 0.101(7) 0.091(7) -0.044(6) -0.001(5) 0.028(6) C6 0.0526(19) 0.0546(18) 0.067(2) -0.0014(16) -0.0085(16) -0.0059(16) N1 0.048(4) 0.110(6) 0.058(4) -0.012(4) -0.022(4) 0.023(4) C7 0.0490(19) 0.0540(18) 0.076(2) -0.0123(18) 0.0110(18) 0.0003(15) N1'' 0.127(9) 0.132(9) 0.067(6) -0.026(6) -0.034(6) 0.039(7) C9 0.055(2) 0.0586(19) 0.095(3) -0.0056(19) -0.0053(19) -0.0080(17) C10 0.047(2) 0.071(2) 0.095(2) -0.003(2) -0.0003(19) -0.0180(18) C11 0.0465(18) 0.065(2) 0.0589(19) -0.0080(17) 0.0032(15) -0.0051(16) C12 0.051(2) 0.0539(19) 0.122(3) -0.016(2) -0.001(2) -0.0047(17) C13 0.0428(19) 0.063(2) 0.103(3) -0.013(2) -0.0035(19) -0.0067(17) C14 0.0515(19) 0.080(2) 0.089(3) -0.014(2) 0.0120(19) -0.0024(18) C15 0.054(2) 0.077(2) 0.109(3) 0.024(2) 0.021(2) -0.0010(19) C16 0.052(2) 0.068(2) 0.152(4) 0.028(2) 0.011(2) -0.0043(19) C17 0.0493(19) 0.061(2) 0.088(3) 0.0173(19) 0.0082(18) 0.0067(16) C18 0.0505(19) 0.074(2) 0.072(2) -0.0118(18) 0.0054(17) -0.0027(18) C19 0.051(2) 0.083(2) 0.057(2) -0.0038(18) 0.0115(16) -0.0092(18) C20 0.104(3) 0.118(3) 0.047(2) 0.005(2) 0.001(2) -0.036(3) C21 0.103(3) 0.119(3) 0.066(3) 0.028(2) 0.018(2) -0.032(3) N2 0.0458(14) 0.0560(15) 0.0536(14) -0.0042(12) -0.0046(12) -0.0039(13) N3 0.0555(15) 0.0669(16) 0.0431(14) 0.0029(13) 0.0021(12) -0.0014(13) O1 0.130(2) 0.0787(16) 0.0647(14) -0.0117(13) -0.0208(16) 0.0170(16) O2 0.0821(18) 0.141(2) 0.0752(17) -0.0453(16) -0.0047(14) 0.0216(18) O3 0.0854(17) 0.0767(16) 0.0623(14) -0.0030(12) -0.0191(13) -0.0071(13) _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 O4 C8 1.274(4) . ? O4 Co1 2.025(2) 7_566 ? C8 O3 1.247(3) . ? C8 C5 1.492(4) . ? C5 C4 1.384(4) . ? C5 C6 1.401(4) . ? C4 C3 1.382(4) . ? C4 H4 0.9300 . ? Co1 O4 2.025(2) 7_565 ? Co1 O2 2.074(2) . ? Co1 N3 2.084(2) 1_455 ? Co1 N2 2.098(2) . ? Co1 O1 2.234(2) . ? C1 O2 1.242(4) . ? C1 O1 1.243(4) . ? C1 C2 1.490(4) . ? C2 C3 1.378(4) . ? C2 C7 1.385(4) . ? C3 N1'' 1.453(8) . ? C3 H3 0.9300 . ? N1' C7 1.325(4) . ? N1' H1C 0.8600 . ? N1' H1D 0.8600 . ? C6 N1 1.377(5) . ? C6 C7 1.396(4) . ? C6 H6 0.9300 . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? C7 H7 0.9300 . ? N1'' H1E 0.8600 . ? N1'' H1F 0.8600 . ? C9 N2 1.327(4) . ? C9 C10 1.365(4) . ? C9 H9 0.9300 . ? C10 C11 1.369(4) . ? C10 H10 0.9300 . ? C11 C12 1.378(4) . ? C11 C14 1.501(4) . ? C12 C13 1.371(4) . ? C12 H12 0.9300 . ? C13 N2 1.332(4) . ? C13 H13 0.9300 . ? C14 C15 1.511(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.524(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.498(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C21 1.365(5) . ? C17 C18 1.371(4) . ? C18 C19 1.368(4) . ? C18 H18 0.9300 . ? C19 N3 1.334(4) . ? C19 H19 0.9300 . ? C20 N3 1.326(4) . ? C20 C21 1.362(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? N3 Co1 2.084(2) 1_655 ? 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 C8 O4 Co1 99.66(19) . 7_566 ? O3 C8 O4 120.9(3) . . ? O3 C8 C5 120.7(3) . . ? O4 C8 C5 118.3(3) . . ? C4 C5 C6 118.5(3) . . ? C4 C5 C8 119.9(3) . . ? C6 C5 C8 121.5(3) . . ? C3 C4 C5 121.6(3) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? O4 Co1 O2 153.74(11) 7_565 . ? O4 Co1 N3 93.41(9) 7_565 1_455 ? O2 Co1 N3 105.83(10) . 1_455 ? O4 Co1 N2 105.88(9) 7_565 . ? O2 Co1 N2 88.21(10) . . ? N3 Co1 N2 100.76(10) 1_455 . ? O4 Co1 O1 102.56(9) 7_565 . ? O2 Co1 O1 59.51(9) . . ? N3 Co1 O1 93.08(10) 1_455 . ? N2 Co1 O1 147.40(10) . . ? O2 C1 O1 119.2(3) . . ? O2 C1 C2 120.0(3) . . ? O1 C1 C2 120.9(3) . . ? C3 C2 C7 118.9(3) . . ? C3 C2 C1 121.0(3) . . ? C7 C2 C1 120.1(3) . . ? C2 C3 C4 120.4(3) . . ? C2 C3 N1'' 126.8(5) . . ? C4 C3 N1'' 111.8(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? N1'' C3 H3 12.5 . . ? C7 N1' H1C 120.0 . . ? C7 N1' H1D 120.0 . . ? H1C N1' H1D 120.0 . . ? N1 C6 C7 115.5(4) . . ? N1 C6 C5 125.0(4) . . ? C7 C6 C5 119.4(3) . . ? N1 C6 H6 5.5 . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 N1 H1A 120.0 . . ? C6 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? N1' C7 C2 129.3(3) . . ? N1' C7 C6 109.0(3) . . ? C2 C7 C6 121.3(3) . . ? N1' C7 H7 12.3 . . ? C2 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C3 N1'' H1E 120.0 . . ? C3 N1'' H1F 120.0 . . ? H1E N1'' H1F 120.0 . . ? N2 C9 C10 124.1(3) . . ? N2 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? C9 C10 C11 120.9(3) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 115.4(3) . . ? C10 C11 C14 122.2(3) . . ? C12 C11 C14 122.3(3) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? N2 C13 C12 123.9(3) . . ? N2 C13 H13 118.0 . . ? C12 C13 H13 118.0 . . ? C11 C14 C15 112.6(3) . . ? C11 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? C11 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 112.7(3) . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C15 112.4(3) . . ? C17 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? C17 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C21 C17 C18 115.8(3) . . ? C21 C17 C16 121.8(3) . . ? C18 C17 C16 122.4(4) . . ? C19 C18 C17 120.2(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? N3 C19 C18 124.1(3) . . ? N3 C19 H19 117.9 . . ? C18 C19 H19 117.9 . . ? N3 C20 C21 124.1(3) . . ? N3 C20 H20 118.0 . . ? C21 C20 H20 118.0 . . ? C20 C21 C17 120.9(3) . . ? C20 C21 H21 119.5 . . ? C17 C21 H21 119.5 . . ? C9 N2 C13 115.2(3) . . ? C9 N2 Co1 117.7(2) . . ? C13 N2 Co1 126.3(2) . . ? C20 N3 C19 114.9(3) . . ? C20 N3 Co1 124.6(2) . 1_655 ? C19 N3 Co1 120.40(19) . 1_655 ? C1 O1 Co1 86.9(2) . . ? C1 O2 Co1 94.4(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.265 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.064 ################################################################