# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email j.w.leeland@sms.ed.ac.uk _publ_contact_author_name 'James Leeland' _publ_author_name J.Love data_jl9040 _database_code_depnum_ccdc_archive 'CCDC 795242' #TrackingRef 'combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'James Leeland' _exptl_crystal_recrystallization_method 'Diffusion of hexane into C6D6 solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H40 Co N4 O5' _chemical_formula_sum 'C35 H40 Co N4 O5' _chemical_formula_weight 655.64 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2650(6) _cell_length_b 23.9628(9) _cell_length_c 18.4445(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.501(2) _cell_angle_gamma 90.00 _cell_volume 6359.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7689 _cell_measurement_theta_min 2.212 _cell_measurement_theta_max 26.381 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.7454 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '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 72807 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.42 _reflns_number_total 12987 _reflns_number_gt 11287 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^ > 2\s(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^)+(0.0427P)^2^+26.3590P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12987 _refine_ls_number_parameters 815 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1837 _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_restrained_S_all 1.226 _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 C101 C 0.3244(3) 0.24936(19) 0.1558(3) 0.0220(9) Uani 1 1 d . . . H101 H 0.2858 0.2216 0.1241 0.026 Uiso 1 1 calc R . . C102 C 0.3263(3) 0.30396(19) 0.1293(3) 0.0219(9) Uani 1 1 d . . . C103 C 0.2806(3) 0.33682(19) 0.0651(3) 0.0238(10) Uani 1 1 d . . . H103 H 0.2383 0.3241 0.0175 0.029 Uiso 1 1 calc R . . C104 C 0.3087(3) 0.39158(19) 0.0842(3) 0.0268(10) Uani 1 1 d . . . H104 H 0.2889 0.4233 0.0519 0.032 Uiso 1 1 calc R . . C105 C 0.3718(3) 0.39160(18) 0.1599(3) 0.0221(9) Uani 1 1 d . . . C106 C 0.4197(3) 0.44138(18) 0.2081(3) 0.0226(9) Uani 1 1 d . . . C107 C 0.3449(3) 0.4766(2) 0.2281(3) 0.0285(11) Uani 1 1 d . . . H10A H 0.3730 0.5126 0.2504 0.034 Uiso 1 1 calc R . . H10B H 0.2935 0.4848 0.1799 0.034 Uiso 1 1 calc R . . C108 C 0.3048(4) 0.4484(3) 0.2841(3) 0.0382(13) Uani 1 1 d . . . H10E H 0.2765 0.4128 0.2625 0.057 Uiso 1 1 calc R . . H10F H 0.2576 0.4727 0.2928 0.057 Uiso 1 1 calc R . . H10G H 0.3547 0.4417 0.3330 0.057 Uiso 1 1 calc R . . C109 C 0.4616(4) 0.47865(19) 0.1599(3) 0.0285(11) Uani 1 1 d . . . H10C H 0.4106 0.4925 0.1146 0.034 Uiso 1 1 calc R . . H10D H 0.4911 0.5115 0.1911 0.034 Uiso 1 1 calc R . . C110 C 0.5330(4) 0.4496(2) 0.1323(4) 0.0418(13) Uani 1 1 d . . . H11A H 0.5831 0.4348 0.1766 0.063 Uiso 1 1 calc R . . H11B H 0.5588 0.4763 0.1046 0.063 Uiso 1 1 calc R . . H11C H 0.5032 0.4188 0.0978 0.063 Uiso 1 1 calc R . . C111 C 0.4939(3) 0.42519(18) 0.2823(3) 0.0224(9) Uani 1 1 d . . . C112 C 0.5569(3) 0.46034(19) 0.3369(3) 0.0247(10) Uani 1 1 d . . . H112 H 0.5634 0.4994 0.3320 0.030 Uiso 1 1 calc R . . C113 C 0.6075(3) 0.42758(18) 0.3989(3) 0.0227(9) Uani 1 1 d . . . H113 H 0.6551 0.4399 0.4440 0.027 Uiso 1 1 calc R . . C114 C 0.5749(3) 0.37349(18) 0.3823(2) 0.0195(9) Uani 1 1 d . . . C115 C 0.5924(3) 0.31956(18) 0.4150(3) 0.0199(9) Uani 1 1 d . . . H115 H 0.6372 0.3135 0.4644 0.024 Uiso 1 1 calc R . . C116 C 0.5622(3) 0.22296(18) 0.4047(3) 0.0200(9) Uani 1 1 d . . . C117 C 0.5751(3) 0.18106(18) 0.3575(3) 0.0219(9) Uani 1 1 d . . . H117 H 0.5762 0.1904 0.3077 0.026 Uiso 1 1 calc R . . C118 C 0.5864(3) 0.12593(19) 0.3811(3) 0.0258(10) Uani 1 1 d . . . H118 H 0.5927 0.0975 0.3473 0.031 Uiso 1 1 calc R . . C119 C 0.5883(3) 0.11285(19) 0.4547(3) 0.0281(11) Uani 1 1 d . . . H119 H 0.5963 0.0752 0.4717 0.034 Uiso 1 1 calc R . . C120 C 0.5784(4) 0.15439(19) 0.5036(3) 0.0282(11) Uani 1 1 d . . . H120 H 0.5811 0.1451 0.5544 0.034 Uiso 1 1 calc R . . C121 C 0.5647(3) 0.20946(18) 0.4790(3) 0.0212(9) Uani 1 1 d . . . C122 C 0.5575(4) 0.2403(2) 0.6002(3) 0.0287(10) Uani 1 1 d . . . H12A H 0.6200 0.2255 0.6291 0.034 Uiso 1 1 calc R . . H12B H 0.5104 0.2123 0.6020 0.034 Uiso 1 1 calc R . . C123 C 0.5411(4) 0.2948(2) 0.6340(3) 0.0318(11) Uani 1 1 d . . . H12E H 0.4833 0.3123 0.6001 0.038 Uiso 1 1 calc R . . H12F H 0.5349 0.2885 0.6851 0.038 Uiso 1 1 calc R . . C124 C 0.6079(4) 0.3863(2) 0.6607(3) 0.0384(13) Uani 1 1 d . . . H12M H 0.6701 0.4039 0.6807 0.046 Uiso 1 1 calc R . . H12N H 0.5807 0.3868 0.7024 0.046 Uiso 1 1 calc R . . C125 C 0.5473(4) 0.4203(2) 0.5940(3) 0.0344(12) Uani 1 1 d . . . H12O H 0.5590 0.4605 0.6050 0.041 Uiso 1 1 calc R . . H12P H 0.5623 0.4113 0.5471 0.041 Uiso 1 1 calc R . . C126 C 0.3916(4) 0.4271(2) 0.5094(3) 0.0339(12) Uani 1 1 d . . . H12G H 0.4171 0.4175 0.4681 0.041 Uiso 1 1 calc R . . H12H H 0.3845 0.4681 0.5102 0.041 Uiso 1 1 calc R . . C127 C 0.2990(4) 0.3992(2) 0.4945(3) 0.0337(12) Uani 1 1 d . . . H12K H 0.2748 0.4093 0.5363 0.040 Uiso 1 1 calc R . . H12L H 0.2549 0.4138 0.4458 0.040 Uiso 1 1 calc R . . C128 C 0.3202(4) 0.3224(2) 0.4227(3) 0.0376(13) Uani 1 1 d . . . H12I H 0.3813 0.3369 0.4236 0.045 Uiso 1 1 calc R . . H12J H 0.2719 0.3373 0.3764 0.045 Uiso 1 1 calc R . . C129 C 0.3202(3) 0.25956(19) 0.4198(3) 0.0252(10) Uani 1 1 d . . . H12C H 0.3663 0.2438 0.4667 0.030 Uiso 1 1 calc R . . H12D H 0.2580 0.2444 0.4145 0.030 Uiso 1 1 calc R . . C130 C 0.3476(3) 0.19320(18) 0.3310(3) 0.0220(9) Uani 1 1 d . . . C131 C 0.3361(3) 0.1468(2) 0.3709(3) 0.0265(10) Uani 1 1 d . . . H131 H 0.3271 0.1505 0.4193 0.032 Uiso 1 1 calc R . . C132 C 0.3378(3) 0.09440(19) 0.3390(3) 0.0285(11) Uani 1 1 d . . . H132 H 0.3297 0.0620 0.3658 0.034 Uiso 1 1 calc R . . C133 C 0.3508(3) 0.08861(19) 0.2695(3) 0.0275(10) Uani 1 1 d . . . H133 H 0.3503 0.0525 0.2482 0.033 Uiso 1 1 calc R . . C134 C 0.3649(3) 0.13552(19) 0.2297(3) 0.0246(10) Uani 1 1 d . . . H134 H 0.3752 0.1315 0.1819 0.030 Uiso 1 1 calc R . . C135 C 0.3637(3) 0.18776(18) 0.2608(3) 0.0217(9) Uani 1 1 d . . . C201 C 0.8084(3) 0.26126(19) 0.7329(3) 0.0234(9) Uani 1 1 d . . . H201 H 0.7702 0.2908 0.7394 0.028 Uiso 1 1 calc R . . C202 C 0.8035(3) 0.2070(2) 0.7618(3) 0.0258(10) Uani 1 1 d . . . C203 C 0.7480(4) 0.1780(2) 0.7951(3) 0.0327(11) Uani 1 1 d . . . H203 H 0.7018 0.1932 0.8134 0.039 Uiso 1 1 calc R . . C204 C 0.7737(4) 0.1218(2) 0.7961(3) 0.0309(11) Uani 1 1 d . . . H204 H 0.7480 0.0917 0.8158 0.037 Uiso 1 1 calc R . . C205 C 0.8443(4) 0.1178(2) 0.7628(3) 0.0266(10) Uani 1 1 d . . . C206 C 0.8927(3) 0.06601(19) 0.7483(3) 0.0261(10) Uani 1 1 d . . . C207 C 0.8185(4) 0.0280(2) 0.6914(3) 0.0308(11) Uani 1 1 d . . . H20A H 0.8477 -0.0083 0.6874 0.037 Uiso 1 1 calc R . . H20B H 0.7682 0.0207 0.7129 0.037 Uiso 1 1 calc R . . C208 C 0.7759(4) 0.0521(2) 0.6113(3) 0.0394(13) Uani 1 1 d . . . H20E H 0.7429 0.0867 0.6141 0.059 Uiso 1 1 calc R . . H20F H 0.7320 0.0252 0.5784 0.059 Uiso 1 1 calc R . . H20G H 0.8251 0.0600 0.5896 0.059 Uiso 1 1 calc R . . C209 C 0.9340(4) 0.0333(2) 0.8242(3) 0.0359(12) Uani 1 1 d . . . H20C H 0.8829 0.0227 0.8433 0.043 Uiso 1 1 calc R . . H20D H 0.9623 -0.0015 0.8134 0.043 Uiso 1 1 calc R . . C210 C 1.0067(5) 0.0652(3) 0.8868(4) 0.0562(18) Uani 1 1 d . . . H21A H 1.0568 0.0768 0.8681 0.084 Uiso 1 1 calc R . . H21B H 1.0321 0.0411 0.9320 0.084 Uiso 1 1 calc R . . H21C H 0.9782 0.0982 0.9010 0.084 Uiso 1 1 calc R . . C211 C 0.9676(3) 0.07767(19) 0.7134(3) 0.0250(10) Uani 1 1 d . . . C212 C 1.0268(4) 0.0393(2) 0.6954(3) 0.0314(11) Uani 1 1 d . . . H212 H 1.0287 0.0002 0.7044 0.038 Uiso 1 1 calc R . . C213 C 1.0820(4) 0.0688(2) 0.6620(3) 0.0309(11) Uani 1 1 d . . . H213 H 1.1286 0.0539 0.6440 0.037 Uiso 1 1 calc R . . C214 C 1.0555(3) 0.12490(19) 0.6602(3) 0.0245(10) Uani 1 1 d . . . C215 C 1.0819(3) 0.1769(2) 0.6381(3) 0.0245(10) Uani 1 1 d . . . H215 H 1.1296 0.1800 0.6159 0.029 Uiso 1 1 calc R . . C216 C 1.0669(3) 0.27454(18) 0.6332(3) 0.0223(9) Uani 1 1 d . . . C217 C 1.0889(3) 0.3150(2) 0.6908(3) 0.0274(10) Uani 1 1 d . . . H217 H 1.0847 0.3062 0.7397 0.033 Uiso 1 1 calc R . . C218 C 1.1166(4) 0.3678(2) 0.6777(3) 0.0331(12) Uani 1 1 d . . . H218 H 1.1323 0.3948 0.7177 0.040 Uiso 1 1 calc R . . C219 C 1.1216(4) 0.3810(2) 0.6071(3) 0.0295(11) Uani 1 1 d . . . H219 H 1.1394 0.4176 0.5979 0.035 Uiso 1 1 calc R . . C220 C 1.1009(3) 0.3415(2) 0.5487(3) 0.0272(10) Uani 1 1 d . . . H220 H 1.1052 0.3512 0.5001 0.033 Uiso 1 1 calc R . . C221 C 1.0740(3) 0.28815(19) 0.5610(3) 0.0230(9) Uani 1 1 d . . . C222 C 1.0495(4) 0.2615(2) 0.4305(3) 0.0270(10) Uani 1 1 d . . . H22A H 1.1096 0.2778 0.4317 0.032 Uiso 1 1 calc R . . H22B H 0.9999 0.2894 0.4084 0.032 Uiso 1 1 calc R . . C223 C 1.0297(3) 0.2090(2) 0.3831(3) 0.0283(10) Uani 1 1 d . . . H22O H 0.9794 0.1876 0.3930 0.034 Uiso 1 1 calc R . . H22P H 1.0098 0.2183 0.3277 0.034 Uiso 1 1 calc R . . C224 C 1.1031(4) 0.1198(2) 0.3810(3) 0.0306(11) Uani 1 1 d . . . H22E H 1.1654 0.1042 0.3876 0.037 Uiso 1 1 calc R . . H22F H 1.0662 0.1181 0.3256 0.037 Uiso 1 1 calc R . . C225 C 1.0568(4) 0.0840(2) 0.4247(3) 0.0346(12) Uani 1 1 d . . . H22G H 1.0758 0.0445 0.4238 0.041 Uiso 1 1 calc R . . H22H H 1.0752 0.0963 0.4789 0.041 Uiso 1 1 calc R . . C226 C 0.9064(4) 0.0714(2) 0.4345(3) 0.0317(11) Uani 1 1 d . . . H22I H 0.9357 0.0840 0.4884 0.038 Uiso 1 1 calc R . . H22J H 0.9019 0.0302 0.4341 0.038 Uiso 1 1 calc R . . C227 C 0.8116(4) 0.0969(2) 0.4004(3) 0.0344(12) Uani 1 1 d . . . H22C H 0.7842 0.0844 0.3463 0.041 Uiso 1 1 calc R . . H22D H 0.7713 0.0829 0.4288 0.041 Uiso 1 1 calc R . . C228 C 0.8254(4) 0.1773(2) 0.4771(3) 0.0316(11) Uani 1 1 d . . . H22K H 0.8860 0.1644 0.5130 0.038 Uiso 1 1 calc R . . H22L H 0.7757 0.1633 0.4956 0.038 Uiso 1 1 calc R . . C229 C 0.8233(3) 0.2403(2) 0.4744(3) 0.0258(10) Uani 1 1 d . . . H22M H 0.8742 0.2552 0.4580 0.031 Uiso 1 1 calc R . . H22N H 0.7631 0.2540 0.4388 0.031 Uiso 1 1 calc R . . C230 C 0.8460(3) 0.31030(19) 0.5735(3) 0.0249(10) Uani 1 1 d . . . C231 C 0.8401(3) 0.3555(2) 0.5261(3) 0.0290(11) Uani 1 1 d . . . H231 H 0.8298 0.3502 0.4728 0.035 Uiso 1 1 calc R . . C232 C 0.8495(4) 0.4091(2) 0.5568(3) 0.0336(12) Uani 1 1 d . . . H232 H 0.8467 0.4403 0.5244 0.040 Uiso 1 1 calc R . . C233 C 0.8629(4) 0.4175(2) 0.6339(3) 0.0353(12) Uani 1 1 d . . . H233 H 0.8677 0.4543 0.6541 0.042 Uiso 1 1 calc R . . C234 C 0.8692(3) 0.3716(2) 0.6822(3) 0.0283(10) Uani 1 1 d . . . H234 H 0.8784 0.3770 0.7352 0.034 Uiso 1 1 calc R . . C235 C 0.8620(3) 0.31813(18) 0.6524(3) 0.0227(9) Uani 1 1 d . . . N101 N 0.3779(3) 0.23832(15) 0.2259(2) 0.0206(8) Uani 1 1 d . . . N102 N 0.3818(3) 0.33889(15) 0.1864(2) 0.0202(8) Uani 1 1 d . . . N103 N 0.5051(3) 0.37307(14) 0.3108(2) 0.0193(8) Uani 1 1 d . . . N104 N 0.5442(2) 0.27834(15) 0.3744(2) 0.0180(7) Uani 1 1 d . . . N201 N 0.8681(3) 0.26878(15) 0.6970(2) 0.0214(8) Uani 1 1 d . . . N202 N 0.8615(3) 0.16973(16) 0.7423(2) 0.0232(8) Uani 1 1 d . . . N203 N 0.9854(3) 0.12892(15) 0.6917(2) 0.0232(8) Uani 1 1 d . . . N204 N 1.0370(3) 0.22099(16) 0.6498(2) 0.0212(8) Uani 1 1 d . . . O101 O 0.5499(2) 0.25219(13) 0.52249(18) 0.0262(7) Uani 1 1 d . . . O102 O 0.6185(3) 0.32986(15) 0.6409(2) 0.0391(9) Uani 1 1 d . . . O103 O 0.4530(2) 0.40818(14) 0.5818(2) 0.0312(8) Uani 1 1 d . . . O104 O 0.3020(3) 0.34007(14) 0.4897(2) 0.0326(8) Uani 1 1 d . . . O105 O 0.3447(2) 0.24744(13) 0.35344(19) 0.0272(7) Uani 1 1 d . . . O201 O 1.0529(2) 0.24624(13) 0.50699(19) 0.0283(7) Uani 1 1 d . . . O202 O 1.1133(2) 0.17660(14) 0.4044(2) 0.0305(8) Uani 1 1 d . . . O203 O 0.9599(2) 0.08916(14) 0.3891(2) 0.0309(8) Uani 1 1 d . . . O204 O 0.8121(2) 0.15665(14) 0.4023(2) 0.0307(8) Uani 1 1 d . . . O205 O 0.8353(3) 0.25558(13) 0.55146(19) 0.0297(8) Uani 1 1 d . . . Co1 Co 0.45087(4) 0.30418(2) 0.27721(3) 0.01795(15) Uani 1 1 d . . . Co2 Co 0.93744(4) 0.20018(2) 0.69220(4) 0.01963(15) 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 C101 0.025(2) 0.022(2) 0.020(2) -0.0079(18) 0.0092(19) -0.0044(18) C102 0.022(2) 0.025(2) 0.017(2) -0.0055(18) 0.0042(17) 0.0019(18) C103 0.029(2) 0.027(2) 0.015(2) -0.0016(18) 0.0066(19) 0.0006(19) C104 0.034(3) 0.021(2) 0.024(2) 0.0026(19) 0.008(2) 0.0037(19) C105 0.029(2) 0.015(2) 0.024(2) -0.0011(18) 0.011(2) 0.0003(18) C106 0.030(2) 0.014(2) 0.024(2) 0.0000(17) 0.009(2) 0.0007(18) C107 0.032(3) 0.024(2) 0.027(3) -0.003(2) 0.007(2) 0.010(2) C108 0.031(3) 0.049(3) 0.035(3) -0.002(3) 0.012(2) 0.004(2) C109 0.039(3) 0.018(2) 0.029(3) 0.0036(19) 0.011(2) -0.002(2) C110 0.050(3) 0.037(3) 0.044(3) -0.002(3) 0.024(3) -0.006(3) C111 0.027(2) 0.017(2) 0.024(2) -0.0010(18) 0.0099(19) 0.0004(18) C112 0.028(2) 0.019(2) 0.028(3) -0.0013(19) 0.011(2) -0.0042(18) C113 0.025(2) 0.019(2) 0.023(2) -0.0050(18) 0.0069(19) -0.0025(18) C114 0.022(2) 0.020(2) 0.017(2) -0.0021(17) 0.0068(17) 0.0005(17) C115 0.021(2) 0.019(2) 0.020(2) -0.0012(17) 0.0078(18) 0.0010(17) C116 0.019(2) 0.018(2) 0.020(2) -0.0013(17) 0.0015(17) -0.0011(17) C117 0.024(2) 0.020(2) 0.020(2) -0.0001(17) 0.0057(18) -0.0011(17) C118 0.030(2) 0.021(2) 0.024(2) -0.0025(19) 0.005(2) -0.0007(19) C119 0.037(3) 0.012(2) 0.034(3) 0.0026(19) 0.009(2) -0.0001(19) C120 0.040(3) 0.021(2) 0.023(2) 0.0050(19) 0.009(2) -0.001(2) C121 0.024(2) 0.018(2) 0.022(2) -0.0006(17) 0.0078(18) -0.0002(17) C122 0.035(3) 0.029(3) 0.023(2) 0.001(2) 0.011(2) -0.001(2) C123 0.043(3) 0.031(3) 0.025(3) -0.006(2) 0.015(2) -0.005(2) C124 0.043(3) 0.030(3) 0.039(3) -0.014(2) 0.010(3) -0.003(2) C125 0.043(3) 0.030(3) 0.035(3) -0.010(2) 0.019(2) -0.005(2) C126 0.053(3) 0.018(2) 0.031(3) -0.004(2) 0.013(2) 0.001(2) C127 0.039(3) 0.028(3) 0.036(3) -0.008(2) 0.015(2) 0.004(2) C128 0.057(4) 0.024(3) 0.040(3) -0.007(2) 0.028(3) -0.002(2) C129 0.031(2) 0.021(2) 0.028(3) -0.0036(19) 0.015(2) -0.0026(19) C130 0.023(2) 0.015(2) 0.029(2) -0.0042(18) 0.0096(19) -0.0040(17) C131 0.029(2) 0.025(2) 0.029(3) -0.002(2) 0.014(2) -0.0027(19) C132 0.028(2) 0.015(2) 0.042(3) 0.003(2) 0.012(2) -0.0029(18) C133 0.029(2) 0.014(2) 0.038(3) -0.0057(19) 0.009(2) -0.0037(18) C134 0.024(2) 0.024(2) 0.026(2) -0.0007(19) 0.0074(19) -0.0041(18) C135 0.019(2) 0.016(2) 0.029(2) 0.0003(18) 0.0061(18) -0.0012(17) C201 0.024(2) 0.023(2) 0.023(2) -0.0041(18) 0.0074(19) 0.0032(18) C202 0.026(2) 0.030(2) 0.022(2) -0.006(2) 0.0088(19) -0.001(2) C203 0.032(3) 0.039(3) 0.032(3) -0.003(2) 0.017(2) -0.004(2) C204 0.039(3) 0.030(3) 0.029(3) 0.002(2) 0.018(2) -0.008(2) C205 0.037(3) 0.023(2) 0.020(2) 0.0011(19) 0.010(2) -0.006(2) C206 0.032(3) 0.019(2) 0.025(2) 0.0025(19) 0.007(2) -0.0036(19) C207 0.035(3) 0.022(2) 0.033(3) 0.000(2) 0.008(2) -0.007(2) C208 0.037(3) 0.037(3) 0.037(3) -0.003(2) 0.003(2) -0.005(2) C209 0.049(3) 0.024(3) 0.031(3) 0.005(2) 0.007(2) -0.002(2) C210 0.073(5) 0.047(4) 0.031(3) 0.002(3) -0.006(3) -0.004(3) C211 0.027(2) 0.020(2) 0.025(2) -0.0023(18) 0.005(2) -0.0011(18) C212 0.036(3) 0.020(2) 0.036(3) -0.002(2) 0.009(2) 0.001(2) C213 0.032(3) 0.022(2) 0.040(3) -0.006(2) 0.014(2) 0.004(2) C214 0.025(2) 0.022(2) 0.028(3) -0.0046(19) 0.010(2) 0.0016(18) C215 0.024(2) 0.029(2) 0.023(2) -0.0020(19) 0.0109(19) 0.0007(19) C216 0.020(2) 0.021(2) 0.029(2) -0.0028(19) 0.0118(19) 0.0011(17) C217 0.031(3) 0.030(3) 0.026(3) -0.006(2) 0.017(2) -0.005(2) C218 0.040(3) 0.030(3) 0.034(3) -0.015(2) 0.020(2) -0.012(2) C219 0.037(3) 0.018(2) 0.037(3) -0.001(2) 0.018(2) -0.007(2) C220 0.031(3) 0.026(2) 0.028(3) 0.002(2) 0.014(2) 0.000(2) C221 0.022(2) 0.025(2) 0.021(2) -0.0038(18) 0.0063(18) 0.0024(18) C222 0.034(3) 0.026(2) 0.023(2) -0.0013(19) 0.012(2) 0.002(2) C223 0.027(2) 0.031(3) 0.025(3) -0.004(2) 0.006(2) 0.005(2) C224 0.030(3) 0.030(3) 0.031(3) -0.006(2) 0.009(2) 0.000(2) C225 0.034(3) 0.032(3) 0.034(3) -0.002(2) 0.007(2) 0.002(2) C226 0.044(3) 0.020(2) 0.039(3) -0.007(2) 0.024(2) -0.004(2) C227 0.037(3) 0.028(3) 0.043(3) -0.013(2) 0.020(2) -0.012(2) C228 0.042(3) 0.028(3) 0.025(3) -0.006(2) 0.013(2) -0.005(2) C229 0.029(2) 0.026(2) 0.024(2) -0.0025(19) 0.010(2) 0.0002(19) C230 0.026(2) 0.018(2) 0.033(3) 0.0010(19) 0.013(2) -0.0003(18) C231 0.030(3) 0.027(2) 0.027(3) 0.002(2) 0.006(2) -0.003(2) C232 0.033(3) 0.022(2) 0.042(3) 0.009(2) 0.009(2) -0.002(2) C233 0.033(3) 0.014(2) 0.052(3) -0.001(2) 0.006(2) -0.002(2) C234 0.028(2) 0.023(2) 0.032(3) -0.004(2) 0.009(2) -0.0004(19) C235 0.020(2) 0.016(2) 0.032(3) -0.0011(18) 0.0095(19) -0.0007(17) N101 0.0240(19) 0.0165(18) 0.0216(19) -0.0029(15) 0.0081(16) -0.0028(15) N102 0.0257(19) 0.0175(18) 0.0152(18) -0.0023(14) 0.0039(15) 0.0015(15) N103 0.0255(19) 0.0111(16) 0.023(2) -0.0034(14) 0.0101(16) -0.0028(14) N104 0.0213(18) 0.0170(18) 0.0171(18) -0.0004(14) 0.0082(15) -0.0003(14) N201 0.0230(19) 0.0175(18) 0.022(2) -0.0032(15) 0.0058(16) 0.0012(15) N202 0.025(2) 0.024(2) 0.021(2) -0.0001(16) 0.0090(16) -0.0002(16) N203 0.028(2) 0.0175(18) 0.025(2) 0.0002(15) 0.0108(17) -0.0001(16) N204 0.0205(18) 0.0229(19) 0.023(2) -0.0025(15) 0.0102(16) -0.0003(15) O101 0.0415(19) 0.0210(16) 0.0204(17) 0.0019(13) 0.0158(15) 0.0035(14) O102 0.036(2) 0.0263(19) 0.051(2) -0.0106(17) 0.0100(18) -0.0015(16) O103 0.0355(19) 0.0302(18) 0.0278(19) -0.0005(15) 0.0104(15) -0.0006(15) O104 0.043(2) 0.0274(18) 0.033(2) -0.0101(15) 0.0208(17) -0.0016(16) O105 0.043(2) 0.0137(15) 0.0310(19) -0.0051(13) 0.0207(16) -0.0031(14) O201 0.041(2) 0.0225(17) 0.0228(17) -0.0006(14) 0.0125(15) -0.0040(15) O202 0.0267(17) 0.0274(18) 0.036(2) -0.0098(15) 0.0091(15) -0.0009(14) O203 0.0321(19) 0.0321(19) 0.0314(19) -0.0024(15) 0.0143(16) -0.0008(15) O204 0.0333(19) 0.0295(18) 0.0295(19) -0.0057(15) 0.0108(15) -0.0017(15) O205 0.049(2) 0.0183(16) 0.0234(18) -0.0025(13) 0.0142(16) -0.0028(15) Co1 0.0240(3) 0.0118(3) 0.0173(3) -0.0006(2) 0.0059(2) -0.0008(2) Co2 0.0242(3) 0.0143(3) 0.0224(3) 0.0003(2) 0.0105(3) -0.0005(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C101 N101 1.305(6) . ? C101 C102 1.401(6) . ? C101 H101 0.9500 . ? C102 N102 1.390(6) . ? C102 C103 1.398(6) . ? C103 C104 1.389(7) . ? C103 H103 0.9500 . ? C104 C105 1.407(7) . ? C104 H104 0.9500 . ? C105 N102 1.345(6) . ? C105 C106 1.522(6) . ? C106 C111 1.508(6) . ? C106 C109 1.541(6) . ? C106 C107 1.559(6) . ? C107 C108 1.522(7) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10E 0.9800 . ? C108 H10F 0.9800 . ? C108 H10G 0.9800 . ? C109 C110 1.518(7) . ? C109 H10C 0.9900 . ? C109 H10D 0.9900 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C111 N103 1.343(6) . ? C111 C112 1.414(6) . ? C112 C113 1.390(7) . ? C112 H112 0.9500 . ? C113 C114 1.386(6) . ? C113 H113 0.9500 . ? C114 N103 1.391(6) . ? C114 C115 1.413(6) . ? C115 N104 1.307(6) . ? C115 H115 0.9500 . ? C116 C117 1.386(6) . ? C116 C121 1.396(6) . ? C116 N104 1.431(5) . ? C117 C118 1.384(6) . ? C117 H117 0.9500 . ? C118 C119 1.384(7) . ? C118 H118 0.9500 . ? C119 C120 1.386(7) . ? C119 H119 0.9500 . ? C120 C121 1.389(6) . ? C120 H120 0.9500 . ? C121 O101 1.365(5) . ? C122 O101 1.428(5) . ? C122 C123 1.503(7) . ? C122 H12A 0.9900 . ? C122 H12B 0.9900 . ? C123 O102 1.420(6) . ? C123 H12E 0.9900 . ? C123 H12F 0.9900 . ? C124 O102 1.424(6) . ? C124 C125 1.508(8) . ? C124 H12M 0.9900 . ? C124 H12N 0.9900 . ? C125 O103 1.410(6) . ? C125 H12O 0.9900 . ? C125 H12P 0.9900 . ? C126 O103 1.424(6) . ? C126 C127 1.504(7) . ? C126 H12G 0.9900 . ? C126 H12H 0.9900 . ? C127 O104 1.421(6) . ? C127 H12K 0.9900 . ? C127 H12L 0.9900 . ? C128 O104 1.418(6) . ? C128 C129 1.507(7) . ? C128 H12I 0.9900 . ? C128 H12J 0.9900 . ? C129 O105 1.425(5) . ? C129 H12C 0.9900 . ? C129 H12D 0.9900 . ? C130 O105 1.369(5) . ? C130 C131 1.378(6) . ? C130 C135 1.402(7) . ? C131 C132 1.391(7) . ? C131 H131 0.9500 . ? C132 C133 1.367(7) . ? C132 H132 0.9500 . ? C133 C134 1.398(7) . ? C133 H133 0.9500 . ? C134 C135 1.379(6) . ? C134 H134 0.9500 . ? C135 N101 1.422(6) . ? C201 N201 1.306(6) . ? C201 C202 1.417(7) . ? C201 H201 0.9500 . ? C202 N202 1.386(6) . ? C202 C203 1.387(7) . ? C203 C204 1.400(7) . ? C203 H203 0.9500 . ? C204 C205 1.411(7) . ? C204 H204 0.9500 . ? C205 N202 1.352(6) . ? C205 C206 1.513(7) . ? C206 C211 1.513(7) . ? C206 C209 1.543(7) . ? C206 C207 1.556(7) . ? C207 C208 1.516(7) . ? C207 H20A 0.9900 . ? C207 H20B 0.9900 . ? C208 H20E 0.9800 . ? C208 H20F 0.9800 . ? C208 H20G 0.9800 . ? C209 C210 1.514(8) . ? C209 H20C 0.9900 . ? C209 H20D 0.9900 . ? C210 H21A 0.9800 . ? C210 H21B 0.9800 . ? C210 H21C 0.9800 . ? C211 N203 1.347(6) . ? C211 C212 1.405(7) . ? C212 C213 1.393(7) . ? C212 H212 0.9500 . ? C213 C214 1.400(6) . ? C213 H213 0.9500 . ? C214 N203 1.381(6) . ? C214 C215 1.411(7) . ? C215 N204 1.315(6) . ? C215 H215 0.9500 . ? C216 C217 1.394(6) . ? C216 C221 1.410(6) . ? C216 N204 1.429(6) . ? C217 C218 1.378(7) . ? C217 H217 0.9500 . ? C218 C219 1.367(7) . ? C218 H218 0.9500 . ? C219 C220 1.388(7) . ? C219 H219 0.9500 . ? C220 C221 1.385(7) . ? C220 H220 0.9500 . ? C221 O201 1.375(5) . ? C222 O201 1.442(6) . ? C222 C223 1.504(6) . ? C222 H22A 0.9900 . ? C222 H22B 0.9900 . ? C223 O202 1.432(6) . ? C223 H22O 0.9900 . ? C223 H22P 0.9900 . ? C224 O202 1.420(6) . ? C224 C225 1.507(7) . ? C224 H22E 0.9900 . ? C224 H22F 0.9900 . ? C225 O203 1.410(6) . ? C225 H22G 0.9900 . ? C225 H22H 0.9900 . ? C226 O203 1.416(6) . ? C226 C227 1.502(8) . ? C226 H22I 0.9900 . ? C226 H22J 0.9900 . ? C227 O204 1.433(6) . ? C227 H22C 0.9900 . ? C227 H22D 0.9900 . ? C228 O204 1.415(6) . ? C228 C229 1.509(7) . ? C228 H22K 0.9900 . ? C228 H22L 0.9900 . ? C229 O205 1.419(5) . ? C229 H22M 0.9900 . ? C229 H22N 0.9900 . ? C230 O205 1.367(5) . ? C230 C231 1.378(7) . ? C230 C235 1.404(7) . ? C231 C232 1.391(7) . ? C231 H231 0.9500 . ? C232 C233 1.382(8) . ? C232 H232 0.9500 . ? C233 C234 1.398(7) . ? C233 H233 0.9500 . ? C234 C235 1.383(6) . ? C234 H234 0.9500 . ? C235 N201 1.426(6) . ? N101 Co1 1.981(4) . ? N102 Co1 1.852(4) . ? N103 Co1 1.858(3) . ? N104 Co1 1.981(4) . ? N201 Co2 1.973(4) . ? N202 Co2 1.856(4) . ? N203 Co2 1.859(4) . ? N204 Co2 1.991(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 N101 C101 C102 117.1(4) . . ? N101 C101 H101 121.4 . . ? C102 C101 H101 121.4 . . ? N102 C102 C103 108.0(4) . . ? N102 C102 C101 112.1(4) . . ? C103 C102 C101 139.4(4) . . ? C104 C103 C102 107.1(4) . . ? C104 C103 H103 126.5 . . ? C102 C103 H103 126.5 . . ? C103 C104 C105 107.6(4) . . ? C103 C104 H104 126.2 . . ? C105 C104 H104 126.2 . . ? N102 C105 C104 108.5(4) . . ? N102 C105 C106 123.3(4) . . ? C104 C105 C106 128.1(4) . . ? C111 C106 C105 113.5(4) . . ? C111 C106 C109 110.1(4) . . ? C105 C106 C109 109.1(4) . . ? C111 C106 C107 108.2(4) . . ? C105 C106 C107 108.4(4) . . ? C109 C106 C107 107.5(4) . . ? C108 C107 C106 114.4(4) . . ? C108 C107 H10A 108.7 . . ? C106 C107 H10A 108.7 . . ? C108 C107 H10B 108.7 . . ? C106 C107 H10B 108.7 . . ? H10A C107 H10B 107.6 . . ? C107 C108 H10E 109.5 . . ? C107 C108 H10F 109.5 . . ? H10E C108 H10F 109.5 . . ? C107 C108 H10G 109.5 . . ? H10E C108 H10G 109.5 . . ? H10F C108 H10G 109.5 . . ? C110 C109 C106 114.2(4) . . ? C110 C109 H10C 108.7 . . ? C106 C109 H10C 108.7 . . ? C110 C109 H10D 108.7 . . ? C106 C109 H10D 108.7 . . ? H10C C109 H10D 107.6 . . ? C109 C110 H11A 109.5 . . ? C109 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C109 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? N103 C111 C112 108.0(4) . . ? N103 C111 C106 123.6(4) . . ? C112 C111 C106 128.2(4) . . ? C113 C112 C111 107.9(4) . . ? C113 C112 H112 126.0 . . ? C111 C112 H112 126.0 . . ? C114 C113 C112 106.6(4) . . ? C114 C113 H113 126.7 . . ? C112 C113 H113 126.7 . . ? C113 C114 N103 108.7(4) . . ? C113 C114 C115 139.3(4) . . ? N103 C114 C115 112.0(4) . . ? N104 C115 C114 117.1(4) . . ? N104 C115 H115 121.4 . . ? C114 C115 H115 121.4 . . ? C117 C116 C121 119.1(4) . . ? C117 C116 N104 118.4(4) . . ? C121 C116 N104 122.5(4) . . ? C118 C117 C116 121.5(4) . . ? C118 C117 H117 119.3 . . ? C116 C117 H117 119.3 . . ? C119 C118 C117 119.0(4) . . ? C119 C118 H118 120.5 . . ? C117 C118 H118 120.5 . . ? C118 C119 C120 120.3(4) . . ? C118 C119 H119 119.8 . . ? C120 C119 H119 119.8 . . ? C119 C120 C121 120.4(4) . . ? C119 C120 H120 119.8 . . ? C121 C120 H120 119.8 . . ? O101 C121 C120 123.8(4) . . ? O101 C121 C116 116.6(4) . . ? C120 C121 C116 119.6(4) . . ? O101 C122 C123 105.8(4) . . ? O101 C122 H12A 110.6 . . ? C123 C122 H12A 110.6 . . ? O101 C122 H12B 110.6 . . ? C123 C122 H12B 110.6 . . ? H12A C122 H12B 108.7 . . ? O102 C123 C122 107.7(4) . . ? O102 C123 H12E 110.2 . . ? C122 C123 H12E 110.2 . . ? O102 C123 H12F 110.2 . . ? C122 C123 H12F 110.2 . . ? H12E C123 H12F 108.5 . . ? O102 C124 C125 113.2(4) . . ? O102 C124 H12M 108.9 . . ? C125 C124 H12M 108.9 . . ? O102 C124 H12N 108.9 . . ? C125 C124 H12N 108.9 . . ? H12M C124 H12N 107.7 . . ? O103 C125 C124 109.6(4) . . ? O103 C125 H12O 109.7 . . ? C124 C125 H12O 109.7 . . ? O103 C125 H12P 109.7 . . ? C124 C125 H12P 109.7 . . ? H12O C125 H12P 108.2 . . ? O103 C126 C127 108.3(4) . . ? O103 C126 H12G 110.0 . . ? C127 C126 H12G 110.0 . . ? O103 C126 H12H 110.0 . . ? C127 C126 H12H 110.0 . . ? H12G C126 H12H 108.4 . . ? O104 C127 C126 114.0(4) . . ? O104 C127 H12K 108.8 . . ? C126 C127 H12K 108.8 . . ? O104 C127 H12L 108.8 . . ? C126 C127 H12L 108.8 . . ? H12K C127 H12L 107.6 . . ? O104 C128 C129 109.4(4) . . ? O104 C128 H12I 109.8 . . ? C129 C128 H12I 109.8 . . ? O104 C128 H12J 109.8 . . ? C129 C128 H12J 109.8 . . ? H12I C128 H12J 108.2 . . ? O105 C129 C128 103.7(4) . . ? O105 C129 H12C 111.0 . . ? C128 C129 H12C 111.0 . . ? O105 C129 H12D 111.0 . . ? C128 C129 H12D 111.0 . . ? H12C C129 H12D 109.0 . . ? O105 C130 C131 125.6(4) . . ? O105 C130 C135 113.6(4) . . ? C131 C130 C135 120.8(4) . . ? C130 C131 C132 118.5(5) . . ? C130 C131 H131 120.7 . . ? C132 C131 H131 120.7 . . ? C133 C132 C131 121.2(4) . . ? C133 C132 H132 119.4 . . ? C131 C132 H132 119.4 . . ? C132 C133 C134 120.4(4) . . ? C132 C133 H133 119.8 . . ? C134 C133 H133 119.8 . . ? C135 C134 C133 119.1(4) . . ? C135 C134 H134 120.5 . . ? C133 C134 H134 120.5 . . ? C134 C135 C130 119.9(4) . . ? C134 C135 N101 124.0(4) . . ? C130 C135 N101 116.1(4) . . ? N201 C201 C202 116.8(4) . . ? N201 C201 H201 121.6 . . ? C202 C201 H201 121.6 . . ? N202 C202 C203 109.2(4) . . ? N202 C202 C201 112.0(4) . . ? C203 C202 C201 138.0(5) . . ? C202 C203 C204 106.1(4) . . ? C202 C203 H203 126.9 . . ? C204 C203 H203 126.9 . . ? C203 C204 C205 108.1(4) . . ? C203 C204 H204 126.0 . . ? C205 C204 H204 126.0 . . ? N202 C205 C204 107.9(4) . . ? N202 C205 C206 123.6(4) . . ? C204 C205 C206 128.5(4) . . ? C211 C206 C205 114.0(4) . . ? C211 C206 C209 109.9(4) . . ? C205 C206 C209 109.3(4) . . ? C211 C206 C207 107.8(4) . . ? C205 C206 C207 108.2(4) . . ? C209 C206 C207 107.4(4) . . ? C208 C207 C206 114.4(4) . . ? C208 C207 H20A 108.7 . . ? C206 C207 H20A 108.7 . . ? C208 C207 H20B 108.7 . . ? C206 C207 H20B 108.7 . . ? H20A C207 H20B 107.6 . . ? C207 C208 H20E 109.5 . . ? C207 C208 H20F 109.5 . . ? H20E C208 H20F 109.5 . . ? C207 C208 H20G 109.5 . . ? H20E C208 H20G 109.5 . . ? H20F C208 H20G 109.5 . . ? C210 C209 C206 114.2(4) . . ? C210 C209 H20C 108.7 . . ? C206 C209 H20C 108.7 . . ? C210 C209 H20D 108.7 . . ? C206 C209 H20D 108.7 . . ? H20C C209 H20D 107.6 . . ? C209 C210 H21A 109.5 . . ? C209 C210 H21B 109.5 . . ? H21A C210 H21B 109.5 . . ? C209 C210 H21C 109.5 . . ? H21A C210 H21C 109.5 . . ? H21B C210 H21C 109.5 . . ? N203 C211 C212 108.5(4) . . ? N203 C211 C206 123.4(4) . . ? C212 C211 C206 128.0(4) . . ? C213 C212 C211 107.7(4) . . ? C213 C212 H212 126.2 . . ? C211 C212 H212 126.2 . . ? C212 C213 C214 106.6(4) . . ? C212 C213 H213 126.7 . . ? C214 C213 H213 126.7 . . ? N203 C214 C213 108.4(4) . . ? N203 C214 C215 113.3(4) . . ? C213 C214 C215 138.3(5) . . ? N204 C215 C214 116.6(4) . . ? N204 C215 H215 121.7 . . ? C214 C215 H215 121.7 . . ? C217 C216 C221 118.9(4) . . ? C217 C216 N204 118.4(4) . . ? C221 C216 N204 122.7(4) . . ? C218 C217 C216 121.0(5) . . ? C218 C217 H217 119.5 . . ? C216 C217 H217 119.5 . . ? C219 C218 C217 119.8(5) . . ? C219 C218 H218 120.1 . . ? C217 C218 H218 120.1 . . ? C218 C219 C220 120.7(4) . . ? C218 C219 H219 119.7 . . ? C220 C219 H219 119.7 . . ? C221 C220 C219 120.4(5) . . ? C221 C220 H220 119.8 . . ? C219 C220 H220 119.8 . . ? O201 C221 C220 124.5(4) . . ? O201 C221 C216 116.3(4) . . ? C220 C221 C216 119.2(4) . . ? O201 C222 C223 106.9(4) . . ? O201 C222 H22A 110.3 . . ? C223 C222 H22A 110.3 . . ? O201 C222 H22B 110.3 . . ? C223 C222 H22B 110.3 . . ? H22A C222 H22B 108.6 . . ? O202 C223 C222 107.8(4) . . ? O202 C223 H22O 110.1 . . ? C222 C223 H22O 110.1 . . ? O202 C223 H22P 110.1 . . ? C222 C223 H22P 110.1 . . ? H22O C223 H22P 108.5 . . ? O202 C224 C225 114.0(4) . . ? O202 C224 H22E 108.8 . . ? C225 C224 H22E 108.8 . . ? O202 C224 H22F 108.8 . . ? C225 C224 H22F 108.8 . . ? H22E C224 H22F 107.6 . . ? O203 C225 C224 107.9(4) . . ? O203 C225 H22G 110.1 . . ? C224 C225 H22G 110.1 . . ? O203 C225 H22H 110.1 . . ? C224 C225 H22H 110.1 . . ? H22G C225 H22H 108.4 . . ? O203 C226 C227 107.2(4) . . ? O203 C226 H22I 110.3 . . ? C227 C226 H22I 110.3 . . ? O203 C226 H22J 110.3 . . ? C227 C226 H22J 110.3 . . ? H22I C226 H22J 108.5 . . ? O204 C227 C226 113.5(4) . . ? O204 C227 H22C 108.9 . . ? C226 C227 H22C 108.9 . . ? O204 C227 H22D 108.9 . . ? C226 C227 H22D 108.9 . . ? H22C C227 H22D 107.7 . . ? O204 C228 C229 108.9(4) . . ? O204 C228 H22K 109.9 . . ? C229 C228 H22K 109.9 . . ? O204 C228 H22L 109.9 . . ? C229 C228 H22L 109.9 . . ? H22K C228 H22L 108.3 . . ? O205 C229 C228 103.4(4) . . ? O205 C229 H22M 111.1 . . ? C228 C229 H22M 111.1 . . ? O205 C229 H22N 111.1 . . ? C228 C229 H22N 111.1 . . ? H22M C229 H22N 109.1 . . ? O205 C230 C231 126.1(5) . . ? O205 C230 C235 113.5(4) . . ? C231 C230 C235 120.3(4) . . ? C230 C231 C232 119.4(5) . . ? C230 C231 H231 120.3 . . ? C232 C231 H231 120.3 . . ? C233 C232 C231 120.9(5) . . ? C233 C232 H232 119.5 . . ? C231 C232 H232 119.5 . . ? C232 C233 C234 119.7(5) . . ? C232 C233 H233 120.2 . . ? C234 C233 H233 120.2 . . ? C235 C234 C233 119.7(5) . . ? C235 C234 H234 120.1 . . ? C233 C234 H234 120.1 . . ? C234 C235 C230 119.9(4) . . ? C234 C235 N201 123.8(4) . . ? C230 C235 N201 116.2(4) . . ? C101 N101 C135 118.8(4) . . ? C101 N101 Co1 112.2(3) . . ? C135 N101 Co1 127.4(3) . . ? C105 N102 C102 108.8(4) . . ? C105 N102 Co1 135.4(3) . . ? C102 N102 Co1 115.7(3) . . ? C111 N103 C114 108.7(4) . . ? C111 N103 Co1 135.3(3) . . ? C114 N103 Co1 115.9(3) . . ? C115 N104 C116 118.6(4) . . ? C115 N104 Co1 112.3(3) . . ? C116 N104 Co1 129.0(3) . . ? C201 N201 C235 119.0(4) . . ? C201 N201 Co2 112.5(3) . . ? C235 N201 Co2 126.7(3) . . ? C205 N202 C202 108.6(4) . . ? C205 N202 Co2 135.5(3) . . ? C202 N202 Co2 115.8(3) . . ? C211 N203 C214 108.9(4) . . ? C211 N203 Co2 135.8(3) . . ? C214 N203 Co2 115.3(3) . . ? C215 N204 C216 117.7(4) . . ? C215 N204 Co2 111.8(3) . . ? C216 N204 Co2 130.5(3) . . ? C121 O101 C122 117.8(4) . . ? C123 O102 C124 115.1(4) . . ? C125 O103 C126 113.7(4) . . ? C128 O104 C127 111.8(4) . . ? C130 O105 C129 119.9(4) . . ? C221 O201 C222 116.6(4) . . ? C224 O202 C223 116.0(4) . . ? C225 O203 C226 114.8(4) . . ? C228 O204 C227 111.9(4) . . ? C230 O205 C229 120.6(4) . . ? N102 Co1 N103 87.62(16) . . ? N102 Co1 N104 168.38(16) . . ? N103 Co1 N104 82.53(16) . . ? N102 Co1 N101 82.29(16) . . ? N103 Co1 N101 169.78(16) . . ? N104 Co1 N101 107.68(15) . . ? N202 Co2 N203 87.37(17) . . ? N202 Co2 N201 82.62(16) . . ? N203 Co2 N201 169.58(16) . . ? N202 Co2 N204 168.40(16) . . ? N203 Co2 N204 82.79(16) . . ? N201 Co2 N204 107.47(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 C101 C102 N102 -4.6(6) . . . . ? N101 C101 C102 C103 -174.2(5) . . . . ? N102 C102 C103 C104 -0.2(5) . . . . ? C101 C102 C103 C104 169.6(6) . . . . ? C102 C103 C104 C105 0.3(5) . . . . ? C103 C104 C105 N102 -0.3(5) . . . . ? C103 C104 C105 C106 -177.7(4) . . . . ? N102 C105 C106 C111 11.7(6) . . . . ? C104 C105 C106 C111 -171.2(5) . . . . ? N102 C105 C106 C109 134.8(5) . . . . ? C104 C105 C106 C109 -48.1(6) . . . . ? N102 C105 C106 C107 -108.4(5) . . . . ? C104 C105 C106 C107 68.6(6) . . . . ? C111 C106 C107 C108 -54.0(5) . . . . ? C105 C106 C107 C108 69.4(5) . . . . ? C109 C106 C107 C108 -172.8(4) . . . . ? C111 C106 C109 C110 65.2(5) . . . . ? C105 C106 C109 C110 -60.0(6) . . . . ? C107 C106 C109 C110 -177.3(4) . . . . ? C105 C106 C111 N103 -12.2(6) . . . . ? C109 C106 C111 N103 -134.8(4) . . . . ? C107 C106 C111 N103 108.0(5) . . . . ? C105 C106 C111 C112 174.0(4) . . . . ? C109 C106 C111 C112 51.4(6) . . . . ? C107 C106 C111 C112 -65.8(6) . . . . ? N103 C111 C112 C113 0.8(5) . . . . ? C106 C111 C112 C113 175.4(4) . . . . ? C111 C112 C113 C114 -0.5(5) . . . . ? C112 C113 C114 N103 0.1(5) . . . . ? C112 C113 C114 C115 178.4(5) . . . . ? C113 C114 C115 N104 -176.7(5) . . . . ? N103 C114 C115 N104 1.6(6) . . . . ? C121 C116 C117 C118 2.8(7) . . . . ? N104 C116 C117 C118 -175.5(4) . . . . ? C116 C117 C118 C119 -2.4(7) . . . . ? C117 C118 C119 C120 0.4(7) . . . . ? C118 C119 C120 C121 1.3(8) . . . . ? C119 C120 C121 O101 176.7(4) . . . . ? C119 C120 C121 C116 -0.9(7) . . . . ? C117 C116 C121 O101 -178.8(4) . . . . ? N104 C116 C121 O101 -0.6(6) . . . . ? C117 C116 C121 C120 -1.1(7) . . . . ? N104 C116 C121 C120 177.1(4) . . . . ? O101 C122 C123 O102 -69.2(5) . . . . ? O102 C124 C125 O103 78.6(6) . . . . ? O103 C126 C127 O104 -61.8(6) . . . . ? O104 C128 C129 O105 -176.5(4) . . . . ? O105 C130 C131 C132 177.8(4) . . . . ? C135 C130 C131 C132 -2.0(7) . . . . ? C130 C131 C132 C133 0.2(7) . . . . ? C131 C132 C133 C134 1.4(7) . . . . ? C132 C133 C134 C135 -1.2(7) . . . . ? C133 C134 C135 C130 -0.7(7) . . . . ? C133 C134 C135 N101 179.5(4) . . . . ? O105 C130 C135 C134 -177.6(4) . . . . ? C131 C130 C135 C134 2.3(7) . . . . ? O105 C130 C135 N101 2.2(6) . . . . ? C131 C130 C135 N101 -177.9(4) . . . . ? N201 C201 C202 N202 -3.4(6) . . . . ? N201 C201 C202 C203 -171.7(6) . . . . ? N202 C202 C203 C204 0.5(6) . . . . ? C201 C202 C203 C204 169.0(6) . . . . ? C202 C203 C204 C205 -0.4(6) . . . . ? C203 C204 C205 N202 0.1(6) . . . . ? C203 C204 C205 C206 -177.7(5) . . . . ? N202 C205 C206 C211 4.1(7) . . . . ? C204 C205 C206 C211 -178.3(5) . . . . ? N202 C205 C206 C209 127.6(5) . . . . ? C204 C205 C206 C209 -54.8(7) . . . . ? N202 C205 C206 C207 -115.7(5) . . . . ? C204 C205 C206 C207 61.9(6) . . . . ? C211 C206 C207 C208 -57.2(6) . . . . ? C205 C206 C207 C208 66.5(6) . . . . ? C209 C206 C207 C208 -175.6(5) . . . . ? C211 C206 C209 C210 64.2(6) . . . . ? C205 C206 C209 C210 -61.7(6) . . . . ? C207 C206 C209 C210 -178.8(5) . . . . ? C205 C206 C211 N203 -4.8(7) . . . . ? C209 C206 C211 N203 -128.0(5) . . . . ? C207 C206 C211 N203 115.2(5) . . . . ? C205 C206 C211 C212 177.8(5) . . . . ? C209 C206 C211 C212 54.6(7) . . . . ? C207 C206 C211 C212 -62.1(6) . . . . ? N203 C211 C212 C213 0.3(6) . . . . ? C206 C211 C212 C213 177.9(5) . . . . ? C211 C212 C213 C214 0.0(6) . . . . ? C212 C213 C214 N203 -0.2(6) . . . . ? C212 C213 C214 C215 177.2(6) . . . . ? N203 C214 C215 N204 -0.3(6) . . . . ? C213 C214 C215 N204 -177.6(6) . . . . ? C221 C216 C217 C218 0.4(7) . . . . ? N204 C216 C217 C218 -178.9(4) . . . . ? C216 C217 C218 C219 0.9(8) . . . . ? C217 C218 C219 C220 -1.4(8) . . . . ? C218 C219 C220 C221 0.6(8) . . . . ? C219 C220 C221 O201 -179.4(4) . . . . ? C219 C220 C221 C216 0.7(7) . . . . ? C217 C216 C221 O201 178.9(4) . . . . ? N204 C216 C221 O201 -1.8(6) . . . . ? C217 C216 C221 C220 -1.2(7) . . . . ? N204 C216 C221 C220 178.1(4) . . . . ? O201 C222 C223 O202 -75.2(5) . . . . ? O202 C224 C225 O203 84.9(5) . . . . ? O203 C226 C227 O204 -62.7(5) . . . . ? O204 C228 C229 O205 178.9(4) . . . . ? O205 C230 C231 C232 177.8(5) . . . . ? C235 C230 C231 C232 -0.5(7) . . . . ? C230 C231 C232 C233 -1.2(8) . . . . ? C231 C232 C233 C234 1.5(8) . . . . ? C232 C233 C234 C235 0.0(8) . . . . ? C233 C234 C235 C230 -1.7(7) . . . . ? C233 C234 C235 N201 179.6(4) . . . . ? O205 C230 C235 C234 -176.6(4) . . . . ? C231 C230 C235 C234 1.9(7) . . . . ? O205 C230 C235 N201 2.2(6) . . . . ? C231 C230 C235 N201 -179.2(4) . . . . ? C102 C101 N101 C135 166.5(4) . . . . ? C102 C101 N101 Co1 -0.5(5) . . . . ? C134 C135 N101 C101 55.9(6) . . . . ? C130 C135 N101 C101 -123.9(5) . . . . ? C134 C135 N101 Co1 -139.2(4) . . . . ? C130 C135 N101 Co1 41.0(5) . . . . ? C104 C105 N102 C102 0.2(5) . . . . ? C106 C105 N102 C102 177.7(4) . . . . ? C104 C105 N102 Co1 179.1(4) . . . . ? C106 C105 N102 Co1 -3.4(7) . . . . ? C103 C102 N102 C105 0.0(5) . . . . ? C101 C102 N102 C105 -172.9(4) . . . . ? C103 C102 N102 Co1 -179.1(3) . . . . ? C101 C102 N102 Co1 8.0(5) . . . . ? C112 C111 N103 C114 -0.8(5) . . . . ? C106 C111 N103 C114 -175.7(4) . . . . ? C112 C111 N103 Co1 179.5(3) . . . . ? C106 C111 N103 Co1 4.6(7) . . . . ? C113 C114 N103 C111 0.5(5) . . . . ? C115 C114 N103 C111 -178.4(4) . . . . ? C113 C114 N103 Co1 -179.7(3) . . . . ? C115 C114 N103 Co1 1.4(5) . . . . ? C114 C115 N104 C116 178.1(4) . . . . ? C114 C115 N104 Co1 -3.7(5) . . . . ? C117 C116 N104 C115 -131.3(4) . . . . ? C121 C116 N104 C115 50.5(6) . . . . ? C117 C116 N104 Co1 50.8(6) . . . . ? C121 C116 N104 Co1 -127.4(4) . . . . ? C202 C201 N201 C235 166.2(4) . . . . ? C202 C201 N201 Co2 0.1(5) . . . . ? C234 C235 N201 C201 59.5(6) . . . . ? C230 C235 N201 C201 -119.2(5) . . . . ? C234 C235 N201 Co2 -136.5(4) . . . . ? C230 C235 N201 Co2 44.7(5) . . . . ? C204 C205 N202 C202 0.2(5) . . . . ? C206 C205 N202 C202 178.2(4) . . . . ? C204 C205 N202 Co2 -176.5(4) . . . . ? C206 C205 N202 Co2 1.5(8) . . . . ? C203 C202 N202 C205 -0.4(6) . . . . ? C201 C202 N202 C205 -172.1(4) . . . . ? C203 C202 N202 Co2 177.0(3) . . . . ? C201 C202 N202 Co2 5.3(5) . . . . ? C212 C211 N203 C214 -0.4(5) . . . . ? C206 C211 N203 C214 -178.2(4) . . . . ? C212 C211 N203 Co2 177.9(4) . . . . ? C206 C211 N203 Co2 0.1(8) . . . . ? C213 C214 N203 C211 0.4(6) . . . . ? C215 C214 N203 C211 -177.7(4) . . . . ? C213 C214 N203 Co2 -178.3(3) . . . . ? C215 C214 N203 Co2 3.6(5) . . . . ? C214 C215 N204 C216 175.5(4) . . . . ? C214 C215 N204 Co2 -2.8(5) . . . . ? C217 C216 N204 C215 -125.9(5) . . . . ? C221 C216 N204 C215 54.8(6) . . . . ? C217 C216 N204 Co2 52.0(6) . . . . ? C221 C216 N204 Co2 -127.3(4) . . . . ? C120 C121 O101 C122 6.0(7) . . . . ? C116 C121 O101 C122 -176.4(4) . . . . ? C123 C122 O101 C121 178.1(4) . . . . ? C122 C123 O102 C124 170.6(4) . . . . ? C125 C124 O102 C123 -77.0(6) . . . . ? C124 C125 O103 C126 -165.2(4) . . . . ? C127 C126 O103 C125 165.3(4) . . . . ? C129 C128 O104 C127 -178.6(4) . . . . ? C126 C127 O104 C128 -68.9(6) . . . . ? C131 C130 O105 C129 -5.8(7) . . . . ? C135 C130 O105 C129 174.1(4) . . . . ? C128 C129 O105 C130 -177.2(4) . . . . ? C220 C221 O201 C222 -6.8(6) . . . . ? C216 C221 O201 C222 173.0(4) . . . . ? C223 C222 O201 C221 177.6(4) . . . . ? C225 C224 O202 C223 -71.8(5) . . . . ? C222 C223 O202 C224 164.5(4) . . . . ? C224 C225 O203 C226 -162.8(4) . . . . ? C227 C226 O203 C225 161.5(4) . . . . ? C229 C228 O204 C227 -178.9(4) . . . . ? C226 C227 O204 C228 -75.0(5) . . . . ? C231 C230 O205 C229 4.8(7) . . . . ? C235 C230 O205 C229 -176.8(4) . . . . ? C228 C229 O205 C230 173.7(4) . . . . ? C105 N102 Co1 N103 -3.8(5) . . . . ? C102 N102 Co1 N103 175.0(3) . . . . ? C105 N102 Co1 N104 -35.8(10) . . . . ? C102 N102 Co1 N104 143.0(7) . . . . ? C105 N102 Co1 N101 174.6(5) . . . . ? C102 N102 Co1 N101 -6.6(3) . . . . ? C111 N103 Co1 N102 3.2(4) . . . . ? C114 N103 Co1 N102 -176.5(3) . . . . ? C111 N103 Co1 N104 177.1(5) . . . . ? C114 N103 Co1 N104 -2.6(3) . . . . ? C111 N103 Co1 N101 -5.6(12) . . . . ? C114 N103 Co1 N101 174.7(8) . . . . ? C115 N104 Co1 N102 35.7(9) . . . . ? C116 N104 Co1 N102 -146.3(7) . . . . ? C115 N104 Co1 N103 3.5(3) . . . . ? C116 N104 Co1 N103 -178.5(4) . . . . ? C115 N104 Co1 N101 -176.0(3) . . . . ? C116 N104 Co1 N101 2.0(4) . . . . ? C101 N101 Co1 N102 3.9(3) . . . . ? C135 N101 Co1 N102 -161.8(4) . . . . ? C101 N101 Co1 N103 12.8(11) . . . . ? C135 N101 Co1 N103 -152.8(8) . . . . ? C101 N101 Co1 N104 -169.9(3) . . . . ? C135 N101 Co1 N104 24.4(4) . . . . ? C205 N202 Co2 N203 -4.8(5) . . . . ? C202 N202 Co2 N203 178.7(3) . . . . ? C205 N202 Co2 N201 172.3(5) . . . . ? C202 N202 Co2 N201 -4.2(3) . . . . ? C205 N202 Co2 N204 -36.6(11) . . . . ? C202 N202 Co2 N204 146.8(7) . . . . ? C211 N203 Co2 N202 4.0(5) . . . . ? C214 N203 Co2 N202 -177.9(4) . . . . ? C211 N203 Co2 N201 -12.2(12) . . . . ? C214 N203 Co2 N201 166.0(8) . . . . ? C211 N203 Co2 N204 177.8(5) . . . . ? C214 N203 Co2 N204 -4.0(3) . . . . ? C201 N201 Co2 N202 2.2(3) . . . . ? C235 N201 Co2 N202 -162.6(4) . . . . ? C201 N201 Co2 N203 18.5(11) . . . . ? C235 N201 Co2 N203 -146.4(8) . . . . ? C201 N201 Co2 N204 -171.9(3) . . . . ? C235 N201 Co2 N204 23.2(4) . . . . ? C215 N204 Co2 N202 35.9(10) . . . . ? C216 N204 Co2 N202 -142.1(7) . . . . ? C215 N204 Co2 N203 3.7(3) . . . . ? C216 N204 Co2 N203 -174.3(4) . . . . ? C215 N204 Co2 N201 -174.4(3) . . . . ? C216 N204 Co2 N201 7.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.202 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.096 _exptl_absorpt_process_details 'SADABS 2007/2' data_jl0031 _database_code_depnum_ccdc_archive 'CCDC 795243' #TrackingRef 'combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H43 Co N4 O7, 1.67(H2 O)' _chemical_formula_sum 'C35 H46.33 Co N4 O8.67' _chemical_formula_weight 720.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 46.262(2) _cell_length_b 46.262(2) _cell_length_c 8.3856(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 15542.0(12) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10057 _cell_measurement_theta_min 1.9083 _cell_measurement_theta_max 73.2561 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.166 _exptl_crystal_size_mid 0.1064 _exptl_crystal_size_min 0.0710 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6852 _exptl_absorpt_coefficient_mu 4.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.41648 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\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_reflns_number 26850 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 73.42 _reflns_number_total 6751 _reflns_number_gt 5092 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== For Documentation: http://www.cryst.chem.uu.nl/spek/platon/CIF-VALIDATION.pdf #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text 601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 179.00 A**3 041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? 042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? 043_ALERT_1_C Check Reported Molecular Weight ................ 720.69 044_ALERT_1_C Calculated and Reported Dx Differ .............. ? 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLATON SQUEEZE used due to unsatisfactory modelling of water molecules in the 'channel' made by the arene backbones. Electron count of 129 consistant with approximately 0.67 water molecules per asymmetric unit, or 4 water molecules per 'channel'. NB: the waters lie on a plane of symmetry Formulae, Mw, Dx and F000 include the missing solvent. 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.38 There is a peak close to the Co which is due to absorption (Cu radiation used) 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 27 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 96 Completeness and resolution meet IUCr limits. 072_ALERT_2_G SHELXL First Parameter in WGHT Unusually Large. 0.11 The data at high angle were quite weak, Rint is thus somewhat high (0.855). The weighting scheme is compensating for poor data quality. 432_ALERT_2_G Short Inter X...Y Contact C3 .. C13 .. 3.18 Ang. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4 731_ALERT_1_C Bond Calc 0.84(4), Rep 0.838(10) ...... 4.00 su-Ra O7 -H39 1.555 1.555 731_ALERT_1_C Bond Calc 0.85(3), Rep 0.847(10) ...... 3.00 su-Ra O100 -H41 1.555 1.555 732_ALERT_1_C Angle Calc 104(4), Rep 103.4(15) ...... 2.67 su-Ra H40 -O100 -H41 1.555 1.555 1.555 Restraints were used for some OH hydrogen positions. Platon has calculated values which without access to the full LS matrix thus slight differences are apparent. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 802_ALERT_4_G CIF Input Record(s) with more than 80 Characters ! No action taken ; _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^)+(0.1142P)^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 6751 _refine_ls_number_parameters 449 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1669 _refine_ls_wR_factor_gt 0.1618 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.80056(8) -0.01536(8) 0.0743(4) 0.0212(7) Uani 1 1 d . . . H1 H 0.8032 -0.0247 -0.0215 0.025 Uiso 1 1 calc R . . C2 C 0.77545(8) -0.00695(8) 0.0886(4) 0.0224(7) Uani 1 1 d . . . C3 C 0.74881(9) -0.00927(9) -0.0007(4) 0.0284(8) Uani 1 1 d . . . H3 H 0.7417 -0.0191 -0.1032 0.034 Uiso 1 1 calc R . . C4 C 0.73480(9) 0.00562(9) 0.0906(5) 0.0299(8) Uani 1 1 d . . . H4 H 0.7163 0.0080 0.0610 0.036 Uiso 1 1 calc R . . C5 C 0.75280(8) 0.01663(8) 0.2345(4) 0.0236(7) Uani 1 1 d . . . C6 C 0.74793(8) 0.03534(8) 0.3692(5) 0.0260(7) Uani 1 1 d . . . C7 C 0.71044(9) 0.01697(10) 0.4181(5) 0.0332(8) Uani 1 1 d . . . H7A H 0.7071 0.0304 0.5003 0.040 Uiso 1 1 calc R . . H7B H 0.6969 0.0155 0.3240 0.040 Uiso 1 1 calc R . . C8 C 0.69802(9) -0.01790(10) 0.4827(5) 0.0382(9) Uani 1 1 d . . . H8A H 0.6744 -0.0280 0.5115 0.057 Uiso 1 1 calc R . . H8B H 0.7110 -0.0167 0.5773 0.057 Uiso 1 1 calc R . . H8C H 0.7006 -0.0316 0.4009 0.057 Uiso 1 1 calc R . . C9 C 0.75741(10) 0.07093(10) 0.3103(5) 0.0359(9) Uani 1 1 d . . . H9A H 0.7436 0.0688 0.2162 0.043 Uiso 1 1 calc R . . H9B H 0.7520 0.0823 0.3953 0.043 Uiso 1 1 calc R . . C10 C 0.79415(11) 0.09264(10) 0.2656(5) 0.0394(9) Uani 1 1 d . . . H10A H 0.7983 0.1146 0.2300 0.059 Uiso 1 1 calc R . . H10B H 0.7997 0.0819 0.1794 0.059 Uiso 1 1 calc R . . H10C H 0.8081 0.0954 0.3588 0.059 Uiso 1 1 calc R . . C11 C 0.76852(8) 0.03869(8) 0.5146(4) 0.0227(7) Uani 1 1 d . . . C12 C 0.76952(9) 0.05381(8) 0.6609(4) 0.0268(7) Uani 1 1 d . . . H12 H 0.7571 0.0644 0.6873 0.032 Uiso 1 1 calc R . . C13 C 0.79170(9) 0.05075(8) 0.7608(4) 0.0257(7) Uani 1 1 d . . . H13 H 0.7973 0.0586 0.8673 0.031 Uiso 1 1 calc R . . C14 C 0.80429(8) 0.03361(7) 0.6725(4) 0.0206(6) Uani 1 1 d . . . C15 C 0.82727(8) 0.02245(7) 0.6938(4) 0.0187(6) Uani 1 1 d . . . H15 H 0.8378 0.0244 0.7937 0.022 Uiso 1 1 calc R . . C16 C 0.85371(8) -0.00566(7) 0.5940(4) 0.0177(6) Uani 1 1 d . . . C17 C 0.88592(8) 0.00892(8) 0.5328(4) 0.0210(6) Uani 1 1 d . . . H17 H 0.8943 0.0285 0.4691 0.025 Uiso 1 1 calc R . . C18 C 0.90602(9) -0.00487(8) 0.5642(4) 0.0266(7) Uani 1 1 d . . . H18 H 0.9282 0.0054 0.5239 0.032 Uiso 1 1 calc R . . C19 C 0.89353(9) -0.03370(9) 0.6545(4) 0.0270(7) Uani 1 1 d . . . H19 H 0.9074 -0.0428 0.6781 0.032 Uiso 1 1 calc R . . C20 C 0.86102(8) -0.04948(8) 0.7111(4) 0.0239(7) Uani 1 1 d . . . H20 H 0.8525 -0.0696 0.7706 0.029 Uiso 1 1 calc R . . C21 C 0.84094(8) -0.03558(8) 0.6798(4) 0.0198(6) Uani 1 1 d . . . C22 C 0.79320(8) -0.08188(8) 0.7988(4) 0.0250(7) Uani 1 1 d . . . H22A H 0.8043 -0.0817 0.9001 0.030 Uiso 1 1 calc R . . H22B H 0.7949 -0.0976 0.7242 0.030 Uiso 1 1 calc R . . C23 C 0.75739(8) -0.09227(8) 0.8280(4) 0.0260(7) Uani 1 1 d . . . H23A H 0.7453 -0.1155 0.8688 0.031 Uiso 1 1 calc R . . H23B H 0.7559 -0.0775 0.9089 0.031 Uiso 1 1 calc R . . C24 C 0.70783(9) -0.10312(9) 0.6961(5) 0.0318(8) Uani 1 1 d . . . H24A H 0.7033 -0.0888 0.7674 0.038 Uiso 1 1 calc R . . H24B H 0.6969 -0.1259 0.7413 0.038 Uiso 1 1 calc R . . C25 C 0.69433(9) -0.10384(10) 0.5319(5) 0.0340(9) Uani 1 1 d . . . H25A H 0.6705 -0.1101 0.5386 0.041 Uiso 1 1 calc R . . H25B H 0.7069 -0.0815 0.4818 0.041 Uiso 1 1 calc R . . C26 C 0.69779(10) -0.12344(11) 0.2714(5) 0.0372(9) Uani 1 1 d . . . H26A H 0.7110 -0.0995 0.2435 0.045 Uiso 1 1 calc R . . H26B H 0.6747 -0.1321 0.2325 0.045 Uiso 1 1 calc R . . C27 C 0.71291(9) -0.14237(11) 0.1947(5) 0.0360(9) Uani 1 1 d . . . H27A H 0.7052 -0.1636 0.2532 0.043 Uiso 1 1 calc R . . H27B H 0.7046 -0.1480 0.0838 0.043 Uiso 1 1 calc R . . C28 C 0.76288(8) -0.12284(8) 0.3447(4) 0.0233(7) Uani 1 1 d . . . H28A H 0.7558 -0.1456 0.3843 0.028 Uiso 1 1 calc R . . H28B H 0.7556 -0.1117 0.4224 0.028 Uiso 1 1 calc R . . C29 C 0.80011(8) -0.10339(8) 0.3260(4) 0.0245(7) Uani 1 1 d . . . H29A H 0.8111 -0.1053 0.4237 0.029 Uiso 1 1 calc R . . H29B H 0.8071 -0.1121 0.2348 0.029 Uiso 1 1 calc R . . C30 C 0.84057(8) -0.04841(8) 0.2384(4) 0.0201(6) Uani 1 1 d . . . C31 C 0.86571(9) -0.05626(9) 0.2266(4) 0.0255(7) Uani 1 1 d . . . H31 H 0.8619 -0.0774 0.2620 0.031 Uiso 1 1 calc R . . C32 C 0.89641(9) -0.03334(9) 0.1631(4) 0.0287(8) Uani 1 1 d . . . H32 H 0.9138 -0.0386 0.1583 0.034 Uiso 1 1 calc R . . C33 C 0.90200(9) -0.00280(9) 0.1064(4) 0.0286(7) Uani 1 1 d . . . H33 H 0.9230 0.0126 0.0612 0.034 Uiso 1 1 calc R . . C34 C 0.87674(9) 0.00502(8) 0.1164(4) 0.0254(7) Uani 1 1 d . . . H34 H 0.8804 0.0259 0.0772 0.031 Uiso 1 1 calc R . . C35 C 0.84636(8) -0.01734(8) 0.1829(4) 0.0194(6) Uani 1 1 d . . . N1 N 0.82010(6) -0.00999(6) 0.1959(3) 0.0185(5) Uani 1 1 d . . . N2 N 0.77679(7) 0.00865(7) 0.2291(3) 0.0212(6) Uani 1 1 d . . . N3 N 0.78964(7) 0.02669(7) 0.5244(3) 0.0200(6) Uani 1 1 d . . . N4 N 0.83361(6) 0.00917(6) 0.5697(3) 0.0176(5) Uani 1 1 d . . . O1 O 0.80863(5) -0.04883(5) 0.7310(3) 0.0207(5) Uani 1 1 d . . . O2 O 0.74281(6) -0.09019(6) 0.6834(3) 0.0269(5) Uani 1 1 d . . . O3 O 0.69771(6) -0.12752(6) 0.4404(3) 0.0307(6) Uani 1 1 d . . . O4 O 0.74834(6) -0.12455(7) 0.1919(3) 0.0331(6) Uani 1 1 d . . . O5 O 0.80942(6) -0.06916(5) 0.2987(3) 0.0229(5) Uani 1 1 d . . . O6 O 0.77341(6) -0.03925(6) 0.4326(3) 0.0219(5) Uani 1 1 d . . . O7 O 0.84171(6) 0.05170(5) 0.3214(3) 0.0220(5) Uani 1 1 d D . . O100 O 0.85790(7) 0.06425(7) 0.0137(3) 0.0337(6) Uani 1 1 d D . . Co1 Co 0.807259(12) 0.008905(12) 0.37868(6) 0.01667(15) Uani 1 1 d . . . H39 H 0.8357(9) 0.0648(8) 0.357(5) 0.025 Uiso 1 1 d D . . H37 H 0.7792(10) -0.0496(10) 0.381(5) 0.025 Uiso 1 1 d . . . H40 H 0.8505(9) 0.0623(8) 0.110(2) 0.025 Uiso 1 1 d D . . H38 H 0.7700(10) -0.0458(10) 0.527(6) 0.025 Uiso 1 1 d . . . H41 H 0.8575(10) 0.0812(6) -0.022(4) 0.025 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0295(16) 0.0211(15) 0.0096(16) 0.0019(11) 0.0019(12) 0.0102(13) C2 0.0253(16) 0.0261(16) 0.0119(17) 0.0022(12) -0.0003(12) 0.0099(13) C3 0.0265(16) 0.0344(18) 0.0176(19) 0.0014(14) -0.0072(13) 0.0101(14) C4 0.0274(17) 0.0385(19) 0.023(2) 0.0046(15) -0.0039(14) 0.0159(15) C5 0.0215(15) 0.0247(15) 0.0231(19) 0.0054(13) 0.0000(13) 0.0103(13) C6 0.0236(16) 0.0274(17) 0.032(2) 0.0006(14) -0.0036(14) 0.0163(14) C7 0.0260(17) 0.040(2) 0.037(2) -0.0083(17) -0.0017(15) 0.0193(16) C8 0.0267(18) 0.039(2) 0.037(2) -0.0020(17) 0.0033(16) 0.0077(16) C9 0.040(2) 0.0341(19) 0.042(2) 0.0016(17) -0.0090(17) 0.0253(17) C10 0.048(2) 0.0292(18) 0.041(3) 0.0061(17) -0.0088(19) 0.0191(18) C11 0.0213(15) 0.0215(15) 0.0264(19) -0.0010(13) 0.0011(13) 0.0116(13) C12 0.0295(17) 0.0269(16) 0.029(2) -0.0039(14) 0.0047(14) 0.0174(14) C13 0.0313(17) 0.0231(16) 0.0216(19) -0.0057(13) 0.0044(14) 0.0127(14) C14 0.0242(15) 0.0181(14) 0.0150(17) -0.0003(12) 0.0005(12) 0.0073(12) C15 0.0234(15) 0.0178(14) 0.0117(16) 0.0009(11) -0.0009(12) 0.0080(12) C16 0.0218(14) 0.0178(14) 0.0124(16) -0.0043(11) -0.0050(12) 0.0092(12) C17 0.0222(15) 0.0205(15) 0.0173(17) -0.0013(12) -0.0017(12) 0.0084(12) C18 0.0247(16) 0.0280(16) 0.0239(19) -0.0040(14) -0.0021(13) 0.0107(14) C19 0.0318(17) 0.0294(17) 0.025(2) -0.0022(14) -0.0043(14) 0.0193(15) C20 0.0313(17) 0.0229(15) 0.0184(18) -0.0007(13) -0.0042(13) 0.0144(14) C21 0.0245(15) 0.0230(15) 0.0102(16) -0.0049(12) -0.0025(12) 0.0106(13) C22 0.0308(17) 0.0226(15) 0.0190(18) 0.0051(13) 0.0040(14) 0.0115(14) C23 0.0290(17) 0.0247(16) 0.0133(17) 0.0013(13) 0.0024(13) 0.0051(13) C24 0.0287(18) 0.0338(19) 0.030(2) 0.0006(15) 0.0087(15) 0.0136(15) C25 0.0213(16) 0.0335(19) 0.045(3) -0.0001(17) -0.0015(15) 0.0122(15) C26 0.0284(18) 0.044(2) 0.028(2) 0.0045(17) -0.0049(15) 0.0095(16) C27 0.0290(18) 0.046(2) 0.0170(19) -0.0036(16) -0.0031(14) 0.0065(16) C28 0.0313(17) 0.0189(14) 0.0170(18) 0.0001(12) 0.0021(13) 0.0105(13) C29 0.0314(17) 0.0180(15) 0.0247(19) 0.0013(13) 0.0019(14) 0.0128(13) C30 0.0237(15) 0.0206(15) 0.0142(17) -0.0050(12) -0.0028(12) 0.0098(12) C31 0.0302(17) 0.0271(16) 0.0228(19) -0.0043(13) -0.0028(14) 0.0171(14) C32 0.0275(17) 0.0370(19) 0.025(2) -0.0079(15) -0.0027(14) 0.0185(15) C33 0.0262(17) 0.0290(17) 0.0239(19) -0.0014(14) 0.0050(14) 0.0088(14) C34 0.0300(17) 0.0258(16) 0.0171(18) -0.0008(13) 0.0021(13) 0.0114(14) C35 0.0252(15) 0.0190(14) 0.0130(16) -0.0042(11) -0.0008(12) 0.0102(12) N1 0.0237(13) 0.0207(12) 0.0098(13) -0.0008(10) 0.0006(10) 0.0101(11) N2 0.0262(13) 0.0214(13) 0.0140(14) 0.0012(10) -0.0006(11) 0.0104(11) N3 0.0224(13) 0.0225(13) 0.0156(15) 0.0020(10) 0.0008(10) 0.0116(11) N4 0.0229(13) 0.0180(12) 0.0106(13) -0.0006(10) -0.0015(10) 0.0092(10) O1 0.0246(11) 0.0192(10) 0.0154(12) 0.0045(8) 0.0029(9) 0.0087(9) O2 0.0243(12) 0.0316(12) 0.0196(13) 0.0020(10) 0.0015(9) 0.0100(10) O3 0.0309(13) 0.0364(13) 0.0213(14) 0.0013(10) -0.0005(10) 0.0142(11) O4 0.0280(12) 0.0372(14) 0.0199(14) 0.0011(10) 0.0009(10) 0.0058(11) O5 0.0250(11) 0.0178(10) 0.0265(13) 0.0019(9) 0.0027(9) 0.0113(9) O6 0.0271(12) 0.0180(11) 0.0177(13) 0.0010(9) 0.0023(9) 0.0092(9) O7 0.0252(11) 0.0193(11) 0.0202(13) -0.0017(9) 0.0005(9) 0.0102(9) O100 0.0476(16) 0.0333(14) 0.0182(14) 0.0005(10) 0.0000(11) 0.0187(12) Co1 0.0207(3) 0.0172(2) 0.0122(3) -0.00049(19) -0.00027(19) 0.0096(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.301(4) . ? C1 C2 1.403(5) . ? C1 H1 0.9500 . ? C2 N2 1.366(4) . ? C2 C3 1.400(5) . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 C5 1.410(5) . ? C4 H4 0.9500 . ? C5 N2 1.334(4) . ? C5 C6 1.507(5) . ? C6 C11 1.507(5) . ? C6 C7 1.557(5) . ? C6 C9 1.557(5) . ? C7 C8 1.516(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.527(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.346(4) . ? C11 C12 1.402(5) . ? C12 C13 1.386(5) . ? C12 H12 0.9500 . ? C13 C14 1.406(4) . ? C13 H13 0.9500 . ? C14 N3 1.374(4) . ? C14 C15 1.406(4) . ? C15 N4 1.314(4) . ? C15 H15 0.9500 . ? C16 C17 1.390(4) . ? C16 C21 1.402(4) . ? C16 N4 1.420(4) . ? C17 C18 1.391(5) . ? C17 H17 0.9500 . ? C18 C19 1.385(5) . ? C18 H18 0.9500 . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C20 C21 1.394(5) . ? C20 H20 0.9500 . ? C21 O1 1.370(4) . ? C22 O1 1.442(4) . ? C22 C23 1.496(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.414(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O2 1.421(4) . ? C24 C25 1.505(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O3 1.409(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O3 1.429(5) . ? C26 C27 1.511(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O4 1.419(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O4 1.431(4) . ? C28 C29 1.500(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O5 1.437(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O5 1.368(4) . ? C30 C31 1.385(5) . ? C30 C35 1.403(4) . ? C31 C32 1.385(5) . ? C31 H31 0.9500 . ? C32 C33 1.387(5) . ? C32 H32 0.9500 . ? C33 C34 1.388(5) . ? C33 H33 0.9500 . ? C34 C35 1.379(5) . ? C34 H34 0.9500 . ? C35 N1 1.420(4) . ? N1 Co1 1.996(3) . ? N2 Co1 1.883(3) . ? N3 Co1 1.872(3) . ? N4 Co1 2.009(3) . ? O6 Co1 2.033(2) . ? O6 H37 0.78(4) . ? O6 H38 0.83(5) . ? O7 Co1 1.880(2) . ? O7 H39 0.838(10) . ? O100 H40 0.860(10) . ? O100 H41 0.847(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 118.2(3) . . ? N1 C1 H1 120.9 . . ? C2 C1 H1 120.9 . . ? N2 C2 C3 107.9(3) . . ? N2 C2 C1 113.3(3) . . ? C3 C2 C1 138.8(3) . . ? C4 C3 C2 106.2(3) . . ? C4 C3 H3 126.9 . . ? C2 C3 H3 126.9 . . ? C3 C4 C5 108.3(3) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? N2 C5 C4 107.1(3) . . ? N2 C5 C6 124.7(3) . . ? C4 C5 C6 128.2(3) . . ? C5 C6 C11 113.4(3) . . ? C5 C6 C7 109.3(3) . . ? C11 C6 C7 108.5(3) . . ? C5 C6 C9 109.0(3) . . ? C11 C6 C9 108.6(3) . . ? C7 C6 C9 108.0(3) . . ? C8 C7 C6 113.6(3) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 113.9(3) . . ? C10 C9 H9A 108.8 . . ? C6 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C6 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 107.6(3) . . ? N3 C11 C6 124.0(3) . . ? C12 C11 C6 128.4(3) . . ? C13 C12 C11 108.6(3) . . ? C13 C12 H12 125.7 . . ? C11 C12 H12 125.7 . . ? C12 C13 C14 106.0(3) . . ? C12 C13 H13 127.0 . . ? C14 C13 H13 127.0 . . ? N3 C14 C15 113.9(3) . . ? N3 C14 C13 108.2(3) . . ? C15 C14 C13 138.0(3) . . ? N4 C15 C14 117.2(3) . . ? N4 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? C17 C16 C21 119.3(3) . . ? C17 C16 N4 121.0(3) . . ? C21 C16 N4 119.8(3) . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 119.5(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 121.0(3) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 119.4(3) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? O1 C21 C20 124.4(3) . . ? O1 C21 C16 115.4(3) . . ? C20 C21 C16 120.2(3) . . ? O1 C22 C23 106.6(3) . . ? O1 C22 H22A 110.4 . . ? C23 C22 H22A 110.4 . . ? O1 C22 H22B 110.4 . . ? C23 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? O2 C23 C22 109.1(3) . . ? O2 C23 H23A 109.9 . . ? C22 C23 H23A 109.9 . . ? O2 C23 H23B 109.9 . . ? C22 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O2 C24 C25 108.3(3) . . ? O2 C24 H24A 110.0 . . ? C25 C24 H24A 110.0 . . ? O2 C24 H24B 110.0 . . ? C25 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? O3 C25 C24 108.0(3) . . ? O3 C25 H25A 110.1 . . ? C24 C25 H25A 110.1 . . ? O3 C25 H25B 110.1 . . ? C24 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? O3 C26 C27 108.5(3) . . ? O3 C26 H26A 110.0 . . ? C27 C26 H26A 110.0 . . ? O3 C26 H26B 110.0 . . ? C27 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? O4 C27 C26 113.9(3) . . ? O4 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? O4 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? O4 C28 C29 107.8(3) . . ? O4 C28 H28A 110.1 . . ? C29 C28 H28A 110.1 . . ? O4 C28 H28B 110.1 . . ? C29 C28 H28B 110.1 . . ? H28A C28 H28B 108.5 . . ? O5 C29 C28 107.4(3) . . ? O5 C29 H29A 110.2 . . ? C28 C29 H29A 110.2 . . ? O5 C29 H29B 110.2 . . ? C28 C29 H29B 110.2 . . ? H29A C29 H29B 108.5 . . ? O5 C30 C31 124.8(3) . . ? O5 C30 C35 115.9(3) . . ? C31 C30 C35 119.3(3) . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 120.6(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C34 119.5(3) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 120.3(3) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C30 120.2(3) . . ? C34 C35 N1 121.6(3) . . ? C30 C35 N1 118.1(3) . . ? C1 N1 C35 119.3(3) . . ? C1 N1 Co1 110.8(2) . . ? C35 N1 Co1 129.9(2) . . ? C5 N2 C2 110.6(3) . . ? C5 N2 Co1 134.4(2) . . ? C2 N2 Co1 114.5(2) . . ? C11 N3 C14 109.5(3) . . ? C11 N3 Co1 135.0(2) . . ? C14 N3 Co1 114.8(2) . . ? C15 N4 C16 117.8(3) . . ? C15 N4 Co1 111.0(2) . . ? C16 N4 Co1 130.8(2) . . ? C21 O1 C22 116.7(2) . . ? C23 O2 C24 112.9(3) . . ? C25 O3 C26 115.5(3) . . ? C27 O4 C28 113.1(3) . . ? C30 O5 C29 117.6(2) . . ? Co1 O6 H37 104(3) . . ? Co1 O6 H38 121(3) . . ? H37 O6 H38 111(4) . . ? Co1 O7 H39 105(3) . . ? H40 O100 H41 103.4(15) . . ? N3 Co1 O7 91.71(11) . . ? N3 Co1 N2 87.05(12) . . ? O7 Co1 N2 94.25(11) . . ? N3 Co1 N1 169.67(12) . . ? O7 Co1 N1 89.09(10) . . ? N2 Co1 N1 82.62(12) . . ? N3 Co1 N4 82.71(11) . . ? O7 Co1 N4 90.28(10) . . ? N2 Co1 N4 168.92(12) . . ? N1 Co1 N4 107.59(11) . . ? N3 Co1 O6 94.03(11) . . ? O7 Co1 O6 173.67(10) . . ? N2 Co1 O6 88.71(11) . . ? N1 Co1 O6 85.74(11) . . ? N4 Co1 O6 87.81(10) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 67.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.944 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.109 data_j10073b _database_code_depnum_ccdc_archive 'CCDC 795244' #TrackingRef 'combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H40 Co I N4 O6' _chemical_formula_sum 'C35 H40 Co I N4 O6' _chemical_formula_weight 798.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.571(3) _cell_length_b 11.471(3) _cell_length_c 15.551(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.408(14) _cell_angle_gamma 90.00 _cell_volume 3469.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7609 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 27.5 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2112 _exptl_crystal_size_mid 0.1551 _exptl_crystal_size_min 0.1002 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81927 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_reflns_number 15746 _diffrn_reflns_av_R_equivalents 0.1087 _diffrn_reflns_av_sigmaI/netI 0.1213 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7609 _reflns_number_gt 4282 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text 971_ALERT_2_B Large Calcd. Non-Metal Positive Residual Density 2.99 eA-3 972_ALERT_2_C Large Calcd. Non-Metal Negative Residual Density -2.07 eA-3 972_ALERT_2_C Large Calcd. Non-Metal Negative Residual Density -1.96 eA-3 973_ALERT_2_B Large Calcd. Positive Residual Density on Co1 1.81 eA-3 All large peaks are either close to the Iodine atom or the Co atom. Such problems are commonly encountered when significant absorption is present as is the case here. 084_ALERT_2_C High wR2 Value ................................. 0.27 072_ALERT_2_G SHELXL First Parameter in WGHT Unusually Large. 0.14 234_ALERT_4_C Large Hirshfeld Difference C7 -- C8 .. 0.19 Ang. 234_ALERT_4_C Large Hirshfeld Difference C26 -- C27 .. 0.19 Ang. 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 13 The data are not very good and are quite weak at high angle. 910_ALERT_3_C Missing # of FCF Reflections Bew Th(Min) ..... 9 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 55 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 288 Completeness and resolution meet IUCr limits. ; _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^)+(0.1442P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7609 _refine_ls_number_parameters 426 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2714 _refine_ls_wR_factor_gt 0.2066 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7566(4) -0.0853(8) 0.0040(5) 0.040(2) Uani 1 1 d . . . H1 H 0.7636 -0.1476 -0.0342 0.048 Uiso 1 1 calc R . . C2 C 0.6950(4) -0.0270(7) -0.0033(5) 0.0340(17) Uani 1 1 d . . . C3 C 0.6301(4) -0.0345(9) -0.0517(6) 0.047(2) Uani 1 1 d . . . H3 H 0.6161 -0.0889 -0.0963 0.056 Uiso 1 1 calc R . . C4 C 0.5907(4) 0.0534(9) -0.0214(6) 0.050(2) Uani 1 1 d . . . H4 H 0.5442 0.0698 -0.0418 0.060 Uiso 1 1 calc R . . C5 C 0.6312(4) 0.1154(9) 0.0454(5) 0.041(2) Uani 1 1 d . . . C6 C 0.6119(4) 0.2169(9) 0.0971(5) 0.042(2) Uani 1 1 d . . . C7 C 0.5407(4) 0.1938(10) 0.1292(6) 0.053(2) Uani 1 1 d U . . H7A H 0.5260 0.2654 0.1575 0.064 Uiso 1 1 calc R . . H7B H 0.5068 0.1786 0.0782 0.064 Uiso 1 1 calc R . . C8 C 0.5386(5) 0.0958(10) 0.1900(7) 0.064(3) Uani 1 1 d U . . H8A H 0.5525 0.0239 0.1626 0.097 Uiso 1 1 calc R . . H8B H 0.4918 0.0869 0.2058 0.097 Uiso 1 1 calc R . . H8C H 0.5702 0.1113 0.2422 0.097 Uiso 1 1 calc R . . C9 C 0.6100(5) 0.3258(10) 0.0417(7) 0.058(3) Uani 1 1 d . . . H9A H 0.6004 0.3929 0.0785 0.070 Uiso 1 1 calc R . . H9B H 0.6565 0.3376 0.0240 0.070 Uiso 1 1 calc R . . C10 C 0.5591(7) 0.3294(14) -0.0389(8) 0.092(4) Uani 1 1 d . . . H10A H 0.5731 0.2738 -0.0814 0.138 Uiso 1 1 calc R . . H10B H 0.5579 0.4082 -0.0635 0.138 Uiso 1 1 calc R . . H10C H 0.5133 0.3088 -0.0240 0.138 Uiso 1 1 calc R . . C11 C 0.6634(4) 0.2406(8) 0.1772(5) 0.040(2) Uani 1 1 d . . . C12 C 0.6559(5) 0.3160(10) 0.2461(6) 0.059(3) Uani 1 1 d . . . H12 H 0.6163 0.3613 0.2533 0.070 Uiso 1 1 calc R . . C13 C 0.7162(5) 0.3135(10) 0.3020(6) 0.054(3) Uani 1 1 d . . . H13 H 0.7252 0.3525 0.3560 0.065 Uiso 1 1 calc R . . C14 C 0.7609(5) 0.2419(8) 0.2626(5) 0.040(2) Uani 1 1 d . . . C15 C 0.8251(4) 0.1857(8) 0.2829(5) 0.040(2) Uani 1 1 d . . . H15 H 0.8526 0.2023 0.3358 0.049 Uiso 1 1 calc R . . C16 C 0.9074(4) 0.0478(8) 0.2528(5) 0.0353(18) Uani 1 1 d . . . C17 C 0.9603(4) 0.0470(9) 0.2018(5) 0.044(2) Uani 1 1 d . . . H17 H 0.9565 0.0925 0.1505 0.053 Uiso 1 1 calc R . . C18 C 1.0188(4) -0.0181(9) 0.2233(6) 0.049(2) Uani 1 1 d . . . H18 H 1.0548 -0.0185 0.1870 0.059 Uiso 1 1 calc R . . C19 C 1.0243(4) -0.0824(9) 0.2980(7) 0.055(3) Uani 1 1 d . . . H19 H 1.0651 -0.1257 0.3140 0.065 Uiso 1 1 calc R . . C20 C 0.9719(5) -0.0856(9) 0.3506(6) 0.054(2) Uani 1 1 d . . . H20 H 0.9761 -0.1317 0.4016 0.065 Uiso 1 1 calc R . . C21 C 0.9124(4) -0.0195(9) 0.3271(5) 0.044(2) Uani 1 1 d . . . C22 C 0.8535(5) -0.0921(10) 0.4448(6) 0.057(3) Uani 1 1 d . . . H22A H 0.8894 -0.0704 0.4919 0.069 Uiso 1 1 calc R . . H22B H 0.8610 -0.1739 0.4280 0.069 Uiso 1 1 calc R . . C23 C 0.7833(5) -0.0780(9) 0.4737(6) 0.052(2) Uani 1 1 d . . . H23A H 0.7790 -0.1258 0.5259 0.062 Uiso 1 1 calc R . . H23B H 0.7747 0.0046 0.4875 0.062 Uiso 1 1 calc R . . C24 C 0.6664(5) -0.1166(11) 0.4258(7) 0.063(3) Uani 1 1 d . . . H24A H 0.6570 -0.0440 0.4569 0.076 Uiso 1 1 calc R . . H24B H 0.6592 -0.1837 0.4638 0.076 Uiso 1 1 calc R . . C25 C 0.6199(5) -0.1252(10) 0.3439(7) 0.061(3) Uani 1 1 d . . . H25A H 0.5715 -0.1167 0.3557 0.074 Uiso 1 1 calc R . . H25B H 0.6304 -0.0624 0.3037 0.074 Uiso 1 1 calc R . . C26 C 0.6067(6) -0.2426(11) 0.2151(8) 0.067(3) Uani 1 1 d U . . H26A H 0.6214 -0.1727 0.1848 0.081 Uiso 1 1 calc R . . H26B H 0.5559 -0.2473 0.2059 0.081 Uiso 1 1 calc R . . C27 C 0.6375(5) -0.3495(12) 0.1807(7) 0.073(3) Uani 1 1 d U . . H27A H 0.6325 -0.4148 0.2212 0.088 Uiso 1 1 calc R . . H27B H 0.6114 -0.3699 0.1245 0.088 Uiso 1 1 calc R . . C28 C 0.7541(5) -0.3503(11) 0.2453(7) 0.064(3) Uani 1 1 d . . . H28A H 0.7484 -0.4276 0.2719 0.076 Uiso 1 1 calc R . . H28B H 0.7456 -0.2893 0.2879 0.076 Uiso 1 1 calc R . . C29 C 0.8248(5) -0.3384(9) 0.2192(7) 0.057(3) Uani 1 1 d . . . H29A H 0.8594 -0.3485 0.2701 0.068 Uiso 1 1 calc R . . H29B H 0.8329 -0.3985 0.1758 0.068 Uiso 1 1 calc R . . C30 C 0.8802(4) -0.2065(8) 0.1290(5) 0.041(2) Uani 1 1 d . . . C31 C 0.9408(4) -0.2664(8) 0.1329(6) 0.041(2) Uani 1 1 d . . . H31 H 0.9505 -0.3246 0.1759 0.049 Uiso 1 1 calc R . . C32 C 0.9882(4) -0.2445(9) 0.0761(7) 0.051(3) Uani 1 1 d . . . H32 H 1.0294 -0.2889 0.0790 0.062 Uiso 1 1 calc R . . C33 C 0.9758(4) -0.1577(9) 0.0148(6) 0.046(2) Uani 1 1 d . . . H33 H 1.0080 -0.1427 -0.0253 0.056 Uiso 1 1 calc R . . C34 C 0.9155(4) -0.0923(9) 0.0126(5) 0.046(2) Uani 1 1 d . . . H34 H 0.9073 -0.0311 -0.0285 0.055 Uiso 1 1 calc R . . C35 C 0.8682(4) -0.1149(8) 0.0683(5) 0.0356(18) Uani 1 1 d . . . Co1 Co 0.77272(5) 0.07928(10) 0.13309(6) 0.0319(3) Uani 1 1 d . . . I1 I 0.82492(3) 0.22802(6) 0.03683(4) 0.0464(2) Uani 1 1 d . . . N1 N 0.8052(3) -0.0546(6) 0.0635(4) 0.0333(15) Uani 1 1 d . . . N2 N 0.6930(3) 0.0637(6) 0.0543(4) 0.0334(15) Uani 1 1 d . . . N3 N 0.7261(3) 0.1953(6) 0.1873(4) 0.0341(15) Uani 1 1 d . . . N4 N 0.8461(3) 0.1113(6) 0.2286(4) 0.0350(15) Uani 1 1 d . . . O1 O 0.8559(3) -0.0173(7) 0.3730(4) 0.0596(19) Uani 1 1 d . . . O2 O 0.7360(3) -0.1162(7) 0.4037(4) 0.0554(18) Uani 1 1 d . . . O3 O 0.6297(4) -0.2347(7) 0.3066(5) 0.064(2) Uani 1 1 d . . . O4 O 0.7073(4) -0.3378(8) 0.1689(4) 0.073(2) Uani 1 1 d . . . O5 O 0.8304(3) -0.2243(6) 0.1832(4) 0.0504(16) Uani 1 1 d . . . O6 O 0.7376(3) -0.0423(6) 0.2119(3) 0.0440(15) 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 0.033(4) 0.051(6) 0.035(4) -0.008(4) 0.001(3) -0.005(4) C2 0.031(4) 0.034(5) 0.036(4) -0.002(4) -0.002(3) -0.006(3) C3 0.041(4) 0.048(6) 0.047(5) -0.012(4) -0.012(4) -0.002(4) C4 0.036(4) 0.052(6) 0.058(5) -0.007(5) -0.013(4) 0.000(4) C5 0.029(4) 0.059(6) 0.033(4) 0.008(4) -0.004(3) 0.004(4) C6 0.032(4) 0.058(7) 0.036(4) -0.002(4) -0.007(3) 0.010(4) C7 0.038(5) 0.064(7) 0.056(5) 0.004(5) -0.001(4) 0.012(5) C8 0.053(6) 0.085(8) 0.058(6) -0.003(5) 0.013(5) -0.007(6) C9 0.062(6) 0.048(7) 0.061(6) 0.015(5) -0.013(5) -0.003(5) C10 0.099(9) 0.102(11) 0.067(7) 0.014(8) -0.033(7) -0.001(9) C11 0.038(4) 0.045(6) 0.035(4) -0.001(4) -0.006(3) 0.007(4) C12 0.048(5) 0.071(8) 0.053(5) -0.011(5) -0.009(4) 0.021(5) C13 0.057(6) 0.059(7) 0.044(5) -0.017(5) -0.007(4) 0.008(5) C14 0.046(5) 0.037(5) 0.036(4) 0.004(4) -0.009(4) 0.000(4) C15 0.045(5) 0.035(5) 0.037(4) -0.007(4) -0.014(4) 0.001(4) C16 0.032(4) 0.038(5) 0.033(4) -0.004(4) -0.010(3) -0.007(3) C17 0.036(4) 0.059(6) 0.035(4) 0.000(4) -0.005(3) -0.014(4) C18 0.034(4) 0.050(6) 0.061(5) -0.011(5) -0.001(4) -0.006(4) C19 0.035(4) 0.049(6) 0.076(7) -0.002(5) -0.008(5) 0.004(4) C20 0.051(5) 0.053(7) 0.054(5) 0.010(5) -0.011(4) 0.009(5) C21 0.038(4) 0.055(6) 0.037(4) 0.009(4) 0.001(3) 0.005(4) C22 0.053(5) 0.071(8) 0.046(5) 0.028(5) -0.002(4) -0.001(5) C23 0.065(6) 0.051(6) 0.039(4) -0.001(4) 0.007(4) -0.007(5) C24 0.052(6) 0.079(9) 0.061(6) -0.018(6) 0.016(5) -0.001(5) C25 0.052(6) 0.055(7) 0.079(7) -0.003(6) 0.016(5) 0.000(5) C26 0.056(6) 0.078(8) 0.067(7) 0.002(6) 0.005(5) -0.007(5) C27 0.059(6) 0.094(9) 0.068(6) -0.006(6) 0.017(5) -0.020(6) C28 0.064(6) 0.070(8) 0.059(6) 0.024(6) 0.018(5) 0.001(6) C29 0.057(6) 0.049(7) 0.067(6) 0.027(5) 0.016(5) 0.004(5) C30 0.032(4) 0.052(6) 0.038(4) -0.006(4) 0.002(3) -0.004(4) C31 0.040(4) 0.032(5) 0.047(5) 0.005(4) -0.008(4) 0.002(4) C32 0.030(4) 0.058(7) 0.065(6) -0.014(5) 0.002(4) 0.006(4) C33 0.039(4) 0.046(6) 0.055(5) -0.005(5) 0.011(4) -0.004(4) C34 0.044(5) 0.054(6) 0.039(4) 0.002(4) 0.002(4) -0.005(4) C35 0.032(4) 0.042(5) 0.032(4) -0.001(4) -0.004(3) 0.000(4) Co1 0.0268(5) 0.0403(7) 0.0273(5) 0.0011(5) -0.0035(4) -0.0016(4) I1 0.0426(3) 0.0551(5) 0.0401(3) 0.0117(3) -0.0018(2) -0.0078(3) N1 0.031(3) 0.035(4) 0.033(3) -0.006(3) 0.000(3) 0.002(3) N2 0.030(3) 0.032(4) 0.037(3) -0.013(3) -0.004(3) -0.004(3) N3 0.038(3) 0.030(4) 0.033(3) -0.011(3) -0.002(3) 0.003(3) N4 0.033(3) 0.038(4) 0.031(3) 0.002(3) -0.009(3) -0.002(3) O1 0.053(4) 0.077(5) 0.050(3) 0.034(4) 0.012(3) 0.018(4) O2 0.045(3) 0.075(5) 0.046(3) -0.013(3) 0.007(3) -0.002(3) O3 0.070(5) 0.061(5) 0.061(4) -0.005(4) 0.005(4) 0.000(4) O4 0.053(4) 0.111(7) 0.057(4) 0.005(5) 0.017(3) -0.005(4) O5 0.046(3) 0.045(4) 0.064(4) 0.022(3) 0.018(3) 0.008(3) O6 0.038(3) 0.057(4) 0.037(3) 0.001(3) 0.006(2) -0.005(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 N1 1.299(9) . ? C1 C2 1.372(11) . ? C1 H1 0.9500 . ? C2 N2 1.375(10) . ? C2 C3 1.405(10) . ? C3 C4 1.384(13) . ? C3 H3 0.9500 . ? C4 C5 1.423(12) . ? C4 H4 0.9500 . ? C5 N2 1.341(10) . ? C5 C6 1.488(13) . ? C6 C9 1.515(14) . ? C6 C11 1.536(11) . ? C6 C7 1.555(12) . ? C7 C8 1.473(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.512(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.325(10) . ? C11 C12 1.397(13) . ? C12 C13 1.386(12) . ? C12 H12 0.9500 . ? C13 C14 1.390(13) . ? C13 H13 0.9500 . ? C14 N3 1.395(10) . ? C14 C15 1.415(12) . ? C15 N4 1.299(11) . ? C15 H15 0.9500 . ? C16 C17 1.373(11) . ? C16 C21 1.384(11) . ? C16 N4 1.417(10) . ? C17 C18 1.377(13) . ? C17 H17 0.9500 . ? C18 C19 1.369(14) . ? C18 H18 0.9500 . ? C19 C20 1.381(14) . ? C19 H19 0.9500 . ? C20 C21 1.404(12) . ? C20 H20 0.9500 . ? C21 O1 1.382(10) . ? C22 O1 1.412(10) . ? C22 C23 1.501(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.417(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O2 1.443(10) . ? C24 C25 1.484(14) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O3 1.406(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O3 1.447(13) . ? C26 C27 1.492(17) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O4 1.405(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O4 1.424(12) . ? C28 C29 1.491(13) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O5 1.432(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.367(12) . ? C30 O5 1.373(10) . ? C30 C35 1.415(12) . ? C31 C32 1.373(13) . ? C31 H31 0.9500 . ? C32 C33 1.381(14) . ? C32 H32 0.9500 . ? C33 C34 1.396(12) . ? C33 H33 0.9500 . ? C34 C35 1.362(11) . ? C34 H34 0.9500 . ? C35 N1 1.408(10) . ? Co1 N3 1.867(6) . ? Co1 N2 1.882(6) . ? Co1 N4 1.983(6) . ? Co1 N1 2.022(7) . ? Co1 O6 2.026(6) . ? Co1 I1 2.5568(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 119.6(8) . . ? N1 C1 H1 120.2 . . ? C2 C1 H1 120.2 . . ? C1 C2 N2 113.7(7) . . ? C1 C2 C3 138.3(8) . . ? N2 C2 C3 107.9(7) . . ? C4 C3 C2 106.0(8) . . ? C4 C3 H3 127.0 . . ? C2 C3 H3 127.0 . . ? C3 C4 C5 109.1(8) . . ? C3 C4 H4 125.4 . . ? C5 C4 H4 125.4 . . ? N2 C5 C4 106.1(8) . . ? N2 C5 C6 124.7(7) . . ? C4 C5 C6 129.2(7) . . ? C5 C6 C9 109.2(8) . . ? C5 C6 C11 113.2(7) . . ? C9 C6 C11 106.7(8) . . ? C5 C6 C7 109.3(8) . . ? C9 C6 C7 110.9(7) . . ? C11 C6 C7 107.5(7) . . ? C8 C7 C6 115.2(8) . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 117.8(10) . . ? C10 C9 H9A 107.9 . . ? C6 C9 H9A 107.9 . . ? C10 C9 H9B 107.9 . . ? C6 C9 H9B 107.9 . . ? H9A C9 H9B 107.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 109.1(7) . . ? N3 C11 C6 122.8(7) . . ? C12 C11 C6 128.0(8) . . ? C13 C12 C11 108.2(8) . . ? C13 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? C12 C13 C14 105.7(8) . . ? C12 C13 H13 127.2 . . ? C14 C13 H13 127.2 . . ? C13 C14 N3 108.9(7) . . ? C13 C14 C15 139.2(8) . . ? N3 C14 C15 110.6(8) . . ? N4 C15 C14 119.5(7) . . ? N4 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C21 119.4(8) . . ? C17 C16 N4 121.4(7) . . ? C21 C16 N4 119.2(7) . . ? C16 C17 C18 121.6(8) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C19 C18 C17 118.8(9) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 121.6(9) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C21 118.7(9) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? O1 C21 C16 115.8(7) . . ? O1 C21 C20 124.3(8) . . ? C16 C21 C20 119.9(8) . . ? O1 C22 C23 106.5(8) . . ? O1 C22 H22A 110.4 . . ? C23 C22 H22A 110.4 . . ? O1 C22 H22B 110.4 . . ? C23 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? O2 C23 C22 106.0(7) . . ? O2 C23 H23A 110.5 . . ? C22 C23 H23A 110.5 . . ? O2 C23 H23B 110.5 . . ? C22 C23 H23B 110.5 . . ? H23A C23 H23B 108.7 . . ? O2 C24 C25 107.5(8) . . ? O2 C24 H24A 110.2 . . ? C25 C24 H24A 110.2 . . ? O2 C24 H24B 110.2 . . ? C25 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? O3 C25 C24 108.3(9) . . ? O3 C25 H25A 110.0 . . ? C24 C25 H25A 110.0 . . ? O3 C25 H25B 110.0 . . ? C24 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? O3 C26 C27 108.1(9) . . ? O3 C26 H26A 110.1 . . ? C27 C26 H26A 110.1 . . ? O3 C26 H26B 110.1 . . ? C27 C26 H26B 110.1 . . ? H26A C26 H26B 108.4 . . ? O4 C27 C26 114.0(10) . . ? O4 C27 H27A 108.7 . . ? C26 C27 H27A 108.7 . . ? O4 C27 H27B 108.7 . . ? C26 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? O4 C28 C29 107.1(8) . . ? O4 C28 H28A 110.3 . . ? C29 C28 H28A 110.3 . . ? O4 C28 H28B 110.3 . . ? C29 C28 H28B 110.3 . . ? H28A C28 H28B 108.6 . . ? O5 C29 C28 107.7(8) . . ? O5 C29 H29A 110.2 . . ? C28 C29 H29A 110.2 . . ? O5 C29 H29B 110.2 . . ? C28 C29 H29B 110.2 . . ? H29A C29 H29B 108.5 . . ? C31 C30 O5 124.8(8) . . ? C31 C30 C35 118.7(8) . . ? O5 C30 C35 116.4(7) . . ? C30 C31 C32 121.7(9) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C31 C32 C33 119.7(8) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 119.2(8) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 121.0(9) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 N1 121.8(8) . . ? C34 C35 C30 119.5(8) . . ? N1 C35 C30 118.6(7) . . ? N3 Co1 N2 87.2(3) . . ? N3 Co1 N4 83.1(3) . . ? N2 Co1 N4 169.9(3) . . ? N3 Co1 N1 169.0(3) . . ? N2 Co1 N1 82.3(3) . . ? N4 Co1 N1 107.3(3) . . ? N3 Co1 O6 90.1(3) . . ? N2 Co1 O6 90.9(3) . . ? N4 Co1 O6 86.6(2) . . ? N1 Co1 O6 87.0(3) . . ? N3 Co1 I1 92.1(2) . . ? N2 Co1 I1 92.2(2) . . ? N4 Co1 I1 90.7(2) . . ? N1 Co1 I1 91.4(2) . . ? O6 Co1 I1 176.27(16) . . ? C1 N1 C35 118.2(7) . . ? C1 N1 Co1 109.7(5) . . ? C35 N1 Co1 132.0(5) . . ? C5 N2 C2 110.9(6) . . ? C5 N2 Co1 134.3(6) . . ? C2 N2 Co1 114.5(5) . . ? C11 N3 C14 108.0(7) . . ? C11 N3 Co1 136.0(6) . . ? C14 N3 Co1 115.8(6) . . ? C15 N4 C16 119.1(6) . . ? C15 N4 Co1 110.7(5) . . ? C16 N4 Co1 128.6(5) . . ? C21 O1 C22 119.8(7) . . ? C23 O2 C24 111.7(7) . . ? C25 O3 C26 114.8(9) . . ? C27 O4 C28 115.2(8) . . ? C30 O5 C29 117.8(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 2.2(12) . . . . ? N1 C1 C2 C3 -175.1(10) . . . . ? C1 C2 C3 C4 177.5(10) . . . . ? N2 C2 C3 C4 0.1(10) . . . . ? C2 C3 C4 C5 0.2(11) . . . . ? C3 C4 C5 N2 -0.5(11) . . . . ? C3 C4 C5 C6 179.6(9) . . . . ? N2 C5 C6 C9 104.9(9) . . . . ? C4 C5 C6 C9 -75.2(12) . . . . ? N2 C5 C6 C11 -13.8(13) . . . . ? C4 C5 C6 C11 166.1(9) . . . . ? N2 C5 C6 C7 -133.6(9) . . . . ? C4 C5 C6 C7 46.3(12) . . . . ? C5 C6 C7 C8 64.8(10) . . . . ? C9 C6 C7 C8 -174.8(9) . . . . ? C11 C6 C7 C8 -58.5(11) . . . . ? C5 C6 C9 C10 61.6(12) . . . . ? C11 C6 C9 C10 -175.6(10) . . . . ? C7 C6 C9 C10 -58.9(13) . . . . ? C5 C6 C11 N3 15.9(13) . . . . ? C9 C6 C11 N3 -104.3(10) . . . . ? C7 C6 C11 N3 136.6(9) . . . . ? C5 C6 C11 C12 -169.1(10) . . . . ? C9 C6 C11 C12 70.7(13) . . . . ? C7 C6 C11 C12 -48.3(14) . . . . ? N3 C11 C12 C13 -1.9(13) . . . . ? C6 C11 C12 C13 -177.5(9) . . . . ? C11 C12 C13 C14 3.8(13) . . . . ? C12 C13 C14 N3 -4.4(12) . . . . ? C12 C13 C14 C15 -168.8(12) . . . . ? C13 C14 C15 N4 171.0(12) . . . . ? N3 C14 C15 N4 6.7(12) . . . . ? C21 C16 C17 C18 -0.8(13) . . . . ? N4 C16 C17 C18 -177.5(8) . . . . ? C16 C17 C18 C19 -0.8(14) . . . . ? C17 C18 C19 C20 1.8(15) . . . . ? C18 C19 C20 C21 -1.2(15) . . . . ? C17 C16 C21 O1 -177.7(8) . . . . ? N4 C16 C21 O1 -0.9(12) . . . . ? C17 C16 C21 C20 1.4(13) . . . . ? N4 C16 C21 C20 178.2(8) . . . . ? C19 C20 C21 O1 178.5(9) . . . . ? C19 C20 C21 C16 -0.5(15) . . . . ? O1 C22 C23 O2 62.8(10) . . . . ? O2 C24 C25 O3 66.1(11) . . . . ? O3 C26 C27 O4 -76.4(12) . . . . ? O4 C28 C29 O5 61.3(12) . . . . ? O5 C30 C31 C32 179.6(8) . . . . ? C35 C30 C31 C32 -4.0(13) . . . . ? C30 C31 C32 C33 1.9(14) . . . . ? C31 C32 C33 C34 1.0(14) . . . . ? C32 C33 C34 C35 -1.7(14) . . . . ? C33 C34 C35 N1 -176.0(8) . . . . ? C33 C34 C35 C30 -0.4(13) . . . . ? C31 C30 C35 C34 3.2(12) . . . . ? O5 C30 C35 C34 180.0(8) . . . . ? C31 C30 C35 N1 178.9(7) . . . . ? O5 C30 C35 N1 -4.3(11) . . . . ? C2 C1 N1 C35 -178.9(8) . . . . ? C2 C1 N1 Co1 0.3(10) . . . . ? C34 C35 N1 C1 78.1(11) . . . . ? C30 C35 N1 C1 -97.5(9) . . . . ? C34 C35 N1 Co1 -101.0(9) . . . . ? C30 C35 N1 Co1 83.4(10) . . . . ? N3 Co1 N1 C1 14.3(18) . . . . ? N2 Co1 N1 C1 -1.9(6) . . . . ? N4 Co1 N1 C1 175.0(6) . . . . ? O6 Co1 N1 C1 89.5(6) . . . . ? I1 Co1 N1 C1 -93.9(6) . . . . ? N3 Co1 N1 C35 -166.6(13) . . . . ? N2 Co1 N1 C35 177.2(8) . . . . ? N4 Co1 N1 C35 -5.9(8) . . . . ? O6 Co1 N1 C35 -91.4(7) . . . . ? I1 Co1 N1 C35 85.2(7) . . . . ? C4 C5 N2 C2 0.6(10) . . . . ? C6 C5 N2 C2 -179.5(8) . . . . ? C4 C5 N2 Co1 -172.8(7) . . . . ? C6 C5 N2 Co1 7.2(14) . . . . ? C1 C2 N2 C5 -178.5(7) . . . . ? C3 C2 N2 C5 -0.4(10) . . . . ? C1 C2 N2 Co1 -3.8(9) . . . . ? C3 C2 N2 Co1 174.3(6) . . . . ? N3 Co1 N2 C5 -0.7(9) . . . . ? N4 Co1 N2 C5 14(2) . . . . ? N1 Co1 N2 C5 176.2(9) . . . . ? O6 Co1 N2 C5 89.4(8) . . . . ? I1 Co1 N2 C5 -92.7(8) . . . . ? N3 Co1 N2 C2 -173.9(6) . . . . ? N4 Co1 N2 C2 -159.5(15) . . . . ? N1 Co1 N2 C2 3.1(5) . . . . ? O6 Co1 N2 C2 -83.8(6) . . . . ? I1 Co1 N2 C2 94.2(5) . . . . ? C12 C11 N3 C14 -0.9(11) . . . . ? C6 C11 N3 C14 175.0(8) . . . . ? C12 C11 N3 Co1 172.1(8) . . . . ? C6 C11 N3 Co1 -12.1(14) . . . . ? C13 C14 N3 C11 3.3(11) . . . . ? C15 C14 N3 C11 172.5(8) . . . . ? C13 C14 N3 Co1 -171.2(7) . . . . ? C15 C14 N3 Co1 -2.0(10) . . . . ? N2 Co1 N3 C11 3.5(9) . . . . ? N4 Co1 N3 C11 -174.0(9) . . . . ? N1 Co1 N3 C11 -13(2) . . . . ? O6 Co1 N3 C11 -87.5(9) . . . . ? I1 Co1 N3 C11 95.6(9) . . . . ? N2 Co1 N3 C14 176.0(6) . . . . ? N4 Co1 N3 C14 -1.5(6) . . . . ? N1 Co1 N3 C14 159.9(13) . . . . ? O6 Co1 N3 C14 85.1(6) . . . . ? I1 Co1 N3 C14 -91.9(6) . . . . ? C14 C15 N4 C16 -174.4(8) . . . . ? C14 C15 N4 Co1 -7.8(11) . . . . ? C17 C16 N4 C15 -126.2(9) . . . . ? C21 C16 N4 C15 57.1(11) . . . . ? C17 C16 N4 Co1 70.0(10) . . . . ? C21 C16 N4 Co1 -106.7(8) . . . . ? N3 Co1 N4 C15 5.0(6) . . . . ? N2 Co1 N4 C15 -9(2) . . . . ? N1 Co1 N4 C15 -171.4(6) . . . . ? O6 Co1 N4 C15 -85.6(6) . . . . ? I1 Co1 N4 C15 97.0(6) . . . . ? N3 Co1 N4 C16 169.9(7) . . . . ? N2 Co1 N4 C16 155.5(15) . . . . ? N1 Co1 N4 C16 -6.4(7) . . . . ? O6 Co1 N4 C16 79.4(7) . . . . ? I1 Co1 N4 C16 -98.1(6) . . . . ? C16 C21 O1 C22 173.7(9) . . . . ? C20 C21 O1 C22 -5.3(15) . . . . ? C23 C22 O1 C21 -173.9(8) . . . . ? C22 C23 O2 C24 175.1(9) . . . . ? C25 C24 O2 C23 164.6(9) . . . . ? C24 C25 O3 C26 -160.1(9) . . . . ? C27 C26 O3 C25 164.5(9) . . . . ? C26 C27 O4 C28 80.1(13) . . . . ? C29 C28 O4 C27 178.5(10) . . . . ? C31 C30 O5 C29 -28.5(13) . . . . ? C35 C30 O5 C29 155.0(8) . . . . ? C28 C29 O5 C30 -158.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.024 _refine_diff_density_min -2.120 _refine_diff_density_rms 0.228