Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_chr03 _database_code_CSD 161550 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Brown, Angelica D.' 'Christou, George' 'Concolino, Thomas E.' 'Dimitrou, Katerina' 'Rheingold, Arnold' _publ_contact_author_name 'Prof George Christou' _publ_contact_author_address ; Prof George Christou Department of Chemistry Indiana University Bloomington IN 47405-4001 USA ; _publ_contact_author_email 'CHRISTOU@INDIANA.EDU' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H49 Cl3 Co4 N11 O27' _chemical_formula_weight 1650.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6330(2) _cell_length_b 14.1304(2) _cell_length_c 20.7165(2) _cell_angle_alpha 91.8195(6) _cell_angle_beta 95.8450(8) _cell_angle_gamma 110.1203(4) _cell_volume 3172.78(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1674 _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_type 'Empirical from DIFABS' _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18626 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10537 _reflns_number_gt 8985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10537 _refine_ls_number_parameters 910 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2279 _refine_ls_wR_factor_gt 0.2089 _refine_ls_goodness_of_fit_ref 1.750 _refine_ls_restrained_S_all 1.750 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.31865(6) -0.11872(5) 0.21024(3) 0.0250(2) Uani 1 1 d . . . Co2 Co 0.14593(6) -0.29928(5) 0.20537(3) 0.0251(2) Uani 1 1 d . . . Co3 Co 0.39406(6) -0.28597(5) 0.24394(3) 0.0252(2) Uani 1 1 d . . . Co4 Co 0.28102(6) -0.21688(5) 0.32966(3) 0.0261(2) Uani 1 1 d . . . Cl1 Cl -0.1068(2) -0.07514(16) 0.38145(10) 0.0680(6) Uani 1 1 d . . . Cl2 Cl -0.2622(3) 0.3138(3) 0.36447(15) 0.1087(10) Uani 1 1 d . . . Cl3 Cl -0.4126(2) 0.3185(2) 0.02695(10) 0.0765(6) Uani 1 1 d . . . O1 O 0.4112(3) -0.1555(3) 0.27977(17) 0.0288(8) Uani 1 1 d . . . O2 O 0.2394(3) -0.3353(3) 0.27466(17) 0.0291(8) Uani 1 1 d . . . O3 O 0.3015(3) -0.2484(3) 0.17591(17) 0.0273(8) Uani 1 1 d . . . O4 O 0.1898(3) -0.1807(3) 0.25951(17) 0.0273(8) Uani 1 1 d . . . O5 O 0.2167(3) -0.0976(3) 0.13637(17) 0.0283(8) Uani 1 1 d . . . O6 O 0.0649(3) -0.2504(3) 0.13320(17) 0.0295(8) Uani 1 1 d . . . O7 O -0.0327(4) -0.0162(3) -0.1620(2) 0.0458(11) Uani 1 1 d . . . O8 O -0.1983(5) -0.1446(4) -0.1543(2) 0.0625(15) Uani 1 1 d . . . O9 O 0.4784(3) -0.3214(3) 0.32035(18) 0.0319(8) Uani 1 1 d . . . O10 O 0.3835(3) -0.2600(3) 0.39267(17) 0.0313(8) Uani 1 1 d . . . O11 O 0.7834(5) -0.4659(4) 0.5812(2) 0.0611(13) Uani 1 1 d . . . O12 O 0.6851(5) -0.4112(5) 0.6463(2) 0.0667(15) Uani 1 1 d . . . O16 O -0.0313(8) -0.0896(6) 0.3369(4) 0.122(3) Uani 1 1 d . . . O15 O -0.0514(13) -0.0538(18) 0.4406(5) 0.282(11) Uani 1 1 d . . . O14 O -0.1302(17) 0.0089(11) 0.3764(8) 0.243(9) Uani 1 1 d . . . O13 O -0.2124(11) -0.1514(9) 0.3779(8) 0.236(8) Uani 1 1 d . . . O24 O -0.3857(5) 0.3429(4) 0.0950(3) 0.0673(15) Uani 1 1 d . . . O23 O -0.3297(7) 0.2730(6) 0.0057(3) 0.091(2) Uani 1 1 d . . . O22 O -0.5359(8) 0.2488(11) 0.0165(5) 0.180(6) Uani 1 1 d . . . O21 O -0.4108(16) 0.3998(11) -0.0094(6) 0.228(8) Uani 1 1 d . . . O20 O -0.3419(8) 0.3677(7) 0.3586(4) 0.118(3) Uani 1 1 d . . . O19 O -0.2618(8) 0.2762(9) 0.2956(4) 0.140(4) Uani 1 1 d . . . O18 O -0.3131(13) 0.2299(10) 0.3972(7) 0.200(6) Uani 1 1 d . . . O17 O -0.1374(11) 0.3587(12) 0.3817(8) 0.226(7) Uani 1 1 d . . . O25 O -0.1421(7) -0.1822(6) 0.5611(4) 0.110(2) Uani 1 1 d . . . O26 O -0.3434(10) 0.0362(11) 0.3181(6) 0.198(6) Uani 1 1 d . . . O27 O -0.3200(8) 0.5932(7) 0.0113(5) 0.129(3) Uani 1 1 d . . . N1 N -0.0943(5) -0.0885(4) -0.1344(2) 0.0385(11) Uani 1 1 d . . . N2 N 0.7075(5) -0.4271(4) 0.5917(2) 0.0427(12) Uani 1 1 d . . . N3 N 0.0899(4) -0.4249(3) 0.1513(2) 0.0301(10) Uani 1 1 d . . . N4 N -0.0157(4) -0.3573(3) 0.2335(2) 0.0310(10) Uani 1 1 d . . . N5 N 0.3407(4) 0.0163(3) 0.2446(2) 0.0285(10) Uani 1 1 d . . . N6 N 0.4539(4) -0.0465(3) 0.1621(2) 0.0293(10) Uani 1 1 d . . . N7 N 0.3819(4) -0.4155(3) 0.2050(2) 0.0281(9) Uani 1 1 d . . . N8 N 0.5517(4) -0.2411(3) 0.2094(2) 0.0293(10) Uani 1 1 d . . . N9 N 0.1531(4) -0.2738(4) 0.3841(2) 0.0375(11) Uani 1 1 d . . . N10 N 0.3191(5) -0.0975(4) 0.3896(2) 0.0395(12) Uani 1 1 d . . . N11 N -0.0697(13) 0.2058(9) 0.1829(6) 0.136(4) Uani 1 1 d . . . C1 C 0.1192(5) -0.1657(4) 0.1110(2) 0.0251(11) Uani 1 1 d . . . C2 C 0.0627(5) -0.1462(4) 0.0467(2) 0.0258(11) Uani 1 1 d . . . C3 C 0.1316(5) -0.0671(4) 0.0125(3) 0.0301(11) Uani 1 1 d . . . H3A H 0.2126 -0.0257 0.0304 0.036 Uiso 1 1 calc R . . C4 C 0.0819(5) -0.0481(4) -0.0484(3) 0.0321(12) Uani 1 1 d . . . H4A H 0.1285 0.0044 -0.0727 0.039 Uiso 1 1 calc R . . C5 C -0.0387(5) -0.1096(4) -0.0716(2) 0.0317(12) Uani 1 1 d . . . C6 C -0.1070(5) -0.1893(4) -0.0381(3) 0.0342(12) Uani 1 1 d . . . H6A H -0.1885 -0.2301 -0.0555 0.041 Uiso 1 1 calc R . . C7 C -0.0551(5) -0.2083(4) 0.0206(3) 0.0319(12) Uani 1 1 d . . . H7A H -0.1000 -0.2640 0.0432 0.038 Uiso 1 1 calc R . . C8 C 0.4555(5) -0.3051(4) 0.3775(2) 0.0261(11) Uani 1 1 d . . . C9 C 0.5207(5) -0.3390(4) 0.4335(2) 0.0269(11) Uani 1 1 d . . . C10 C 0.6053(5) -0.3850(4) 0.4216(3) 0.0363(13) Uani 1 1 d . . . H10A H 0.6210 -0.3956 0.3784 0.044 Uiso 1 1 calc R . . C11 C 0.6667(5) -0.4154(4) 0.4733(3) 0.0368(13) Uani 1 1 d . . . H11A H 0.7251 -0.4468 0.4662 0.044 Uiso 1 1 calc R . . C12 C 0.6402(5) -0.3984(4) 0.5360(3) 0.0352(13) Uani 1 1 d . . . C13 C 0.5549(6) -0.3561(4) 0.5483(3) 0.0364(13) Uani 1 1 d . . . H13A H 0.5379 -0.3466 0.5914 0.044 Uiso 1 1 calc R . . C14 C 0.4932(6) -0.3269(4) 0.4955(3) 0.0366(13) Uani 1 1 d . . . H14A H 0.4320 -0.2985 0.5026 0.044 Uiso 1 1 calc R . . C15 C 0.1478(5) -0.4462(4) 0.1021(3) 0.0343(12) Uani 1 1 d . . . H15A H 0.2251 -0.3994 0.0942 0.041 Uiso 1 1 calc R . . C16 C 0.0951(6) -0.5358(5) 0.0634(3) 0.0483(16) Uani 1 1 d . . . H16A H 0.1362 -0.5499 0.0290 0.058 Uiso 1 1 calc R . . C17 C -0.0148(6) -0.6031(5) 0.0747(4) 0.0561(19) Uani 1 1 d . . . H17A H -0.0501 -0.6648 0.0485 0.067 Uiso 1 1 calc R . . C18 C -0.0756(6) -0.5825(5) 0.1239(4) 0.0491(16) Uani 1 1 d . . . H18A H -0.1528 -0.6293 0.1321 0.059 Uiso 1 1 calc R . . C19 C -0.0217(5) -0.4919(4) 0.1614(3) 0.0354(13) Uani 1 1 d . . . C20 C -0.0823(5) -0.4518(4) 0.2093(3) 0.0337(12) Uani 1 1 d . . . C21 C -0.2005(6) -0.5016(5) 0.2256(3) 0.0513(17) Uani 1 1 d . . . H21A H -0.2463 -0.5689 0.2089 0.062 Uiso 1 1 calc R . . C22 C -0.2498(6) -0.4503(6) 0.2668(4) 0.0564(19) Uani 1 1 d . . . H22A H -0.3290 -0.4831 0.2799 0.068 Uiso 1 1 calc R . . C23 C -0.1838(6) -0.3525(5) 0.2883(3) 0.0460(15) Uani 1 1 d . . . H23A H -0.2184 -0.3160 0.3149 0.055 Uiso 1 1 calc R . . C24 C -0.0666(5) -0.3069(4) 0.2716(3) 0.0352(13) Uani 1 1 d . . . H24A H -0.0208 -0.2389 0.2871 0.042 Uiso 1 1 calc R . . C25 C 0.2682(6) 0.0414(5) 0.2822(3) 0.0383(13) Uani 1 1 d . . . H25A H 0.1986 -0.0105 0.2944 0.046 Uiso 1 1 calc R . . C26 C 0.2901(6) 0.1413(5) 0.3044(3) 0.0451(15) Uani 1 1 d . . . H26A H 0.2390 0.1571 0.3327 0.054 Uiso 1 1 calc R . . C27 C 0.3888(6) 0.2162(5) 0.2838(3) 0.0472(16) Uani 1 1 d . . . H27A H 0.4056 0.2848 0.2977 0.057 Uiso 1 1 calc R . . C28 C 0.4630(6) 0.1918(4) 0.2431(3) 0.0437(15) Uani 1 1 d . . . H28A H 0.5305 0.2430 0.2286 0.052 Uiso 1 1 calc R . . C29 C 0.4370(5) 0.0911(4) 0.2240(3) 0.0329(12) Uani 1 1 d . . . C30 C 0.5001(5) 0.0544(4) 0.1765(3) 0.0342(13) Uani 1 1 d . . . C31 C 0.5954(6) 0.1151(5) 0.1442(4) 0.0489(16) Uani 1 1 d . . . H31A H 0.6309 0.1856 0.1557 0.059 Uiso 1 1 calc R . . C32 C 0.6373(6) 0.0724(5) 0.0959(4) 0.0545(18) Uani 1 1 d . . . H32A H 0.7046 0.1124 0.0749 0.065 Uiso 1 1 calc R . . C33 C 0.5808(6) -0.0302(5) 0.0778(3) 0.0440(15) Uani 1 1 d . . . H33A H 0.6051 -0.0598 0.0423 0.053 Uiso 1 1 calc R . . C34 C 0.4891(5) -0.0886(5) 0.1120(3) 0.0349(12) Uani 1 1 d . . . H34A H 0.4506 -0.1588 0.1000 0.042 Uiso 1 1 calc R . . C35 C 0.2974(5) -0.5051(4) 0.2143(3) 0.0351(13) Uani 1 1 d . . . H35A H 0.2336 -0.5066 0.2399 0.042 Uiso 1 1 calc R . . C36 C 0.3005(6) -0.5960(5) 0.1876(3) 0.0431(15) Uani 1 1 d . . . H36A H 0.2402 -0.6587 0.1948 0.052 Uiso 1 1 calc R . . C37 C 0.3921(6) -0.5924(4) 0.1508(3) 0.0421(14) Uani 1 1 d . . . H37A H 0.3948 -0.6534 0.1316 0.051 Uiso 1 1 calc R . . C38 C 0.4815(6) -0.5013(4) 0.1409(3) 0.0397(14) Uani 1 1 d . . . H38A H 0.5450 -0.4994 0.1150 0.048 Uiso 1 1 calc R . . C39 C 0.4762(5) -0.4132(4) 0.1696(3) 0.0324(12) Uani 1 1 d . . . C40 C 0.5721(5) -0.3124(4) 0.1713(3) 0.0331(12) Uani 1 1 d . . . C41 C 0.6827(6) -0.2906(5) 0.1447(3) 0.0445(15) Uani 1 1 d . . . H41A H 0.6968 -0.3399 0.1175 0.053 Uiso 1 1 calc R . . C42 C 0.7718(6) -0.1955(5) 0.1589(3) 0.0479(16) Uani 1 1 d . . . H42A H 0.8478 -0.1792 0.1411 0.057 Uiso 1 1 calc R . . C43 C 0.7510(6) -0.1252(5) 0.1982(3) 0.0462(15) Uani 1 1 d . . . H43A H 0.8123 -0.0602 0.2082 0.055 Uiso 1 1 calc R . . C44 C 0.6407(5) -0.1494(4) 0.2230(3) 0.0392(14) Uani 1 1 d . . . H44A H 0.6263 -0.1006 0.2505 0.047 Uiso 1 1 calc R . . C45 C 0.0834(5) -0.3734(5) 0.3830(4) 0.0512(18) Uani 1 1 d . . . H45A H 0.0889 -0.4192 0.3498 0.061 Uiso 1 1 calc R . . C46 C 0.0051(7) -0.4088(8) 0.4291(5) 0.081(3) Uani 1 1 d . . . H46A H -0.0424 -0.4786 0.4289 0.097 Uiso 1 1 calc R . . C47 C -0.0021(8) -0.3386(11) 0.4762(4) 0.093(4) Uani 1 1 d . . . H47A H -0.0581 -0.3611 0.5075 0.112 Uiso 1 1 calc R . . C48 C 0.0687(8) -0.2393(9) 0.4783(4) 0.079(3) Uani 1 1 d . . . H48A H 0.0642 -0.1922 0.5109 0.095 Uiso 1 1 calc R . . C49 C 0.1461(6) -0.2098(5) 0.4321(3) 0.0441(15) Uani 1 1 d . . . C50 C 0.2375(7) -0.1089(6) 0.4341(3) 0.0510(17) Uani 1 1 d . . . C51 C 0.2591(11) -0.0253(8) 0.4800(4) 0.082(3) Uani 1 1 d . . . H51A H 0.2024 -0.0278 0.5103 0.099 Uiso 1 1 calc R . . C52 C 0.3625(13) 0.0582(7) 0.4797(6) 0.100(4) Uani 1 1 d . . . H52A H 0.3767 0.1138 0.5102 0.120 Uiso 1 1 calc R . . C53 C 0.4431(12) 0.0642(6) 0.4384(5) 0.089(4) Uani 1 1 d . . . H53A H 0.5163 0.1218 0.4406 0.106 Uiso 1 1 calc R . . C54 C 0.4201(7) -0.0133(5) 0.3924(3) 0.058(2) Uani 1 1 d . . . H54A H 0.4766 -0.0078 0.3615 0.070 Uiso 1 1 calc R . . C55 C 0.0014(12) 0.2364(15) 0.3050(7) 0.151(7) Uani 1 1 d . . . C56 C -0.0388(10) 0.2183(8) 0.2374(6) 0.084(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0322(4) 0.0295(4) 0.0153(4) 0.0015(3) 0.0009(3) 0.0139(3) Co2 0.0311(4) 0.0271(4) 0.0173(4) 0.0020(3) 0.0018(3) 0.0109(3) Co3 0.0341(4) 0.0276(4) 0.0165(4) 0.0012(3) 0.0007(3) 0.0148(3) Co4 0.0345(4) 0.0295(4) 0.0160(4) 0.0033(3) 0.0026(3) 0.0135(3) Cl1 0.0914(14) 0.0734(12) 0.0446(11) -0.0111(9) -0.0096(10) 0.0418(11) Cl2 0.0858(18) 0.158(3) 0.0792(19) 0.0166(19) -0.0075(14) 0.0428(19) Cl3 0.1086(17) 0.1039(16) 0.0429(11) 0.0103(10) 0.0065(11) 0.0701(15) O1 0.0350(19) 0.038(2) 0.0181(18) 0.0037(15) 0.0040(15) 0.0175(16) O2 0.0370(19) 0.0365(19) 0.0168(18) 0.0004(15) 0.0037(15) 0.0167(16) O3 0.0384(19) 0.0304(18) 0.0160(18) 0.0013(14) 0.0018(14) 0.0161(15) O4 0.0320(18) 0.0317(18) 0.0198(18) 0.0023(14) 0.0026(14) 0.0133(15) O5 0.0346(19) 0.0280(18) 0.0202(19) 0.0031(15) 0.0012(15) 0.0088(16) O6 0.0364(19) 0.0331(19) 0.0189(18) 0.0051(15) 0.0017(15) 0.0123(16) O7 0.060(3) 0.048(2) 0.027(2) 0.0137(19) -0.0019(19) 0.017(2) O8 0.062(3) 0.057(3) 0.047(3) 0.014(2) -0.030(2) 0.003(2) O9 0.041(2) 0.038(2) 0.022(2) 0.0041(16) 0.0020(16) 0.0198(17) O10 0.043(2) 0.041(2) 0.0157(18) 0.0055(15) 0.0022(15) 0.0222(17) O11 0.066(3) 0.079(3) 0.051(3) 0.016(3) -0.002(2) 0.043(3) O12 0.096(4) 0.097(4) 0.024(3) 0.011(3) -0.005(2) 0.058(3) O16 0.158(7) 0.111(6) 0.109(6) -0.013(5) 0.064(6) 0.050(5) O15 0.211(13) 0.62(3) 0.079(7) -0.094(13) -0.049(8) 0.248(19) O14 0.40(2) 0.209(13) 0.272(16) 0.114(12) 0.184(16) 0.250(16) O13 0.163(10) 0.153(10) 0.310(18) -0.104(11) 0.114(11) -0.061(8) O24 0.082(4) 0.073(3) 0.055(3) -0.017(3) 0.004(3) 0.040(3) O23 0.116(5) 0.113(5) 0.065(4) -0.018(4) 0.023(4) 0.066(4) O22 0.097(6) 0.319(16) 0.134(8) -0.093(10) -0.042(6) 0.110(8) O21 0.39(2) 0.238(14) 0.188(12) 0.156(11) 0.123(13) 0.238(15) O20 0.111(6) 0.119(6) 0.131(7) 0.004(5) 0.044(5) 0.040(5) O19 0.107(6) 0.219(11) 0.093(6) -0.025(6) -0.014(5) 0.065(7) O18 0.242(14) 0.187(12) 0.221(14) 0.104(11) 0.105(11) 0.107(11) O17 0.134(9) 0.285(17) 0.241(15) -0.122(13) -0.073(10) 0.088(10) O25 0.110(5) 0.090(5) 0.121(7) -0.009(5) 0.029(5) 0.020(4) O26 0.162(9) 0.301(16) 0.151(10) -0.121(10) -0.060(8) 0.142(11) O27 0.125(7) 0.125(7) 0.124(7) -0.012(6) 0.016(6) 0.030(5) N1 0.048(3) 0.038(3) 0.026(3) 0.002(2) -0.008(2) 0.014(2) N2 0.048(3) 0.051(3) 0.029(3) 0.010(2) -0.004(2) 0.018(2) N3 0.041(2) 0.033(2) 0.020(2) 0.0002(18) -0.0040(19) 0.021(2) N4 0.038(2) 0.037(2) 0.019(2) 0.0067(19) 0.0004(18) 0.015(2) N5 0.034(2) 0.030(2) 0.022(2) 0.0002(18) -0.0074(18) 0.0152(19) N6 0.034(2) 0.031(2) 0.022(2) 0.0031(18) 0.0004(18) 0.0104(19) N7 0.030(2) 0.034(2) 0.023(2) 0.0084(18) 0.0015(18) 0.0151(19) N8 0.034(2) 0.031(2) 0.026(2) 0.0025(18) -0.0010(18) 0.0160(19) N9 0.040(3) 0.052(3) 0.026(3) 0.017(2) 0.002(2) 0.022(2) N10 0.052(3) 0.042(3) 0.026(3) 0.000(2) -0.009(2) 0.022(2) N11 0.220(14) 0.130(9) 0.095(8) -0.001(7) 0.030(9) 0.106(9) C1 0.033(3) 0.029(3) 0.017(2) 0.000(2) 0.001(2) 0.017(2) C2 0.031(3) 0.027(2) 0.020(3) 0.000(2) -0.001(2) 0.013(2) C3 0.034(3) 0.035(3) 0.024(3) 0.000(2) 0.001(2) 0.015(2) C4 0.039(3) 0.038(3) 0.020(3) 0.005(2) 0.002(2) 0.015(2) C5 0.044(3) 0.038(3) 0.016(3) -0.003(2) -0.005(2) 0.021(2) C6 0.040(3) 0.027(3) 0.028(3) -0.005(2) -0.009(2) 0.006(2) C7 0.046(3) 0.028(3) 0.022(3) 0.001(2) 0.002(2) 0.013(2) C8 0.032(3) 0.025(2) 0.020(3) 0.005(2) 0.002(2) 0.009(2) C9 0.033(3) 0.027(2) 0.021(3) 0.003(2) -0.002(2) 0.012(2) C10 0.038(3) 0.039(3) 0.030(3) 0.004(2) -0.003(2) 0.013(2) C11 0.035(3) 0.045(3) 0.034(3) 0.004(3) 0.004(2) 0.019(3) C12 0.043(3) 0.029(3) 0.027(3) 0.003(2) -0.010(2) 0.007(2) C13 0.051(3) 0.044(3) 0.019(3) 0.000(2) -0.002(2) 0.024(3) C14 0.050(3) 0.038(3) 0.026(3) 0.001(2) 0.001(2) 0.022(3) C15 0.039(3) 0.037(3) 0.025(3) -0.002(2) -0.001(2) 0.012(2) C16 0.054(4) 0.055(4) 0.041(4) -0.008(3) 0.007(3) 0.026(3) C17 0.052(4) 0.047(4) 0.064(5) -0.021(3) -0.001(3) 0.015(3) C18 0.047(4) 0.033(3) 0.060(4) -0.009(3) 0.006(3) 0.005(3) C19 0.042(3) 0.028(3) 0.035(3) 0.002(2) 0.003(2) 0.010(2) C20 0.038(3) 0.036(3) 0.027(3) 0.004(2) 0.002(2) 0.012(2) C21 0.043(3) 0.048(4) 0.049(4) -0.004(3) 0.008(3) -0.001(3) C22 0.041(3) 0.065(4) 0.051(4) 0.002(4) 0.016(3) 0.000(3) C23 0.043(3) 0.064(4) 0.031(3) 0.002(3) 0.012(3) 0.017(3) C24 0.041(3) 0.038(3) 0.028(3) 0.001(2) 0.005(2) 0.015(3) C25 0.050(3) 0.047(3) 0.021(3) 0.003(2) 0.002(2) 0.022(3) C26 0.068(4) 0.045(3) 0.029(3) -0.009(3) -0.006(3) 0.033(3) C27 0.064(4) 0.038(3) 0.036(4) -0.013(3) -0.018(3) 0.020(3) C28 0.053(4) 0.033(3) 0.036(3) -0.004(3) -0.010(3) 0.008(3) C29 0.036(3) 0.036(3) 0.024(3) -0.003(2) -0.010(2) 0.013(2) C30 0.033(3) 0.039(3) 0.030(3) 0.007(2) -0.007(2) 0.013(2) C31 0.047(3) 0.037(3) 0.059(4) 0.009(3) 0.011(3) 0.009(3) C32 0.050(4) 0.052(4) 0.066(5) 0.022(3) 0.030(3) 0.016(3) C33 0.045(3) 0.057(4) 0.040(4) 0.018(3) 0.018(3) 0.026(3) C34 0.042(3) 0.044(3) 0.021(3) 0.009(2) 0.005(2) 0.019(3) C35 0.041(3) 0.039(3) 0.026(3) 0.006(2) 0.001(2) 0.016(2) C36 0.046(3) 0.035(3) 0.045(4) 0.004(3) -0.004(3) 0.011(3) C37 0.055(4) 0.032(3) 0.041(4) -0.003(3) -0.006(3) 0.020(3) C38 0.048(3) 0.040(3) 0.039(3) -0.002(3) 0.006(3) 0.026(3) C39 0.041(3) 0.040(3) 0.022(3) 0.004(2) 0.004(2) 0.021(2) C40 0.037(3) 0.039(3) 0.025(3) 0.005(2) 0.003(2) 0.015(2) C41 0.047(3) 0.049(4) 0.044(4) 0.004(3) 0.010(3) 0.024(3) C42 0.035(3) 0.057(4) 0.049(4) 0.010(3) 0.009(3) 0.010(3) C43 0.041(3) 0.042(3) 0.048(4) 0.005(3) -0.001(3) 0.008(3) C44 0.043(3) 0.039(3) 0.035(3) -0.002(3) -0.010(3) 0.018(3) C45 0.036(3) 0.057(4) 0.053(4) 0.029(3) -0.007(3) 0.008(3) C46 0.050(4) 0.100(7) 0.070(6) 0.058(6) -0.007(4) -0.004(4) C47 0.062(5) 0.183(12) 0.037(5) 0.036(6) 0.017(4) 0.040(7) C48 0.071(5) 0.131(9) 0.053(5) 0.023(5) 0.033(4) 0.048(6) C49 0.054(4) 0.074(4) 0.021(3) 0.009(3) 0.006(3) 0.044(4) C50 0.074(4) 0.066(4) 0.025(3) -0.011(3) -0.009(3) 0.045(4) C51 0.127(8) 0.105(8) 0.043(5) -0.023(5) -0.005(5) 0.083(7) C52 0.170(12) 0.056(6) 0.068(7) -0.032(5) -0.055(7) 0.056(7) C53 0.157(10) 0.045(4) 0.048(5) -0.012(4) -0.045(6) 0.033(5) C54 0.081(5) 0.038(3) 0.036(4) 0.003(3) -0.028(3) 0.006(3) C55 0.103(9) 0.28(2) 0.100(10) 0.009(12) -0.015(8) 0.109(12) C56 0.092(7) 0.093(7) 0.082(7) 0.013(6) 0.020(6) 0.049(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 1.876(3) . ? Co1 O3 1.882(4) . ? Co1 O1 1.903(4) . ? Co1 O5 1.934(4) . ? Co1 N5 1.938(4) . ? Co1 N6 1.947(4) . ? Co1 Co2 2.6406(9) . ? Co1 Co3 2.8720(10) . ? Co1 Co4 2.8735(9) . ? Co2 O4 1.871(4) . ? Co2 O3 1.877(4) . ? Co2 O2 1.900(4) . ? Co2 N4 1.934(5) . ? Co2 N3 1.939(4) . ? Co2 O6 1.956(4) . ? Co2 Co3 2.8553(10) . ? Co2 Co4 2.8605(9) . ? Co3 O2 1.878(4) . ? Co3 O3 1.886(4) . ? Co3 O1 1.902(4) . ? Co3 N7 1.931(5) . ? Co3 N8 1.942(5) . ? Co3 O9 1.948(4) . ? Co3 Co4 2.6618(10) . ? Co4 O2 1.882(4) . ? Co4 O1 1.894(4) . ? Co4 O4 1.899(4) . ? Co4 N9 1.926(5) . ? Co4 O10 1.931(4) . ? Co4 N10 1.956(5) . ? Cl1 O15 1.299(9) . ? Cl1 O14 1.311(9) . ? Cl1 O13 1.320(10) . ? Cl1 O16 1.393(7) . ? Cl2 O18 1.366(11) . ? Cl2 O17 1.372(11) . ? Cl2 O20 1.386(9) . ? Cl2 O19 1.508(9) . ? Cl3 O21 1.389(9) . ? Cl3 O24 1.417(6) . ? Cl3 O22 1.423(11) . ? Cl3 O23 1.427(6) . ? O5 C1 1.258(6) . ? O6 C1 1.272(6) . ? O7 N1 1.225(6) . ? O8 N1 1.216(6) . ? O9 C8 1.272(6) . ? O10 C8 1.271(6) . ? O11 N2 1.222(7) . ? O12 N2 1.217(7) . ? N1 C5 1.478(7) . ? N2 C12 1.474(7) . ? N3 C15 1.358(7) . ? N3 C19 1.359(7) . ? N4 C20 1.342(7) . ? N4 C24 1.353(7) . ? N5 C25 1.328(7) . ? N5 C29 1.366(7) . ? N6 C34 1.346(7) . ? N6 C30 1.351(7) . ? N7 C35 1.342(7) . ? N7 C39 1.373(7) . ? N8 C44 1.350(7) . ? N8 C40 1.359(7) . ? N9 C49 1.350(8) . ? N9 C45 1.360(8) . ? N10 C54 1.349(9) . ? N10 C50 1.363(9) . ? N11 C56 1.139(14) . ? C1 C2 1.500(7) . ? C2 C7 1.390(7) . ? C2 C3 1.395(7) . ? C3 C4 1.405(7) . ? C4 C5 1.397(8) . ? C5 C6 1.388(8) . ? C6 C7 1.378(8) . ? C8 C9 1.501(7) . ? C9 C14 1.375(8) . ? C9 C10 1.389(8) . ? C10 C11 1.387(8) . ? C11 C12 1.398(8) . ? C12 C13 1.363(9) . ? C13 C14 1.397(8) . ? C15 C16 1.386(9) . ? C16 C17 1.353(10) . ? C17 C18 1.378(10) . ? C18 C19 1.385(8) . ? C19 C20 1.479(8) . ? C20 C21 1.394(8) . ? C21 C22 1.388(10) . ? C22 C23 1.363(10) . ? C23 C24 1.379(8) . ? C25 C26 1.398(9) . ? C26 C27 1.383(10) . ? C27 C28 1.383(10) . ? C28 C29 1.383(8) . ? C29 C30 1.468(8) . ? C30 C31 1.395(8) . ? C31 C32 1.366(10) . ? C32 C33 1.390(10) . ? C33 C34 1.380(8) . ? C35 C36 1.396(9) . ? C36 C37 1.360(9) . ? C37 C38 1.385(9) . ? C38 C39 1.387(8) . ? C39 C40 1.473(8) . ? C40 C41 1.391(8) . ? C41 C42 1.386(9) . ? C42 C43 1.366(10) . ? C43 C44 1.368(9) . ? C45 C46 1.373(11) . ? C46 C47 1.399(16) . ? C47 C48 1.358(16) . ? C48 C49 1.358(10) . ? C49 C50 1.452(10) . ? C50 C51 1.427(10) . ? C51 C52 1.366(16) . ? C52 C53 1.314(16) . ? C53 C54 1.365(12) . ? C55 C56 1.415(17) . ? 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 O4 Co1 O3 87.97(15) . . ? O4 Co1 O1 81.42(15) . . ? O3 Co1 O1 81.39(15) . . ? O4 Co1 O5 96.51(15) . . ? O3 Co1 O5 92.34(15) . . ? O1 Co1 O5 173.44(15) . . ? O4 Co1 N5 93.59(17) . . ? O3 Co1 N5 178.40(18) . . ? O1 Co1 N5 98.44(17) . . ? O5 Co1 N5 87.87(16) . . ? O4 Co1 N6 176.48(17) . . ? O3 Co1 N6 95.52(17) . . ? O1 Co1 N6 98.59(17) . . ? O5 Co1 N6 83.86(16) . . ? N5 Co1 N6 82.93(19) . . ? O4 Co1 Co2 45.12(11) . . ? O3 Co1 Co2 45.30(11) . . ? O1 Co1 Co2 89.73(11) . . ? O5 Co1 Co2 84.46(10) . . ? N5 Co1 Co2 136.31(14) . . ? N6 Co1 Co2 138.36(13) . . ? O4 Co1 Co3 83.34(11) . . ? O3 Co1 Co3 40.40(11) . . ? O1 Co1 Co3 40.99(11) . . ? O5 Co1 Co3 132.73(11) . . ? N5 Co1 Co3 139.40(13) . . ? N6 Co1 Co3 99.00(14) . . ? Co2 Co1 Co3 62.22(2) . . ? O4 Co1 Co4 40.73(11) . . ? O3 Co1 Co4 83.32(11) . . ? O1 Co1 Co4 40.70(11) . . ? O5 Co1 Co4 136.96(11) . . ? N5 Co1 Co4 97.61(13) . . ? N6 Co1 Co4 139.14(13) . . ? Co2 Co1 Co4 62.33(2) . . ? Co3 Co1 Co4 55.20(2) . . ? O4 Co2 O3 88.27(15) . . ? O4 Co2 O2 81.62(16) . . ? O3 Co2 O2 81.37(15) . . ? O4 Co2 N4 94.27(18) . . ? O3 Co2 N4 177.45(18) . . ? O2 Co2 N4 98.74(17) . . ? O4 Co2 N3 176.21(17) . . ? O3 Co2 N3 95.51(18) . . ? O2 Co2 N3 99.07(17) . . ? N4 Co2 N3 81.95(19) . . ? O4 Co2 O6 95.30(15) . . ? O3 Co2 O6 93.58(15) . . ? O2 Co2 O6 174.14(15) . . ? N4 Co2 O6 86.43(17) . . ? N3 Co2 O6 84.32(16) . . ? O4 Co2 Co1 45.29(11) . . ? O3 Co2 Co1 45.45(11) . . ? O2 Co2 Co1 89.89(11) . . ? N4 Co2 Co1 137.05(14) . . ? N3 Co2 Co1 138.28(14) . . ? O6 Co2 Co1 84.42(11) . . ? O4 Co2 Co3 83.90(11) . . ? O3 Co2 Co3 40.77(11) . . ? O2 Co2 Co3 40.61(11) . . ? N4 Co2 Co3 139.25(13) . . ? N3 Co2 Co3 99.07(13) . . ? O6 Co2 Co3 134.32(11) . . ? Co1 Co2 Co3 62.87(2) . . ? O4 Co2 Co4 41.01(11) . . ? O3 Co2 Co4 83.77(11) . . ? O2 Co2 Co4 40.62(11) . . ? N4 Co2 Co4 97.99(13) . . ? N3 Co2 Co4 139.50(13) . . ? O6 Co2 Co4 136.17(11) . . ? Co1 Co2 Co4 62.83(2) . . ? Co3 Co2 Co4 55.51(2) . . ? O2 Co3 O3 81.72(15) . . ? O2 Co3 O1 88.09(15) . . ? O3 Co3 O1 81.29(15) . . ? O2 Co3 N7 94.25(17) . . ? O3 Co3 N7 98.05(16) . . ? O1 Co3 N7 177.46(17) . . ? O2 Co3 N8 177.16(17) . . ? O3 Co3 N8 97.90(17) . . ? O1 Co3 N8 94.65(17) . . ? N7 Co3 N8 83.00(18) . . ? O2 Co3 O9 93.32(15) . . ? O3 Co3 O9 173.92(15) . . ? O1 Co3 O9 95.08(15) . . ? N7 Co3 O9 85.78(17) . . ? N8 Co3 O9 87.22(17) . . ? O2 Co3 Co4 44.99(11) . . ? O3 Co3 Co4 89.41(11) . . ? O1 Co3 Co4 45.35(11) . . ? N7 Co3 Co4 137.17(13) . . ? N8 Co3 Co4 137.85(13) . . ? O9 Co3 Co4 84.59(11) . . ? O2 Co3 Co2 41.21(11) . . ? O3 Co3 Co2 40.52(11) . . ? O1 Co3 Co2 83.52(11) . . ? N7 Co3 Co2 97.59(13) . . ? N8 Co3 Co2 138.31(13) . . ? O9 Co3 Co2 134.47(11) . . ? Co4 Co3 Co2 62.34(2) . . ? O2 Co3 Co1 83.56(12) . . ? O3 Co3 Co1 40.29(11) . . ? O1 Co3 Co1 41.00(11) . . ? N7 Co3 Co1 138.27(13) . . ? N8 Co3 Co1 97.99(13) . . ? O9 Co3 Co1 135.93(11) . . ? Co4 Co3 Co1 62.43(2) . . ? Co2 Co3 Co1 54.91(2) . . ? O2 Co4 O1 88.21(15) . . ? O2 Co4 O4 81.38(16) . . ? O1 Co4 O4 81.08(15) . . ? O2 Co4 N9 94.69(19) . . ? O1 Co4 N9 176.93(19) . . ? O4 Co4 N9 100.35(17) . . ? O2 Co4 O10 93.32(16) . . ? O1 Co4 O10 93.80(15) . . ? O4 Co4 O10 172.70(15) . . ? N9 Co4 O10 85.02(17) . . ? O2 Co4 N10 177.31(19) . . ? O1 Co4 N10 94.42(19) . . ? O4 Co4 N10 99.58(18) . . ? N9 Co4 N10 82.7(2) . . ? O10 Co4 N10 85.94(18) . . ? O2 Co4 Co3 44.86(11) . . ? O1 Co4 Co3 45.61(11) . . ? O4 Co4 Co3 89.03(11) . . ? N9 Co4 Co3 136.87(16) . . ? O10 Co4 Co3 83.67(11) . . ? N10 Co4 Co3 137.49(16) . . ? O2 Co4 Co2 41.10(11) . . ? O1 Co4 Co2 83.52(11) . . ? O4 Co4 Co2 40.28(11) . . ? N9 Co4 Co2 99.34(15) . . ? O10 Co4 Co2 134.29(12) . . ? N10 Co4 Co2 139.76(14) . . ? Co3 Co4 Co2 62.15(2) . . ? O2 Co4 Co1 83.45(11) . . ? O1 Co4 Co1 40.93(11) . . ? O4 Co4 Co1 40.15(10) . . ? N9 Co4 Co1 140.40(14) . . ? O10 Co4 Co1 134.56(11) . . ? N10 Co4 Co1 98.92(15) . . ? Co3 Co4 Co1 62.37(2) . . ? Co2 Co4 Co1 54.84(2) . . ? O15 Cl1 O14 96.3(12) . . ? O15 Cl1 O13 111.9(12) . . ? O14 Cl1 O13 108.6(11) . . ? O15 Cl1 O16 112.9(6) . . ? O14 Cl1 O16 114.1(7) . . ? O13 Cl1 O16 112.2(7) . . ? O18 Cl2 O17 112.8(10) . . ? O18 Cl2 O20 109.2(7) . . ? O17 Cl2 O20 123.1(8) . . ? O18 Cl2 O19 106.1(8) . . ? O17 Cl2 O19 99.2(7) . . ? O20 Cl2 O19 104.1(6) . . ? O21 Cl3 O24 114.3(7) . . ? O21 Cl3 O22 106.2(9) . . ? O24 Cl3 O22 106.1(5) . . ? O21 Cl3 O23 110.3(6) . . ? O24 Cl3 O23 109.5(4) . . ? O22 Cl3 O23 110.4(6) . . ? Co4 O1 Co3 89.04(15) . . ? Co4 O1 Co1 98.37(16) . . ? Co3 O1 Co1 98.00(16) . . ? Co3 O2 Co4 90.14(16) . . ? Co3 O2 Co2 98.18(16) . . ? Co4 O2 Co2 98.27(17) . . ? Co2 O3 Co1 89.26(15) . . ? Co2 O3 Co3 98.70(16) . . ? Co1 O3 Co3 99.31(16) . . ? Co2 O4 Co1 89.60(15) . . ? Co2 O4 Co4 98.71(17) . . ? Co1 O4 Co4 99.12(16) . . ? C1 O5 Co1 122.4(3) . . ? C1 O6 Co2 120.8(3) . . ? C8 O9 Co3 121.8(3) . . ? C8 O10 Co4 123.7(3) . . ? O8 N1 O7 125.3(5) . . ? O8 N1 C5 116.9(5) . . ? O7 N1 C5 117.8(5) . . ? O12 N2 O11 122.8(5) . . ? O12 N2 C12 118.6(5) . . ? O11 N2 C12 118.6(5) . . ? C15 N3 C19 119.0(5) . . ? C15 N3 Co2 125.3(4) . . ? C19 N3 Co2 115.5(4) . . ? C20 N4 C24 119.5(5) . . ? C20 N4 Co2 116.0(4) . . ? C24 N4 Co2 124.3(4) . . ? C25 N5 C29 118.9(5) . . ? C25 N5 Co1 126.3(4) . . ? C29 N5 Co1 114.6(4) . . ? C34 N6 C30 120.8(5) . . ? C34 N6 Co1 124.2(4) . . ? C30 N6 Co1 114.3(4) . . ? C35 N7 C39 119.1(5) . . ? C35 N7 Co3 125.9(4) . . ? C39 N7 Co3 114.7(3) . . ? C44 N8 C40 119.8(5) . . ? C44 N8 Co3 125.5(4) . . ? C40 N8 Co3 114.7(4) . . ? C49 N9 C45 119.0(6) . . ? C49 N9 Co4 115.2(4) . . ? C45 N9 Co4 125.1(5) . . ? C54 N10 C50 120.7(6) . . ? C54 N10 Co4 125.6(5) . . ? C50 N10 Co4 113.5(4) . . ? O5 C1 O6 127.0(5) . . ? O5 C1 C2 116.6(4) . . ? O6 C1 C2 116.3(4) . . ? C7 C2 C3 120.4(5) . . ? C7 C2 C1 120.5(5) . . ? C3 C2 C1 119.1(4) . . ? C2 C3 C4 120.4(5) . . ? C5 C4 C3 117.4(5) . . ? C6 C5 C4 122.4(5) . . ? C6 C5 N1 119.3(5) . . ? C4 C5 N1 118.3(5) . . ? C7 C6 C5 119.2(5) . . ? C6 C7 C2 120.1(5) . . ? O10 C8 O9 126.0(5) . . ? O10 C8 C9 115.6(4) . . ? O9 C8 C9 118.3(5) . . ? C14 C9 C10 120.8(5) . . ? C14 C9 C8 119.6(5) . . ? C10 C9 C8 119.5(5) . . ? C11 C10 C9 119.7(5) . . ? C10 C11 C12 118.1(5) . . ? C13 C12 C11 122.9(5) . . ? C13 C12 N2 118.2(5) . . ? C11 C12 N2 118.9(5) . . ? C12 C13 C14 118.1(5) . . ? C9 C14 C13 120.3(5) . . ? N3 C15 C16 120.6(5) . . ? C17 C16 C15 120.0(6) . . ? C16 C17 C18 120.3(6) . . ? C17 C18 C19 118.5(6) . . ? N3 C19 C18 121.5(6) . . ? N3 C19 C20 112.9(5) . . ? C18 C19 C20 125.2(5) . . ? N4 C20 C21 121.4(6) . . ? N4 C20 C19 113.4(5) . . ? C21 C20 C19 125.0(5) . . ? C22 C21 C20 118.4(6) . . ? C23 C22 C21 119.6(6) . . ? C22 C23 C24 119.9(6) . . ? N4 C24 C23 121.1(6) . . ? N5 C25 C26 122.6(6) . . ? C27 C26 C25 117.7(6) . . ? C28 C27 C26 120.4(6) . . ? C27 C28 C29 118.6(6) . . ? N5 C29 C28 121.6(6) . . ? N5 C29 C30 113.4(5) . . ? C28 C29 C30 124.8(6) . . ? N6 C30 C31 120.0(6) . . ? N6 C30 C29 114.5(5) . . ? C31 C30 C29 125.4(5) . . ? C32 C31 C30 119.5(6) . . ? C31 C32 C33 119.4(6) . . ? C34 C33 C32 119.5(6) . . ? N6 C34 C33 120.3(6) . . ? N7 C35 C36 122.1(6) . . ? C37 C36 C35 118.2(6) . . ? C36 C37 C38 121.2(6) . . ? C37 C38 C39 118.5(6) . . ? N7 C39 C38 120.8(5) . . ? N7 C39 C40 113.6(5) . . ? C38 C39 C40 125.4(5) . . ? N8 C40 C41 120.4(5) . . ? N8 C40 C39 113.6(5) . . ? C41 C40 C39 125.4(5) . . ? C42 C41 C40 118.6(6) . . ? C43 C42 C41 120.4(6) . . ? C42 C43 C44 119.2(6) . . ? N8 C44 C43 121.6(6) . . ? N9 C45 C46 120.9(8) . . ? C45 C46 C47 117.7(9) . . ? C48 C47 C46 121.8(8) . . ? C47 C48 C49 117.4(9) . . ? N9 C49 C48 123.2(8) . . ? N9 C49 C50 114.1(5) . . ? C48 C49 C50 122.5(7) . . ? N10 C50 C51 117.1(8) . . ? N10 C50 C49 114.3(5) . . ? C51 C50 C49 128.4(8) . . ? C52 C51 C50 119.1(9) . . ? C53 C52 C51 122.1(9) . . ? C52 C53 C54 119.1(10) . . ? N10 C54 C53 121.7(9) . . ? N11 C56 C55 178.6(16) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.478 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.128