# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Scott, Peter' _publ_contact_author_email peter.scott@warwick.ac.uk _publ_section_title ; TTF salts of optically pure cobalt pyridine amidates; detection of soluble assemblies with stoichiometry corresponding to the solid state ; _publ_author_name P.Scott # Attachment '- 18C6KCoL1.cif' data_nc17 _database_code_depnum_ccdc_archive 'CCDC 786086' #TrackingRef '- 18C6KCoL1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H71 Co K N7 O11' _chemical_formula_weight 1164.27 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' K K 0.2009 0.2494 '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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3421(2) _cell_length_b 23.3274(5) _cell_length_c 13.6888(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.304(2) _cell_angle_gamma 90.00 _cell_volume 2890.66(12) _cell_formula_units_Z 2 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used 15568 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 29.32 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 1.0\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model with freely rotating methyl groups except the Hs on the water which were located a difference map. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameters equal to 1.2 (or 1.5 for methyl or OH hydrogen atoms) times the equivalent isotropic displacement parameter of the atom to which the H-atom is attached. Several ellipsoids of atoms in one wing of the crown were rather elongated. SIMU restraints were used to make these atoms have similar thermal parameters to neighbouring atoms in the crown. ; _diffrn_ambient_temperature 95(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 28920 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 29.38 _reflns_number_total 13656 _reflns_number_gt 11264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 6290 Friedel pairs' _refine_ls_abs_structure_Flack 0.012(9) _chemical_absolute_configuration rmad _refine_ls_number_reflns 13656 _refine_ls_number_parameters 731 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.60490(3) 0.073356(14) 0.35933(2) 0.01127(8) Uani 1 1 d . . . K1 K 0.31942(6) -0.10274(3) -0.02900(5) 0.01980(13) Uani 1 1 d . . . O1 O 0.4628(2) -0.03989(8) 0.12998(14) 0.0204(4) Uani 1 1 d . . . N1 N 0.6078(2) 0.02850(9) 0.23385(16) 0.0141(5) Uani 1 1 d . . . C1 C 0.7508(3) 0.12250(13) 0.0946(2) 0.0258(7) Uani 1 1 d . . . H1A H 0.8160 0.1335 0.1567 0.031 Uiso 1 1 calc R . . N2 N 0.4348(2) 0.03008(9) 0.35086(16) 0.0127(4) Uani 1 1 d . . . O2 O 0.37962(19) 0.08515(8) 0.57731(14) 0.0190(4) Uani 1 1 d . . . C2 C 0.7197(4) 0.16095(14) 0.0153(3) 0.0350(8) Uani 1 1 d . . . H2A H 0.7623 0.1982 0.0237 0.042 Uiso 1 1 calc R . . N3 N 0.5539(2) 0.10243(9) 0.48349(16) 0.0121(4) Uani 1 1 d . . . C3 C 0.6275(4) 0.14576(14) -0.0757(3) 0.0407(9) Uani 1 1 d . . . H3A H 0.6070 0.1722 -0.1302 0.049 Uiso 1 1 calc R . . O3 O 0.58762(19) 0.22421(8) 0.21321(14) 0.0185(4) Uani 1 1 d . . . C4 C 0.5649(4) 0.09170(14) -0.0871(2) 0.0382(9) Uani 1 1 d . . . H4A H 0.5013 0.0810 -0.1500 0.046 Uiso 1 1 calc R . . O4 O 0.98299(18) 0.01744(8) 0.54465(14) 0.0173(4) Uani 1 1 d . . . N4 N 0.5156(2) 0.14033(9) 0.27915(16) 0.0138(5) Uani 1 1 d . . . C5 C 0.5938(3) 0.05339(13) -0.0085(2) 0.0266(7) Uani 1 1 d . . . H5A H 0.5490 0.0166 -0.0177 0.032 Uiso 1 1 calc R . . N5 N 0.7740(2) 0.11758(9) 0.37637(16) 0.0125(4) Uani 1 1 d . . . O5 O 0.3836(3) -0.20263(9) 0.08793(16) 0.0330(5) Uani 1 1 d U . . C6 C 0.6881(3) 0.06757(13) 0.0851(2) 0.0201(6) Uani 1 1 d . . . N6 N 0.7447(2) 0.01925(9) 0.44167(16) 0.0123(4) Uani 1 1 d . . . O6 O 0.5866(2) -0.15712(9) -0.02427(16) 0.0272(5) Uani 1 1 d . . . C7 C 0.7166(3) 0.02473(11) 0.1705(2) 0.0165(6) Uani 1 1 d . . . H7A H 0.7024 -0.0140 0.1381 0.020 Uiso 1 1 calc R . . O7 O 0.4567(2) -0.09031(8) -0.19611(15) 0.0232(4) Uani 1 1 d . . . N7 N 0.0911(4) 0.21822(17) 0.7903(3) 0.0749(12) Uani 1 1 d . . . C8 C 0.8764(3) 0.02637(13) 0.2334(2) 0.0220(6) Uani 1 1 d . . . H8A H 0.8878 0.0000 0.2906 0.033 Uiso 1 1 calc R . . H8B H 0.9011 0.0654 0.2584 0.033 Uiso 1 1 calc R . . H8C H 0.9426 0.0147 0.1915 0.033 Uiso 1 1 calc R . . O8 O 0.2091(2) -0.02293(9) -0.19270(15) 0.0280(5) Uani 1 1 d . . . C9 C 0.4930(3) -0.00716(11) 0.2047(2) 0.0153(6) Uani 1 1 d . . . O9 O 0.0205(2) -0.06235(11) -0.06705(16) 0.0355(5) Uani 1 1 d U . . C10 C 0.3943(3) -0.00741(10) 0.27541(19) 0.0130(5) Uani 1 1 d . . . O10 O 0.1379(2) -0.13471(10) 0.09388(16) 0.0326(4) Uani 1 1 d U . . C11 C 0.2768(3) -0.04403(11) 0.2725(2) 0.0162(6) Uani 1 1 d . . . H11A H 0.2471 -0.0711 0.2196 0.019 Uiso 1 1 calc R . . C12 C 0.2030(3) -0.04009(11) 0.3493(2) 0.0181(6) Uani 1 1 d . . . H12A H 0.1227 -0.0651 0.3491 0.022 Uiso 1 1 calc R . . C13 C 0.2458(3) -0.00008(11) 0.4260(2) 0.0171(6) Uani 1 1 d . . . H13A H 0.1947 0.0033 0.4777 0.021 Uiso 1 1 calc R . . C14 C 0.3659(3) 0.03489(11) 0.4247(2) 0.0140(5) Uani 1 1 d . . . C15 C 0.4341(3) 0.07787(13) 0.50379(19) 0.0152(5) Uani 1 1 d . . . C16 C 0.6471(3) 0.14088(11) 0.5590(2) 0.0154(5) Uani 1 1 d . . . H16A H 0.7413 0.1452 0.5374 0.019 Uiso 1 1 calc R . . C17 C 0.6925(3) 0.11513(12) 0.6654(2) 0.0220(6) Uani 1 1 d . . . H17A H 0.7377 0.0775 0.6626 0.033 Uiso 1 1 calc R . . H17B H 0.6050 0.1109 0.6922 0.033 Uiso 1 1 calc R . . H17C H 0.7638 0.1406 0.7095 0.033 Uiso 1 1 calc R . . C18 C 0.5868(3) 0.20153(11) 0.5603(2) 0.0160(6) Uani 1 1 d . . . C19 C 0.4537(3) 0.21357(13) 0.5845(2) 0.0236(6) Uani 1 1 d . . . H19A H 0.3947 0.1830 0.5987 0.028 Uiso 1 1 calc R . . C20 C 0.4062(3) 0.26953(13) 0.5882(2) 0.0275(7) Uani 1 1 d . . . H20A H 0.3154 0.2770 0.6054 0.033 Uiso 1 1 calc R . . C21 C 0.4897(3) 0.31463(13) 0.5673(2) 0.0249(7) Uani 1 1 d . . . H21A H 0.4567 0.3530 0.5698 0.030 Uiso 1 1 calc R . . C22 C 0.6216(3) 0.30338(12) 0.5425(2) 0.0245(7) Uani 1 1 d . . . H22A H 0.6799 0.3341 0.5279 0.029 Uiso 1 1 calc R . . C23 C 0.6689(3) 0.24717(12) 0.5390(2) 0.0200(6) Uani 1 1 d . . . H23A H 0.7595 0.2399 0.5217 0.024 Uiso 1 1 calc R . . C24 C 0.1417(3) 0.21068(12) 0.1640(2) 0.0193(6) Uani 1 1 d . . . H24A H 0.1041 0.1852 0.1097 0.023 Uiso 1 1 calc R . . C25 C 0.0609(3) 0.25880(13) 0.1759(2) 0.0215(6) Uani 1 1 d . . . H25A H -0.0317 0.2659 0.1299 0.026 Uiso 1 1 calc R . . C26 C 0.1134(3) 0.29648(12) 0.2539(2) 0.0199(6) Uani 1 1 d . . . H26A H 0.0583 0.3297 0.2616 0.024 Uiso 1 1 calc R . . C27 C 0.2486(3) 0.28527(12) 0.3213(2) 0.0197(6) Uani 1 1 d . . . H27A H 0.2863 0.3110 0.3754 0.024 Uiso 1 1 calc R . . C28 C 0.3285(3) 0.23670(11) 0.3096(2) 0.0167(6) Uani 1 1 d . . . H28A H 0.4197 0.2292 0.3569 0.020 Uiso 1 1 calc R . . C29 C 0.2783(3) 0.19915(11) 0.2312(2) 0.0147(6) Uani 1 1 d . . . C30 C 0.3610(3) 0.14379(12) 0.2175(2) 0.0186(6) Uani 1 1 d . . . H30A H 0.3068 0.1119 0.2416 0.022 Uiso 1 1 calc R . . C31 C 0.3541(3) 0.13035(13) 0.1067(2) 0.0268(7) Uani 1 1 d . . . H31A H 0.3994 0.0929 0.1020 0.040 Uiso 1 1 calc R . . H31B H 0.4078 0.1599 0.0793 0.040 Uiso 1 1 calc R . . H31C H 0.2508 0.1297 0.0679 0.040 Uiso 1 1 calc R . . C32 C 0.6107(3) 0.18054(11) 0.2675(2) 0.0144(5) Uani 1 1 d . . . C33 C 0.7630(3) 0.16891(11) 0.3325(2) 0.0141(5) Uani 1 1 d . . . C34 C 0.8861(3) 0.20419(11) 0.3489(2) 0.0166(6) Uani 1 1 d . . . H34A H 0.8808 0.2409 0.3180 0.020 Uiso 1 1 calc R . . C35 C 1.0181(3) 0.18453(12) 0.4120(2) 0.0187(6) Uani 1 1 d . . . H35A H 1.1040 0.2078 0.4232 0.022 Uiso 1 1 calc R . . C36 C 1.0251(3) 0.13148(12) 0.4583(2) 0.0183(6) Uani 1 1 d . . . H36A H 1.1146 0.1182 0.5017 0.022 Uiso 1 1 calc R . . C37 C 0.8981(3) 0.09821(11) 0.43956(19) 0.0137(5) Uani 1 1 d . . . C38 C 0.8794(3) 0.04016(11) 0.4810(2) 0.0148(5) Uani 1 1 d . . . C39 C 0.7085(3) -0.03917(11) 0.4685(2) 0.0154(6) Uani 1 1 d . . . H39A H 0.6081 -0.0475 0.4247 0.018 Uiso 1 1 calc R . . C40 C 0.6923(3) -0.04206(12) 0.5764(2) 0.0201(6) Uani 1 1 d . . . H40A H 0.6186 -0.0140 0.5854 0.030 Uiso 1 1 calc R . . H40B H 0.7875 -0.0335 0.6232 0.030 Uiso 1 1 calc R . . H40C H 0.6604 -0.0806 0.5900 0.030 Uiso 1 1 calc R . . C41 C 0.8106(3) -0.08520(11) 0.4427(2) 0.0147(5) Uani 1 1 d . . . C42 C 0.9236(3) -0.11075(12) 0.5153(2) 0.0189(6) Uani 1 1 d . . . H42A H 0.9441 -0.0977 0.5831 0.023 Uiso 1 1 calc R . . C43 C 1.0063(3) -0.15500(12) 0.4900(2) 0.0247(7) Uani 1 1 d . . . H43A H 1.0825 -0.1722 0.5405 0.030 Uiso 1 1 calc R . . C44 C 0.9791(3) -0.17427(12) 0.3921(2) 0.0217(6) Uani 1 1 d . . . H44A H 1.0365 -0.2045 0.3749 0.026 Uiso 1 1 calc R . . C45 C 0.8674(3) -0.14934(11) 0.3191(2) 0.0196(6) Uani 1 1 d . . . H45A H 0.8474 -0.1626 0.2515 0.024 Uiso 1 1 calc R . . C46 C 0.7843(3) -0.10487(11) 0.3445(2) 0.0172(6) Uani 1 1 d . . . H46A H 0.7084 -0.0877 0.2937 0.021 Uiso 1 1 calc R . . C47 C 0.1607(4) -0.18975(15) 0.1391(3) 0.0353(5) Uani 1 1 d U . . H47A H 0.1140 -0.2194 0.0896 0.042 Uiso 1 1 calc R . . H47B H 0.1151 -0.1916 0.1971 0.042 Uiso 1 1 calc R . . C48 C 0.3213(4) -0.20047(15) 0.1735(2) 0.0351(5) Uani 1 1 d U . . H48A H 0.3688 -0.1695 0.2197 0.042 Uiso 1 1 calc R . . H48B H 0.3391 -0.2372 0.2107 0.042 Uiso 1 1 calc R . . C49 C 0.5404(4) -0.20746(15) 0.1172(3) 0.0365(8) Uani 1 1 d . . . H49A H 0.5691 -0.2419 0.1598 0.044 Uiso 1 1 calc R . . H49B H 0.5834 -0.1734 0.1569 0.044 Uiso 1 1 calc R . . C50 C 0.5980(4) -0.21202(14) 0.0239(3) 0.0351(8) Uani 1 1 d . . . H50A H 0.7024 -0.2246 0.0424 0.042 Uiso 1 1 calc R . . H50B H 0.5397 -0.2407 -0.0228 0.042 Uiso 1 1 calc R . . C51 C 0.6321(3) -0.15984(14) -0.1160(2) 0.0282(7) Uani 1 1 d . . . H51A H 0.5729 -0.1890 -0.1611 0.034 Uiso 1 1 calc R . . H51B H 0.7373 -0.1711 -0.1019 0.034 Uiso 1 1 calc R . . C52 C 0.6112(3) -0.10256(14) -0.1660(2) 0.0264(7) Uani 1 1 d . . . H52A H 0.6626 -0.0728 -0.1187 0.032 Uiso 1 1 calc R . . H52B H 0.6532 -0.1027 -0.2256 0.032 Uiso 1 1 calc R . . C53 C 0.4218(4) -0.03959(14) -0.2543(3) 0.0310(7) Uani 1 1 d . . . H53A H 0.4590 -0.0426 -0.3159 0.037 Uiso 1 1 calc R . . H53B H 0.4700 -0.0062 -0.2148 0.037 Uiso 1 1 calc R . . C54 C 0.2597(4) -0.03144(14) -0.2824(2) 0.0303(7) Uani 1 1 d . . . H54A H 0.2340 0.0023 -0.3273 0.036 Uiso 1 1 calc R . . H54B H 0.2112 -0.0656 -0.3192 0.036 Uiso 1 1 calc R . . C55 C 0.0509(3) -0.01997(16) -0.2159(3) 0.0359(8) Uani 1 1 d . . . H55A H 0.0080 -0.0561 -0.2485 0.043 Uiso 1 1 calc R . . H55B H 0.0156 0.0120 -0.2633 0.043 Uiso 1 1 calc R . . C56 C 0.0033(4) -0.01082(16) -0.1218(3) 0.0405(9) Uani 1 1 d . . . H56A H 0.0637 0.0197 -0.0812 0.049 Uiso 1 1 calc R . . H56B H -0.1015 0.0013 -0.1379 0.049 Uiso 1 1 calc R . . C57 C -0.0184(4) -0.05753(16) 0.0253(3) 0.0365(5) Uani 1 1 d U . . H57A H -0.1195 -0.0417 0.0143 0.044 Uiso 1 1 calc R . . H57B H 0.0507 -0.0313 0.0708 0.044 Uiso 1 1 calc R . . C58 C -0.0120(3) -0.11519(16) 0.0714(3) 0.0365(5) Uani 1 1 d U . . H58A H -0.0470 -0.1134 0.1340 0.044 Uiso 1 1 calc R . . H58B H -0.0763 -0.1420 0.0241 0.044 Uiso 1 1 calc R . . C59 C 0.1283(4) 0.17503(17) 0.7674(3) 0.0435(9) Uani 1 1 d . . . C60 C 0.1773(5) 0.12043(17) 0.7372(3) 0.0498(10) Uani 1 1 d . . . H60A H 0.1935 0.0936 0.7939 0.075 Uiso 1 1 calc R . . H60B H 0.2698 0.1258 0.7167 0.075 Uiso 1 1 calc R . . H60C H 0.1017 0.1050 0.6805 0.075 Uiso 1 1 calc R . . O11 O 0.2483(2) -0.17871(10) -0.20020(19) 0.0296(5) Uani 1 1 d . . . H01A H 0.286(4) -0.2102(17) -0.196(3) 0.044 Uiso 1 1 d . . . H01B H 0.305(4) -0.1555(17) -0.218(3) 0.044 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.00975(15) 0.01081(16) 0.01449(17) -0.00055(15) 0.00535(12) -0.00053(15) K1 0.0180(3) 0.0228(3) 0.0203(3) -0.0046(3) 0.0078(2) -0.0022(2) O1 0.0222(10) 0.0223(10) 0.0170(11) -0.0077(8) 0.0054(8) -0.0023(8) N1 0.0151(10) 0.0146(11) 0.0138(12) 0.0014(9) 0.0060(8) 0.0014(9) C1 0.0351(17) 0.0241(16) 0.0204(16) -0.0023(13) 0.0112(13) -0.0039(13) N2 0.0116(10) 0.0111(10) 0.0164(12) 0.0029(9) 0.0053(9) 0.0004(8) O2 0.0184(9) 0.0220(11) 0.0204(10) -0.0037(8) 0.0120(7) -0.0014(8) C2 0.056(2) 0.0227(17) 0.030(2) -0.0039(14) 0.0177(16) -0.0088(15) N3 0.0124(10) 0.0137(11) 0.0114(11) -0.0036(9) 0.0054(8) -0.0007(9) C3 0.073(3) 0.0264(18) 0.0259(19) 0.0062(14) 0.0186(17) 0.0019(17) O3 0.0184(9) 0.0170(10) 0.0208(11) 0.0058(8) 0.0059(8) 0.0025(8) C4 0.059(2) 0.038(2) 0.0151(17) 0.0002(13) 0.0058(15) -0.0028(16) O4 0.0129(9) 0.0194(10) 0.0197(10) 0.0030(8) 0.0045(7) 0.0013(7) N4 0.0133(10) 0.0121(11) 0.0161(12) 0.0018(9) 0.0037(9) 0.0015(9) C5 0.0398(18) 0.0203(14) 0.0211(17) -0.0013(12) 0.0099(13) -0.0046(13) N5 0.0114(10) 0.0131(11) 0.0151(12) -0.0029(9) 0.0074(8) -0.0029(8) O5 0.0448(10) 0.0319(10) 0.0241(10) -0.0028(8) 0.0120(8) -0.0031(9) C6 0.0231(13) 0.0221(15) 0.0199(14) -0.0025(13) 0.0145(10) 0.0009(13) N6 0.0114(10) 0.0129(11) 0.0137(12) -0.0006(9) 0.0049(8) 0.0025(8) O6 0.0277(11) 0.0265(11) 0.0277(13) -0.0054(9) 0.0076(9) 0.0048(9) C7 0.0158(12) 0.0190(14) 0.0171(15) -0.0032(11) 0.0084(11) -0.0002(11) O7 0.0179(10) 0.0239(11) 0.0300(12) 0.0006(9) 0.0100(8) -0.0013(8) N7 0.079(3) 0.045(2) 0.105(3) -0.002(2) 0.029(2) 0.012(2) C8 0.0190(14) 0.0280(16) 0.0227(16) -0.0021(12) 0.0120(12) 0.0002(12) O8 0.0266(11) 0.0371(13) 0.0207(12) 0.0012(9) 0.0068(9) 0.0071(9) C9 0.0163(13) 0.0130(13) 0.0171(15) 0.0019(11) 0.0054(11) 0.0043(11) O9 0.0248(9) 0.0592(12) 0.0242(10) -0.0054(9) 0.0096(8) 0.0039(9) C10 0.0126(12) 0.0100(12) 0.0151(14) -0.0010(10) 0.0011(10) 0.0024(10) O10 0.0284(8) 0.0451(9) 0.0272(9) -0.0044(7) 0.0126(7) -0.0104(7) C11 0.0156(13) 0.0140(13) 0.0179(15) -0.0034(11) 0.0021(11) 0.0003(10) C12 0.0129(13) 0.0139(13) 0.0278(17) 0.0017(11) 0.0056(11) -0.0022(10) C13 0.0120(12) 0.0184(14) 0.0228(16) 0.0047(11) 0.0076(11) 0.0017(10) C14 0.0112(12) 0.0158(13) 0.0155(14) 0.0024(10) 0.0044(10) 0.0034(10) C15 0.0171(12) 0.0142(13) 0.0156(13) 0.0004(12) 0.0063(10) 0.0031(12) C16 0.0111(12) 0.0196(14) 0.0159(14) -0.0054(11) 0.0040(10) -0.0017(10) C17 0.0240(14) 0.0230(15) 0.0170(15) -0.0033(12) 0.0011(11) -0.0007(12) C18 0.0135(12) 0.0179(13) 0.0165(15) -0.0050(11) 0.0033(10) -0.0013(10) C19 0.0188(14) 0.0218(15) 0.0335(18) -0.0075(13) 0.0128(12) -0.0021(12) C20 0.0200(15) 0.0278(17) 0.0373(19) -0.0072(14) 0.0119(13) 0.0025(13) C21 0.0235(15) 0.0181(15) 0.0323(18) -0.0038(13) 0.0054(13) 0.0072(12) C22 0.0273(15) 0.0177(14) 0.0301(18) -0.0010(12) 0.0102(13) -0.0042(12) C23 0.0180(13) 0.0204(14) 0.0231(16) -0.0027(12) 0.0079(11) 0.0019(11) C24 0.0164(13) 0.0217(15) 0.0180(15) -0.0015(12) 0.0005(11) 0.0008(11) C25 0.0103(13) 0.0301(16) 0.0239(16) 0.0058(13) 0.0036(11) 0.0039(11) C26 0.0170(13) 0.0162(14) 0.0307(17) 0.0051(12) 0.0137(12) 0.0041(11) C27 0.0191(14) 0.0170(14) 0.0264(16) -0.0035(12) 0.0121(11) -0.0033(11) C28 0.0145(13) 0.0173(13) 0.0187(15) 0.0037(11) 0.0049(11) -0.0016(11) C29 0.0116(12) 0.0177(13) 0.0167(15) 0.0027(11) 0.0071(10) -0.0006(10) C30 0.0162(13) 0.0146(13) 0.0235(16) 0.0005(11) 0.0018(11) -0.0010(11) C31 0.0260(15) 0.0276(17) 0.0237(17) -0.0038(13) 0.0004(12) 0.0086(13) C32 0.0154(13) 0.0126(13) 0.0170(15) -0.0013(11) 0.0072(10) 0.0007(10) C33 0.0168(13) 0.0124(13) 0.0173(15) -0.0004(10) 0.0120(11) 0.0019(10) C34 0.0182(13) 0.0127(13) 0.0215(15) 0.0003(11) 0.0098(11) -0.0005(10) C35 0.0131(13) 0.0201(14) 0.0257(16) -0.0021(12) 0.0102(11) -0.0018(11) C36 0.0134(12) 0.0191(14) 0.0239(16) -0.0003(11) 0.0076(11) 0.0012(11) C37 0.0135(12) 0.0177(13) 0.0110(14) -0.0027(10) 0.0050(10) -0.0001(10) C38 0.0148(13) 0.0151(13) 0.0169(15) -0.0039(11) 0.0085(11) 0.0006(10) C39 0.0132(12) 0.0142(13) 0.0193(15) 0.0000(11) 0.0053(11) -0.0001(10) C40 0.0218(14) 0.0165(14) 0.0254(16) 0.0051(11) 0.0123(12) 0.0002(11) C41 0.0136(12) 0.0097(12) 0.0228(15) 0.0040(10) 0.0083(11) -0.0003(10) C42 0.0163(13) 0.0199(14) 0.0205(15) 0.0011(11) 0.0047(11) 0.0008(11) C43 0.0184(14) 0.0213(15) 0.0334(19) 0.0076(13) 0.0046(12) 0.0044(12) C44 0.0205(14) 0.0119(14) 0.0370(19) 0.0028(12) 0.0151(13) 0.0022(11) C45 0.0199(14) 0.0176(14) 0.0251(16) -0.0009(12) 0.0123(12) -0.0035(11) C46 0.0144(12) 0.0144(13) 0.0241(15) 0.0053(11) 0.0074(11) 0.0004(11) C47 0.0409(9) 0.0406(9) 0.0277(9) -0.0039(8) 0.0149(8) -0.0099(9) C48 0.0461(10) 0.0355(10) 0.0260(10) -0.0027(8) 0.0134(8) -0.0056(9) C49 0.042(2) 0.0329(19) 0.030(2) 0.0029(15) 0.0004(15) 0.0053(15) C50 0.0360(18) 0.0286(18) 0.037(2) -0.0027(15) 0.0027(15) 0.0100(14) C51 0.0153(14) 0.0361(18) 0.033(2) -0.0126(14) 0.0062(13) 0.0017(13) C52 0.0162(13) 0.0323(17) 0.0339(18) -0.0092(14) 0.0124(12) -0.0076(13) C53 0.0376(18) 0.0315(18) 0.0303(19) 0.0019(14) 0.0206(14) -0.0025(14) C54 0.0408(19) 0.0318(18) 0.0188(17) 0.0016(14) 0.0086(14) 0.0046(14) C55 0.0234(16) 0.049(2) 0.032(2) 0.0027(16) 0.0024(14) 0.0074(15) C56 0.0248(17) 0.050(2) 0.047(2) -0.0055(19) 0.0101(15) 0.0079(16) C57 0.0247(9) 0.0604(11) 0.0267(10) -0.0056(9) 0.0109(8) 0.0019(9) C58 0.0263(8) 0.0569(10) 0.0285(9) -0.0049(9) 0.0113(8) -0.0057(9) C59 0.043(2) 0.032(2) 0.055(3) 0.0034(18) 0.0133(18) -0.0011(17) C60 0.056(2) 0.049(2) 0.051(3) 0.0051(19) 0.0236(19) 0.0073(19) O11 0.0196(11) 0.0206(11) 0.0505(16) -0.0120(11) 0.0122(10) -0.0039(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 1.853(2) . ? Co1 N2 1.862(2) . ? Co1 N6 1.960(2) . ? Co1 N4 1.972(2) . ? Co1 N3 1.994(2) . ? Co1 N1 2.017(2) . ? K1 O1 2.6906(19) . ? K1 O10 2.769(2) . ? K1 O6 2.786(2) . ? K1 O5 2.807(2) . ? K1 O9 2.870(2) . ? K1 O11 2.882(2) . ? K1 O8 2.900(2) . ? K1 O7 2.900(2) . ? K1 C49 3.492(3) . ? K1 H01B 2.84(4) . ? O1 C9 1.251(3) . ? N1 C9 1.337(3) . ? N1 C7 1.493(3) . ? C1 C2 1.383(4) . ? C1 C6 1.402(4) . ? C1 H1A 0.9500 . ? N2 C14 1.330(3) . ? N2 C10 1.335(3) . ? O2 C15 1.247(3) . ? C2 C3 1.374(5) . ? C2 H2A 0.9500 . ? N3 C15 1.346(3) . ? N3 C16 1.479(3) . ? C3 C4 1.382(5) . ? C3 H3A 0.9500 . ? O3 C32 1.248(3) . ? C4 C5 1.373(4) . ? C4 H4A 0.9500 . ? O4 C38 1.249(3) . ? N4 C32 1.328(3) . ? N4 C30 1.484(3) . ? C5 C6 1.404(4) . ? C5 H5A 0.9500 . ? N5 C33 1.332(3) . ? N5 C37 1.342(3) . ? O5 C49 1.424(4) . ? O5 C48 1.433(4) . ? C6 C7 1.510(4) . ? N6 C38 1.333(3) . ? N6 C39 1.472(3) . ? O6 C51 1.423(4) . ? O6 C50 1.432(4) . ? C7 C8 1.529(4) . ? C7 H7A 1.0000 . ? O7 C53 1.419(4) . ? O7 C52 1.428(3) . ? N7 C59 1.134(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O8 C55 1.435(4) . ? O8 C54 1.435(4) . ? C9 C10 1.493(4) . ? O9 C57 1.404(4) . ? O9 C56 1.405(4) . ? C10 C11 1.384(4) . ? O10 C47 1.418(4) . ? O10 C58 1.432(4) . ? C11 C12 1.395(4) . ? C11 H11A 0.9500 . ? C12 C13 1.388(4) . ? C12 H12A 0.9500 . ? C13 C14 1.391(4) . ? C13 H13A 0.9500 . ? C14 C15 1.498(4) . ? C16 C18 1.525(4) . ? C16 C17 1.535(4) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.384(4) . ? C18 C19 1.393(4) . ? C19 C20 1.384(4) . ? C19 H19A 0.9500 . ? C20 C21 1.382(4) . ? C20 H20A 0.9500 . ? C21 C22 1.382(4) . ? C21 H21A 0.9500 . ? C22 C23 1.388(4) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.385(4) . ? C24 C29 1.402(4) . ? C24 H24A 0.9500 . ? C25 C26 1.376(4) . ? C25 H25A 0.9500 . ? C26 C27 1.392(4) . ? C26 H26A 0.9500 . ? C27 C28 1.387(4) . ? C27 H27A 0.9500 . ? C28 C29 1.375(4) . ? C28 H28A 0.9500 . ? C29 C30 1.540(4) . ? C30 C31 1.535(4) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.504(4) . ? C33 C34 1.387(4) . ? C34 C35 1.396(4) . ? C34 H34A 0.9500 . ? C35 C36 1.384(4) . ? C35 H35A 0.9500 . ? C36 C37 1.388(4) . ? C36 H36A 0.9500 . ? C37 C38 1.495(4) . ? C39 C40 1.523(4) . ? C39 C41 1.534(4) . ? C39 H39A 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C46 1.384(4) . ? C41 C42 1.392(4) . ? C42 C43 1.384(4) . ? C42 H42A 0.9500 . ? C43 C44 1.376(4) . ? C43 H43A 0.9500 . ? C44 C45 1.382(4) . ? C44 H44A 0.9500 . ? C45 C46 1.390(4) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.479(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.507(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.492(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.480(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.479(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.480(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.448(5) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O11 H01A 0.81(4) . ? O11 H01B 0.84(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 N5 Co1 N2 176.25(10) . . ? N5 Co1 N6 81.94(9) . . ? N2 Co1 N6 97.11(9) . . ? N5 Co1 N4 81.90(9) . . ? N2 Co1 N4 99.09(9) . . ? N6 Co1 N4 163.80(8) . . ? N5 Co1 N3 94.55(9) . . ? N2 Co1 N3 81.80(9) . . ? N6 Co1 N3 89.69(9) . . ? N4 Co1 N3 92.73(9) . . ? N5 Co1 N1 101.87(9) . . ? N2 Co1 N1 81.74(9) . . ? N6 Co1 N1 90.49(9) . . ? N4 Co1 N1 91.71(9) . . ? N3 Co1 N1 163.43(8) . . ? O1 K1 O10 84.98(6) . . ? O1 K1 O6 88.01(6) . . ? O10 K1 O6 122.86(7) . . ? O1 K1 O5 89.86(6) . . ? O10 K1 O5 60.44(7) . . ? O6 K1 O5 62.92(7) . . ? O1 K1 O9 103.61(6) . . ? O10 K1 O9 58.96(7) . . ? O6 K1 O9 168.37(7) . . ? O5 K1 O9 115.94(7) . . ? O1 K1 O11 164.07(6) . . ? O10 K1 O11 105.99(7) . . ? O6 K1 O11 76.37(6) . . ? O5 K1 O11 85.82(7) . . ? O9 K1 O11 92.04(6) . . ? O1 K1 O8 106.62(6) . . ? O10 K1 O8 119.22(7) . . ? O6 K1 O8 117.10(7) . . ? O5 K1 O8 163.51(7) . . ? O9 K1 O8 60.32(6) . . ? O11 K1 O8 78.46(7) . . ? O1 K1 O7 110.78(6) . . ? O10 K1 O7 164.23(6) . . ? O6 K1 O7 59.72(6) . . ? O5 K1 O7 117.32(6) . . ? O9 K1 O7 115.09(6) . . ? O11 K1 O7 58.55(6) . . ? O8 K1 O7 57.88(6) . . ? O1 K1 C49 79.16(7) . . ? O10 K1 C49 80.06(8) . . ? O6 K1 C49 43.02(7) . . ? O5 K1 C49 23.00(7) . . ? O9 K1 C49 138.12(8) . . ? O11 K1 C49 91.20(8) . . ? O8 K1 C49 159.89(8) . . ? O7 K1 C49 102.01(7) . . ? O1 K1 H01B 151.1(8) . . ? O10 K1 H01B 122.6(8) . . ? O6 K1 H01B 70.4(8) . . ? O5 K1 H01B 96.6(8) . . ? O9 K1 H01B 98.7(8) . . ? O11 K1 H01B 16.8(8) . . ? O8 K1 H01B 69.3(8) . . ? O7 K1 H01B 41.8(8) . . ? C49 K1 H01B 96.2(8) . . ? C9 O1 K1 163.81(17) . . ? C9 N1 C7 113.6(2) . . ? C9 N1 Co1 113.49(18) . . ? C7 N1 Co1 132.81(17) . . ? C2 C1 C6 121.2(3) . . ? C2 C1 H1A 119.4 . . ? C6 C1 H1A 119.4 . . ? C14 N2 C10 123.0(2) . . ? C14 N2 Co1 118.22(18) . . ? C10 N2 Co1 118.55(17) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C15 N3 C16 119.3(2) . . ? C15 N3 Co1 114.66(17) . . ? C16 N3 Co1 125.35(16) . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C32 N4 C30 118.6(2) . . ? C32 N4 Co1 115.03(16) . . ? C30 N4 Co1 125.29(17) . . ? C4 C5 C6 121.3(3) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C33 N5 C37 123.5(2) . . ? C33 N5 Co1 118.35(17) . . ? C37 N5 Co1 117.89(17) . . ? C49 O5 C48 111.7(2) . . ? C49 O5 K1 106.65(18) . . ? C48 O5 K1 111.38(18) . . ? C1 C6 C5 117.0(3) . . ? C1 C6 C7 122.9(2) . . ? C5 C6 C7 120.1(3) . . ? C38 N6 C39 119.4(2) . . ? C38 N6 Co1 115.16(17) . . ? C39 N6 Co1 125.30(16) . . ? C51 O6 C50 111.2(2) . . ? C51 O6 K1 117.43(16) . . ? C50 O6 K1 112.46(18) . . ? N1 C7 C6 113.3(2) . . ? N1 C7 C8 112.4(2) . . ? C6 C7 C8 112.4(2) . . ? N1 C7 H7A 106.0 . . ? C6 C7 H7A 106.0 . . ? C8 C7 H7A 106.0 . . ? C53 O7 C52 113.8(2) . . ? C53 O7 K1 116.20(16) . . ? C52 O7 K1 111.37(16) . . ? 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 . . ? C55 O8 C54 110.9(2) . . ? C55 O8 K1 110.62(18) . . ? C54 O8 K1 116.31(16) . . ? O1 C9 N1 128.8(3) . . ? O1 C9 C10 118.5(2) . . ? N1 C9 C10 112.7(2) . . ? C57 O9 C56 113.0(3) . . ? C57 O9 K1 108.65(17) . . ? C56 O9 K1 110.85(18) . . ? N2 C10 C11 119.8(2) . . ? N2 C10 C9 113.4(2) . . ? C11 C10 C9 126.6(2) . . ? C47 O10 C58 114.5(2) . . ? C47 O10 K1 117.42(19) . . ? C58 O10 K1 119.80(18) . . ? C10 C11 C12 118.3(2) . . ? C10 C11 H11A 120.9 . . ? C12 C11 H11A 120.9 . . ? C13 C12 C11 120.7(2) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 C14 117.8(3) . . ? C12 C13 H13A 121.1 . . ? C14 C13 H13A 121.1 . . ? N2 C14 C13 120.3(2) . . ? N2 C14 C15 114.0(2) . . ? C13 C14 C15 125.7(2) . . ? O2 C15 N3 129.4(2) . . ? O2 C15 C14 119.3(2) . . ? N3 C15 C14 111.3(2) . . ? N3 C16 C18 114.5(2) . . ? N3 C16 C17 113.8(2) . . ? C18 C16 C17 111.6(2) . . ? N3 C16 H16A 105.3 . . ? C18 C16 H16A 105.3 . . ? C17 C16 H16A 105.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 117.9(3) . . ? C23 C18 C16 119.1(2) . . ? C19 C18 C16 123.0(2) . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 119.3(3) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 119.9(3) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C18 C23 C22 121.5(3) . . ? C18 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C25 C24 C29 120.8(3) . . ? C25 C24 H24A 119.6 . . ? C29 C24 H24A 119.6 . . ? C26 C25 C24 120.6(2) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 119.0(3) . . ? C25 C26 H26A 120.5 . . ? C27 C26 H26A 120.5 . . ? C28 C27 C26 120.2(3) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 C27 121.4(2) . . ? C29 C28 H28A 119.3 . . ? C27 C28 H28A 119.3 . . ? C28 C29 C24 118.0(2) . . ? C28 C29 C30 123.0(2) . . ? C24 C29 C30 118.9(2) . . ? N4 C30 C31 110.3(2) . . ? N4 C30 C29 115.1(2) . . ? C31 C30 C29 113.1(2) . . ? N4 C30 H30A 105.9 . . ? C31 C30 H30A 105.9 . . ? C29 C30 H30A 105.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O3 C32 N4 128.8(2) . . ? O3 C32 C33 119.9(2) . . ? N4 C32 C33 111.4(2) . . ? N5 C33 C34 119.4(2) . . ? N5 C33 C32 112.7(2) . . ? C34 C33 C32 127.9(2) . . ? C33 C34 C35 118.4(2) . . ? C33 C34 H34A 120.8 . . ? C35 C34 H34A 120.8 . . ? C36 C35 C34 120.8(2) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C35 C36 C37 118.3(2) . . ? C35 C36 H36A 120.9 . . ? C37 C36 H36A 120.9 . . ? N5 C37 C36 119.6(2) . . ? N5 C37 C38 112.7(2) . . ? C36 C37 C38 127.7(2) . . ? O4 C38 N6 128.2(2) . . ? O4 C38 C37 120.4(2) . . ? N6 C38 C37 111.4(2) . . ? N6 C39 C40 111.5(2) . . ? N6 C39 C41 113.4(2) . . ? C40 C39 C41 114.1(2) . . ? N6 C39 H39A 105.7 . . ? C40 C39 H39A 105.7 . . ? C41 C39 H39A 105.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C46 C41 C42 118.2(2) . . ? C46 C41 C39 119.0(2) . . ? C42 C41 C39 122.7(2) . . ? C43 C42 C41 120.8(3) . . ? C43 C42 H42A 119.6 . . ? C41 C42 H42A 119.6 . . ? C44 C43 C42 120.5(3) . . ? C44 C43 H43A 119.8 . . ? C42 C43 H43A 119.8 . . ? C43 C44 C45 119.4(3) . . ? C43 C44 H44A 120.3 . . ? C45 C44 H44A 120.3 . . ? C44 C45 C46 120.1(3) . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C41 C46 C45 120.9(2) . . ? C41 C46 H46A 119.5 . . ? C45 C46 H46A 119.5 . . ? O10 C47 C48 108.8(3) . . ? O10 C47 H47A 109.9 . . ? C48 C47 H47A 109.9 . . ? O10 C47 H47B 109.9 . . ? C48 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? O5 C48 C47 109.3(3) . . ? O5 C48 H48A 109.8 . . ? C47 C48 H48A 109.8 . . ? O5 C48 H48B 109.8 . . ? C47 C48 H48B 109.8 . . ? H48A C48 H48B 108.3 . . ? O5 C49 C50 108.9(3) . . ? O5 C49 K1 50.35(14) . . ? C50 C49 K1 81.24(17) . . ? O5 C49 H49A 109.9 . . ? C50 C49 H49A 109.9 . . ? K1 C49 H49A 160.2 . . ? O5 C49 H49B 109.9 . . ? C50 C49 H49B 109.9 . . ? K1 C49 H49B 81.7 . . ? H49A C49 H49B 108.3 . . ? O6 C50 C49 109.0(3) . . ? O6 C50 H50A 109.9 . . ? C49 C50 H50A 109.9 . . ? O6 C50 H50B 109.9 . . ? C49 C50 H50B 109.9 . . ? H50A C50 H50B 108.3 . . ? O6 C51 C52 109.3(2) . . ? O6 C51 H51A 109.8 . . ? C52 C51 H51A 109.8 . . ? O6 C51 H51B 109.8 . . ? C52 C51 H51B 109.8 . . ? H51A C51 H51B 108.3 . . ? O7 C52 C51 108.7(2) . . ? O7 C52 H52A 110.0 . . ? C51 C52 H52A 110.0 . . ? O7 C52 H52B 110.0 . . ? C51 C52 H52B 110.0 . . ? H52A C52 H52B 108.3 . . ? O7 C53 C54 109.3(3) . . ? O7 C53 H53A 109.8 . . ? C54 C53 H53A 109.8 . . ? O7 C53 H53B 109.8 . . ? C54 C53 H53B 109.8 . . ? H53A C53 H53B 108.3 . . ? O8 C54 C53 109.1(2) . . ? O8 C54 H54A 109.9 . . ? C53 C54 H54A 109.9 . . ? O8 C54 H54B 109.9 . . ? C53 C54 H54B 109.9 . . ? H54A C54 H54B 108.3 . . ? O8 C55 C56 109.2(2) . . ? O8 C55 H55A 109.8 . . ? C56 C55 H55A 109.8 . . ? O8 C55 H55B 109.8 . . ? C56 C55 H55B 109.8 . . ? H55A C55 H55B 108.3 . . ? O9 C56 C55 108.8(3) . . ? O9 C56 H56A 109.9 . . ? C55 C56 H56A 109.9 . . ? O9 C56 H56B 109.9 . . ? C55 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? O9 C57 C58 108.6(3) . . ? O9 C57 H57A 110.0 . . ? C58 C57 H57A 110.0 . . ? O9 C57 H57B 110.0 . . ? C58 C57 H57B 110.0 . . ? H57A C57 H57B 108.4 . . ? O10 C58 C57 108.4(3) . . ? O10 C58 H58A 110.0 . . ? C57 C58 H58A 110.0 . . ? O10 C58 H58B 110.0 . . ? C57 C58 H58B 110.0 . . ? H58A C58 H58B 108.4 . . ? N7 C59 C60 179.0(5) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? K1 O11 H01A 120(3) . . ? K1 O11 H01B 79(3) . . ? H01A O11 H01B 108(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H01A O3 0.81(4) 1.98(4) 2.765(3) 162(4) 2_645 O11 H01B O7 0.84(4) 2.05(4) 2.827(3) 154(4) . _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.713 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.063 # Attachment '- 18C6KFeL1.cif' data_ch1 _database_code_depnum_ccdc_archive 'CCDC 786087' #TrackingRef '- 18C6KFeL1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H66 Fe K N6 O10' _chemical_formula_weight 1102.12 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.5438(10) _cell_length_b 13.1192(9) _cell_length_c 26.7367(17) _cell_angle_alpha 90.00 _cell_angle_beta 99.309(3) _cell_angle_gamma 90.00 _cell_volume 5380.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7268 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2324 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9122 _exptl_absorpt_correction_T_max 0.9792 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; We are greatful to the EPSRC Crystallographic Service for recording the data for CH1. The crystal had basically no diffraction out by 25 degrees so has an A alert in the cif checker for weak data. It also required many restraints (SIMU, DELU and ISOR) to make the disordered components of the crown and alpha-methylbenzylamine components have chemically sensible bond lengths and thermal parameters. The asymmetric unit contains two potassium/crown counterions with two bis amide anions with iron. There is a large distortion in one of the crowns from O16-O20 and this was modelled as disordered over two positions about the potassium ion in the ratio of 64:36. The minor component was refined isotropically. The disorder is a change in the kinks/ruffle of the ethyleneoxide chains of the crown around the potassium. There is also disorder in one of the phenyls of an alpha methyl benzamide group (C70-C77). This was traced over the whole phenyl and out to the alpha methyl. This was modelled as 60:40 major minor and involves a tilt in the phenyl group from the major component. The minor component was refined isotropically. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 32109 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.1670 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.03 _reflns_number_total 15168 _reflns_number_gt 8834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+18.2602P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 6068 Friedel pairs' _refine_ls_abs_structure_Flack 0.15(3) _chemical_absolute_configuration rmad _refine_ls_number_reflns 15168 _refine_ls_number_parameters 1434 _refine_ls_number_restraints 1902 _refine_ls_R_factor_all 0.1895 _refine_ls_R_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.1766 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.25119(9) -0.15689(11) 1.89564(6) 0.0273(4) Uani 1 1 d U . . K1 K -0.26904(16) -0.1018(2) 1.16374(10) 0.0452(7) Uani 1 1 d U . . Fe2 Fe -0.23603(9) 0.08921(10) 1.39706(6) 0.0257(4) Uani 1 1 d U A . K2 K -0.29035(15) 0.01597(19) 1.65873(9) 0.0356(6) Uani 1 1 d U . . C1 C -0.2974(7) 0.1472(8) 1.8459(4) 0.036(3) Uani 1 1 d U . . H1A H -0.3300 0.0899 1.8319 0.044 Uiso 1 1 calc R . . C2 C -0.2731(7) 0.2222(8) 1.8136(5) 0.037(3) Uani 1 1 d U . . H2A H -0.2877 0.2160 1.7778 0.044 Uiso 1 1 calc R . . C3 C -0.2268(7) 0.3059(8) 1.8356(5) 0.038(3) Uani 1 1 d U . . H3A H -0.2109 0.3583 1.8143 0.045 Uiso 1 1 calc R . . C4 C -0.2040(7) 0.3147(8) 1.8860(5) 0.045(3) Uani 1 1 d U . . H4A H -0.1716 0.3724 1.8999 0.054 Uiso 1 1 calc R . . C5 C -0.2275(7) 0.2401(8) 1.9178(5) 0.036(3) Uani 1 1 d U . . H5A H -0.2115 0.2462 1.9535 0.043 Uiso 1 1 calc R . . C6 C -0.2752(6) 0.1553(8) 1.8968(4) 0.028(2) Uani 1 1 d U . . C7 C -0.2977(6) 0.0708(7) 1.9315(4) 0.031(2) Uani 1 1 d U . . H7A H -0.2850 0.0988 1.9667 0.037 Uiso 1 1 calc R . . C8 C -0.3942(6) 0.0443(8) 1.9224(4) 0.040(3) Uani 1 1 d U . . H8A H -0.4039 -0.0169 1.9417 0.060 Uiso 1 1 calc R . . H8B H -0.4135 0.0317 1.8862 0.060 Uiso 1 1 calc R . . H8C H -0.4275 0.1012 1.9334 0.060 Uiso 1 1 calc R . . N1 N -0.2388(5) -0.0197(6) 1.9308(3) 0.0255(18) Uani 1 1 d U . . O1 O -0.1368(4) 0.0701(5) 1.9869(3) 0.0289(17) Uani 1 1 d U . . C9 C -0.1595(6) -0.0067(8) 1.9612(4) 0.024(2) Uani 1 1 d U . . C10 C -0.1045(6) -0.0980(8) 1.9639(4) 0.027(2) Uani 1 1 d U . . C11 C -0.0248(6) -0.1107(9) 1.9941(4) 0.034(3) Uani 1 1 d U . . H11A H 0.0018 -0.0558 2.0140 0.040 Uiso 1 1 calc R . . C12 C 0.0157(7) -0.2033(8) 1.9950(4) 0.032(3) Uani 1 1 d U . . H12A H 0.0709 -0.2129 2.0156 0.039 Uiso 1 1 calc R . . C13 C -0.0240(7) -0.2835(8) 1.9658(4) 0.031(2) Uani 1 1 d U . . H13A H 0.0025 -0.3489 1.9671 0.037 Uiso 1 1 calc R . . N2 N -0.1394(5) -0.1736(6) 1.9345(3) 0.0225(17) Uani 1 1 d U . . C14 C -0.1015(7) -0.2662(8) 1.9353(4) 0.030(2) Uani 1 1 d U . . O2 O -0.1309(4) -0.4308(5) 1.9003(3) 0.0352(18) Uani 1 1 d U . . C15 C -0.1556(7) -0.3411(8) 1.9014(4) 0.028(2) Uani 1 1 d U . . N3 N -0.2272(5) -0.2978(6) 1.8749(3) 0.0290(19) Uani 1 1 d U . . C16 C -0.2885(7) -0.3565(8) 1.8372(4) 0.038(2) Uani 1 1 d U . . H16A H -0.3380 -0.3089 1.8257 0.045 Uiso 1 1 calc R . . C17 C -0.3295(7) -0.4476(8) 1.8613(4) 0.043(3) Uani 1 1 d U . . H17A H -0.3557 -0.4237 1.8902 0.064 Uiso 1 1 calc R . . H17B H -0.2843 -0.4981 1.8730 0.064 Uiso 1 1 calc R . . H17C H -0.3746 -0.4788 1.8361 0.064 Uiso 1 1 calc R . . C18 C -0.2553(7) -0.3880(8) 1.7895(4) 0.038(2) Uani 1 1 d U . . C19 C -0.3045(8) -0.3629(9) 1.7440(5) 0.053(3) Uani 1 1 d U . . H19A H -0.3570 -0.3257 1.7434 0.063 Uiso 1 1 calc R . . C20 C -0.2788(8) -0.3911(10) 1.6988(4) 0.057(3) Uani 1 1 d U . . H20A H -0.3138 -0.3716 1.6679 0.068 Uiso 1 1 calc R . . C21 C -0.2038(8) -0.4468(10) 1.6973(5) 0.059(3) Uani 1 1 d U . . H21A H -0.1878 -0.4678 1.6660 0.070 Uiso 1 1 calc R . . C22 C -0.1540(8) -0.4702(8) 1.7421(5) 0.043(3) Uani 1 1 d U . . H22A H -0.1008 -0.5056 1.7420 0.052 Uiso 1 1 calc R . . C23 C -0.1783(7) -0.4440(8) 1.7881(4) 0.037(3) Uani 1 1 d U . . H23A H -0.1429 -0.4640 1.8189 0.044 Uiso 1 1 calc R . . C24 C -0.2663(8) -0.4267(9) 1.9928(4) 0.041(3) Uani 1 1 d U . . H24A H -0.2193 -0.4031 1.9771 0.049 Uiso 1 1 calc R . . C25 C -0.2738(8) -0.5301(9) 1.9999(5) 0.044(3) Uani 1 1 d U . . H25A H -0.2349 -0.5764 1.9878 0.053 Uiso 1 1 calc R . . C26 C -0.3393(8) -0.5652(9) 2.0249(5) 0.045(3) Uani 1 1 d U . . H26A H -0.3453 -0.6361 2.0308 0.054 Uiso 1 1 calc R . . C27 C -0.3953(8) -0.4966(10) 2.0410(5) 0.050(3) Uani 1 1 d U . . H27A H -0.4404 -0.5204 2.0581 0.060 Uiso 1 1 calc R . . C28 C -0.3871(7) -0.3933(9) 2.0328(4) 0.041(3) Uani 1 1 d U . . H28A H -0.4261 -0.3474 2.0451 0.049 Uiso 1 1 calc R . . C29 C -0.3233(7) -0.3550(9) 2.0071(4) 0.035(2) Uani 1 1 d U . . C30 C -0.3124(7) -0.2425(8) 2.0004(4) 0.036(2) Uani 1 1 d U . . H30A H -0.3606 -0.2103 2.0155 0.043 Uiso 1 1 calc R . . C31 C -0.2300(6) -0.2024(8) 2.0309(4) 0.040(3) Uani 1 1 d U . . H31A H -0.2298 -0.2168 2.0669 0.060 Uiso 1 1 calc R . . H31B H -0.2265 -0.1286 2.0259 0.060 Uiso 1 1 calc R . . H31C H -0.1797 -0.2356 2.0200 0.060 Uiso 1 1 calc R . . N4 N -0.3280(5) -0.2100(6) 1.9455(3) 0.0277(18) Uani 1 1 d U . . O3 O -0.4757(4) -0.2350(5) 1.9486(3) 0.0386(19) Uani 1 1 d U . . C32 C -0.4151(6) -0.2098(7) 1.9264(4) 0.029(2) Uani 1 1 d U . . C33 C -0.4329(6) -0.1724(8) 1.8733(4) 0.029(2) Uani 1 1 d U . . C34 C -0.5142(6) -0.1624(9) 1.8448(4) 0.043(3) Uani 1 1 d U . . H34A H -0.5647 -0.1829 1.8580 0.051 Uiso 1 1 calc R . . C35 C -0.5215(7) -0.1221(8) 1.7965(4) 0.040(3) Uani 1 1 d U . . H35A H -0.5776 -0.1135 1.7767 0.048 Uiso 1 1 calc R . . C36 C -0.4477(7) -0.0939(9) 1.7765(4) 0.040(3) Uani 1 1 d U . . H36A H -0.4512 -0.0672 1.7432 0.047 Uiso 1 1 calc R . . N5 N -0.3624(5) -0.1428(6) 1.8555(3) 0.0238(17) Uani 1 1 d U . . C37 C -0.3690(6) -0.1073(8) 1.8082(4) 0.027(2) Uani 1 1 d U . . O4 O -0.2780(5) -0.0550(6) 1.7496(3) 0.0399(19) Uani 1 1 d U . . C38 C -0.2801(7) -0.0832(7) 1.7924(4) 0.027(2) Uani 1 1 d U . . N6 N -0.2143(5) -0.1063(7) 1.8307(3) 0.0312(19) Uani 1 1 d U . . C39 C -0.1283(6) -0.0969(8) 1.8145(4) 0.035(2) Uani 1 1 d U . . H39A H -0.1386 -0.0493 1.7849 0.042 Uiso 1 1 calc R . . C40 C -0.1027(7) -0.1965(8) 1.7922(4) 0.050(3) Uani 1 1 d U . . H40A H -0.1491 -0.2182 1.7650 0.075 Uiso 1 1 calc R . . H40B H -0.0940 -0.2488 1.8187 0.075 Uiso 1 1 calc R . . H40C H -0.0485 -0.1870 1.7785 0.075 Uiso 1 1 calc R . . C41 C -0.0602(7) -0.0442(8) 1.8521(4) 0.028(2) Uani 1 1 d U . . C42 C 0.0195(7) -0.0890(8) 1.8693(4) 0.030(2) Uani 1 1 d U . . H42A H 0.0302 -0.1566 1.8591 0.036 Uiso 1 1 calc R . . C43 C 0.0850(7) -0.0370(9) 1.9016(4) 0.040(3) Uani 1 1 d U . . H43A H 0.1392 -0.0692 1.9132 0.048 Uiso 1 1 calc R . . C44 C 0.0704(7) 0.0611(9) 1.9165(4) 0.041(3) Uani 1 1 d U . . H44A H 0.1147 0.0975 1.9379 0.049 Uiso 1 1 calc R . . C45 C -0.0080(7) 0.1051(8) 1.9003(4) 0.040(3) Uani 1 1 d U . . H45A H -0.0192 0.1714 1.9120 0.048 Uiso 1 1 calc R . . C46 C -0.0721(7) 0.0558(8) 1.8672(4) 0.031(2) Uani 1 1 d U . . H46A H -0.1248 0.0904 1.8545 0.038 Uiso 1 1 calc R . . C47 C -0.2960(6) -0.2333(7) 1.3346(4) 0.024(2) Uani 1 1 d U . . H47A H -0.3210 -0.1768 1.3152 0.029 Uiso 1 1 calc R . . C48 C -0.2763(8) -0.3206(8) 1.3105(4) 0.037(3) Uani 1 1 d U . . H48A H -0.2850 -0.3224 1.2745 0.045 Uiso 1 1 calc R . . C49 C -0.2448(7) -0.4041(9) 1.3370(4) 0.040(3) Uani 1 1 d U . . H49A H -0.2328 -0.4643 1.3196 0.049 Uiso 1 1 calc R . . C50 C -0.2297(7) -0.4013(9) 1.3901(4) 0.035(3) Uani 1 1 d U . . H50A H -0.2077 -0.4596 1.4091 0.042 Uiso 1 1 calc R . . C51 C -0.2475(6) -0.3115(8) 1.4147(4) 0.031(2) Uani 1 1 d U . . H51A H -0.2371 -0.3091 1.4507 0.038 Uiso 1 1 calc R . . C52 C -0.2795(6) -0.2269(7) 1.3880(4) 0.023(2) Uani 1 1 d U . . C53 C -0.3034(6) -0.1303(7) 1.4141(4) 0.026(2) Uani 1 1 d U . . H53A H -0.3505 -0.0977 1.3894 0.032 Uiso 1 1 calc R . . C54 C -0.3443(6) -0.1488(8) 1.4614(4) 0.038(3) Uani 1 1 d U . . H54A H -0.3660 -0.0842 1.4729 0.057 Uiso 1 1 calc R . . H54B H -0.3003 -0.1771 1.4883 0.057 Uiso 1 1 calc R . . H54C H -0.3927 -0.1970 1.4535 0.057 Uiso 1 1 calc R . . N7 N -0.2332(5) -0.0540(6) 1.4227(3) 0.0240(18) Uani 1 1 d U . . O5 O -0.1473(4) -0.1599(6) 1.4797(3) 0.0314(17) Uani 1 1 d U . . C55 C -0.1637(7) -0.0782(8) 1.4558(4) 0.027(2) Uani 1 1 d U . . C56 C -0.0977(6) 0.0093(8) 1.4667(4) 0.024(2) Uani 1 1 d U . . C57 C -0.0217(6) 0.0114(8) 1.5008(4) 0.030(2) Uani 1 1 d U . . H57A H -0.0018 -0.0473 1.5200 0.036 Uiso 1 1 calc R . . C58 C 0.0244(6) 0.1000(9) 1.5062(4) 0.036(3) Uani 1 1 d U . . H58A H 0.0771 0.1024 1.5298 0.043 Uiso 1 1 calc R . . C59 C -0.0026(6) 0.1857(8) 1.4789(4) 0.029(2) Uani 1 1 d U . . H59A H 0.0309 0.2466 1.4828 0.035 Uiso 1 1 calc R . . N8 N -0.1264(5) 0.0926(7) 1.4398(3) 0.0232(17) Uani 1 1 d U . . C60 C -0.0820(6) 0.1802(7) 1.4447(4) 0.021(2) Uani 1 1 d U . . O6 O -0.0903(4) 0.3494(5) 1.4130(2) 0.0312(16) Uani 1 1 d U . . C61 C -0.1251(7) 0.2632(8) 1.4129(4) 0.032(2) Uani 1 1 d U . . N9 N -0.2019(5) 0.2335(6) 1.3859(3) 0.0247(18) Uani 1 1 d U . . C62 C -0.2503(6) 0.3140(7) 1.3547(4) 0.029(2) Uani 1 1 d U . . H62A H -0.2257 0.3797 1.3697 0.034 Uiso 1 1 calc R . . C63 C -0.3468(6) 0.3188(7) 1.3571(4) 0.033(3) Uani 1 1 d U . . H63A H -0.3553 0.3230 1.3926 0.049 Uiso 1 1 calc R . . H63B H -0.3755 0.2574 1.3416 0.049 Uiso 1 1 calc R . . H63C H -0.3722 0.3791 1.3388 0.049 Uiso 1 1 calc R . . C64 C -0.2308(6) 0.3134(7) 1.3002(4) 0.023(2) Uani 1 1 d U . . C65 C -0.2824(7) 0.2592(8) 1.2613(4) 0.031(2) Uani 1 1 d U . . H65A H -0.3290 0.2182 1.2688 0.037 Uiso 1 1 calc R . . C66 C -0.2661(8) 0.2648(8) 1.2121(4) 0.044(3) Uani 1 1 d U . . H66A H -0.3041 0.2318 1.1856 0.053 Uiso 1 1 calc R . . C67 C -0.1943(7) 0.3186(8) 1.2012(4) 0.045(3) Uani 1 1 d U . . H67A H -0.1818 0.3212 1.1676 0.054 Uiso 1 1 calc R . . C68 C -0.1417(7) 0.3679(7) 1.2400(5) 0.038(3) Uani 1 1 d U . . H68A H -0.0931 0.4059 1.2329 0.045 Uiso 1 1 calc R . . C69 C -0.1583(7) 0.3631(8) 1.2884(4) 0.034(3) Uani 1 1 d U . . H69A H -0.1190 0.3948 1.3148 0.041 Uiso 1 1 calc R . . C75 C -0.0556(16) -0.0304(18) 1.3481(11) 0.031(3) Uani 0.60 1 d PU A 1 C70 C 0.0262(14) -0.0212(16) 1.3767(9) 0.032(4) Uani 0.60 1 d PU A 1 H70A H 0.0531 0.0439 1.3804 0.039 Uiso 0.60 1 calc PR A 1 C71 C 0.0703(14) -0.1051(17) 1.4003(9) 0.045(4) Uani 0.60 1 d PU A 1 H71A H 0.1256 -0.0953 1.4208 0.054 Uiso 0.60 1 calc PR A 1 C72 C 0.0362(14) -0.2004(16) 1.3948(8) 0.047(4) Uani 0.60 1 d PU A 1 H72A H 0.0661 -0.2567 1.4120 0.056 Uiso 0.60 1 calc PR A 1 C73 C -0.0450(13) -0.2138(16) 1.3629(8) 0.048(4) Uani 0.60 1 d PU A 1 H73A H -0.0688 -0.2802 1.3569 0.058 Uiso 0.60 1 calc PR A 1 C74 C -0.0899(13) -0.1298(17) 1.3402(9) 0.046(5) Uani 0.60 1 d PU A 1 H74A H -0.1445 -0.1394 1.3190 0.055 Uiso 0.60 1 calc PR A 1 C76 C -0.1057(13) 0.0645(17) 1.3258(9) 0.032(3) Uani 0.60 1 d PRU A 1 H76A H -0.0815 0.1248 1.3463 0.039 Uiso 0.60 1 calc PR A 1 C77 C -0.091(3) 0.079(5) 1.2759(14) 0.043(9) Uani 0.60 1 d PU A 1 H77A H -0.1311 0.1305 1.2591 0.065 Uiso 0.60 1 calc PR A 1 H77B H -0.0994 0.0148 1.2572 0.065 Uiso 0.60 1 calc PR A 1 H77C H -0.0305 0.1027 1.2765 0.065 Uiso 0.60 1 calc PR A 1 C75A C -0.0490(18) -0.0228(19) 1.3523(14) 0.031(3) Uani 0.40 1 d PGU A 2 C74A C -0.0767(14) -0.123(2) 1.3559(11) 0.032(8) Uiso 0.40 1 d PGU A 2 H74B H -0.1334 -0.1425 1.3400 0.038 Uiso 0.40 1 calc PR A 2 C73A C -0.0215(15) -0.1942(15) 1.3828(9) 0.033(7) Uiso 0.40 1 d PGU A 2 H73B H -0.0404 -0.2626 1.3853 0.040 Uiso 0.40 1 calc PR A 2 C72A C 0.0615(13) -0.1655(15) 1.4062(9) 0.038(6) Uiso 0.40 1 d PGU A 2 H72B H 0.0992 -0.2143 1.4246 0.046 Uiso 0.40 1 calc PR A 2 C71A C 0.0892(13) -0.0654(17) 1.4025(10) 0.039(6) Uiso 0.40 1 d PGU A 2 H71B H 0.1459 -0.0458 1.4184 0.047 Uiso 0.40 1 calc PR A 2 C70A C 0.0339(19) 0.0059(14) 1.3756(13) 0.039(6) Uiso 0.40 1 d PGU A 2 H70B H 0.0529 0.0743 1.3731 0.046 Uiso 0.40 1 calc PR A 2 C76A C -0.108(3) 0.056(3) 1.3230(17) 0.032(3) Uani 0.40 1 d PU A 2 H76B H -0.0866 0.1200 1.3416 0.039 Uiso 0.40 1 calc PR A 2 C77A C -0.086(5) 0.083(7) 1.2643(19) 0.035(10) Uani 0.40 1 d PU A 2 H77D H -0.1193 0.1440 1.2512 0.053 Uiso 0.40 1 calc PR A 2 H77E H -0.1039 0.0254 1.2418 0.053 Uiso 0.40 1 calc PR A 2 H77F H -0.0239 0.0959 1.2661 0.053 Uiso 0.40 1 calc PR A 2 N10 N -0.1976(5) 0.0517(6) 1.3328(3) 0.0260(17) Uani 1 1 d U . . O7 O -0.2566(4) -0.0172(6) 1.2528(3) 0.0352(17) Uani 1 1 d U A . C78 C -0.2608(7) 0.0211(8) 1.2962(4) 0.030(2) Uani 1 1 d U A . C79 C -0.3495(6) 0.0349(7) 1.3110(4) 0.024(2) Uani 1 1 d U . . C80 C -0.4291(6) 0.0079(8) 1.2829(4) 0.032(2) Uani 1 1 d U A . H80A H -0.4326 -0.0162 1.2491 0.038 Uiso 1 1 calc R . . C81 C -0.5029(6) 0.0168(8) 1.3048(4) 0.033(2) Uani 1 1 d U . . H81A H -0.5581 -0.0022 1.2864 0.039 Uiso 1 1 calc R A . C82 C -0.4965(6) 0.0537(7) 1.3542(4) 0.0232(14) Uani 1 1 d U A . H82A H -0.5471 0.0587 1.3697 0.028 Uiso 1 1 calc R . . N11 N -0.3450(5) 0.0708(6) 1.3570(3) 0.0232(14) Uani 1 1 d U A . C83 C -0.4161(6) 0.0831(7) 1.3805(4) 0.024(2) Uani 1 1 d U . . O8 O -0.4539(4) 0.1320(5) 1.4594(3) 0.0349(18) Uani 1 1 d U . . C84 C -0.3941(6) 0.1205(7) 1.4341(4) 0.025(2) Uani 1 1 d U A . N12 N -0.3088(5) 0.1356(6) 1.4470(3) 0.0228(17) Uani 1 1 d U . . C85 C -0.2753(7) 0.1748(8) 1.4987(4) 0.030(2) Uani 1 1 d U A . H85A H -0.2111 0.1837 1.4999 0.036 Uiso 1 1 calc R . . C86 C -0.2850(7) 0.0971(8) 1.5396(4) 0.040(3) Uani 1 1 d U . . H86A H -0.2579 0.0326 1.5320 0.060 Uiso 1 1 calc R A . H86B H -0.3470 0.0859 1.5407 0.060 Uiso 1 1 calc R . . H86C H -0.2562 0.1226 1.5726 0.060 Uiso 1 1 calc R . . C87 C -0.3107(6) 0.2818(8) 1.5077(4) 0.031(2) Uani 1 1 d U . . C88 C -0.2669(6) 0.3638(8) 1.4952(4) 0.030(2) Uani 1 1 d U A . H88A H -0.2181 0.3546 1.4785 0.036 Uiso 1 1 calc R . . C89 C -0.2922(8) 0.4626(8) 1.5066(4) 0.039(3) Uani 1 1 d U . . H89A H -0.2605 0.5197 1.4974 0.047 Uiso 1 1 calc R A . C90 C -0.3629(7) 0.4773(8) 1.5310(4) 0.039(3) Uani 1 1 d U A . H90A H -0.3808 0.5441 1.5384 0.047 Uiso 1 1 calc R . . C91 C -0.4072(7) 0.3927(9) 1.5446(4) 0.043(3) Uani 1 1 d U . . H91A H -0.4555 0.4009 1.5619 0.051 Uiso 1 1 calc R A . C92 C -0.3808(7) 0.2966(8) 1.5329(4) 0.033(3) Uani 1 1 d U A . H92A H -0.4115 0.2390 1.5424 0.039 Uiso 1 1 calc R . . O9 O -0.1292(4) 0.1192(6) 1.6713(3) 0.051(2) Uani 1 1 d U . . C93 C -0.1243(9) 0.1955(11) 1.7093(5) 0.072(3) Uani 1 1 d U . . H93A H -0.0667 0.2295 1.7137 0.086 Uiso 1 1 calc R . . H93B H -0.1322 0.1647 1.7420 0.086 Uiso 1 1 calc R . . C94 C -0.1959(8) 0.2718(10) 1.6923(5) 0.060(3) Uani 1 1 d U . . H94A H -0.1922 0.3293 1.7166 0.072 Uiso 1 1 calc R . . H94B H -0.1904 0.2992 1.6585 0.072 Uiso 1 1 calc R . . O10 O -0.2777(5) 0.2193(6) 1.6904(3) 0.0460(19) Uani 1 1 d U . . C95 C -0.3478(8) 0.2895(9) 1.6778(5) 0.054(3) Uani 1 1 d U . . H95A H -0.3473 0.3178 1.6435 0.065 Uiso 1 1 calc R . . H95B H -0.3415 0.3465 1.7023 0.065 Uiso 1 1 calc R . . C96 C -0.4322(8) 0.2339(9) 1.6792(5) 0.059(3) Uani 1 1 d U . . H96A H -0.4323 0.2039 1.7132 0.070 Uiso 1 1 calc R . . H96B H -0.4820 0.2815 1.6717 0.070 Uiso 1 1 calc R . . O11 O -0.4389(5) 0.1553(6) 1.6416(3) 0.0410(18) Uani 1 1 d U . . C97 C -0.5190(7) 0.1028(9) 1.6377(5) 0.049(3) Uani 1 1 d U . . H97A H -0.5682 0.1508 1.6290 0.059 Uiso 1 1 calc R . . H97B H -0.5241 0.0694 1.6703 0.059 Uiso 1 1 calc R . . C98 C -0.5201(7) 0.0238(9) 1.5964(4) 0.043(3) Uani 1 1 d U . . H98A H -0.5785 -0.0082 1.5889 0.051 Uiso 1 1 calc R . . H98B H -0.5077 0.0568 1.5650 0.051 Uiso 1 1 calc R . . O12 O -0.4564(5) -0.0514(5) 1.6125(3) 0.0388(17) Uani 1 1 d U . . C99 C -0.4570(7) -0.1276(9) 1.5749(4) 0.050(3) Uani 1 1 d U . . H99A H -0.4491 -0.0960 1.5423 0.060 Uiso 1 1 calc R . . H99B H -0.5135 -0.1640 1.5698 0.060 Uiso 1 1 calc R . . C100 C -0.3844(8) -0.2010(9) 1.5917(5) 0.055(3) Uani 1 1 d U . . H10A H -0.3894 -0.2276 1.6258 0.065 Uiso 1 1 calc R . . H10B H -0.3883 -0.2592 1.5679 0.065 Uiso 1 1 calc R . . O13 O -0.3032(5) -0.1509(6) 1.5933(3) 0.0467(19) Uani 1 1 d U . . C101 C -0.2324(8) -0.2175(10) 1.6052(5) 0.065(3) Uani 1 1 d U . . H10C H -0.2390 -0.2757 1.5813 0.078 Uiso 1 1 calc R . . H10D H -0.2305 -0.2444 1.6399 0.078 Uiso 1 1 calc R . . C102 C -0.1494(8) -0.1609(11) 1.6016(5) 0.059(3) Uani 1 1 d U . . H10E H -0.0993 -0.2084 1.6070 0.071 Uiso 1 1 calc R . . H10F H -0.1528 -0.1300 1.5675 0.071 Uiso 1 1 calc R . . O14 O -0.1383(5) -0.0837(6) 1.6393(3) 0.0492(19) Uani 1 1 d U . . C103 C -0.0645(8) -0.0201(10) 1.6371(5) 0.060(3) Uani 1 1 d U . . H10G H -0.0722 0.0176 1.6046 0.072 Uiso 1 1 calc R . . H10H H -0.0111 -0.0621 1.6395 0.072 Uiso 1 1 calc R . . C104 C -0.0567(8) 0.0521(10) 1.6799(5) 0.064(3) Uani 1 1 d U . . H10I H -0.0561 0.0146 1.7121 0.077 Uiso 1 1 calc R . . H10J H -0.0017 0.0912 1.6823 0.077 Uiso 1 1 calc R . . O15 O -0.1359(5) -0.2499(6) 1.1673(3) 0.0491(19) Uani 1 1 d U B . C105 C -0.1490(9) -0.3390(10) 1.1948(5) 0.065(3) Uani 1 1 d U . . H10K H -0.1451 -0.3223 1.2312 0.078 Uiso 1 1 calc R B . H10L H -0.1031 -0.3897 1.1913 0.078 Uiso 1 1 calc R . . C106 C -0.2340(9) -0.3813(10) 1.1757(5) 0.072(3) Uani 1 1 d U B . H10M H -0.2385 -0.3959 1.1390 0.087 Uiso 1 1 calc R . . H10N H -0.2421 -0.4461 1.1934 0.087 Uiso 1 1 calc R . . O16 O -0.2998(6) -0.3107(7) 1.1837(3) 0.058(2) Uani 1 1 d DU B . C107 C -0.3749(13) -0.3718(16) 1.1766(9) 0.054(4) Uani 0.634(9) 1 d PU B 1 H10O H -0.3745 -0.4219 1.2043 0.065 Uiso 0.634(9) 1 calc PR B 1 H10P H -0.3827 -0.4078 1.1436 0.065 Uiso 0.634(9) 1 calc PR B 1 C108 C -0.4425(16) -0.2908(17) 1.1778(9) 0.058(4) Uani 0.634(9) 1 d PU B 1 H10Q H -0.5011 -0.3224 1.1736 0.069 Uiso 0.634(9) 1 calc PR B 1 H10R H -0.4321 -0.2557 1.2110 0.069 Uiso 0.634(9) 1 calc PR B 1 O17 O -0.4391(8) -0.2200(11) 1.1389(5) 0.052(3) Uani 0.634(9) 1 d PU B 1 C109 C -0.5112(13) -0.1557(17) 1.1312(8) 0.052(4) Uani 0.634(9) 1 d PDU B 1 H10S H -0.5146 -0.1155 1.1622 0.062 Uiso 0.634(9) 1 calc PR B 1 H10T H -0.5655 -0.1958 1.1226 0.062 Uiso 0.634(9) 1 calc PR B 1 C110 C -0.4996(13) -0.0859(18) 1.0879(8) 0.050(4) Uani 0.634(9) 1 d PDU B 1 H11B H -0.4931 -0.1269 1.0576 0.060 Uiso 0.634(9) 1 calc PR B 1 H11C H -0.5516 -0.0419 1.0792 0.060 Uiso 0.634(9) 1 calc PR B 1 O18 O -0.4245(10) -0.0246(11) 1.1021(5) 0.047(3) Uani 0.634(9) 1 d PU B 1 C111 C -0.4064(13) 0.0432(16) 1.0622(7) 0.048(4) Uani 0.634(9) 1 d PU B 1 H11D H -0.4574 0.0875 1.0510 0.058 Uiso 0.634(9) 1 calc PR B 1 H11E H -0.3946 0.0029 1.0327 0.058 Uiso 0.634(9) 1 calc PR B 1 C112 C -0.3307(15) 0.105(2) 1.0817(10) 0.054(5) Uani 0.634(9) 1 d PU B 1 H11F H -0.3221 0.1573 1.0561 0.065 Uiso 0.634(9) 1 calc PR B 1 H11G H -0.3413 0.1413 1.1126 0.065 Uiso 0.634(9) 1 calc PR B 1 O19 O -0.2571(9) 0.0475(10) 1.0928(5) 0.051(3) Uani 0.634(9) 1 d PU B 1 C113 C -0.1786(14) 0.0997(18) 1.1075(9) 0.054(3) Uani 0.634(9) 1 d PU B 1 H11H H -0.1802 0.1330 1.1406 0.064 Uiso 0.634(9) 1 calc PR B 1 H11I H -0.1738 0.1541 1.0824 0.064 Uiso 0.634(9) 1 calc PR B 1 C114 C -0.0945(8) 0.0300(9) 1.1124(4) 0.052(3) Uani 0.634(9) 1 d PU B 1 H11J H -0.0896 -0.0007 1.0792 0.062 Uiso 0.634(9) 1 calc PR B 1 H11K H -0.0416 0.0712 1.1238 0.062 Uiso 0.634(9) 1 calc PR B 1 C07A C -0.3999(13) -0.315(3) 1.1698(18) 0.063(7) Uiso 0.366(9) 1 d PDU B 2 H07A H -0.4137 -0.3251 1.1327 0.075 Uiso 0.366(9) 1 calc PR B 2 H07B H -0.4195 -0.3767 1.1858 0.075 Uiso 0.366(9) 1 calc PR B 2 C08A C -0.455(2) -0.230(3) 1.1824(14) 0.052(6) Uiso 0.366(9) 1 d PU B 2 H08A H -0.5167 -0.2491 1.1714 0.063 Uiso 0.366(9) 1 calc PR B 2 H08B H -0.4461 -0.2226 1.2197 0.063 Uiso 0.366(9) 1 calc PR B 2 O17A O -0.4422(12) -0.1293(14) 1.1611(7) 0.041(5) Uiso 0.366(9) 1 d PU B 2 C09A C -0.494(2) -0.114(3) 1.1111(15) 0.043(6) Uiso 0.366(9) 1 d PU B 2 H09A H -0.5567 -0.1196 1.1128 0.051 Uiso 0.366(9) 1 calc PR B 2 H09B H -0.4786 -0.1665 1.0871 0.051 Uiso 0.366(9) 1 calc PR B 2 C10A C -0.471(2) -0.010(3) 1.0946(15) 0.044(6) Uiso 0.366(9) 1 d PU B 2 H10U H -0.5080 0.0061 1.0616 0.053 Uiso 0.366(9) 1 calc PR B 2 H10V H -0.4855 0.0407 1.1197 0.053 Uiso 0.366(9) 1 calc PR B 2 O18A O -0.3815(14) 0.0005(16) 1.0897(9) 0.035(5) Uiso 0.366(9) 1 d PU B 2 C11A C -0.362(2) 0.100(4) 1.0716(17) 0.043(6) Uiso 0.366(9) 1 d PU B 2 H11L H -0.3814 0.1534 1.0935 0.052 Uiso 0.366(9) 1 calc PR B 2 H11M H -0.3932 0.1101 1.0366 0.052 Uiso 0.366(9) 1 calc PR B 2 C12A C -0.262(2) 0.106(3) 1.0729(11) 0.039(5) Uiso 0.366(9) 1 d PU B 2 H12B H -0.2429 0.0484 1.0539 0.047 Uiso 0.366(9) 1 calc PR B 2 H12C H -0.2480 0.1703 1.0564 0.047 Uiso 0.366(9) 1 calc PR B 2 O19A O -0.2186(13) 0.1040(17) 1.1241(8) 0.037(5) Uiso 0.366(9) 1 d PU B 2 C13A C -0.126(2) 0.116(2) 1.1274(12) 0.038(6) Uiso 0.366(9) 1 d PU B 2 H13B H -0.1135 0.1729 1.1055 0.046 Uiso 0.366(9) 1 calc PR B 2 H13C H -0.0997 0.1312 1.1627 0.046 Uiso 0.366(9) 1 calc PR B 2 C14A C -0.0945(8) 0.0300(9) 1.1124(4) 0.052(3) Uani 0.366(9) 1 d PU B 2 H14A H -0.0324 0.0394 1.1093 0.062 Uiso 0.366(9) 1 calc PR B 2 H14B H -0.1267 0.0103 1.0788 0.062 Uiso 0.366(9) 1 calc PR B 2 O20 O -0.1027(5) -0.0473(6) 1.1482(3) 0.0443(18) Uani 1 1 d U B . C115 C -0.0399(7) -0.1246(9) 1.1474(4) 0.048(3) Uani 1 1 d U . . H11N H 0.0194 -0.0953 1.1561 0.057 Uiso 1 1 calc R B . H11O H -0.0456 -0.1541 1.1129 0.057 Uiso 1 1 calc R . . C116 C -0.0523(7) -0.2050(9) 1.1841(4) 0.054(3) Uani 1 1 d U B . H11P H -0.0059 -0.2571 1.1856 0.064 Uiso 1 1 calc R . . H11Q H -0.0501 -0.1754 1.2184 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0237(8) 0.0267(8) 0.0309(9) 0.0004(8) 0.0024(7) -0.0031(7) K1 0.0395(16) 0.0635(18) 0.0338(15) 0.0059(14) 0.0093(12) 0.0135(13) Fe2 0.0253(9) 0.0255(8) 0.0258(9) 0.0001(8) 0.0027(7) -0.0014(7) K2 0.0343(14) 0.0414(14) 0.0310(14) -0.0002(12) 0.0053(12) 0.0070(12) C1 0.048(7) 0.023(5) 0.036(5) -0.002(5) 0.001(5) -0.006(5) C2 0.042(7) 0.030(6) 0.036(6) 0.004(5) 0.000(5) 0.014(5) C3 0.040(7) 0.029(6) 0.044(6) 0.015(5) 0.009(6) -0.002(5) C4 0.050(7) 0.025(6) 0.052(6) 0.004(5) -0.009(6) -0.016(5) C5 0.036(7) 0.032(6) 0.036(6) 0.009(5) -0.003(5) -0.004(5) C6 0.021(6) 0.026(5) 0.038(5) -0.001(4) 0.011(5) 0.011(4) C7 0.019(5) 0.033(5) 0.039(6) 0.000(4) 0.000(5) -0.003(4) C8 0.022(5) 0.047(7) 0.053(7) 0.002(6) 0.013(5) 0.001(5) N1 0.022(4) 0.025(4) 0.028(5) 0.000(3) 0.000(3) -0.004(3) O1 0.023(4) 0.032(4) 0.032(4) -0.001(3) 0.004(3) -0.001(3) C9 0.018(5) 0.035(5) 0.020(6) 0.000(4) 0.006(4) -0.005(4) C10 0.016(5) 0.034(5) 0.032(6) 0.002(5) 0.005(4) 0.003(4) C11 0.024(6) 0.042(5) 0.033(6) -0.005(5) -0.001(4) -0.003(5) C12 0.024(6) 0.044(6) 0.029(6) 0.005(5) 0.004(5) 0.004(4) C13 0.034(6) 0.039(6) 0.018(6) 0.001(5) 0.002(4) 0.006(5) N2 0.020(4) 0.028(4) 0.019(4) 0.010(3) 0.004(3) 0.000(3) C14 0.025(5) 0.026(5) 0.038(7) 0.009(5) 0.002(4) -0.002(4) O2 0.028(4) 0.034(4) 0.044(5) -0.006(4) 0.008(3) 0.000(3) C15 0.019(6) 0.030(5) 0.035(6) 0.007(5) 0.006(4) -0.005(4) N3 0.016(4) 0.031(4) 0.039(5) -0.007(4) 0.003(3) -0.010(3) C16 0.026(6) 0.037(6) 0.048(6) -0.007(5) 0.001(4) -0.009(5) C17 0.043(7) 0.036(6) 0.052(8) -0.019(5) 0.016(6) -0.012(5) C18 0.042(6) 0.034(6) 0.035(5) -0.001(5) 0.002(4) -0.010(5) C19 0.041(7) 0.069(8) 0.046(5) 0.010(6) -0.003(5) -0.016(5) C20 0.049(7) 0.085(10) 0.037(5) 0.024(6) 0.005(5) -0.030(6) C21 0.049(7) 0.081(10) 0.046(6) -0.007(7) 0.011(5) -0.038(6) C22 0.049(7) 0.040(7) 0.044(6) 0.001(6) 0.013(5) -0.017(5) C23 0.053(7) 0.025(6) 0.032(5) 0.002(5) 0.003(5) -0.005(5) C24 0.050(7) 0.044(5) 0.030(7) 0.000(6) 0.014(5) -0.012(5) C25 0.045(7) 0.044(5) 0.042(7) -0.011(6) 0.003(5) 0.007(6) C26 0.051(6) 0.028(5) 0.053(6) 0.005(5) -0.002(5) -0.011(4) C27 0.040(7) 0.056(6) 0.055(8) 0.006(7) 0.010(6) -0.011(6) C28 0.037(6) 0.042(5) 0.047(7) 0.004(6) 0.013(5) 0.007(5) C29 0.038(7) 0.037(5) 0.028(6) -0.005(5) -0.003(5) -0.008(4) C30 0.042(6) 0.043(5) 0.023(5) 0.001(5) 0.010(4) -0.005(5) C31 0.037(7) 0.037(6) 0.042(7) -0.006(6) -0.004(5) -0.001(5) N4 0.022(4) 0.033(5) 0.027(4) -0.002(4) 0.004(3) 0.000(4) O3 0.025(4) 0.037(4) 0.058(5) 0.005(4) 0.020(4) -0.004(3) C32 0.016(5) 0.021(5) 0.051(6) -0.002(5) 0.005(4) 0.002(4) C33 0.023(4) 0.025(6) 0.040(5) -0.003(5) 0.008(3) 0.003(5) C34 0.018(4) 0.049(7) 0.058(6) 0.004(6) -0.002(4) -0.004(5) C35 0.027(5) 0.038(7) 0.049(6) -0.009(5) -0.011(4) -0.004(5) C36 0.034(5) 0.038(6) 0.039(6) 0.002(5) -0.016(4) -0.007(5) N5 0.014(3) 0.027(5) 0.027(4) -0.009(4) -0.006(3) -0.007(3) C37 0.024(4) 0.022(5) 0.034(5) 0.000(5) -0.003(4) -0.006(5) O4 0.053(5) 0.042(4) 0.024(3) 0.006(3) 0.007(3) -0.001(4) C38 0.034(5) 0.016(5) 0.031(5) -0.003(5) 0.001(4) -0.003(5) N6 0.026(4) 0.043(5) 0.024(4) 0.001(4) 0.004(3) -0.001(4) C39 0.028(5) 0.043(6) 0.036(6) -0.004(5) 0.007(4) 0.002(5) C40 0.046(6) 0.047(5) 0.060(6) -0.015(5) 0.018(5) -0.006(4) C41 0.025(5) 0.028(5) 0.032(6) 0.009(4) 0.010(4) -0.005(4) C42 0.036(6) 0.024(5) 0.032(6) -0.004(5) 0.012(4) 0.002(4) C43 0.028(6) 0.056(6) 0.036(7) 0.000(6) 0.005(5) 0.004(5) C44 0.031(6) 0.052(7) 0.040(7) -0.017(6) 0.010(5) -0.016(5) C45 0.044(6) 0.031(6) 0.047(7) -0.009(5) 0.020(5) -0.015(5) C46 0.036(6) 0.031(5) 0.028(6) 0.011(4) 0.010(4) 0.008(4) C47 0.030(6) 0.019(5) 0.021(5) 0.004(4) -0.004(5) -0.012(4) C48 0.060(8) 0.023(5) 0.028(6) -0.003(4) 0.004(6) -0.009(5) C49 0.059(7) 0.022(5) 0.039(6) -0.005(5) 0.003(6) -0.003(5) C50 0.042(6) 0.022(5) 0.034(5) 0.010(5) -0.012(5) 0.001(5) C51 0.019(6) 0.036(5) 0.032(6) -0.001(4) -0.016(5) 0.001(5) C52 0.017(5) 0.022(4) 0.030(5) 0.003(4) 0.000(4) 0.009(4) C53 0.023(5) 0.027(5) 0.030(6) -0.001(4) 0.004(4) 0.000(4) C54 0.039(6) 0.032(6) 0.048(7) 0.002(6) 0.022(5) 0.006(5) N7 0.022(4) 0.025(4) 0.026(5) -0.001(3) 0.007(3) -0.001(3) O5 0.028(4) 0.034(4) 0.031(4) 0.006(4) 0.001(3) 0.006(4) C55 0.031(6) 0.028(5) 0.022(6) -0.001(4) 0.009(4) -0.001(4) C56 0.022(5) 0.026(4) 0.023(6) -0.009(4) 0.002(4) 0.010(4) C57 0.029(6) 0.029(5) 0.031(6) 0.004(5) 0.004(4) 0.005(4) C58 0.023(6) 0.039(5) 0.042(7) -0.001(5) -0.003(5) 0.006(5) C59 0.014(5) 0.034(5) 0.041(7) -0.004(5) 0.012(4) -0.004(4) N8 0.012(4) 0.034(4) 0.022(4) -0.004(4) -0.001(3) -0.001(3) C60 0.021(5) 0.027(4) 0.017(5) -0.002(4) 0.012(4) -0.002(4) O6 0.037(4) 0.024(3) 0.035(4) 0.000(3) 0.012(3) -0.007(3) C61 0.033(6) 0.037(5) 0.026(6) 0.001(5) 0.008(4) -0.014(4) N9 0.027(4) 0.016(4) 0.028(5) 0.004(3) -0.004(3) -0.004(3) C62 0.036(5) 0.022(5) 0.030(5) 0.001(4) 0.011(4) 0.010(4) C63 0.036(5) 0.032(6) 0.034(6) 0.005(5) 0.016(5) 0.012(5) C64 0.025(5) 0.015(5) 0.032(5) -0.001(4) 0.012(4) 0.007(4) C65 0.032(6) 0.024(5) 0.037(5) -0.002(5) 0.006(5) 0.005(4) C66 0.053(7) 0.044(7) 0.036(6) -0.008(6) 0.006(5) 0.001(5) C67 0.056(7) 0.049(8) 0.034(6) 0.003(5) 0.022(5) 0.015(5) C68 0.046(7) 0.018(6) 0.054(6) 0.007(5) 0.026(5) 0.005(5) C69 0.030(6) 0.034(7) 0.039(5) -0.001(6) 0.005(5) -0.004(5) C75 0.019(5) 0.041(5) 0.033(6) 0.005(5) 0.008(4) 0.005(4) C70 0.033(6) 0.036(6) 0.028(7) 0.000(6) 0.005(5) -0.002(5) C71 0.044(6) 0.048(6) 0.042(7) 0.004(6) 0.001(5) 0.008(5) C72 0.046(7) 0.048(6) 0.047(7) 0.010(6) 0.012(5) 0.005(6) C73 0.048(7) 0.048(6) 0.052(7) 0.006(6) 0.018(6) 0.001(5) C74 0.029(9) 0.045(7) 0.063(13) 0.003(9) 0.005(8) -0.006(6) C76 0.021(4) 0.040(6) 0.038(6) 0.007(5) 0.009(4) 0.005(4) C77 0.035(15) 0.045(18) 0.053(16) 0.017(17) 0.019(13) -0.005(14) C75A 0.019(5) 0.041(5) 0.033(6) 0.005(5) 0.008(4) 0.005(4) C76A 0.021(4) 0.040(6) 0.038(6) 0.007(5) 0.009(4) 0.005(4) C77A 0.05(2) 0.04(2) 0.027(16) 0.000(15) 0.013(13) 0.00(2) N10 0.019(3) 0.030(4) 0.029(4) 0.002(3) 0.002(3) 0.002(3) O7 0.033(4) 0.039(4) 0.033(4) -0.002(3) 0.002(3) 0.000(3) C78 0.031(4) 0.025(6) 0.032(5) -0.002(5) 0.003(4) 0.002(5) C79 0.028(4) 0.019(5) 0.022(5) 0.007(4) -0.004(4) 0.001(4) C80 0.035(5) 0.031(6) 0.028(6) -0.001(5) 0.003(4) -0.005(5) C81 0.024(5) 0.026(6) 0.043(6) -0.009(5) -0.010(4) -0.003(5) C82 0.015(3) 0.025(4) 0.030(3) 0.002(3) 0.002(2) -0.001(3) N11 0.015(3) 0.025(4) 0.030(3) 0.002(3) 0.002(2) -0.001(3) C83 0.027(5) 0.014(5) 0.031(5) 0.001(4) 0.002(4) -0.007(4) O8 0.027(4) 0.048(5) 0.033(4) 0.007(4) 0.015(3) 0.000(4) C84 0.021(4) 0.023(5) 0.030(5) 0.005(4) 0.002(4) -0.001(4) N12 0.015(4) 0.020(4) 0.034(4) 0.001(3) 0.004(3) -0.001(3) C85 0.027(6) 0.033(5) 0.025(5) 0.000(4) -0.007(4) 0.010(5) C86 0.055(7) 0.033(5) 0.033(5) -0.007(5) 0.007(5) -0.004(6) C87 0.021(6) 0.030(4) 0.041(7) -0.004(5) 0.008(5) 0.002(4) C88 0.029(6) 0.036(5) 0.028(6) -0.003(5) 0.015(5) -0.006(4) C89 0.062(8) 0.028(5) 0.028(6) -0.003(5) 0.009(5) -0.009(6) C90 0.054(7) 0.028(5) 0.031(6) -0.007(5) -0.006(5) 0.014(5) C91 0.038(7) 0.043(6) 0.047(7) -0.016(6) 0.006(5) 0.001(5) C92 0.028(6) 0.035(5) 0.037(7) -0.013(5) 0.009(5) -0.007(5) O9 0.029(4) 0.081(5) 0.043(5) -0.012(4) 0.007(4) -0.004(3) C93 0.056(5) 0.086(6) 0.072(7) -0.020(5) 0.009(5) -0.013(4) C94 0.066(7) 0.059(7) 0.061(9) -0.024(7) 0.026(7) -0.024(5) O10 0.047(4) 0.039(4) 0.054(5) -0.005(4) 0.013(4) -0.004(3) C95 0.079(7) 0.034(6) 0.047(8) -0.007(6) 0.005(7) 0.008(5) C96 0.055(6) 0.042(7) 0.075(9) -0.014(6) 0.000(7) 0.018(5) O11 0.038(4) 0.036(4) 0.048(5) 0.001(3) 0.004(4) 0.004(3) C97 0.044(6) 0.045(6) 0.059(8) 0.004(6) 0.010(6) 0.003(5) C98 0.034(6) 0.049(6) 0.043(7) 0.005(5) 0.000(5) -0.004(5) O12 0.038(4) 0.033(4) 0.044(5) 0.008(3) 0.001(3) -0.004(3) C99 0.038(6) 0.053(7) 0.061(8) -0.010(6) 0.017(6) -0.013(5) C100 0.058(6) 0.034(6) 0.077(9) -0.009(6) 0.026(7) -0.005(5) O13 0.042(4) 0.041(4) 0.058(5) -0.005(4) 0.011(4) 0.004(3) C101 0.059(6) 0.063(7) 0.079(10) -0.003(7) 0.027(7) 0.019(5) C102 0.049(6) 0.076(8) 0.053(8) -0.009(6) 0.012(6) 0.020(5) O14 0.046(4) 0.066(5) 0.038(4) 0.001(4) 0.017(4) 0.017(3) C103 0.046(5) 0.075(6) 0.057(6) 0.002(5) 0.005(5) 0.010(4) C104 0.041(5) 0.089(6) 0.059(6) -0.006(5) -0.002(5) 0.005(4) O15 0.054(4) 0.043(4) 0.051(5) 0.010(4) 0.010(4) 0.015(3) C105 0.076(5) 0.059(5) 0.060(6) 0.014(5) 0.015(5) 0.012(4) C106 0.089(6) 0.064(5) 0.067(7) 0.004(5) 0.023(5) -0.009(4) O16 0.065(4) 0.063(4) 0.047(5) -0.003(4) 0.012(4) -0.024(4) C107 0.066(8) 0.055(8) 0.042(11) -0.011(9) 0.015(10) -0.010(6) C108 0.054(6) 0.054(7) 0.061(7) -0.005(6) 0.003(6) -0.005(5) O17 0.044(5) 0.063(7) 0.048(8) -0.011(5) 0.000(6) -0.004(4) C109 0.047(6) 0.060(7) 0.048(8) -0.016(6) 0.002(6) 0.001(5) C110 0.037(8) 0.066(11) 0.047(10) -0.012(7) 0.004(7) 0.011(7) O18 0.043(5) 0.058(6) 0.040(5) -0.014(5) 0.001(5) 0.011(4) C111 0.052(6) 0.046(7) 0.044(6) -0.004(5) 0.000(5) 0.012(5) C112 0.063(7) 0.051(9) 0.044(11) -0.005(8) -0.007(9) 0.004(6) O19 0.058(5) 0.045(6) 0.050(7) 0.004(5) 0.008(6) 0.005(4) C113 0.063(5) 0.049(5) 0.046(6) 0.005(5) 0.002(5) -0.003(4) C114 0.068(6) 0.044(6) 0.045(7) -0.007(5) 0.014(5) -0.015(5) C14A 0.068(6) 0.044(6) 0.045(7) -0.007(5) 0.014(5) -0.015(5) O20 0.052(4) 0.043(4) 0.042(5) -0.003(3) 0.017(4) -0.001(3) C115 0.032(6) 0.070(7) 0.041(7) -0.008(5) 0.005(5) 0.000(5) C116 0.047(6) 0.066(7) 0.046(7) 0.006(6) 0.000(6) 0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.887(7) . ? Fe1 N5 1.891(7) . ? Fe1 N3 1.982(8) . ? Fe1 N1 2.025(8) . ? Fe1 N6 2.027(8) . ? Fe1 N4 2.050(9) . ? K1 O7 2.606(8) . ? K1 O17A 2.704(19) . ? K1 O19 2.755(14) . ? K1 O18A 2.77(2) . ? K1 O20 2.779(8) . ? K1 O15 2.829(8) . ? K1 O16 2.846(9) . ? K1 O18 2.880(15) . ? K1 O17 3.044(13) . ? K1 O19A 3.05(2) . ? K1 C08A 3.45(4) . ? K1 C113 3.45(2) . ? Fe2 N11 1.867(8) . ? Fe2 N8 1.892(7) . ? Fe2 N10 1.971(8) . ? Fe2 N12 1.981(8) . ? Fe2 N7 1.998(8) . ? Fe2 N9 2.002(8) . ? K2 O4 2.580(8) . ? K2 O13 2.790(8) . ? K2 O10 2.796(8) . ? K2 O12 2.817(8) . ? K2 O9 2.819(8) . ? K2 O14 2.822(8) . ? K2 O11 2.922(8) . ? C1 C6 1.353(14) . ? C1 C2 1.401(15) . ? C1 H1A 0.9500 . ? C2 C3 1.390(15) . ? C2 H2A 0.9500 . ? C3 C4 1.344(15) . ? C3 H3A 0.9500 . ? C4 C5 1.383(15) . ? C4 H4A 0.9500 . ? C5 C6 1.403(14) . ? C5 H5A 0.9500 . ? C6 C7 1.523(14) . ? C7 N1 1.501(12) . ? C7 C8 1.520(13) . ? C7 H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N1 C9 1.374(12) . ? O1 C9 1.238(11) . ? C9 C10 1.465(14) . ? C10 N2 1.327(12) . ? C10 C11 1.375(13) . ? C11 C12 1.366(13) . ? C11 H11A 0.9500 . ? C12 C13 1.394(14) . ? C12 H12A 0.9500 . ? C13 C14 1.359(13) . ? C13 H13A 0.9500 . ? N2 C14 1.349(13) . ? C14 C15 1.499(14) . ? O2 C15 1.241(12) . ? C15 N3 1.344(12) . ? N3 C16 1.487(12) . ? C16 C18 1.510(14) . ? C16 C17 1.544(14) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.368(15) . ? C18 C23 1.409(14) . ? C19 C20 1.382(16) . ? C19 H19A 0.9500 . ? C20 C21 1.382(16) . ? C20 H20A 0.9500 . ? C21 C22 1.351(15) . ? C21 H21A 0.9500 . ? C22 C23 1.388(14) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.377(16) . ? C24 C29 1.389(15) . ? C24 H24A 0.9500 . ? C25 C26 1.384(15) . ? C25 H25A 0.9500 . ? C26 C27 1.369(16) . ? C26 H26A 0.9500 . ? C27 C28 1.382(16) . ? C27 H27A 0.9500 . ? C28 C29 1.388(15) . ? C28 H28A 0.9500 . ? C29 C30 1.500(15) . ? C30 C31 1.500(13) . ? C30 N4 1.508(13) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N4 C32 1.368(12) . ? O3 C32 1.237(12) . ? C32 C33 1.483(15) . ? C33 N5 1.323(12) . ? C33 C34 1.373(13) . ? C34 C35 1.383(15) . ? C34 H34A 0.9500 . ? C35 C36 1.392(15) . ? C35 H35A 0.9500 . ? C36 C37 1.382(13) . ? C36 H36A 0.9500 . ? N5 C37 1.335(12) . ? C37 C38 1.542(15) . ? O4 C38 1.210(12) . ? C38 N6 1.358(12) . ? N6 C39 1.475(12) . ? C39 C41 1.505(14) . ? C39 C40 1.515(14) . ? C39 H39A 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.381(14) . ? C41 C46 1.394(14) . ? C42 C43 1.401(14) . ? C42 H42A 0.9500 . ? C43 C44 1.376(14) . ? C43 H43A 0.9500 . ? C44 C45 1.354(14) . ? C44 H44A 0.9500 . ? C45 C46 1.382(14) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.373(14) . ? C47 C52 1.410(13) . ? C47 H47A 0.9500 . ? C48 C49 1.353(15) . ? C48 H48A 0.9500 . ? C49 C50 1.403(14) . ? C49 H49A 0.9500 . ? C50 C51 1.399(15) . ? C50 H50A 0.9500 . ? C51 C52 1.370(13) . ? C51 H51A 0.9500 . ? C52 C53 1.523(13) . ? C53 N7 1.471(12) . ? C53 C54 1.523(12) . ? C53 H53A 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? N7 C55 1.318(12) . ? O5 C55 1.254(12) . ? C55 C56 1.536(14) . ? C56 N8 1.345(12) . ? C56 C57 1.369(13) . ? C57 C58 1.361(15) . ? C57 H57A 0.9500 . ? C58 C59 1.370(14) . ? C58 H58A 0.9500 . ? C59 C60 1.414(13) . ? C59 H59A 0.9500 . ? N8 C60 1.337(12) . ? C60 C61 1.473(14) . ? O6 C61 1.253(11) . ? C61 N9 1.349(12) . ? N9 C62 1.474(11) . ? C62 C63 1.514(13) . ? C62 C64 1.534(13) . ? C62 H62A 1.0000 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C69 1.382(13) . ? C64 C65 1.400(13) . ? C65 C66 1.381(14) . ? C65 H65A 0.9500 . ? C66 C67 1.391(15) . ? C66 H66A 0.9500 . ? C67 C68 1.373(15) . ? C67 H67A 0.9500 . ? C68 C69 1.363(14) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C75 C70 1.38(2) . ? C75 C74 1.41(3) . ? C75 C76 1.54(3) . ? C70 C71 1.39(3) . ? C70 H70A 0.9500 . ? C71 C72 1.36(3) . ? C71 H71A 0.9500 . ? C72 C73 1.42(3) . ? C72 H72A 0.9500 . ? C73 C74 1.39(3) . ? C73 H73A 0.9500 . ? C74 H74A 0.9500 . ? C76 C77 1.41(3) . ? C76 N10 1.48(2) . ? C76 H76A 1.0000 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C75A C74A 1.3900 . ? C75A C70A 1.3900 . ? C75A C76A 1.52(4) . ? C74A C73A 1.3900 . ? C74A H74B 0.9500 . ? C73A C72A 1.3900 . ? C73A H73B 0.9500 . ? C72A C71A 1.3900 . ? C72A H72B 0.9500 . ? C71A C70A 1.3900 . ? C71A H71B 0.9500 . ? C70A H70B 0.9500 . ? C76A N10 1.46(4) . ? C76A C77A 1.69(5) . ? C76A H76B 1.0000 . ? C77A H77D 0.9800 . ? C77A H77E 0.9800 . ? C77A H77F 0.9800 . ? N10 C78 1.331(12) . ? O7 C78 1.277(12) . ? C78 C79 1.505(15) . ? C79 N11 1.309(12) . ? C79 C80 1.385(13) . ? C80 C81 1.376(14) . ? C80 H80A 0.9500 . ? C81 C82 1.394(13) . ? C81 H81A 0.9500 . ? C82 C83 1.387(13) . ? C82 H82A 0.9500 . ? N11 C83 1.364(12) . ? C83 C84 1.501(14) . ? O8 C84 1.245(12) . ? C84 N12 1.328(12) . ? N12 C85 1.488(12) . ? C85 C86 1.521(13) . ? C85 C87 1.542(14) . ? C85 H85A 1.0000 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.343(14) . ? C87 C92 1.384(14) . ? C88 C89 1.402(15) . ? C88 H88A 0.9500 . ? C89 C90 1.379(15) . ? C89 H89A 0.9500 . ? C90 C91 1.386(15) . ? C90 H90A 0.9500 . ? C91 C92 1.376(14) . ? C91 H91A 0.9500 . ? C92 H92A 0.9500 . ? O9 C93 1.420(14) . ? O9 C104 1.420(13) . ? C93 C94 1.511(17) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 O10 1.439(13) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? O10 C95 1.424(13) . ? C95 C96 1.507(17) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 O11 1.432(13) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? O11 C97 1.411(13) . ? C97 C98 1.513(15) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 O12 1.415(12) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? O12 C99 1.417(12) . ? C99 C100 1.495(15) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 O13 1.419(12) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? O13 C101 1.400(13) . ? C101 C102 1.505(16) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 O14 1.419(14) . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? O14 C103 1.427(14) . ? C103 C104 1.475(16) . ? C103 H10G 0.9900 . ? C103 H10H 0.9900 . ? C104 H10I 0.9900 . ? C104 H10J 0.9900 . ? O15 C105 1.414(14) . ? O15 C116 1.432(13) . ? C105 C106 1.449(17) . ? C105 H10K 0.9900 . ? C105 H10L 0.9900 . ? C106 O16 1.422(15) . ? C106 H10M 0.9900 . ? C106 H10N 0.9900 . ? O16 C107 1.40(2) . ? O16 C07A 1.542(18) . ? C107 C108 1.50(3) . ? C107 H10O 0.9900 . ? C107 H10P 0.9900 . ? C108 O17 1.40(3) . ? C108 H10Q 0.9900 . ? C108 H10R 0.9900 . ? O17 C109 1.39(2) . ? C109 C110 1.510(16) . ? C109 H10S 0.9900 . ? C109 H10T 0.9900 . ? C110 O18 1.42(2) . ? C110 H11B 0.9900 . ? C110 H11C 0.9900 . ? O18 C111 1.45(2) . ? C111 C112 1.46(3) . ? C111 H11D 0.9900 . ? C111 H11E 0.9900 . ? C112 O19 1.36(3) . ? C112 H11F 0.9900 . ? C112 H11G 0.9900 . ? O19 C113 1.40(2) . ? C113 C114 1.58(2) . ? C113 H11H 0.9900 . ? C113 H11I 0.9900 . ? C114 O20 1.414(13) . ? C114 H11J 0.9900 . ? C114 H11K 0.9900 . ? C07A C08A 1.48(5) . ? C07A H07A 0.9900 . ? C07A H07B 0.9900 . ? C08A O17A 1.46(4) . ? C08A H08A 0.9900 . ? C08A H08B 0.9900 . ? O17A C09A 1.45(4) . ? C09A C10A 1.50(5) . ? C09A H09A 0.9900 . ? C09A H09B 0.9900 . ? C10A O18A 1.43(4) . ? C10A H10U 0.9900 . ? C10A H10V 0.9900 . ? O18A C11A 1.44(5) . ? C11A C12A 1.55(5) . ? C11A H11L 0.9900 . ? C11A H11M 0.9900 . ? C12A O19A 1.43(4) . ? C12A H12B 0.9900 . ? C12A H12C 0.9900 . ? O19A C13A 1.43(4) . ? C13A H13B 0.9900 . ? C13A H13C 0.9900 . ? O20 C115 1.410(12) . ? C115 C116 1.476(15) . ? C115 H11N 0.9900 . ? C115 H11O 0.9900 . ? C116 H11P 0.9900 . ? C116 H11Q 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N5 178.4(4) . . ? N2 Fe1 N3 81.2(4) . . ? N5 Fe1 N3 97.4(4) . . ? N2 Fe1 N1 80.7(4) . . ? N5 Fe1 N1 100.7(3) . . ? N3 Fe1 N1 161.9(3) . . ? N2 Fe1 N6 98.4(3) . . ? N5 Fe1 N6 80.8(3) . . ? N3 Fe1 N6 88.5(4) . . ? N1 Fe1 N6 95.0(3) . . ? N2 Fe1 N4 100.6(3) . . ? N5 Fe1 N4 80.1(3) . . ? N3 Fe1 N4 91.2(4) . . ? N1 Fe1 N4 91.2(3) . . ? N6 Fe1 N4 160.7(3) . . ? O7 K1 O17A 90.4(4) . . ? O7 K1 O19 108.8(3) . . ? O17A K1 O19 104.7(5) . . ? O7 K1 O18A 113.1(5) . . ? O17A K1 O18A 62.3(6) . . ? O19 K1 O18A 42.9(5) . . ? O7 K1 O20 95.4(2) . . ? O17A K1 O20 167.6(4) . . ? O19 K1 O20 63.0(3) . . ? O18A K1 O20 105.3(5) . . ? O7 K1 O15 108.5(2) . . ? O17A K1 O15 128.9(4) . . ? O19 K1 O15 112.4(3) . . ? O18A K1 O15 137.0(5) . . ? O20 K1 O15 59.2(2) . . ? O7 K1 O16 103.2(3) . . ? O17A K1 O16 71.3(4) . . ? O19 K1 O16 147.8(3) . . ? O18A K1 O16 119.7(5) . . ? O20 K1 O16 117.7(3) . . ? O15 K1 O16 58.5(2) . . ? O7 K1 O18 107.7(3) . . ? O17A K1 O18 45.0(5) . . ? O19 K1 O18 59.9(4) . . ? O18A K1 O18 17.3(4) . . ? O20 K1 O18 122.6(4) . . ? O15 K1 O18 143.3(3) . . ? O16 K1 O18 107.2(4) . . ? O7 K1 O17 110.5(3) . . ? O17A K1 O17 26.0(5) . . ? O19 K1 O17 111.4(4) . . ? O18A K1 O17 70.4(5) . . ? O20 K1 O17 153.5(3) . . ? O15 K1 O17 105.2(3) . . ? O16 K1 O17 52.0(3) . . ? O18 K1 O17 55.6(4) . . ? O7 K1 O19A 87.4(4) . . ? O17A K1 O19A 114.8(6) . . ? O19 K1 O19A 23.2(4) . . ? O18A K1 O19A 59.3(6) . . ? O20 K1 O19A 54.7(4) . . ? O15 K1 O19A 113.1(4) . . ? O16 K1 O19A 167.9(5) . . ? O18 K1 O19A 74.2(5) . . ? O17 K1 O19A 129.6(5) . . ? O7 K1 C08A 90.9(6) . . ? O17A K1 C08A 23.7(7) . . ? O19 K1 C08A 126.6(7) . . ? O18A K1 C08A 83.8(8) . . ? O20 K1 C08A 165.8(6) . . ? O15 K1 C08A 106.7(6) . . ? O16 K1 C08A 48.3(6) . . ? O18 K1 C08A 66.9(7) . . ? O17 K1 C08A 20.7(6) . . ? O19A K1 C08A 138.5(7) . . ? O7 K1 C113 95.5(4) . . ? O17A K1 C113 124.3(5) . . ? O19 K1 C113 22.7(4) . . ? O18A K1 C113 64.6(6) . . ? O20 K1 C113 44.2(4) . . ? O15 K1 C113 101.2(4) . . ? O16 K1 C113 155.7(4) . . ? O18 K1 C113 81.0(5) . . ? O17 K1 C113 134.1(5) . . ? O19A K1 C113 12.7(5) . . ? C08A K1 C113 147.7(7) . . ? N11 Fe2 N8 173.6(4) . . ? N11 Fe2 N10 81.0(3) . . ? N8 Fe2 N10 99.3(3) . . ? N11 Fe2 N12 82.0(3) . . ? N8 Fe2 N12 98.2(3) . . ? N10 Fe2 N12 162.1(3) . . ? N11 Fe2 N7 92.5(4) . . ? N8 Fe2 N7 81.2(4) . . ? N10 Fe2 N7 94.1(3) . . ? N12 Fe2 N7 92.3(3) . . ? N11 Fe2 N9 106.0(3) . . ? N8 Fe2 N9 80.4(4) . . ? N10 Fe2 N9 88.9(4) . . ? N12 Fe2 N9 90.2(3) . . ? N7 Fe2 N9 161.6(3) . . ? O4 K2 O13 107.1(3) . . ? O4 K2 O10 93.9(3) . . ? O13 K2 O10 158.9(3) . . ? O4 K2 O12 102.9(2) . . ? O13 K2 O12 60.7(2) . . ? O10 K2 O12 116.5(2) . . ? O4 K2 O9 97.6(2) . . ? O13 K2 O9 115.0(2) . . ? O10 K2 O9 59.2(2) . . ? O12 K2 O9 159.4(2) . . ? O4 K2 O14 94.0(2) . . ? O13 K2 O14 59.8(2) . . ? O10 K2 O14 118.6(3) . . ? O12 K2 O14 120.6(2) . . ? O9 K2 O14 59.4(2) . . ? O4 K2 O11 108.1(2) . . ? O13 K2 O11 114.7(2) . . ? O10 K2 O11 57.7(2) . . ? O12 K2 O11 58.9(2) . . ? O9 K2 O11 112.5(2) . . ? O14 K2 O11 157.7(2) . . ? C6 C1 C2 121.0(10) . . ? C6 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? C3 C2 C1 117.8(11) . . ? C3 C2 H2A 121.1 . . ? C1 C2 H2A 121.1 . . ? C4 C3 C2 121.8(11) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C3 C4 C5 120.1(11) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 119.4(11) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C1 C6 C5 119.8(10) . . ? C1 C6 C7 120.7(10) . . ? C5 C6 C7 119.5(10) . . ? N1 C7 C8 113.9(8) . . ? N1 C7 C6 111.6(8) . . ? C8 C7 C6 112.7(8) . . ? N1 C7 H7A 106.0 . . ? C8 C7 H7A 106.0 . . ? C6 C7 H7A 106.0 . . ? 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 . . ? C9 N1 C7 112.7(8) . . ? C9 N1 Fe1 113.2(7) . . ? C7 N1 Fe1 134.2(6) . . ? O1 C9 N1 125.2(9) . . ? O1 C9 C10 121.7(9) . . ? N1 C9 C10 112.9(9) . . ? N2 C10 C11 120.0(10) . . ? N2 C10 C9 113.7(9) . . ? C11 C10 C9 126.2(10) . . ? C12 C11 C10 119.2(10) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 120.0(10) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 118.6(10) . . ? C14 C13 H13A 120.7 . . ? C12 C13 H13A 120.7 . . ? C10 N2 C14 121.9(9) . . ? C10 N2 Fe1 119.4(7) . . ? C14 N2 Fe1 118.4(7) . . ? N2 C14 C13 120.2(10) . . ? N2 C14 C15 112.2(9) . . ? C13 C14 C15 127.5(10) . . ? O2 C15 N3 128.4(10) . . ? O2 C15 C14 119.4(9) . . ? N3 C15 C14 112.2(9) . . ? C15 N3 C16 121.6(9) . . ? C15 N3 Fe1 115.1(7) . . ? C16 N3 Fe1 122.9(6) . . ? N3 C16 C18 116.5(9) . . ? N3 C16 C17 112.3(9) . . ? C18 C16 C17 111.2(9) . . ? N3 C16 H16A 105.2 . . ? C18 C16 H16A 105.2 . . ? C17 C16 H16A 105.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 117.2(11) . . ? C19 C18 C16 117.8(11) . . ? C23 C18 C16 124.9(10) . . ? C18 C19 C20 120.9(13) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C21 122.1(12) . . ? C19 C20 H20A 118.9 . . ? C21 C20 H20A 118.9 . . ? C22 C21 C20 117.3(12) . . ? C22 C21 H21A 121.4 . . ? C20 C21 H21A 121.4 . . ? C21 C22 C23 122.1(12) . . ? C21 C22 H22A 119.0 . . ? C23 C22 H22A 119.0 . . ? C22 C23 C18 120.3(11) . . ? C22 C23 H23A 119.8 . . ? C18 C23 H23A 119.8 . . ? C25 C24 C29 123.8(11) . . ? C25 C24 H24A 118.1 . . ? C29 C24 H24A 118.1 . . ? C24 C25 C26 118.7(12) . . ? C24 C25 H25A 120.6 . . ? C26 C25 H25A 120.6 . . ? C27 C26 C25 119.2(11) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C26 C27 C28 121.0(12) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? C27 C28 C29 121.6(11) . . ? C27 C28 H28A 119.2 . . ? C29 C28 H28A 119.2 . . ? C28 C29 C24 115.5(11) . . ? C28 C29 C30 121.3(11) . . ? C24 C29 C30 122.9(11) . . ? C29 C30 C31 112.5(9) . . ? C29 C30 N4 113.1(9) . . ? C31 C30 N4 114.8(9) . . ? C29 C30 H30A 105.1 . . ? C31 C30 H30A 105.1 . . ? N4 C30 H30A 105.1 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 N4 C30 111.0(9) . . ? C32 N4 Fe1 113.6(7) . . ? C30 N4 Fe1 135.2(6) . . ? O3 C32 N4 127.2(10) . . ? O3 C32 C33 120.6(9) . . ? N4 C32 C33 112.2(9) . . ? N5 C33 C34 120.9(10) . . ? N5 C33 C32 113.9(9) . . ? C34 C33 C32 125.1(10) . . ? C33 C34 C35 119.0(10) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C34 C35 C36 120.8(10) . . ? C34 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C37 C36 C35 115.7(11) . . ? C37 C36 H36A 122.2 . . ? C35 C36 H36A 122.2 . . ? C33 N5 C37 120.2(8) . . ? C33 N5 Fe1 120.0(7) . . ? C37 N5 Fe1 119.7(7) . . ? N5 C37 C36 123.4(10) . . ? N5 C37 C38 113.2(8) . . ? C36 C37 C38 123.4(10) . . ? C38 O4 K2 173.3(7) . . ? O4 C38 N6 130.4(10) . . ? O4 C38 C37 119.0(9) . . ? N6 C38 C37 110.4(9) . . ? C38 N6 C39 111.6(9) . . ? C38 N6 Fe1 115.8(7) . . ? C39 N6 Fe1 132.4(7) . . ? N6 C39 C41 114.5(9) . . ? N6 C39 C40 110.6(9) . . ? C41 C39 C40 117.2(9) . . ? N6 C39 H39A 104.3 . . ? C41 C39 H39A 104.3 . . ? C40 C39 H39A 104.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 117.3(10) . . ? C42 C41 C39 121.6(9) . . ? C46 C41 C39 120.9(10) . . ? C41 C42 C43 121.4(10) . . ? C41 C42 H42A 119.3 . . ? C43 C42 H42A 119.3 . . ? C44 C43 C42 119.8(10) . . ? C44 C43 H43A 120.1 . . ? C42 C43 H43A 120.1 . . ? C45 C44 C43 119.1(11) . . ? C45 C44 H44A 120.4 . . ? C43 C44 H44A 120.4 . . ? C44 C45 C46 121.6(10) . . ? C44 C45 H45A 119.2 . . ? C46 C45 H45A 119.2 . . ? C45 C46 C41 120.7(10) . . ? C45 C46 H46A 119.7 . . ? C41 C46 H46A 119.7 . . ? C48 C47 C52 120.5(10) . . ? C48 C47 H47A 119.8 . . ? C52 C47 H47A 119.8 . . ? C49 C48 C47 121.2(11) . . ? C49 C48 H48A 119.4 . . ? C47 C48 H48A 119.4 . . ? C48 C49 C50 119.8(11) . . ? C48 C49 H49A 120.1 . . ? C50 C49 H49A 120.1 . . ? C51 C50 C49 119.0(10) . . ? C51 C50 H50A 120.5 . . ? C49 C50 H50A 120.5 . . ? C52 C51 C50 121.3(10) . . ? C52 C51 H51A 119.4 . . ? C50 C51 H51A 119.4 . . ? C51 C52 C47 118.1(10) . . ? C51 C52 C53 122.0(9) . . ? C47 C52 C53 119.7(9) . . ? N7 C53 C52 114.1(8) . . ? N7 C53 C54 112.1(8) . . ? C52 C53 C54 114.5(8) . . ? N7 C53 H53A 105.0 . . ? C52 C53 H53A 105.0 . . ? C54 C53 H53A 105.0 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C55 N7 C53 116.6(8) . . ? C55 N7 Fe2 115.3(7) . . ? C53 N7 Fe2 127.7(6) . . ? O5 C55 N7 128.7(10) . . ? O5 C55 C56 117.9(9) . . ? N7 C55 C56 113.4(9) . . ? N8 C56 C57 121.1(10) . . ? N8 C56 C55 110.6(8) . . ? C57 C56 C55 128.2(10) . . ? C58 C57 C56 118.1(10) . . ? C58 C57 H57A 121.0 . . ? C56 C57 H57A 121.0 . . ? C57 C58 C59 122.2(9) . . ? C57 C58 H58A 118.9 . . ? C59 C58 H58A 118.9 . . ? C58 C59 C60 117.6(10) . . ? C58 C59 H59A 121.2 . . ? C60 C59 H59A 121.2 . . ? C60 N8 C56 121.6(8) . . ? C60 N8 Fe2 118.7(7) . . ? C56 N8 Fe2 119.5(7) . . ? N8 C60 C59 119.3(9) . . ? N8 C60 C61 113.5(9) . . ? C59 C60 C61 127.1(9) . . ? O6 C61 N9 127.2(10) . . ? O6 C61 C60 120.7(9) . . ? N9 C61 C60 112.1(9) . . ? C61 N9 C62 115.0(8) . . ? C61 N9 Fe2 115.2(7) . . ? C62 N9 Fe2 129.7(6) . . ? N9 C62 C63 115.1(8) . . ? N9 C62 C64 111.9(7) . . ? C63 C62 C64 113.0(8) . . ? N9 C62 H62A 105.3 . . ? C63 C62 H62A 105.3 . . ? C64 C62 H62A 105.3 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C69 C64 C65 117.4(10) . . ? C69 C64 C62 120.5(9) . . ? C65 C64 C62 122.0(9) . . ? C66 C65 C64 120.6(10) . . ? C66 C65 H65A 119.7 . . ? C64 C65 H65A 119.7 . . ? C65 C66 C67 120.3(11) . . ? C65 C66 H66A 119.9 . . ? C67 C66 H66A 119.9 . . ? C68 C67 C66 118.7(11) . . ? C68 C67 H67A 120.7 . . ? C66 C67 H67A 120.7 . . ? C69 C68 C67 121.0(11) . . ? C69 C68 H68A 119.5 . . ? C67 C68 H68A 119.5 . . ? C68 C69 C64 121.7(10) . . ? C68 C69 H69A 119.2 . . ? C64 C69 H69A 119.2 . . ? C70 C75 C74 117.1(18) . . ? C70 C75 C76 120.6(19) . . ? C74 C75 C76 122(2) . . ? C75 C70 C71 121.6(19) . . ? C75 C70 H70A 119.2 . . ? C71 C70 H70A 119.2 . . ? C72 C71 C70 121.6(19) . . ? C72 C71 H71A 119.2 . . ? C70 C71 H71A 119.2 . . ? C71 C72 C73 118.3(19) . . ? C71 C72 H72A 120.9 . . ? C73 C72 H72A 120.9 . . ? C74 C73 C72 120(2) . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C75 121(2) . . ? C73 C74 H74A 119.5 . . ? C75 C74 H74A 119.4 . . ? C77 C76 N10 117(3) . . ? C77 C76 C75 109(3) . . ? N10 C76 C75 107.3(14) . . ? C77 C76 H76A 107.8 . . ? N10 C76 H76A 107.8 . . ? C75 C76 H76A 107.8 . . ? C74A C75A C70A 120.0 . . ? C74A C75A C76A 121(2) . . ? C70A C75A C76A 119(2) . . ? C73A C74A C75A 120.0 . . ? C73A C74A H74B 120.0 . . ? C75A C74A H74B 120.0 . . ? C74A C73A C72A 120.0 . . ? C74A C73A H73B 120.0 . . ? C72A C73A H73B 120.0 . . ? C71A C72A C73A 120.0 . . ? C71A C72A H72B 120.0 . . ? C73A C72A H72B 120.0 . . ? C70A C71A C72A 120.0 . . ? C70A C71A H71B 120.0 . . ? C72A C71A H71B 120.0 . . ? C71A C70A C75A 120.0 . . ? C71A C70A H70B 120.0 . . ? C75A C70A H70B 120.0 . . ? N10 C76A C75A 113(3) . . ? N10 C76A C77A 121(4) . . ? C75A C76A C77A 115(3) . . ? N10 C76A H76B 101.0 . . ? C75A C76A H76B 101.0 . . ? C77A C76A H76B 101.1 . . ? C76A C77A H77D 109.4 . . ? C76A C77A H77E 109.5 . . ? H77D C77A H77E 109.5 . . ? C76A C77A H77F 109.5 . . ? H77D C77A H77F 109.5 . . ? H77E C77A H77F 109.5 . . ? C78 N10 C76A 120(2) . . ? C78 N10 C76 123.7(12) . . ? C76A N10 C76 5(3) . . ? C78 N10 Fe2 115.0(7) . . ? C76A N10 Fe2 125.4(19) . . ? C76 N10 Fe2 121.1(11) . . ? C78 O7 K1 172.6(7) . . ? O7 C78 N10 130.3(10) . . ? O7 C78 C79 118.0(9) . . ? N10 C78 C79 111.7(9) . . ? N11 C79 C80 120.6(9) . . ? N11 C79 C78 112.2(9) . . ? C80 C79 C78 127.1(10) . . ? C81 C80 C79 118.8(10) . . ? C81 C80 H80A 120.6 . . ? C79 C80 H80A 120.6 . . ? C80 C81 C82 119.7(9) . . ? C80 C81 H81A 120.2 . . ? C82 C81 H81A 120.2 . . ? C83 C82 C81 119.8(9) . . ? C83 C82 H82A 120.1 . . ? C81 C82 H82A 120.1 . . ? C79 N11 C83 123.4(8) . . ? C79 N11 Fe2 119.4(7) . . ? C83 N11 Fe2 116.6(7) . . ? N11 C83 C82 117.7(9) . . ? N11 C83 C84 113.6(8) . . ? C82 C83 C84 128.5(9) . . ? O8 C84 N12 129.9(10) . . ? O8 C84 C83 118.9(9) . . ? N12 C84 C83 111.1(9) . . ? C84 N12 C85 118.5(8) . . ? C84 N12 Fe2 115.7(7) . . ? C85 N12 Fe2 125.4(6) . . ? N12 C85 C86 112.1(8) . . ? N12 C85 C87 112.4(8) . . ? C86 C85 C87 114.7(9) . . ? N12 C85 H85A 105.6 . . ? C86 C85 H85A 105.6 . . ? C87 C85 H85A 105.6 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 C92 118.6(10) . . ? C88 C87 C85 118.8(9) . . ? C92 C87 C85 122.2(10) . . ? C87 C88 C89 121.0(10) . . ? C87 C88 H88A 119.5 . . ? C89 C88 H88A 119.5 . . ? C90 C89 C88 120.3(11) . . ? C90 C89 H89A 119.9 . . ? C88 C89 H89A 119.9 . . ? C89 C90 C91 118.7(10) . . ? C89 C90 H90A 120.7 . . ? C91 C90 H90A 120.7 . . ? C92 C91 C90 119.7(11) . . ? C92 C91 H91A 120.2 . . ? C90 C91 H91A 120.2 . . ? C91 C92 C87 121.7(11) . . ? C91 C92 H92A 119.2 . . ? C87 C92 H92A 119.2 . . ? C93 O9 C104 111.8(9) . . ? C93 O9 K2 111.6(7) . . ? C104 O9 K2 112.9(7) . . ? O9 C93 C94 107.5(10) . . ? O9 C93 H93A 110.2 . . ? C94 C93 H93A 110.2 . . ? O9 C93 H93B 110.2 . . ? C94 C93 H93B 110.2 . . ? H93A C93 H93B 108.5 . . ? O10 C94 C93 107.3(10) . . ? O10 C94 H94A 110.3 . . ? C93 C94 H94A 110.3 . . ? O10 C94 H94B 110.3 . . ? C93 C94 H94B 110.3 . . ? H94A C94 H94B 108.5 . . ? C95 O10 C94 109.7(9) . . ? C95 O10 K2 122.1(6) . . ? C94 O10 K2 119.1(7) . . ? O10 C95 C96 108.5(10) . . ? O10 C95 H95A 110.0 . . ? C96 C95 H95A 110.0 . . ? O10 C95 H95B 110.0 . . ? C96 C95 H95B 110.0 . . ? H95A C95 H95B 108.4 . . ? O11 C96 C95 107.2(11) . . ? O11 C96 H96A 110.3 . . ? C95 C96 H96A 110.3 . . ? O11 C96 H96B 110.3 . . ? C95 C96 H96B 110.3 . . ? H96A C96 H96B 108.5 . . ? C97 O11 C96 111.5(9) . . ? C97 O11 K2 111.8(6) . . ? C96 O11 K2 112.0(6) . . ? O11 C97 C98 107.1(9) . . ? O11 C97 H97A 110.3 . . ? C98 C97 H97A 110.3 . . ? O11 C97 H97B 110.3 . . ? C98 C97 H97B 110.3 . . ? H97A C97 H97B 108.5 . . ? O12 C98 C97 109.3(9) . . ? O12 C98 H98A 109.8 . . ? C97 C98 H98A 109.8 . . ? O12 C98 H98B 109.8 . . ? C97 C98 H98B 109.8 . . ? H98A C98 H98B 108.3 . . ? C98 O12 C99 110.6(8) . . ? C98 O12 K2 117.5(6) . . ? C99 O12 K2 115.7(6) . . ? O12 C99 C100 108.8(9) . . ? O12 C99 H99A 109.9 . . ? C100 C99 H99A 109.9 . . ? O12 C99 H99B 109.9 . . ? C100 C99 H99B 109.9 . . ? H99A C99 H99B 108.3 . . ? O13 C100 C99 109.6(9) . . ? O13 C100 H10A 109.8 . . ? C99 C100 H10A 109.8 . . ? O13 C100 H10B 109.8 . . ? C99 C100 H10B 109.8 . . ? H10A C100 H10B 108.2 . . ? C101 O13 C100 112.4(9) . . ? C101 O13 K2 111.9(7) . . ? C100 O13 K2 110.7(6) . . ? O13 C101 C102 109.1(10) . . ? O13 C101 H10C 109.9 . . ? C102 C101 H10C 109.9 . . ? O13 C101 H10D 109.9 . . ? C102 C101 H10D 109.9 . . ? H10C C101 H10D 108.3 . . ? O14 C102 C101 108.3(10) . . ? O14 C102 H10E 110.0 . . ? C101 C102 H10E 110.0 . . ? O14 C102 H10F 110.0 . . ? C101 C102 H10F 110.0 . . ? H10E C102 H10F 108.4 . . ? C102 O14 C103 113.3(9) . . ? C102 O14 K2 116.9(6) . . ? C103 O14 K2 116.0(7) . . ? O14 C103 C104 108.1(10) . . ? O14 C103 H10G 110.1 . . ? C104 C103 H10G 110.1 . . ? O14 C103 H10H 110.1 . . ? C104 C103 H10H 110.1 . . ? H10G C103 H10H 108.4 . . ? O9 C104 C103 107.9(10) . . ? O9 C104 H10I 110.1 . . ? C103 C104 H10I 110.1 . . ? O9 C104 H10J 110.1 . . ? C103 C104 H10J 110.1 . . ? H10I C104 H10J 108.4 . . ? C105 O15 C116 112.1(9) . . ? C105 O15 K1 114.8(7) . . ? C116 O15 K1 110.5(6) . . ? O15 C105 C106 109.4(11) . . ? O15 C105 H10K 109.8 . . ? C106 C105 H10K 109.8 . . ? O15 C105 H10L 109.8 . . ? C106 C105 H10L 109.8 . . ? H10K C105 H10L 108.2 . . ? O16 C106 C105 109.5(11) . . ? O16 C106 H10M 109.8 . . ? C105 C106 H10M 109.8 . . ? O16 C106 H10N 109.8 . . ? C105 C106 H10N 109.8 . . ? H10M C106 H10N 108.2 . . ? C107 O16 C106 102.1(12) . . ? C107 O16 C07A 33.1(16) . . ? C106 O16 C07A 132(2) . . ? C107 O16 K1 133.3(11) . . ? C106 O16 K1 116.9(7) . . ? C07A O16 K1 100.4(18) . . ? O16 C107 C108 99.4(16) . . ? O16 C107 H10O 111.9 . . ? C108 C107 H10O 111.9 . . ? O16 C107 H10P 111.9 . . ? C108 C107 H10P 111.9 . . ? H10O C107 H10P 109.6 . . ? O17 C108 C107 110(2) . . ? O17 C108 H10Q 109.7 . . ? C107 C108 H10Q 109.7 . . ? O17 C108 H10R 109.7 . . ? C107 C108 H10R 109.7 . . ? H10Q C108 H10R 108.2 . . ? C109 O17 C108 112.7(17) . . ? C109 O17 K1 112.0(11) . . ? C108 O17 K1 108.1(12) . . ? O17 C109 C110 106.7(17) . . ? O17 C109 H10S 110.4 . . ? C110 C109 H10S 110.4 . . ? O17 C109 H10T 110.4 . . ? C110 C109 H10T 110.4 . . ? H10S C109 H10T 108.6 . . ? O18 C110 C109 109.5(16) . . ? O18 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? O18 C110 H11C 109.8 . . ? C109 C110 H11C 109.8 . . ? H11B C110 H11C 108.2 . . ? C110 O18 C111 113.6(15) . . ? C110 O18 K1 122.1(12) . . ? C111 O18 K1 113.1(13) . . ? O18 C111 C112 108.8(18) . . ? O18 C111 H11D 109.9 . . ? C112 C111 H11D 109.9 . . ? O18 C111 H11E 109.9 . . ? C112 C111 H11E 109.9 . . ? H11D C111 H11E 108.3 . . ? O19 C112 C111 112(2) . . ? O19 C112 K1 45.8(11) . . ? C111 C112 K1 85.0(14) . . ? O19 C112 H11F 109.3 . . ? C111 C112 H11F 109.3 . . ? K1 C112 H11F 155.1 . . ? O19 C112 H11G 109.3 . . ? C111 C112 H11G 109.3 . . ? K1 C112 H11G 85.0 . . ? H11F C112 H11G 108.0 . . ? C112 O19 C113 116.8(17) . . ? C112 O19 K1 113.5(14) . . ? C113 O19 K1 107.9(12) . . ? O19 C113 C114 114.3(17) . . ? O19 C113 K1 49.4(10) . . ? C114 C113 K1 84.9(10) . . ? O19 C113 H11H 108.7 . . ? C114 C113 H11H 108.7 . . ? K1 C113 H11H 83.0 . . ? O19 C113 H11I 108.7 . . ? C114 C113 H11I 108.7 . . ? K1 C113 H11I 158.1 . . ? H11H C113 H11I 107.6 . . ? O20 C114 C113 107.9(12) . . ? O20 C114 H11J 110.1 . . ? C113 C114 H11J 110.1 . . ? O20 C114 H11K 110.1 . . ? C113 C114 H11K 110.1 . . ? H11J C114 H11K 108.4 . . ? C08A C07A O16 121(3) . . ? C08A C07A K1 77(2) . . ? O16 C07A K1 53.7(13) . . ? C08A C07A H07A 107.0 . . ? O16 C07A H07A 107.0 . . ? K1 C07A H07A 95.6 . . ? C08A C07A H07B 107.0 . . ? O16 C07A H07B 107.0 . . ? K1 C07A H07B 154.7 . . ? H07A C07A H07B 106.8 . . ? O17A C08A C07A 118(3) . . ? O17A C08A K1 48.3(13) . . ? C07A C08A K1 78.7(19) . . ? O17A C08A H08A 107.8 . . ? C07A C08A H08A 107.8 . . ? K1 C08A H08A 151.4 . . ? O17A C08A H08B 107.8 . . ? C07A C08A H08B 107.8 . . ? K1 C08A H08B 96.7 . . ? H08A C08A H08B 107.1 . . ? C09A O17A C08A 113(3) . . ? C09A O17A K1 113.8(19) . . ? C08A O17A K1 108.0(17) . . ? O17A C09A C10A 106(3) . . ? O17A C09A H09A 110.6 . . ? C10A C09A H09A 110.6 . . ? O17A C09A H09B 110.6 . . ? C10A C09A H09B 110.6 . . ? H09A C09A H09B 108.7 . . ? O18A C10A C09A 113(3) . . ? O18A C10A H10U 109.1 . . ? C09A C10A H10U 109.1 . . ? O18A C10A H10V 109.1 . . ? C09A C10A H10V 109.0 . . ? H10U C10A H10V 107.8 . . ? C10A O18A C11A 112(3) . . ? C10A O18A K1 114(2) . . ? C11A O18A K1 123(2) . . ? O18A C11A C12A 108(3) . . ? O18A C11A H11L 110.2 . . ? C12A C11A H11L 110.2 . . ? O18A C11A H11M 110.2 . . ? C12A C11A H11M 110.2 . . ? H11L C11A H11M 108.5 . . ? O19A C12A C11A 110(3) . . ? O19A C12A H12B 109.7 . . ? C11A C12A H12B 109.7 . . ? O19A C12A H12C 109.7 . . ? C11A C12A H12C 109.7 . . ? H12B C12A H12C 108.2 . . ? C12A O19A C13A 112(2) . . ? C12A O19A K1 104.1(19) . . ? C13A O19A K1 112.7(16) . . ? O19A C13A H13B 110.1 . . ? O19A C13A H13C 110.1 . . ? H13B C13A H13C 108.4 . . ? C115 O20 C114 111.6(9) . . ? C115 O20 K1 118.7(6) . . ? C114 O20 K1 118.2(7) . . ? O20 C115 C116 109.8(9) . . ? O20 C115 H11N 109.7 . . ? C116 C115 H11N 109.7 . . ? O20 C115 H11O 109.7 . . ? C116 C115 H11O 109.7 . . ? H11N C115 H11O 108.2 . . ? O15 C116 C115 107.1(9) . . ? O15 C116 H11P 110.3 . . ? C115 C116 H11P 110.3 . . ? O15 C116 H11Q 110.3 . . ? C115 C116 H11Q 110.3 . . ? H11P C116 H11Q 108.5 . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.661 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.107 # Attachment '- KCoL1.cif' data_nc3 _database_code_depnum_ccdc_archive 'CCDC 786088' #TrackingRef '- KCoL1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H46 Co K N6 O5' _chemical_formula_weight 872.93 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' K K 0.2009 0.2494 '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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.8734(2) _cell_length_b 17.1654(3) _cell_length_c 12.4840(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.238(2) _cell_angle_gamma 90.00 _cell_volume 2106.96(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12009 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 29.13 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; A crystal was mounted on a glass fibre with Araldite and the data recorded at room temperature. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of six sets of exposures with different \f angles for the crystal; each 10 s exposure covered 1.0\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model except the OH which was located in a difference map. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl and OH H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. Some parts of the structure had large thermal elipsoids. The thermal parameters of the bound water molecules and a phenyl of one of the alpha-methylbenzyl group were subject to restraints (SIMU, DELU and ISOR) to give them chemically reasonable thermal parameters in line with similar parts of the structure. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 22326 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 29.22 _reflns_number_total 9979 _reflns_number_gt 7669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881,4595 Friedel pairs' _refine_ls_abs_structure_Flack 0.016(8) _chemical_absolute_configuration rmad _refine_ls_number_reflns 9979 _refine_ls_number_parameters 549 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.22645(3) 0.328471(14) 0.82307(2) 0.02858(8) Uani 1 1 d . . . K1 K 0.27516(6) 0.06924(3) 1.20631(5) 0.04757(15) Uani 1 1 d DU . . C1 C 0.2413(4) 0.38100(19) 1.1566(2) 0.0692(9) Uani 1 1 d . . . H1A H 0.3285 0.3900 1.1369 0.083 Uiso 1 1 calc R . . C2 C 0.2243(5) 0.3397(3) 1.2517(3) 0.0980(11) Uani 1 1 d U . . H2A H 0.2991 0.3199 1.2936 0.118 Uiso 1 1 calc R . . C3 C 0.0950(5) 0.3291(3) 1.2818(3) 0.1007(11) Uani 1 1 d U . . H3A H 0.0825 0.3029 1.3453 0.121 Uiso 1 1 calc R . . C4 C -0.0145(5) 0.3567(2) 1.2195(3) 0.0926(11) Uani 1 1 d U . . H4A H -0.1016 0.3501 1.2408 0.111 Uiso 1 1 calc R . . C5 C 0.0043(4) 0.3943(2) 1.1250(2) 0.0686(9) Uani 1 1 d U . . H5A H -0.0717 0.4108 1.0816 0.082 Uiso 1 1 calc R . . C6 C 0.1305(3) 0.40839(15) 1.0921(2) 0.0481(7) Uani 1 1 d . . . C7 C 0.1434(3) 0.45544(15) 0.99021(19) 0.0388(6) Uani 1 1 d . . . H7A H 0.0715 0.4949 0.9882 0.047 Uiso 1 1 calc R . . C8 C 0.2757(3) 0.50005(17) 0.9906(2) 0.0502(7) Uani 1 1 d . . . H8A H 0.2769 0.5286 0.9246 0.075 Uiso 1 1 calc R . . H8B H 0.3506 0.4642 0.9973 0.075 Uiso 1 1 calc R . . H8C H 0.2836 0.5356 1.0502 0.075 Uiso 1 1 calc R . . N1 N 0.11317(18) 0.40731(11) 0.89210(14) 0.0306(4) Uani 1 1 d . . . C9 C -0.0103(2) 0.41716(14) 0.84220(18) 0.0335(5) Uani 1 1 d . . . O1 O -0.10267(17) 0.46200(10) 0.86606(15) 0.0479(4) Uani 1 1 d . . . C10 C -0.0358(2) 0.36693(13) 0.74482(18) 0.0331(5) Uani 1 1 d . . . N2 N 0.07222(16) 0.32359(12) 0.72636(13) 0.0298(4) Uani 1 1 d . . . C11 C -0.1542(2) 0.36247(16) 0.6759(2) 0.0430(6) Uani 1 1 d . . . H11A H -0.2307 0.3913 0.6891 0.052 Uiso 1 1 calc R . . C12 C -0.1553(2) 0.31423(17) 0.5874(2) 0.0486(7) Uani 1 1 d . . . H12A H -0.2337 0.3101 0.5405 0.058 Uiso 1 1 calc R . . C13 C -0.0407(3) 0.27201(16) 0.5679(2) 0.0447(6) Uani 1 1 d . . . H13A H -0.0404 0.2405 0.5074 0.054 Uiso 1 1 calc R . . C14 C 0.0733(2) 0.27777(13) 0.64037(18) 0.0347(5) Uani 1 1 d . . . C15 C 0.2061(3) 0.23721(14) 0.6344(2) 0.0385(6) Uani 1 1 d . . . O2 O 0.22736(19) 0.20053(11) 0.55140(14) 0.0540(5) Uani 1 1 d . . . N3 N 0.2917(2) 0.24955(11) 0.72183(16) 0.0336(5) Uani 1 1 d . . . C16 C 0.4282(2) 0.21218(14) 0.7252(2) 0.0403(6) Uani 1 1 d . . . H16A H 0.4754 0.2270 0.7946 0.048 Uiso 1 1 calc R . . C17 C 0.5130(3) 0.24623(17) 0.6400(2) 0.0543(7) Uani 1 1 d . . . H17A H 0.5210 0.3016 0.6498 0.081 Uiso 1 1 calc R . . H17B H 0.4693 0.2354 0.5697 0.081 Uiso 1 1 calc R . . H17C H 0.6019 0.2231 0.6469 0.081 Uiso 1 1 calc R . . C18 C 0.4216(2) 0.12332(16) 0.7260(2) 0.0462(7) Uani 1 1 d . . . C19 C 0.4176(3) 0.07842(17) 0.6337(3) 0.0580(8) Uani 1 1 d . . . H19A H 0.4188 0.1024 0.5670 0.070 Uiso 1 1 calc R . . C20 C 0.4116(4) -0.0018(2) 0.6403(4) 0.0807(12) Uani 1 1 d . . . H20A H 0.4092 -0.0315 0.5778 0.097 Uiso 1 1 calc R . . C21 C 0.4093(4) -0.0382(2) 0.7380(4) 0.0838(11) Uani 1 1 d U . . H21A H 0.4042 -0.0922 0.7416 0.101 Uiso 1 1 calc R . . C22 C 0.4144(3) 0.0044(2) 0.8281(3) 0.0737(10) Uani 1 1 d . . . H22A H 0.4122 -0.0202 0.8943 0.088 Uiso 1 1 calc R . . C23 C 0.4228(3) 0.08469(17) 0.8237(3) 0.0570(8) Uani 1 1 d . . . H23A H 0.4295 0.1133 0.8873 0.068 Uiso 1 1 calc R . . C24 C 0.1973(4) 0.58574(18) 0.7196(2) 0.0608(8) Uani 1 1 d . . . H24A H 0.1274 0.5591 0.7488 0.073 Uiso 1 1 calc R . . C25 C 0.2021(5) 0.6663(2) 0.7294(3) 0.0802(11) Uani 1 1 d . . . H25A H 0.1360 0.6929 0.7633 0.096 Uiso 1 1 calc R . . C26 C 0.3055(5) 0.70551(19) 0.6882(3) 0.0780(11) Uani 1 1 d U . . H26A H 0.3105 0.7594 0.6944 0.094 Uiso 1 1 calc R . . C27 C 0.4018(4) 0.6659(2) 0.6380(3) 0.0760(11) Uani 1 1 d U . . H27A H 0.4726 0.6928 0.6104 0.091 Uiso 1 1 calc R . . C28 C 0.3935(4) 0.58550(18) 0.6282(3) 0.0600(8) Uani 1 1 d . . . H28A H 0.4588 0.5590 0.5932 0.072 Uiso 1 1 calc R . . C29 C 0.2901(3) 0.54399(16) 0.66955(19) 0.0421(6) Uani 1 1 d . . . C30 C 0.2743(3) 0.45595(15) 0.65500(19) 0.0403(6) Uani 1 1 d . . . H30A H 0.1760 0.4465 0.6464 0.048 Uiso 1 1 calc R . . C31 C 0.3278(3) 0.42424(16) 0.5534(2) 0.0566(8) Uani 1 1 d . . . H31A H 0.2965 0.3717 0.5416 0.085 Uiso 1 1 calc R . . H31B H 0.4255 0.4249 0.5612 0.085 Uiso 1 1 calc R . . H31C H 0.2953 0.4560 0.4932 0.085 Uiso 1 1 calc R . . N4 N 0.32581(19) 0.41067(11) 0.75138(15) 0.0323(5) Uani 1 1 d . . . C32 C 0.4556(2) 0.41949(14) 0.78897(18) 0.0337(5) Uani 1 1 d . . . O3 O 0.54473(17) 0.46104(10) 0.75359(14) 0.0470(4) Uani 1 1 d . . . C33 C 0.4918(2) 0.36762(13) 0.88353(18) 0.0333(5) Uani 1 1 d . . . N5 N 0.38806(16) 0.32490(12) 0.91136(13) 0.0318(4) Uani 1 1 d . . . C34 C 0.6200(2) 0.35798(15) 0.9381(2) 0.0426(6) Uani 1 1 d . . . H34A H 0.6934 0.3879 0.9207 0.051 Uiso 1 1 calc R . . C35 C 0.6355(3) 0.30242(16) 1.0192(2) 0.0500(7) Uani 1 1 d . . . H35A H 0.7198 0.2957 1.0578 0.060 Uiso 1 1 calc R . . C36 C 0.5275(3) 0.25758(16) 1.0426(2) 0.0481(7) Uani 1 1 d . . . H36A H 0.5382 0.2197 1.0960 0.058 Uiso 1 1 calc R . . C37 C 0.4019(2) 0.26936(14) 0.98548(18) 0.0365(6) Uani 1 1 d . . . C38 C 0.2735(3) 0.22340(14) 0.99324(19) 0.0408(6) Uani 1 1 d . . . O4 O 0.2778(2) 0.16855(11) 1.06003(17) 0.0608(5) Uani 1 1 d U . . N6 N 0.17234(19) 0.24812(11) 0.92514(15) 0.0338(5) Uani 1 1 d . . . C39 C 0.0320(2) 0.22127(14) 0.9283(2) 0.0402(6) Uani 1 1 d . . . H39A H -0.0256 0.2673 0.9142 0.048 Uiso 1 1 calc R . . C40 C -0.0042(3) 0.18840(18) 1.0365(2) 0.0555(7) Uani 1 1 d . . . H40A H 0.0299 0.2226 1.0936 0.083 Uiso 1 1 calc R . . H40B H 0.0360 0.1378 1.0476 0.083 Uiso 1 1 calc R . . H40C H -0.1013 0.1843 1.0360 0.083 Uiso 1 1 calc R . . C41 C -0.0119(2) 0.16306(14) 0.8399(2) 0.0399(6) Uani 1 1 d . . . C42 C 0.0773(3) 0.11047(16) 0.8027(2) 0.0513(7) Uani 1 1 d . . . H42A H 0.1679 0.1111 0.8308 0.062 Uiso 1 1 calc R . . C43 C 0.0361(3) 0.05730(19) 0.7255(3) 0.0684(9) Uani 1 1 d . . . H43A H 0.0992 0.0236 0.6994 0.082 Uiso 1 1 calc R . . C44 C -0.0974(4) 0.0533(2) 0.6862(3) 0.0736(10) Uani 1 1 d . . . H44A H -0.1259 0.0159 0.6351 0.088 Uiso 1 1 calc R . . C45 C -0.1883(3) 0.1039(2) 0.7220(3) 0.0744(10) Uani 1 1 d U . . H45A H -0.2792 0.1012 0.6953 0.089 Uiso 1 1 calc R . . C46 C -0.1466(3) 0.15968(18) 0.7979(3) 0.0588(8) Uani 1 1 d . . . H46A H -0.2092 0.1950 0.8209 0.071 Uiso 1 1 calc R . . O5 O 0.1744(3) 0.10123(18) 1.3896(2) 0.1066(8) Uani 1 1 d DU . . H5 H 0.208(4) 0.1466(19) 1.423(3) 0.160 Uiso 1 1 d D . . C47 C 0.1069(5) 0.0479(3) 1.4402(3) 0.1067(9) Uani 1 1 d U . . H47A H 0.0364 0.0727 1.4760 0.160 Uiso 1 1 calc R . . H47B H 0.1683 0.0215 1.4921 0.160 Uiso 1 1 calc R . . H47C H 0.0670 0.0109 1.3889 0.160 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02194(14) 0.03187(15) 0.03164(15) 0.00094(15) 0.00086(11) -0.00014(16) K1 0.0458(3) 0.0405(3) 0.0558(3) 0.0100(3) 0.0015(3) 0.0014(3) C1 0.090(3) 0.075(2) 0.0419(16) -0.0013(15) -0.0005(16) 0.0065(19) C2 0.135(3) 0.095(3) 0.0610(19) 0.004(2) -0.010(2) 0.008(3) C3 0.151(2) 0.086(2) 0.0676(18) 0.0014(19) 0.0236(18) -0.022(2) C4 0.109(2) 0.094(2) 0.081(2) -0.0153(17) 0.0380(19) -0.044(2) C5 0.071(2) 0.080(2) 0.0579(17) -0.0152(15) 0.0227(16) -0.0299(18) C6 0.0599(18) 0.0480(15) 0.0374(13) -0.0111(12) 0.0094(13) -0.0095(14) C7 0.0345(13) 0.0435(13) 0.0384(13) -0.0090(11) 0.0041(11) -0.0002(11) C8 0.0512(17) 0.0519(16) 0.0472(15) -0.0090(13) 0.0025(13) -0.0142(14) N1 0.0243(10) 0.0357(10) 0.0321(10) -0.0009(8) 0.0035(8) -0.0010(9) C9 0.0250(12) 0.0348(12) 0.0412(13) 0.0033(10) 0.0055(10) -0.0023(10) O1 0.0314(10) 0.0502(10) 0.0617(12) -0.0123(9) 0.0019(9) 0.0110(9) C10 0.0237(11) 0.0355(12) 0.0398(13) 0.0044(10) 0.0020(10) -0.0010(10) N2 0.0233(8) 0.0349(9) 0.0310(8) 0.0007(10) 0.0026(7) -0.0016(10) C11 0.0259(13) 0.0555(15) 0.0467(15) 0.0033(12) -0.0020(11) 0.0010(12) C12 0.0337(13) 0.065(2) 0.0446(14) -0.0029(14) -0.0081(11) -0.0038(14) C13 0.0411(15) 0.0551(16) 0.0368(13) -0.0094(12) -0.0017(12) -0.0056(13) C14 0.0331(13) 0.0370(13) 0.0344(12) 0.0010(10) 0.0043(10) -0.0049(10) C15 0.0382(14) 0.0398(13) 0.0381(14) -0.0047(11) 0.0065(12) -0.0031(11) O2 0.0545(12) 0.0586(11) 0.0494(11) -0.0181(10) 0.0072(9) 0.0034(10) N3 0.0268(11) 0.0348(10) 0.0396(11) -0.0016(9) 0.0052(9) 0.0020(9) C16 0.0282(13) 0.0455(14) 0.0482(15) -0.0069(12) 0.0080(11) 0.0047(11) C17 0.0377(15) 0.0534(16) 0.0746(19) -0.0030(14) 0.0207(14) -0.0009(13) C18 0.0232(13) 0.0478(15) 0.0680(19) -0.0043(14) 0.0066(12) 0.0065(11) C19 0.0490(18) 0.0493(17) 0.077(2) -0.0129(16) 0.0131(16) 0.0060(14) C20 0.060(2) 0.058(2) 0.124(3) -0.028(2) 0.007(2) 0.0067(18) C21 0.063(2) 0.0476(18) 0.139(3) 0.002(2) 0.001(2) 0.0089(17) C22 0.055(2) 0.062(2) 0.102(3) 0.025(2) -0.0001(19) 0.0130(17) C23 0.0407(16) 0.0529(17) 0.076(2) 0.0098(15) -0.0003(14) 0.0089(13) C24 0.070(2) 0.0573(18) 0.0572(17) 0.0100(14) 0.0200(16) 0.0088(16) C25 0.124(3) 0.056(2) 0.064(2) 0.0014(16) 0.028(2) 0.024(2) C26 0.132(3) 0.0420(17) 0.0592(19) 0.0010(15) 0.004(2) -0.002(2) C27 0.105(3) 0.054(2) 0.071(2) 0.0175(17) 0.017(2) -0.020(2) C28 0.071(2) 0.0491(18) 0.0628(19) 0.0086(15) 0.0219(17) -0.0031(16) C29 0.0471(16) 0.0450(14) 0.0341(13) 0.0106(11) 0.0032(12) 0.0010(12) C30 0.0334(14) 0.0452(14) 0.0415(14) 0.0084(11) -0.0011(11) -0.0014(12) C31 0.082(2) 0.0495(16) 0.0382(14) 0.0023(12) 0.0044(15) 0.0032(16) N4 0.0267(11) 0.0353(10) 0.0348(10) 0.0032(9) 0.0019(9) -0.0006(9) C32 0.0266(12) 0.0356(12) 0.0391(13) -0.0019(10) 0.0047(10) -0.0032(10) O3 0.0316(9) 0.0478(10) 0.0618(11) 0.0124(9) 0.0057(8) -0.0088(8) C33 0.0236(12) 0.0370(12) 0.0393(13) -0.0027(10) 0.0030(10) -0.0036(10) N5 0.0259(9) 0.0358(9) 0.0331(9) -0.0014(10) 0.0005(7) 0.0005(11) C34 0.0246(12) 0.0476(14) 0.0543(16) -0.0025(12) -0.0032(11) -0.0020(11) C35 0.0318(14) 0.0650(18) 0.0505(15) 0.0025(13) -0.0118(12) 0.0035(13) C36 0.0412(15) 0.0522(15) 0.0486(15) 0.0119(13) -0.0078(12) 0.0034(13) C37 0.0348(13) 0.0399(13) 0.0338(12) 0.0047(10) -0.0026(11) 0.0029(11) C38 0.0403(15) 0.0418(14) 0.0400(14) 0.0117(11) 0.0018(12) -0.0011(12) O4 0.0492(12) 0.0554(12) 0.0757(12) 0.0285(10) -0.0052(10) -0.0054(10) N6 0.0283(11) 0.0343(10) 0.0389(11) 0.0047(9) 0.0034(9) -0.0035(9) C39 0.0299(13) 0.0401(13) 0.0510(15) 0.0070(11) 0.0063(11) -0.0006(11) C40 0.0467(17) 0.0659(18) 0.0559(17) 0.0091(14) 0.0154(14) -0.0115(15) C41 0.0314(13) 0.0386(13) 0.0497(15) 0.0114(11) 0.0036(11) -0.0044(11) C42 0.0316(14) 0.0499(16) 0.0716(19) -0.0042(14) -0.0001(13) -0.0016(12) C43 0.056(2) 0.0583(19) 0.090(2) -0.0205(17) 0.0053(17) -0.0042(16) C44 0.068(2) 0.063(2) 0.086(2) -0.0195(18) -0.0133(19) -0.0135(18) C45 0.0435(17) 0.074(2) 0.101(3) 0.0007(19) -0.0205(18) -0.0116(17) C46 0.0318(15) 0.0611(18) 0.082(2) 0.0034(16) -0.0019(14) -0.0012(14) O5 0.1325(19) 0.1242(18) 0.0671(11) -0.0294(11) 0.0308(12) -0.0231(15) C47 0.1255(18) 0.1230(18) 0.0753(13) -0.0184(13) 0.0295(12) -0.0145(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 1.8556(15) . ? Co1 N2 1.8568(15) . ? Co1 N4 1.978(2) . ? Co1 N6 1.9838(19) . ? Co1 N3 1.999(2) . ? Co1 N1 2.0002(19) . ? K1 O4 2.5000(19) . ? K1 O3 2.5885(18) 2_647 ? K1 O1 2.6123(18) 2_547 ? K1 O5 2.635(3) . ? C1 C6 1.381(4) . ? C1 C2 1.407(5) . ? C1 H1A 0.9300 . ? C2 C3 1.374(6) . ? C2 H2A 0.9300 . ? C3 C4 1.358(6) . ? C3 H3A 0.9300 . ? C4 C5 1.373(5) . ? C4 H4A 0.9300 . ? C5 C6 1.369(4) . ? C5 H5A 0.9300 . ? C6 C7 1.521(4) . ? C7 N1 1.485(3) . ? C7 C8 1.514(4) . ? C7 H7A 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N1 C9 1.328(3) . ? C9 O1 1.250(3) . ? C9 C10 1.493(3) . ? O1 K1 2.6123(18) 2_557 ? C10 N2 1.338(3) . ? C10 C11 1.388(3) . ? N2 C14 1.332(3) . ? C11 C12 1.380(4) . ? C11 H11A 0.9300 . ? C12 C13 1.384(4) . ? C12 H12A 0.9300 . ? C13 C14 1.381(3) . ? C13 H13A 0.9300 . ? C14 C15 1.492(4) . ? C15 O2 1.247(3) . ? C15 N3 1.335(3) . ? N3 C16 1.490(3) . ? C16 C18 1.527(4) . ? C16 C17 1.529(4) . ? C16 H16A 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.384(4) . ? C18 C23 1.387(4) . ? C19 C20 1.381(5) . ? C19 H19A 0.9300 . ? C20 C21 1.373(6) . ? C20 H20A 0.9300 . ? C21 C22 1.339(5) . ? C21 H21A 0.9300 . ? C22 C23 1.382(4) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C29 1.359(4) . ? C24 C25 1.388(5) . ? C24 H24A 0.9300 . ? C25 C26 1.362(5) . ? C25 H25A 0.9300 . ? C26 C27 1.367(5) . ? C26 H26A 0.9300 . ? C27 C28 1.387(4) . ? C27 H27A 0.9300 . ? C28 C29 1.383(4) . ? C28 H28A 0.9300 . ? C29 C30 1.528(4) . ? C30 N4 1.483(3) . ? C30 C31 1.519(4) . ? C30 H30A 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N4 C32 1.333(3) . ? C32 O3 1.245(3) . ? C32 C33 1.496(3) . ? O3 K1 2.5885(18) 2_657 ? C33 N5 1.332(3) . ? C33 C34 1.391(3) . ? N5 C37 1.327(3) . ? C34 C35 1.389(4) . ? C34 H34A 0.9300 . ? C35 C36 1.368(4) . ? C35 H35A 0.9300 . ? C36 C37 1.388(3) . ? C36 H36A 0.9300 . ? C37 C38 1.504(4) . ? C38 O4 1.256(3) . ? C38 N6 1.321(3) . ? N6 C39 1.465(3) . ? C39 C41 1.522(4) . ? C39 C40 1.536(4) . ? C39 H39A 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.372(4) . ? C41 C46 1.385(3) . ? C42 C43 1.362(4) . ? C42 H42A 0.9300 . ? C43 C44 1.366(4) . ? C43 H43A 0.9300 . ? C44 C45 1.354(5) . ? C44 H44A 0.9300 . ? C45 C46 1.383(4) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? O5 C47 1.326(5) . ? O5 H5 0.93(2) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Co1 N2 173.92(9) . . ? N5 Co1 N4 81.79(8) . . ? N2 Co1 N4 98.58(8) . . ? N5 Co1 N6 82.12(8) . . ? N2 Co1 N6 97.66(8) . . ? N4 Co1 N6 163.76(7) . . ? N5 Co1 N3 92.53(8) . . ? N2 Co1 N3 81.41(8) . . ? N4 Co1 N3 89.76(8) . . ? N6 Co1 N3 93.22(9) . . ? N5 Co1 N1 104.52(8) . . ? N2 Co1 N1 81.55(8) . . ? N4 Co1 N1 91.85(8) . . ? N6 Co1 N1 89.98(8) . . ? N3 Co1 N1 162.93(7) . . ? O4 K1 O3 125.30(7) . 2_647 ? O4 K1 O1 106.13(6) . 2_547 ? O3 K1 O1 88.62(6) 2_647 2_547 ? O4 K1 O5 121.48(9) . . ? O3 K1 O5 106.77(9) 2_647 . ? O1 K1 O5 99.29(8) 2_547 . ? C6 C1 C2 121.0(4) . . ? C6 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C4 C3 C2 120.6(4) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 122.7(4) . . ? C6 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? C5 C6 C1 117.3(3) . . ? C5 C6 C7 119.5(3) . . ? C1 C6 C7 123.1(3) . . ? N1 C7 C8 113.1(2) . . ? N1 C7 C6 111.6(2) . . ? C8 C7 C6 113.8(2) . . ? N1 C7 H7A 105.9 . . ? C8 C7 H7A 105.9 . . ? C6 C7 H7A 105.9 . . ? 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 . . ? C9 N1 C7 115.00(19) . . ? C9 N1 Co1 114.17(15) . . ? C7 N1 Co1 130.82(15) . . ? O1 C9 N1 128.7(2) . . ? O1 C9 C10 118.5(2) . . ? N1 C9 C10 112.8(2) . . ? C9 O1 K1 144.92(16) . 2_557 ? N2 C10 C11 120.1(2) . . ? N2 C10 C9 112.53(18) . . ? C11 C10 C9 127.3(2) . . ? C14 N2 C10 122.16(18) . . ? C14 N2 Co1 118.99(15) . . ? C10 N2 Co1 118.85(15) . . ? C12 C11 C10 118.3(2) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? C11 C12 C13 120.5(2) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 118.5(2) . . ? C14 C13 H13A 120.7 . . ? C12 C13 H13A 120.7 . . ? N2 C14 C13 120.3(2) . . ? N2 C14 C15 112.77(19) . . ? C13 C14 C15 126.9(2) . . ? O2 C15 N3 128.1(2) . . ? O2 C15 C14 119.5(2) . . ? N3 C15 C14 112.3(2) . . ? C15 N3 C16 117.3(2) . . ? C15 N3 Co1 114.08(16) . . ? C16 N3 Co1 128.08(16) . . ? N3 C16 C18 113.1(2) . . ? N3 C16 C17 111.6(2) . . ? C18 C16 C17 114.4(2) . . ? N3 C16 H16A 105.7 . . ? C18 C16 H16A 105.7 . . ? C17 C16 H16A 105.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 117.6(3) . . ? C19 C18 C16 123.3(3) . . ? C23 C18 C16 119.1(3) . . ? C20 C19 C18 120.3(4) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C21 C20 C19 120.7(4) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C21 C22 C23 120.6(4) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C22 C23 C18 121.1(3) . . ? C22 C23 H23A 119.5 . . ? C18 C23 H23A 119.5 . . ? C29 C24 C25 123.1(3) . . ? C29 C24 H24A 118.4 . . ? C25 C24 H24A 118.4 . . ? C26 C25 C24 118.7(3) . . ? C26 C25 H25A 120.7 . . ? C24 C25 H25A 120.7 . . ? C25 C26 C27 120.3(3) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C26 C27 C28 119.8(4) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C29 C28 C27 121.3(3) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C24 C29 C28 116.8(3) . . ? C24 C29 C30 120.7(3) . . ? C28 C29 C30 122.4(3) . . ? N4 C30 C31 111.7(2) . . ? N4 C30 C29 113.5(2) . . ? C31 C30 C29 114.5(2) . . ? N4 C30 H30A 105.4 . . ? C31 C30 H30A 105.4 . . ? C29 C30 H30A 105.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 N4 C30 118.3(2) . . ? C32 N4 Co1 114.99(15) . . ? C30 N4 Co1 126.41(15) . . ? O3 C32 N4 128.9(2) . . ? O3 C32 C33 119.7(2) . . ? N4 C32 C33 111.3(2) . . ? C32 O3 K1 146.93(16) . 2_657 ? N5 C33 C34 119.6(2) . . ? N5 C33 C32 113.54(18) . . ? C34 C33 C32 126.8(2) . . ? C37 N5 C33 123.03(18) . . ? C37 N5 Co1 117.77(15) . . ? C33 N5 Co1 117.86(15) . . ? C35 C34 C33 118.2(2) . . ? C35 C34 H34A 120.9 . . ? C33 C34 H34A 120.9 . . ? C36 C35 C34 120.4(2) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C35 C36 C37 119.1(2) . . ? C35 C36 H36A 120.5 . . ? C37 C36 H36A 120.5 . . ? N5 C37 C36 119.5(2) . . ? N5 C37 C38 112.86(19) . . ? C36 C37 C38 127.6(2) . . ? O4 C38 N6 130.2(2) . . ? O4 C38 C37 117.3(2) . . ? N6 C38 C37 112.5(2) . . ? C38 O4 K1 173.9(2) . . ? C38 N6 C39 122.9(2) . . ? C38 N6 Co1 113.86(16) . . ? C39 N6 Co1 123.19(15) . . ? N6 C39 C41 113.2(2) . . ? N6 C39 C40 115.9(2) . . ? C41 C39 C40 108.8(2) . . ? N6 C39 H39A 106.0 . . ? C41 C39 H39A 106.0 . . ? C40 C39 H39A 106.0 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 117.9(3) . . ? C42 C41 C39 121.9(2) . . ? C46 C41 C39 120.1(3) . . ? C43 C42 C41 121.4(3) . . ? C43 C42 H42A 119.3 . . ? C41 C42 H42A 119.3 . . ? C42 C43 C44 120.2(3) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C45 C44 C43 119.8(3) . . ? C45 C44 H44A 120.1 . . ? C43 C44 H44A 120.1 . . ? C44 C45 C46 120.4(3) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C45 C46 C41 120.2(3) . . ? C45 C46 H46A 119.9 . . ? C41 C46 H46A 119.9 . . ? C47 O5 K1 121.0(2) . . ? C47 O5 H5 123(2) . . ? K1 O5 H5 114.7(19) . . ? O5 C47 H47A 109.5 . . ? O5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O2 0.93(2) 1.845(19) 2.658(3) 145(3) 1_556 C7 H7A O1 0.98 2.26 2.762(3) 110.4 . C17 H17B O2 0.96 2.45 3.037(3) 119.0 . C19 H19A O2 0.93 2.53 2.937(4) 107.0 . C34 H34A O1 0.93 2.53 3.456(3) 176.3 1_655 C40 H40B O4 0.96 2.44 2.794(4) 101.7 . _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.391 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.039 # Attachment '- KCoL2.cif' data_nc7 _database_code_depnum_ccdc_archive 'CCDC 786089' #TrackingRef '- KCoL2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 Co K N6 O11' _chemical_formula_weight 766.77 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' K K 0.2009 0.2494 '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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5953(2) _cell_length_b 16.0147(2) _cell_length_c 11.11937(18) _cell_angle_alpha 90.00 _cell_angle_beta 106.5681(19) _cell_angle_gamma 90.00 _cell_volume 1808.41(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12350 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 29.34 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model except the OHs on the bound waters which were located in a difference map. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl and OH H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. Some of the OH hydrogen atoms were refined with DFIX retrains. Several atoms had had very elongated thermal parameters so SIMU, DELU and ISOR restraints were used to give them similar thermal parameters to neighbouring atoms. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 17987 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 29.41 _reflns_number_total 8485 _reflns_number_gt 7654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, Friedel pairs' _refine_ls_abs_structure_Flack 0.009(9) _chemical_absolute_configuration rmad _refine_ls_number_reflns 8485 _refine_ls_number_parameters 465 _refine_ls_number_restraints 460 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24342(3) 0.959396(18) 0.49411(2) 0.00693(7) Uani 1 1 d U . . C1 C 0.6006(3) 0.86885(16) 1.0492(2) 0.0209(5) Uani 1 1 d U . . H1A H 0.6013 0.8146 1.0902 0.031 Uiso 1 1 calc R . . H1B H 0.5564 0.9101 1.0882 0.031 Uiso 1 1 calc R . . H1C H 0.6913 0.8868 1.0585 0.031 Uiso 1 1 calc R . . O1 O 0.53218(18) 0.86161(10) 0.91978(15) 0.0185(3) Uani 1 1 d U . . C2 C 0.5279(3) 0.93946(14) 0.8545(2) 0.0151(3) Uani 1 1 d U . . H2A H 0.6162 0.9655 0.8754 0.018 Uiso 1 1 calc R . . H2B H 0.4658 0.9788 0.8764 0.018 Uiso 1 1 calc R . . C3 C 0.4805(2) 0.91600(13) 0.7150(2) 0.0126(3) Uani 1 1 d U . . H3A H 0.4211 0.8667 0.7090 0.015 Uiso 1 1 calc R . . C4 C 0.5954(3) 0.88652(16) 0.6691(2) 0.0187(5) Uani 1 1 d U . . H4A H 0.5633 0.8719 0.5800 0.028 Uiso 1 1 calc R . . H4B H 0.6360 0.8374 0.7174 0.028 Uiso 1 1 calc R . . H4C H 0.6608 0.9313 0.6804 0.028 Uiso 1 1 calc R . . N1 N 0.40162(19) 0.98086(11) 0.63333(17) 0.0105(3) Uani 1 1 d U . . C5 C 0.4394(2) 1.06048(14) 0.6500(2) 0.0117(3) Uani 1 1 d U . . O2 O 0.54075(17) 1.09016(10) 0.72651(15) 0.0161(3) Uani 1 1 d U . . C6 C 0.3422(2) 1.11715(13) 0.5637(2) 0.0106(3) Uani 1 1 d U . . N2 N 0.24311(18) 1.07512(13) 0.48507(16) 0.0100(3) Uani 1 1 d U . . C7 C 0.3434(2) 1.20408(13) 0.5603(2) 0.0127(3) Uani 1 1 d U . . H7A H 0.4121 1.2349 0.6163 0.015 Uiso 1 1 calc R . . C8 C 0.2410(2) 1.24468(15) 0.4723(2) 0.0135(3) Uani 1 1 d U . . H8A H 0.2400 1.3039 0.4682 0.016 Uiso 1 1 calc R . . C9 C 0.1405(2) 1.19939(14) 0.3908(2) 0.0128(3) Uani 1 1 d U . . H9A H 0.0713 1.2268 0.3303 0.015 Uiso 1 1 calc R . . C10 C 0.1441(2) 1.11340(13) 0.4001(2) 0.0110(3) Uani 1 1 d U . . C11 C 0.0470(2) 1.05219(13) 0.3227(2) 0.0106(3) Uani 1 1 d U . . O3 O -0.05369(16) 1.07849(10) 0.24085(15) 0.0153(3) Uani 1 1 d U . . N3 N 0.08456(18) 0.97371(11) 0.35249(16) 0.0103(3) Uani 1 1 d U . . C12 C 0.0043(2) 0.90496(14) 0.2815(2) 0.0127(3) Uani 1 1 d U . . H12A H 0.0575 0.8529 0.3062 0.015 Uiso 1 1 calc R . . C13 C -0.1210(2) 0.89233(15) 0.3194(2) 0.0168(4) Uani 1 1 d U . . H13A H -0.0990 0.8864 0.4108 0.025 Uiso 1 1 calc R . . H13B H -0.1660 0.8418 0.2792 0.025 Uiso 1 1 calc R . . H13C H -0.1789 0.9407 0.2928 0.025 Uiso 1 1 calc R . . C14 C -0.0198(3) 0.91456(14) 0.1394(2) 0.0161(3) Uani 1 1 d U . . H14A H -0.0928 0.9542 0.1046 0.019 Uiso 1 1 calc R . . H14B H 0.0604 0.9359 0.1208 0.019 Uiso 1 1 calc R . . O4 O -0.05246(19) 0.83431(10) 0.08623(16) 0.0199(3) Uani 1 1 d U . . C15 C -0.0728(3) 0.83525(17) -0.0456(2) 0.0265(5) Uani 1 1 d U . . H15A H -0.0951 0.7789 -0.0792 0.040 Uiso 1 1 calc R . . H15B H 0.0078 0.8541 -0.0639 0.040 Uiso 1 1 calc R . . H15C H -0.1451 0.8734 -0.0846 0.040 Uiso 1 1 calc R . . C16 C 0.3861(3) 1.15646(18) 0.1646(3) 0.0343(6) Uani 1 1 d U . . H16A H 0.4322 1.1976 0.1273 0.051 Uiso 1 1 calc R . . H16B H 0.4137 1.1627 0.2561 0.051 Uiso 1 1 calc R . . H16C H 0.2909 1.1654 0.1327 0.051 Uiso 1 1 calc R . . O5 O 0.41748(18) 1.07428(11) 0.13231(17) 0.0239(3) Uani 1 1 d U . . C17 C 0.3539(3) 1.00990(16) 0.1832(2) 0.0185(3) Uani 1 1 d U . . H17A H 0.3582 0.9567 0.1392 0.022 Uiso 1 1 calc R . . H17B H 0.2600 1.0245 0.1690 0.022 Uiso 1 1 calc R . . C18 C 0.4193(2) 0.99852(14) 0.3239(2) 0.0142(3) Uani 1 1 d U . . H18A H 0.4110 1.0530 0.3649 0.017 Uiso 1 1 calc R . . C19 C 0.5666(2) 0.97985(15) 0.3536(2) 0.0172(4) Uani 1 1 d U . . H19A H 0.6042 0.9730 0.4444 0.026 Uiso 1 1 calc R . . H19B H 0.6107 1.0262 0.3245 0.026 Uiso 1 1 calc R . . H19C H 0.5794 0.9284 0.3108 0.026 Uiso 1 1 calc R . . N4 N 0.34896(19) 0.93592(11) 0.37758(17) 0.0111(3) Uani 1 1 d U . . C20 C 0.3592(2) 0.85527(14) 0.3505(2) 0.0112(3) Uani 1 1 d U . . O6 O 0.41163(16) 0.82280(10) 0.27475(15) 0.0129(3) Uani 1 1 d U . . C21 C 0.3018(2) 0.80029(13) 0.4310(2) 0.0110(3) Uani 1 1 d U . . N5 N 0.24300(18) 0.84343(13) 0.50279(16) 0.0096(3) Uani 1 1 d U . . C22 C 0.3087(2) 0.71372(13) 0.4398(2) 0.0138(3) Uani 1 1 d U . . H22A H 0.3497 0.6821 0.3891 0.017 Uiso 1 1 calc R . . C23 C 0.2541(2) 0.67477(15) 0.5250(2) 0.0151(3) Uani 1 1 d U . . H23A H 0.2591 0.6157 0.5334 0.018 Uiso 1 1 calc R . . C24 C 0.1921(2) 0.72097(13) 0.5983(2) 0.0135(3) Uani 1 1 d U . . H24A H 0.1542 0.6946 0.6562 0.016 Uiso 1 1 calc R . . C25 C 0.1880(2) 0.80729(13) 0.5829(2) 0.0108(3) Uani 1 1 d U . . C26 C 0.1265(2) 0.86876(13) 0.6509(2) 0.0106(3) Uani 1 1 d U . . O7 O 0.07249(16) 0.84355(9) 0.73074(15) 0.0132(3) Uani 1 1 d U . . N6 N 0.13897(19) 0.94688(11) 0.61435(16) 0.0110(3) Uani 1 1 d U . . C27 C 0.0814(2) 1.01469(14) 0.6713(2) 0.0138(3) Uani 1 1 d U . . H27A H 0.0970 1.0681 0.6312 0.017 Uiso 1 1 calc R . . C28 C -0.0673(3) 1.00584(16) 0.6483(2) 0.0217(5) Uani 1 1 d U . . H28A H -0.1103 1.0017 0.5579 0.033 Uiso 1 1 calc R . . H28B H -0.1011 1.0548 0.6821 0.033 Uiso 1 1 calc R . . H28C H -0.0859 0.9553 0.6901 0.033 Uiso 1 1 calc R . . C29 C 0.1529(3) 1.02177(15) 0.8127(2) 0.0179(3) Uani 1 1 d U A . H29A H 0.1252 0.9751 0.8577 0.021 Uiso 1 1 calc R . . H29B H 0.2490 1.0170 0.8258 0.021 Uiso 1 1 calc R . . O8 O 0.12508(18) 1.09871(11) 0.86343(16) 0.0200(3) Uani 1 1 d U . . C30 C 0.2129(7) 1.1638(3) 0.8471(5) 0.0228(6) Uani 0.701(12) 1 d PU A 1 H30A H 0.1918 1.2159 0.8832 0.034 Uiso 0.701(12) 1 calc PR A 1 H30B H 0.2025 1.1717 0.7574 0.034 Uiso 0.701(12) 1 calc PR A 1 H30C H 0.3040 1.1478 0.8895 0.034 Uiso 0.701(12) 1 calc PR A 1 C30A C 0.1621(15) 1.1741(6) 0.8143(11) 0.0228(9) Uiso 0.299(12) 1 d PU A 2 H30D H 0.0845 1.1991 0.7552 0.034 Uiso 0.299(12) 1 calc PR A 2 H30E H 0.2284 1.1618 0.7707 0.034 Uiso 0.299(12) 1 calc PR A 2 H30F H 0.1990 1.2132 0.8831 0.034 Uiso 0.299(12) 1 calc PR A 2 K1 K 0.69243(5) 1.19244(3) 0.89382(4) 0.01734(12) Uani 1 1 d U . . O9 O 0.6738(2) 1.09528(14) 1.08650(18) 0.0333(4) Uani 1 1 d DU . . H9B H 0.598(3) 1.087(2) 1.111(3) 0.050 Uiso 1 1 d D . . H9C H 0.753(2) 1.080(2) 1.138(3) 0.050 Uiso 1 1 d D . . O10 O 0.9303(2) 1.12689(15) 0.9857(2) 0.0355(5) Uani 1 1 d U . . H10A H 1.004(4) 1.113(2) 0.954(3) 0.053 Uiso 1 1 d . . . H10B H 0.944(3) 1.109(2) 1.081(3) 0.053 Uiso 1 1 d . . . O11 O 0.7189(2) 1.32111(14) 1.0486(2) 0.0341(5) Uani 1 1 d DU . . H11A H 0.634(4) 1.333(2) 1.069(3) 0.051 Uiso 1 1 d . . . H11B H 0.787(3) 1.325(2) 1.125(2) 0.051 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 Co1 0.00789(14) 0.00505(11) 0.00803(13) -0.00013(11) 0.00258(10) 0.00001(11) C1 0.0206(12) 0.0262(11) 0.0126(8) 0.0041(8) -0.0005(9) 0.0012(10) O1 0.0191(8) 0.0193(7) 0.0132(6) 0.0043(5) -0.0020(6) -0.0019(6) C2 0.0158(8) 0.0160(7) 0.0114(6) 0.0012(5) 0.0004(6) 0.0004(6) C3 0.0124(7) 0.0129(6) 0.0111(6) 0.0005(5) 0.0009(5) 0.0007(6) C4 0.0168(10) 0.0223(11) 0.0154(10) -0.0007(9) 0.0019(8) 0.0072(8) N1 0.0107(5) 0.0104(5) 0.0106(5) -0.0003(5) 0.0031(4) -0.0001(4) C5 0.0120(6) 0.0104(5) 0.0136(6) -0.0023(5) 0.0049(5) -0.0007(5) O2 0.0156(6) 0.0127(6) 0.0193(6) -0.0009(5) 0.0039(5) -0.0028(5) C6 0.0113(6) 0.0084(5) 0.0140(6) -0.0018(5) 0.0065(5) -0.0015(5) N2 0.0098(6) 0.0082(4) 0.0133(6) -0.0005(4) 0.0055(4) 0.0001(4) C7 0.0127(7) 0.0092(6) 0.0173(7) -0.0012(6) 0.0062(6) -0.0011(6) C8 0.0132(8) 0.0101(6) 0.0187(7) 0.0008(6) 0.0071(6) 0.0005(6) C9 0.0119(7) 0.0108(6) 0.0170(7) 0.0022(6) 0.0062(6) 0.0014(6) C10 0.0103(6) 0.0098(5) 0.0141(6) 0.0017(5) 0.0055(5) 0.0013(5) C11 0.0093(6) 0.0109(5) 0.0123(6) 0.0017(5) 0.0042(5) 0.0014(5) O3 0.0110(7) 0.0146(7) 0.0182(7) 0.0027(6) 0.0006(5) 0.0027(6) N3 0.0097(5) 0.0103(5) 0.0109(5) 0.0007(5) 0.0029(4) 0.0000(5) C12 0.0129(7) 0.0130(6) 0.0115(6) -0.0007(6) 0.0022(5) -0.0029(6) C13 0.0158(10) 0.0199(10) 0.0152(9) -0.0025(9) 0.0053(8) -0.0064(8) C14 0.0182(8) 0.0177(7) 0.0118(6) -0.0018(6) 0.0035(6) -0.0047(7) O4 0.0241(8) 0.0212(7) 0.0132(6) -0.0048(6) 0.0034(6) -0.0042(6) C15 0.0331(14) 0.0310(12) 0.0143(8) -0.0071(9) 0.0051(10) -0.0062(11) C16 0.0356(10) 0.0272(7) 0.0391(9) 0.0086(7) 0.0091(8) 0.0002(7) O5 0.0211(8) 0.0258(7) 0.0259(7) 0.0120(6) 0.0085(6) -0.0003(6) C17 0.0164(8) 0.0212(7) 0.0193(7) 0.0066(6) 0.0073(6) 0.0004(6) C18 0.0135(7) 0.0151(6) 0.0160(6) 0.0015(6) 0.0075(6) -0.0006(6) C19 0.0132(8) 0.0220(11) 0.0172(10) 0.0019(8) 0.0057(7) -0.0029(8) N4 0.0109(6) 0.0115(5) 0.0122(6) -0.0006(5) 0.0052(5) 0.0005(5) C20 0.0109(6) 0.0118(5) 0.0105(6) -0.0021(5) 0.0024(5) 0.0017(5) O6 0.0135(7) 0.0140(6) 0.0109(6) -0.0024(5) 0.0032(5) 0.0025(6) C21 0.0106(6) 0.0099(5) 0.0116(6) -0.0021(5) 0.0017(5) 0.0013(5) N5 0.0091(7) 0.0084(4) 0.0106(6) -0.0003(4) 0.0016(5) 0.0001(4) C22 0.0132(7) 0.0105(6) 0.0162(7) -0.0023(6) 0.0018(6) 0.0018(6) C23 0.0148(7) 0.0108(6) 0.0179(6) 0.0002(5) 0.0017(5) 0.0014(5) C24 0.0131(7) 0.0106(6) 0.0155(7) 0.0018(6) 0.0018(6) -0.0004(6) C25 0.0103(6) 0.0099(5) 0.0111(6) 0.0008(5) 0.0015(5) -0.0012(5) C26 0.0104(7) 0.0109(5) 0.0102(6) 0.0006(5) 0.0024(5) -0.0017(5) O7 0.0132(8) 0.0148(7) 0.0123(7) 0.0012(6) 0.0045(6) -0.0037(6) N6 0.0122(6) 0.0109(6) 0.0108(5) 0.0002(5) 0.0049(5) -0.0003(5) C27 0.0159(7) 0.0134(6) 0.0142(6) -0.0006(6) 0.0075(6) 0.0021(6) C28 0.0168(7) 0.0244(9) 0.0243(8) -0.0031(7) 0.0066(6) 0.0047(7) C29 0.0212(7) 0.0165(6) 0.0165(6) -0.0035(6) 0.0065(6) 0.0024(6) O8 0.0247(7) 0.0179(6) 0.0195(6) -0.0056(5) 0.0100(6) 0.0003(6) C30 0.0245(10) 0.0203(8) 0.0234(10) -0.0024(8) 0.0067(8) -0.0014(7) K1 0.0203(3) 0.0157(2) 0.0135(2) -0.0003(2) 0.0009(2) -0.0011(2) O9 0.0206(10) 0.0543(11) 0.0232(8) 0.0165(8) 0.0033(8) -0.0033(10) O10 0.0196(8) 0.0553(12) 0.0327(11) 0.0137(9) 0.0095(7) 0.0125(8) O11 0.0263(12) 0.0415(9) 0.0289(11) -0.0181(8) -0.0010(9) -0.0006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.856(2) . ? Co1 N5 1.860(2) . ? Co1 N1 1.961(2) . ? Co1 N3 1.9631(19) . ? Co1 N6 1.9740(17) . ? Co1 N4 1.9741(18) . ? C1 O1 1.419(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O1 C2 1.437(3) . ? C2 C3 1.534(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.473(3) . ? C3 C4 1.523(3) . ? C3 H3A 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N1 C5 1.333(3) . ? C5 O2 1.258(3) . ? C5 C6 1.497(3) . ? O2 K1 2.6498(17) . ? C6 N2 1.340(3) . ? C6 C7 1.393(3) . ? N2 C10 1.343(3) . ? C7 C8 1.398(3) . ? C7 H7A 0.9500 . ? C8 C9 1.389(3) . ? C8 H8A 0.9500 . ? C9 C10 1.381(3) . ? C9 H9A 0.9500 . ? C10 C11 1.501(3) . ? C11 O3 1.261(3) . ? C11 N3 1.331(3) . ? N3 C12 1.475(3) . ? C12 C13 1.517(3) . ? C12 C14 1.535(3) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 O4 1.416(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O4 C15 1.419(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O5 1.428(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O5 C17 1.433(3) . ? C17 C18 1.531(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N4 1.473(3) . ? C18 C19 1.530(3) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N4 C20 1.338(3) . ? C20 O6 1.247(3) . ? C20 C21 1.502(3) . ? O6 K1 2.8123(16) 2_646 ? C21 N5 1.337(3) . ? C21 C22 1.390(3) . ? N5 C25 1.328(3) . ? C22 C23 1.390(3) . ? C22 H22A 0.9500 . ? C23 C24 1.396(3) . ? C23 H23A 0.9500 . ? C24 C25 1.392(3) . ? C24 H24A 0.9500 . ? C25 C26 1.499(3) . ? C26 O7 1.252(3) . ? C26 N6 1.334(3) . ? N6 C27 1.474(3) . ? C27 C28 1.530(4) . ? C27 C29 1.542(3) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O8 1.421(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O8 C30A 1.426(10) . ? O8 C30 1.442(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? K1 O11 2.648(2) . ? K1 O10 2.651(2) . ? K1 O9 2.7003(19) . ? K1 O6 2.8123(16) 2_656 ? O9 H9B 0.92(2) . ? O9 H9C 0.91(2) . ? O10 H10A 0.97(4) . ? O10 H10B 1.07(4) . ? O11 H11A 1.00(4) . ? O11 H11B 0.95(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N5 179.76(9) . . ? N2 Co1 N1 81.70(8) . . ? N5 Co1 N1 98.53(8) . . ? N2 Co1 N3 81.49(8) . . ? N5 Co1 N3 98.28(8) . . ? N1 Co1 N3 163.19(7) . . ? N2 Co1 N6 98.36(7) . . ? N5 Co1 N6 81.57(7) . . ? N1 Co1 N6 90.07(8) . . ? N3 Co1 N6 92.13(8) . . ? N2 Co1 N4 98.47(7) . . ? N5 Co1 N4 81.61(7) . . ? N1 Co1 N4 92.00(8) . . ? N3 Co1 N4 90.71(8) . . ? N6 Co1 N4 163.17(7) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 O1 C2 112.00(18) . . ? O1 C2 C3 104.61(17) . . ? O1 C2 H2A 110.8 . . ? C3 C2 H2A 110.8 . . ? O1 C2 H2B 110.8 . . ? C3 C2 H2B 110.8 . . ? H2A C2 H2B 108.9 . . ? N1 C3 C4 112.27(18) . . ? N1 C3 C2 114.54(17) . . ? C4 C3 C2 110.6(2) . . ? N1 C3 H3A 106.3 . . ? C4 C3 H3A 106.3 . . ? C2 C3 H3A 106.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 N1 C3 119.57(19) . . ? C5 N1 Co1 115.63(15) . . ? C3 N1 Co1 124.77(14) . . ? O2 C5 N1 128.3(2) . . ? O2 C5 C6 120.20(19) . . ? N1 C5 C6 111.5(2) . . ? C5 O2 K1 159.81(15) . . ? N2 C6 C7 119.7(2) . . ? N2 C6 C5 112.43(19) . . ? C7 C6 C5 127.8(2) . . ? C6 N2 C10 122.6(2) . . ? C6 N2 Co1 118.50(16) . . ? C10 N2 Co1 118.87(16) . . ? C6 C7 C8 118.2(2) . . ? C6 C7 H7A 120.9 . . ? C8 C7 H7A 120.9 . . ? C9 C8 C7 120.8(2) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C10 C9 C8 118.2(2) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? N2 C10 C9 120.5(2) . . ? N2 C10 C11 112.03(19) . . ? C9 C10 C11 127.5(2) . . ? O3 C11 N3 128.8(2) . . ? O3 C11 C10 119.72(19) . . ? N3 C11 C10 111.5(2) . . ? C11 N3 C12 119.07(19) . . ? C11 N3 Co1 115.90(15) . . ? C12 N3 Co1 125.01(14) . . ? N3 C12 C13 111.52(18) . . ? N3 C12 C14 112.20(18) . . ? C13 C12 C14 113.4(2) . . ? N3 C12 H12A 106.4 . . ? C13 C12 H12A 106.4 . . ? C14 C12 H12A 106.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 C14 C12 106.73(18) . . ? O4 C14 H14A 110.4 . . ? C12 C14 H14A 110.4 . . ? O4 C14 H14B 110.4 . . ? C12 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C14 O4 C15 111.62(18) . . ? O4 C15 H15A 109.5 . . ? O4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 H16A 109.5 . . ? O5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C16 O5 C17 113.2(2) . . ? O5 C17 C18 111.3(2) . . ? O5 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? O5 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N4 C18 C19 112.50(19) . . ? N4 C18 C17 111.2(2) . . ? C19 C18 C17 112.31(19) . . ? N4 C18 H18A 106.8 . . ? C19 C18 H18A 106.8 . . ? C17 C18 H18A 106.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 N4 C18 118.91(18) . . ? C20 N4 Co1 115.40(15) . . ? C18 N4 Co1 125.65(14) . . ? O6 C20 N4 129.4(2) . . ? O6 C20 C21 119.48(19) . . ? N4 C20 C21 111.07(18) . . ? C20 O6 K1 126.45(15) . 2_646 ? N5 C21 C22 119.8(2) . . ? N5 C21 C20 112.93(19) . . ? C22 C21 C20 127.2(2) . . ? C25 N5 C21 122.9(2) . . ? C25 N5 Co1 118.55(15) . . ? C21 N5 Co1 118.48(15) . . ? C21 C22 C23 118.1(2) . . ? C21 C22 H22A 120.9 . . ? C23 C22 H22A 120.9 . . ? C22 C23 C24 121.1(2) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C25 C24 C23 117.2(2) . . ? C25 C24 H24A 121.4 . . ? C23 C24 H24A 121.4 . . ? N5 C25 C24 120.7(2) . . ? N5 C25 C26 112.91(18) . . ? C24 C25 C26 126.4(2) . . ? O7 C26 N6 128.6(2) . . ? O7 C26 C25 119.88(19) . . ? N6 C26 C25 111.53(18) . . ? C26 N6 C27 118.09(18) . . ? C26 N6 Co1 115.17(14) . . ? C27 N6 Co1 126.64(14) . . ? N6 C27 C28 113.10(19) . . ? N6 C27 C29 110.46(19) . . ? C28 C27 C29 111.1(2) . . ? N6 C27 H27A 107.3 . . ? C28 C27 H27A 107.3 . . ? C29 C27 H27A 107.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O8 C29 C27 111.82(19) . . ? O8 C29 H29A 109.3 . . ? C27 C29 H29A 109.3 . . ? O8 C29 H29B 109.3 . . ? C27 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? C29 O8 C30A 118.1(4) . . ? C29 O8 C30 111.2(2) . . ? C30A O8 C30 23.4(5) . . ? O8 C30 H30A 109.5 . . ? O8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O8 C30A H30D 109.5 . . ? O8 C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? O8 C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? O11 K1 O2 150.23(7) . . ? O11 K1 O10 98.32(7) . . ? O2 K1 O10 110.21(7) . . ? O11 K1 O9 87.19(7) . . ? O2 K1 O9 91.95(6) . . ? O10 K1 O9 75.08(7) . . ? O11 K1 O6 78.71(6) . 2_656 ? O2 K1 O6 86.96(5) . 2_656 ? O10 K1 O6 134.41(6) . 2_656 ? O9 K1 O6 148.55(6) . 2_656 ? K1 O9 H9B 125(2) . . ? K1 O9 H9C 113(2) . . ? H9B O9 H9C 121(3) . . ? K1 O10 H10A 137(2) . . ? K1 O10 H10B 109.5(19) . . ? H10A O10 H10B 114(3) . . ? K1 O11 H11A 111(2) . . ? K1 O11 H11B 123(2) . . ? H11A O11 H11B 107(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9B O5 0.92(2) 2.01(2) 2.922(3) 170(3) 1_556 O9 H9C O3 0.91(2) 2.04(2) 2.920(3) 164(3) 1_656 O10 H10B O3 1.07(4) 1.83(4) 2.899(3) 173(3) 1_656 O10 H10A O8 0.97(4) 1.86(4) 2.813(3) 168(3) 1_655 O11 H11A O1 1.00(4) 1.86(4) 2.856(3) 171(3) 2_657 O11 H11B O7 0.95(2) 1.88(2) 2.818(3) 175(3) 2_657 _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.943 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.068 # Attachment '- TTFCoL1.cif' data_nc1 _database_code_depnum_ccdc_archive 'CCDC 786090' #TrackingRef '- TTFCoL1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H46 Co N6 O4 S4' _chemical_formula_weight 1006.12 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 15.8680(8) _cell_length_b 10.5601(4) _cell_length_c 15.6312(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.222(5) _cell_angle_gamma 90.00 _cell_volume 2473.26(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1747 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1046 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8146 _exptl_absorpt_correction_T_max 0.9832 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; We are greatful to Oxford Diffraction at Abingdon for recording the data for nc1. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. One of the benzyl groups (C18-C23) had some rather elliptical thermal parameters. SIMU and DELU restraints were used to give these atoms thermal parameters in line with other atoms in the benzyl group. Attempts to produce a suitable model of possible disorder required more restraints and gave a poorer R factor. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra' _diffrn_measurement_method '\w - scans' _diffrn_detector_area_resol_mean 10.3317 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10074 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5410 _reflns_number_gt 3920 _reflns_threshold_expression >2sigma(I) _computing_data_collection ;CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2479 Friedel pairs' _refine_ls_abs_structure_Flack 0.026(14) _chemical_absolute_configuration rmad _refine_ls_number_reflns 5410 _refine_ls_number_parameters 305 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.82847(5) 0.5000 0.01148(15) Uani 1 2 d S . . C1 C -0.1497(2) 0.6936(4) 0.2201(2) 0.0326(9) Uani 1 1 d . . . H1A H -0.0912 0.6956 0.2163 0.039 Uiso 1 1 calc R . . C2 C -0.2216(2) 0.7286(4) 0.1456(3) 0.0395(10) Uani 1 1 d U . . H2A H -0.2116 0.7559 0.0918 0.047 Uiso 1 1 calc R . . C3 C -0.3073(2) 0.7245(4) 0.1484(2) 0.0333(9) Uani 1 1 d . . . H3A H -0.3564 0.7464 0.0966 0.040 Uiso 1 1 calc R . . C4 C -0.3208(2) 0.6882(4) 0.2274(3) 0.0336(9) Uani 1 1 d . . . H4A H -0.3795 0.6870 0.2307 0.040 Uiso 1 1 calc R . . C5 C -0.2491(2) 0.6536(3) 0.3019(3) 0.0260(8) Uani 1 1 d . . . H5A H -0.2593 0.6276 0.3558 0.031 Uiso 1 1 calc R . . C6 C -0.16195(19) 0.6561(3) 0.2992(2) 0.0162(7) Uani 1 1 d . . . C7 C -0.08540(19) 0.6093(3) 0.3799(2) 0.0164(7) Uani 1 1 d . . . H7A H -0.1096 0.6049 0.4313 0.020 Uiso 1 1 calc R . . C8 C -0.0619(2) 0.4725(3) 0.3636(2) 0.0213(8) Uani 1 1 d . . . H8A H -0.0122 0.4430 0.4158 0.032 Uiso 1 1 calc R . . H8B H -0.0444 0.4690 0.3090 0.032 Uiso 1 1 calc R . . H8C H -0.1139 0.4180 0.3554 0.032 Uiso 1 1 calc R . . N1 N -0.00882(15) 0.6959(2) 0.40989(17) 0.0122(6) Uani 1 1 d . . . C9 C 0.06371(19) 0.6817(3) 0.3862(2) 0.0138(7) Uani 1 1 d . . . O1 O 0.07613(13) 0.61093(19) 0.32701(15) 0.0184(5) Uani 1 1 d . . . N3 N 0.11719(14) 0.8344(3) 0.50250(15) 0.0113(5) Uani 1 1 d . . . C10 C 0.13867(19) 0.7645(3) 0.4413(2) 0.0116(7) Uani 1 1 d . . . C11 C 0.22341(19) 0.7754(3) 0.4351(2) 0.0156(7) Uani 1 1 d . . . H11A H 0.2407 0.7262 0.3928 0.019 Uiso 1 1 calc R . . C12 C 0.28228(19) 0.8600(3) 0.4922(2) 0.0171(8) Uani 1 1 d . . . H12A H 0.3408 0.8683 0.4890 0.020 Uiso 1 1 calc R . . C13 C 0.25771(18) 0.9328(3) 0.5541(2) 0.0137(7) Uani 1 1 d . . . H13A H 0.2983 0.9905 0.5933 0.016 Uiso 1 1 calc R . . C14 C 0.17130(18) 0.9181(3) 0.5566(2) 0.0127(7) Uani 1 1 d . . . C15 C 0.12768(19) 0.9947(3) 0.6115(2) 0.0143(7) Uani 1 1 d . . . O2 O 0.16922(12) 1.08196(18) 0.66147(14) 0.0165(5) Uani 1 1 d . . . N2 N 0.04310(15) 0.9584(2) 0.59543(18) 0.0111(6) Uani 1 1 d . . . C16 C -0.01175(18) 1.0302(3) 0.6396(2) 0.0162(7) Uani 1 1 d . . . H16A H -0.0699 0.9840 0.6240 0.019 Uiso 1 1 calc R . . C17 C -0.0344(2) 1.1612(3) 0.5975(2) 0.0195(8) Uani 1 1 d . . . H17A H -0.0659 1.1527 0.5323 0.029 Uiso 1 1 calc R . . H17B H 0.0208 1.2094 0.6072 0.029 Uiso 1 1 calc R . . H17C H -0.0725 1.2058 0.6258 0.029 Uiso 1 1 calc R . . C18 C 0.0249(2) 1.0335(4) 0.7424(2) 0.0275(5) Uani 1 1 d U . . C19 C 0.0672(2) 1.1381(3) 0.7927(2) 0.0289(5) Uani 1 1 d U . . H19A H 0.0795 1.2099 0.7622 0.035 Uiso 1 1 calc R . . C20 C 0.0916(2) 1.1395(4) 0.8857(2) 0.0333(5) Uani 1 1 d U . . H20A H 0.1189 1.2130 0.9181 0.040 Uiso 1 1 calc R . . C21 C 0.0771(2) 1.0370(4) 0.9322(3) 0.0406(6) Uani 1 1 d U . . H21A H 0.0975 1.0370 0.9966 0.049 Uiso 1 1 calc R . . C22 C 0.0325(3) 0.9330(4) 0.8846(3) 0.0428(6) Uani 1 1 d U . . H22A H 0.0192 0.8627 0.9160 0.051 Uiso 1 1 calc R . . C23 C 0.0070(3) 0.9322(4) 0.7901(3) 0.0389(6) Uani 1 1 d U . . H23A H -0.0234 0.8604 0.7577 0.047 Uiso 1 1 calc R . . S1 S 0.04349(5) 0.54790(10) 0.14680(6) 0.0303(2) Uani 1 1 d . . . S2 S 0.14226(5) 0.53597(11) 0.01986(6) 0.0359(3) Uani 1 1 d . . . C24 C 0.03953(19) 0.5380(4) 0.0358(2) 0.0273(8) Uani 1 1 d . . . C25 C 0.2034(2) 0.5466(4) 0.1335(2) 0.0335(9) Uani 1 1 d . . . H25A H 0.2668 0.5476 0.1541 0.040 Uiso 1 1 calc R . . C26 C 0.1582(2) 0.5532(4) 0.1906(2) 0.0280(8) Uani 1 1 d . . . H26A H 0.1880 0.5606 0.2540 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0082(3) 0.0111(3) 0.0144(3) 0.000 0.0027(3) 0.000 C1 0.0196(18) 0.055(3) 0.025(2) 0.008(2) 0.0099(17) 0.0143(19) C2 0.038(2) 0.059(3) 0.024(2) 0.0089(19) 0.0139(19) 0.015(2) C3 0.025(2) 0.042(2) 0.024(2) -0.0025(18) -0.0044(17) 0.0073(18) C4 0.0144(18) 0.041(2) 0.042(3) 0.002(2) 0.0047(19) -0.0027(17) C5 0.0170(18) 0.031(2) 0.029(2) 0.0017(17) 0.0075(17) -0.0036(16) C6 0.0152(17) 0.0140(17) 0.0182(19) -0.0047(14) 0.0039(15) -0.0026(13) C7 0.0115(16) 0.0164(17) 0.021(2) -0.0002(15) 0.0053(15) 0.0005(14) C8 0.0196(18) 0.0143(17) 0.029(2) -0.0023(15) 0.0072(17) -0.0026(14) N1 0.0126(14) 0.0100(13) 0.0134(14) -0.0015(12) 0.0037(12) 0.0012(11) C9 0.0115(16) 0.0125(16) 0.0143(18) 0.0037(14) -0.0001(14) 0.0047(13) O1 0.0161(11) 0.0222(13) 0.0160(13) -0.0051(10) 0.0042(11) 0.0033(10) N3 0.0105(12) 0.0108(12) 0.0134(13) 0.0050(14) 0.0049(11) 0.0040(13) C10 0.0132(16) 0.0101(15) 0.0112(17) 0.0029(13) 0.0035(14) 0.0045(13) C11 0.0116(16) 0.0136(16) 0.0226(19) 0.0013(15) 0.0067(15) 0.0050(13) C12 0.0082(15) 0.018(2) 0.026(2) 0.0062(14) 0.0064(15) 0.0026(13) C13 0.0076(15) 0.0089(16) 0.0224(19) 0.0013(14) 0.0019(15) 0.0000(13) C14 0.0111(16) 0.0112(16) 0.0141(17) 0.0023(14) 0.0018(15) -0.0013(14) C15 0.0095(16) 0.0156(18) 0.0143(18) 0.0033(14) -0.0008(14) -0.0013(13) O2 0.0120(11) 0.0173(12) 0.0198(13) -0.0051(10) 0.0048(10) -0.0047(9) N2 0.0099(13) 0.0087(13) 0.0163(15) -0.0019(11) 0.0064(12) -0.0021(11) C16 0.0095(15) 0.0193(17) 0.0202(17) 0.0010(16) 0.0053(14) 0.0013(14) C17 0.0188(17) 0.0175(18) 0.0205(19) -0.0051(15) 0.0042(15) 0.0071(14) C18 0.0319(12) 0.0345(12) 0.0211(11) -0.0051(10) 0.0156(10) -0.0005(10) C19 0.0315(12) 0.0366(12) 0.0229(11) -0.0064(10) 0.0149(10) -0.0019(10) C20 0.0368(12) 0.0406(12) 0.0247(11) -0.0071(10) 0.0133(10) -0.0020(10) C21 0.0519(12) 0.0431(12) 0.0249(11) -0.0051(10) 0.0100(10) -0.0007(11) C22 0.0518(12) 0.0413(12) 0.0259(11) -0.0021(10) 0.0091(11) -0.0017(11) C23 0.0539(12) 0.0373(12) 0.0238(11) -0.0038(10) 0.0107(11) -0.0012(11) S1 0.0205(4) 0.0522(6) 0.0161(5) -0.0026(5) 0.0030(4) 0.0031(5) S2 0.0218(5) 0.0635(7) 0.0226(5) -0.0023(5) 0.0075(4) -0.0031(5) C24 0.0224(17) 0.040(2) 0.0174(19) 0.0004(18) 0.0040(15) 0.0014(17) C25 0.0180(17) 0.054(3) 0.024(2) -0.001(2) 0.0001(16) -0.006(2) C26 0.0200(17) 0.039(2) 0.0189(19) -0.0052(19) -0.0020(15) 0.0011(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.848(2) . ? Co1 N3 1.848(2) 2_556 ? Co1 N1 1.958(2) . ? Co1 N1 1.958(2) 2_556 ? Co1 N2 1.976(3) . ? Co1 N2 1.976(2) 2_556 ? C1 C6 1.372(4) . ? C1 C2 1.386(5) . ? C1 H1A 0.9500 . ? C2 C3 1.375(5) . ? C2 H2A 0.9500 . ? C3 C4 1.374(5) . ? C3 H3A 0.9500 . ? C4 C5 1.382(5) . ? C4 H4A 0.9500 . ? C5 C6 1.398(4) . ? C5 H5A 0.9500 . ? C6 C7 1.517(4) . ? C7 N1 1.469(4) . ? C7 C8 1.535(4) . ? C7 H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N1 C9 1.329(3) . ? C9 O1 1.254(3) . ? C9 C10 1.499(4) . ? N3 C14 1.325(4) . ? N3 C10 1.338(4) . ? C10 C11 1.385(4) . ? C11 C12 1.385(4) . ? C11 H11A 0.9500 . ? C12 C13 1.388(4) . ? C12 H12A 0.9500 . ? C13 C14 1.393(4) . ? C13 H13A 0.9500 . ? C14 C15 1.504(4) . ? C15 O2 1.247(3) . ? C15 N2 1.338(3) . ? N2 C16 1.486(3) . ? C16 C18 1.518(4) . ? C16 C17 1.523(4) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.385(5) . ? C18 C19 1.394(5) . ? C19 C20 1.376(5) . ? C19 H19A 0.9500 . ? C20 C21 1.365(5) . ? C20 H20A 0.9500 . ? C21 C22 1.384(5) . ? C21 H21A 0.9500 . ? C22 C23 1.398(5) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? S1 C24 1.719(3) . ? S1 C26 1.722(3) . ? S2 C25 1.725(3) . ? S2 C24 1.728(3) . ? C24 C24 1.379(6) 2 ? C25 C26 1.318(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? 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 N3 Co1 N3 176.13(19) . 2_556 ? N3 Co1 N1 82.67(11) . . ? N3 Co1 N1 100.12(10) 2_556 . ? N3 Co1 N1 100.12(10) . 2_556 ? N3 Co1 N1 82.67(11) 2_556 2_556 ? N1 Co1 N1 88.71(15) . 2_556 ? N3 Co1 N2 82.23(11) . . ? N3 Co1 N2 95.07(10) 2_556 . ? N1 Co1 N2 164.72(9) . . ? N1 Co1 N2 91.62(9) 2_556 . ? N3 Co1 N2 95.07(10) . 2_556 ? N3 Co1 N2 82.23(11) 2_556 2_556 ? N1 Co1 N2 91.62(9) . 2_556 ? N1 Co1 N2 164.72(9) 2_556 2_556 ? N2 Co1 N2 92.05(15) . 2_556 ? C6 C1 C2 120.8(3) . . ? C6 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? C4 C3 C2 119.1(3) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C1 C6 C5 117.9(3) . . ? C1 C6 C7 122.1(3) . . ? C5 C6 C7 119.9(3) . . ? N1 C7 C6 114.5(2) . . ? N1 C7 C8 114.7(2) . . ? C6 C7 C8 109.9(3) . . ? N1 C7 H7A 105.6 . . ? C6 C7 H7A 105.6 . . ? C8 C7 H7A 105.6 . . ? 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 . . ? C9 N1 C7 122.8(3) . . ? C9 N1 Co1 114.7(2) . . ? C7 N1 Co1 122.05(17) . . ? O1 C9 N1 129.3(3) . . ? O1 C9 C10 119.0(2) . . ? N1 C9 C10 111.7(3) . . ? C14 N3 C10 124.0(2) . . ? C14 N3 Co1 118.2(2) . . ? C10 N3 Co1 117.2(2) . . ? N3 C10 C11 119.1(3) . . ? N3 C10 C9 113.1(2) . . ? C11 C10 C9 127.8(3) . . ? C10 C11 C12 118.2(3) . . ? C10 C11 H11A 120.9 . . ? C12 C11 H11A 120.9 . . ? C11 C12 C13 121.5(3) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C12 C13 C14 117.5(3) . . ? C12 C13 H13A 121.2 . . ? C14 C13 H13A 121.2 . . ? N3 C14 C13 119.6(3) . . ? N3 C14 C15 113.5(2) . . ? C13 C14 C15 126.7(3) . . ? O2 C15 N2 128.3(3) . . ? O2 C15 C14 120.5(2) . . ? N2 C15 C14 111.1(3) . . ? C15 N2 C16 118.1(2) . . ? C15 N2 Co1 114.66(19) . . ? C16 N2 Co1 126.57(18) . . ? N2 C16 C18 115.1(2) . . ? N2 C16 C17 110.7(2) . . ? C18 C16 C17 113.0(3) . . ? N2 C16 H16A 105.7 . . ? C18 C16 H16A 105.7 . . ? C17 C16 H16A 105.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 117.0(3) . . ? C23 C18 C16 118.5(3) . . ? C19 C18 C16 124.1(3) . . ? C20 C19 C18 121.4(3) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C21 C20 C19 121.0(4) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 119.3(4) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 119.5(4) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C18 C23 C22 121.6(4) . . ? C18 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C24 S1 C26 94.95(15) . . ? C25 S2 C24 95.08(15) . . ? C24 C24 S1 122.7(3) 2 . ? C24 C24 S2 122.2(3) 2 . ? S1 C24 S2 115.05(18) . . ? C26 C25 S2 117.0(3) . . ? C26 C25 H25A 121.5 . . ? S2 C25 H25A 121.5 . . ? C25 C26 S1 117.9(3) . . ? C25 C26 H26A 121.0 . . ? S1 C26 H26A 121.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C26 H26A O1 0.95 2.46 2.905(4) 108.3 . C26 H26A O2 0.95 2.23 2.961(4) 133.4 4_546 C25 H25A O2 0.95 2.75 3.198(4) 109.9 4_546 C13 H13A O1 0.95 2.35 3.274(4) 165.4 4_556 C11 H11A O2 0.95 2.42 3.323(3) 157.8 4_546 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.501 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.061 # Attachment '- TTFCoL2.cif' data_nc16 _database_code_depnum_ccdc_archive 'CCDC 786091' #TrackingRef '- TTFCoL2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H54 Co N6 O10 S4' _chemical_formula_weight 966.06 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' S S 0.3331 0.5567 '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 monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.58540(10) _cell_length_b 25.4527(3) _cell_length_c 9.74480(10) _cell_angle_alpha 90.00 _cell_angle_beta 113.302(2) _cell_angle_gamma 90.00 _cell_volume 2183.55(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11656 _cell_measurement_theta_min 3.46 _cell_measurement_theta_max 61.83 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 5.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 150 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 13998 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 61.94 _reflns_number_total 6707 _reflns_number_gt 6425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 3235 Friedel pairs' _refine_ls_abs_structure_Flack 0.026(2) _chemical_absolute_configuration rmad _refine_ls_number_reflns 6707 _refine_ls_number_parameters 560 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36200(4) 0.754420(16) 0.51177(4) 0.01091(11) Uani 1 1 d . . . N1 N 0.4713(2) 0.70048(9) 0.6592(3) 0.0147(5) Uani 1 1 d . . . C1 C 0.7852(4) 0.63195(15) 0.4979(4) 0.0350(8) Uani 1 1 d . . . H1A H 0.8706 0.6127 0.4909 0.052 Uiso 1 1 calc R . . H1B H 0.8186 0.6672 0.5376 0.052 Uiso 1 1 calc R . . H1C H 0.7031 0.6347 0.3985 0.052 Uiso 1 1 calc R . . O1 O 0.7326(2) 0.60509(9) 0.5933(3) 0.0305(5) Uani 1 1 d . . . O2 O 0.4516(2) 0.65286(8) 0.8561(2) 0.0204(4) Uani 1 1 d . . . N2 N 0.2403(2) 0.75419(9) 0.6199(2) 0.0122(4) Uani 1 1 d . . . C2 C 0.5961(3) 0.62626(12) 0.5949(4) 0.0260(7) Uani 1 1 d . . . H2A H 0.5525 0.6009 0.6443 0.031 Uiso 1 1 calc R . . H2B H 0.5218 0.6309 0.4907 0.031 Uiso 1 1 calc R . . O3 O 0.0057(2) 0.85511(7) 0.4052(2) 0.0154(4) Uani 1 1 d . . . N3 N 0.2215(2) 0.81178(8) 0.4048(2) 0.0118(5) Uani 1 1 d . . . C3 C 0.6192(3) 0.67833(12) 0.6750(3) 0.0197(6) Uani 1 1 d . . . H3A H 0.6605 0.7027 0.6197 0.024 Uiso 1 1 calc R . . C4 C 0.7398(3) 0.67563(13) 0.8343(3) 0.0259(7) Uani 1 1 d . . . H4A H 0.7414 0.7089 0.8857 0.039 Uiso 1 1 calc R . . H4B H 0.8396 0.6695 0.8316 0.039 Uiso 1 1 calc R . . H4C H 0.7157 0.6468 0.8880 0.039 Uiso 1 1 calc R . . O4 O 0.2863(3) 0.93053(8) 0.2213(2) 0.0258(5) Uani 1 1 d . . . C5 C 0.4095(3) 0.68668(10) 0.7544(3) 0.0151(6) Uani 1 1 d . . . C6 C 0.2709(3) 0.71928(10) 0.7319(3) 0.0137(6) Uani 1 1 d . . . C7 C 0.1806(3) 0.71697(11) 0.8123(3) 0.0163(6) Uani 1 1 d . . . H7A H 0.2010 0.6924 0.8912 0.020 Uiso 1 1 calc R . . C8 C 0.0586(3) 0.75168(11) 0.7745(3) 0.0168(6) Uani 1 1 d . . . H8A H -0.0040 0.7513 0.8295 0.020 Uiso 1 1 calc R . . C9 C 0.0276(3) 0.78704(11) 0.6566(3) 0.0161(6) Uani 1 1 d . . . H9A H -0.0561 0.8105 0.6297 0.019 Uiso 1 1 calc R . . C10 C 0.1220(3) 0.78686(10) 0.5803(3) 0.0124(5) Uani 1 1 d . . . C11 C 0.1107(3) 0.82183(10) 0.4519(3) 0.0132(6) Uani 1 1 d . . . C12 C 0.2271(3) 0.84413(11) 0.2813(3) 0.0145(6) Uani 1 1 d . . . H12A H 0.3220 0.8340 0.2684 0.017 Uiso 1 1 calc R . . C13 C 0.0951(3) 0.83275(12) 0.1332(3) 0.0246(7) Uani 1 1 d . . . H13A H 0.0960 0.7955 0.1083 0.037 Uiso 1 1 calc R . . H13B H 0.1054 0.8543 0.0543 0.037 Uiso 1 1 calc R . . H13C H -0.0009 0.8412 0.1418 0.037 Uiso 1 1 calc R . . C14 C 0.2417(4) 0.90226(11) 0.3219(3) 0.0224(7) Uani 1 1 d . . . H14A H 0.1432 0.9158 0.3174 0.027 Uiso 1 1 calc R . . H14B H 0.3182 0.9070 0.4251 0.027 Uiso 1 1 calc R . . C15 C 0.3013(4) 0.98478(12) 0.2587(4) 0.0348(8) Uani 1 1 d . . . H15A H 0.3151 1.0048 0.1790 0.052 Uiso 1 1 calc R . . H15B H 0.3896 0.9900 0.3527 0.052 Uiso 1 1 calc R . . H15C H 0.2095 0.9970 0.2701 0.052 Uiso 1 1 calc R . . N4 N 0.5194(2) 0.80454(9) 0.6299(3) 0.0140(5) Uani 1 1 d . . . N5 N 0.4728(2) 0.75571(9) 0.3938(2) 0.0124(4) Uani 1 1 d . . . O5 O 0.4474(2) 0.90076(8) 0.8819(2) 0.0221(5) Uani 1 1 d . . . O6 O 0.7135(2) 0.85514(8) 0.6095(2) 0.0190(4) Uani 1 1 d . . . N6 N 0.2444(2) 0.70146(9) 0.3622(3) 0.0129(5) Uani 1 1 d . . . O7 O 0.2259(2) 0.66809(7) 0.1318(2) 0.0175(4) Uani 1 1 d . . . O8 O 0.2231(2) 0.58479(8) 0.3895(3) 0.0308(5) Uani 1 1 d . . . C16 C 0.3425(3) 0.87398(12) 0.9288(3) 0.0245(7) Uani 1 1 d . . . H16A H 0.3301 0.8938 1.0094 0.037 Uiso 1 1 calc R . . H16B H 0.3814 0.8388 0.9649 0.037 Uiso 1 1 calc R . . H16C H 0.2440 0.8709 0.8442 0.037 Uiso 1 1 calc R . . C17 C 0.4546(3) 0.87913(11) 0.7512(3) 0.0189(6) Uani 1 1 d . . . H17A H 0.5087 0.9041 0.7115 0.023 Uiso 1 1 calc R . . H17B H 0.3500 0.8751 0.6748 0.023 Uiso 1 1 calc R . . C18 C 0.5348(3) 0.82576(11) 0.7756(3) 0.0141(6) Uani 1 1 d . . . H18A H 0.4784 0.8015 0.8163 0.017 Uiso 1 1 calc R . . C19 C 0.6974(3) 0.82958(12) 0.8932(3) 0.0202(6) Uani 1 1 d . . . H19A H 0.7475 0.7954 0.9036 0.030 Uiso 1 1 calc R . . H19B H 0.6953 0.8399 0.9893 0.030 Uiso 1 1 calc R . . H19C H 0.7536 0.8559 0.8622 0.030 Uiso 1 1 calc R . . C20 C 0.6144(3) 0.82068(10) 0.5679(3) 0.0147(6) Uani 1 1 d . . . C21 C 0.5893(3) 0.78975(10) 0.4279(3) 0.0131(6) Uani 1 1 d . . . C22 C 0.6682(3) 0.79447(11) 0.3366(3) 0.0164(6) Uani 1 1 d . . . H22A H 0.7503 0.8185 0.3599 0.020 Uiso 1 1 calc R . . C23 C 0.6238(3) 0.76302(11) 0.2093(3) 0.0173(6) Uani 1 1 d . . . H23A H 0.6781 0.7648 0.1464 0.021 Uiso 1 1 calc R . . C24 C 0.5015(3) 0.72915(11) 0.1736(3) 0.0158(6) Uani 1 1 d . . . H24A H 0.4700 0.7083 0.0858 0.019 Uiso 1 1 calc R . . C25 C 0.4257(3) 0.72633(10) 0.2689(3) 0.0132(6) Uani 1 1 d . . . C26 C 0.2865(3) 0.69483(10) 0.2476(3) 0.0143(6) Uani 1 1 d . . . C27 C 0.1069(3) 0.67414(11) 0.3570(3) 0.0156(6) Uani 1 1 d . . . H27A H 0.1067 0.6758 0.4595 0.019 Uiso 1 1 calc R . . C28 C -0.0373(3) 0.70185(13) 0.2503(4) 0.0250(7) Uani 1 1 d . . . H28A H -0.0355 0.7387 0.2803 0.038 Uiso 1 1 calc R . . H28B H -0.1268 0.6844 0.2541 0.038 Uiso 1 1 calc R . . H28C H -0.0416 0.7002 0.1482 0.038 Uiso 1 1 calc R . . C29 C 0.0941(3) 0.61627(12) 0.3110(4) 0.0245(7) Uani 1 1 d . . . H29A H 0.0057 0.6009 0.3248 0.029 Uiso 1 1 calc R . . H29B H 0.0731 0.6145 0.2031 0.029 Uiso 1 1 calc R . . C30 C 0.2314(4) 0.56861(14) 0.5316(4) 0.0367(8) Uani 1 1 d . . . H30A H 0.3176 0.5447 0.5770 0.055 Uiso 1 1 calc R . . H30B H 0.1372 0.5505 0.5202 0.055 Uiso 1 1 calc R . . H30C H 0.2450 0.5995 0.5958 0.055 Uiso 1 1 calc R . . S1 S 0.61810(8) 0.56737(3) 0.07182(8) 0.02035(16) Uani 1 1 d . . . S2 S 0.57673(8) 0.51715(3) 0.32050(8) 0.02036(16) Uani 1 1 d . . . S3 S 0.89272(8) 0.45380(3) 0.40373(8) 0.01983(16) Uani 1 1 d . . . S4 S 0.92060(8) 0.49713(3) 0.13939(8) 0.02185(17) Uani 1 1 d . . . C31 C 0.4613(3) 0.58569(11) 0.1053(3) 0.0204(6) Uani 1 1 d . . . H31A H 0.3912 0.6110 0.0446 0.024 Uiso 1 1 calc R . . C32 C 0.4427(3) 0.56269(12) 0.2206(3) 0.0219(6) Uani 1 1 d . . . H32A H 0.3593 0.5712 0.2459 0.026 Uiso 1 1 calc R . . C33 C 0.6857(3) 0.52342(11) 0.2179(3) 0.0179(6) Uani 1 1 d . . . C34 C 0.8193(3) 0.49479(11) 0.2511(3) 0.0186(6) Uani 1 1 d . . . C35 C 1.0445(3) 0.43287(12) 0.3658(3) 0.0225(7) Uani 1 1 d . . . H35A H 1.1159 0.4082 0.4281 0.027 Uiso 1 1 calc R . . C36 C 1.0573(3) 0.45303(12) 0.2444(3) 0.0236(7) Uani 1 1 d . . . H36A H 1.1387 0.4434 0.2172 0.028 Uiso 1 1 calc R . . O9 O 1.1969(3) 0.50103(9) -0.1940(3) 0.0381(6) Uani 1 1 d . . . O10 O 1.1152(3) 0.49335(12) -0.0126(3) 0.0558(8) Uani 1 1 d . . . C37 C 1.3581(5) 0.43881(16) -0.2380(5) 0.0476(10) Uani 1 1 d . . . H37A H 1.3875 0.4017 -0.2311 0.071 Uiso 1 1 calc R . . H37B H 1.4480 0.4603 -0.1839 0.071 Uiso 1 1 calc R . . H37C H 1.3137 0.4495 -0.3432 0.071 Uiso 1 1 calc R . . C38 C 1.2479(4) 0.44605(13) -0.1729(4) 0.0391(9) Uani 1 1 d . . . H38A H 1.2941 0.4376 -0.0650 0.047 Uiso 1 1 calc R . . H38B H 1.1603 0.4223 -0.2216 0.047 Uiso 1 1 calc R . . C39 C 1.1307(4) 0.51973(15) -0.1076(4) 0.0370(8) Uani 1 1 d . . . C40 C 1.0802(4) 0.57537(14) -0.1425(4) 0.0393(9) Uani 1 1 d . . . H40A H 1.0993 0.5944 -0.0493 0.059 Uiso 1 1 calc R . . H40B H 0.9713 0.5762 -0.2057 0.059 Uiso 1 1 calc R . . H40C H 1.1368 0.5921 -0.1953 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0103(2) 0.0119(2) 0.0107(2) 0.00018(18) 0.00435(16) -0.00020(17) N1 0.0125(11) 0.0146(11) 0.0176(12) 0.0012(10) 0.0066(10) 0.0012(9) C1 0.0313(18) 0.042(2) 0.038(2) -0.0064(17) 0.0211(16) 0.0027(16) O1 0.0278(12) 0.0327(12) 0.0320(13) -0.0032(10) 0.0129(10) 0.0101(10) O2 0.0222(10) 0.0198(10) 0.0193(10) 0.0079(9) 0.0084(9) 0.0042(8) N2 0.0118(10) 0.0111(10) 0.0126(11) -0.0012(10) 0.0035(9) 0.0001(10) C2 0.0196(15) 0.0277(17) 0.0288(17) -0.0028(14) 0.0074(13) 0.0064(13) O3 0.0120(9) 0.0150(10) 0.0189(10) 0.0024(8) 0.0057(8) 0.0025(8) N3 0.0121(11) 0.0132(11) 0.0114(11) -0.0025(9) 0.0060(9) -0.0019(9) C3 0.0177(15) 0.0243(15) 0.0192(15) 0.0023(12) 0.0095(12) 0.0054(12) C4 0.0177(15) 0.0305(17) 0.0275(17) -0.0010(14) 0.0067(13) 0.0039(13) O4 0.0449(13) 0.0169(10) 0.0204(11) -0.0003(8) 0.0177(10) -0.0075(9) C5 0.0143(14) 0.0153(14) 0.0147(14) -0.0013(11) 0.0048(11) -0.0012(11) C6 0.0181(14) 0.0112(13) 0.0115(14) -0.0012(11) 0.0054(11) -0.0025(11) C7 0.0181(14) 0.0167(14) 0.0144(14) 0.0006(11) 0.0067(12) -0.0056(11) C8 0.0162(13) 0.0196(14) 0.0164(14) -0.0026(12) 0.0084(11) -0.0049(12) C9 0.0128(13) 0.0181(15) 0.0180(15) -0.0036(12) 0.0068(12) -0.0024(11) C10 0.0103(13) 0.0122(13) 0.0137(13) -0.0029(11) 0.0036(11) 0.0004(10) C11 0.0141(13) 0.0111(13) 0.0129(14) -0.0028(11) 0.0039(11) -0.0031(11) C12 0.0129(14) 0.0175(14) 0.0133(14) 0.0049(11) 0.0054(12) 0.0046(11) C13 0.0260(16) 0.0293(17) 0.0143(15) 0.0008(13) 0.0035(13) -0.0044(13) C14 0.0330(17) 0.0186(15) 0.0198(16) -0.0002(12) 0.0148(14) -0.0041(13) C15 0.056(2) 0.0191(16) 0.0300(18) 0.0016(14) 0.0181(17) -0.0098(15) N4 0.0144(11) 0.0132(11) 0.0148(12) 0.0001(9) 0.0064(10) 0.0003(9) N5 0.0141(10) 0.0084(10) 0.0139(11) 0.0022(10) 0.0047(9) 0.0030(10) O5 0.0233(11) 0.0235(11) 0.0210(11) -0.0054(8) 0.0104(9) -0.0009(9) O6 0.0173(10) 0.0197(11) 0.0215(11) -0.0050(9) 0.0091(9) -0.0063(8) N6 0.0115(11) 0.0139(11) 0.0132(12) 0.0035(9) 0.0049(9) 0.0012(9) O7 0.0203(10) 0.0189(10) 0.0129(10) -0.0055(8) 0.0062(8) -0.0025(8) O8 0.0334(12) 0.0280(12) 0.0369(13) 0.0054(10) 0.0202(11) 0.0027(10) C16 0.0269(16) 0.0283(17) 0.0209(16) -0.0025(13) 0.0122(13) 0.0026(13) C17 0.0207(15) 0.0188(15) 0.0180(15) -0.0045(12) 0.0086(12) 0.0009(12) C18 0.0145(13) 0.0161(13) 0.0120(14) -0.0009(11) 0.0054(11) -0.0022(11) C19 0.0167(15) 0.0230(15) 0.0161(15) -0.0019(12) 0.0015(12) -0.0012(12) C20 0.0146(14) 0.0140(13) 0.0148(14) 0.0014(11) 0.0051(12) 0.0018(11) C21 0.0085(12) 0.0135(13) 0.0152(13) 0.0016(11) 0.0023(11) 0.0018(10) C22 0.0114(13) 0.0191(14) 0.0190(15) 0.0023(12) 0.0065(12) 0.0019(11) C23 0.0173(14) 0.0197(15) 0.0161(14) 0.0043(12) 0.0079(11) 0.0031(12) C24 0.0164(14) 0.0179(14) 0.0133(14) 0.0022(12) 0.0061(11) 0.0047(11) C25 0.0142(13) 0.0118(13) 0.0129(14) 0.0015(11) 0.0046(11) 0.0020(11) C26 0.0146(13) 0.0121(13) 0.0160(15) 0.0030(12) 0.0057(12) 0.0037(11) C27 0.0132(14) 0.0192(14) 0.0152(14) -0.0026(11) 0.0066(12) -0.0024(11) C28 0.0146(14) 0.0283(16) 0.0285(17) 0.0017(14) 0.0047(13) 0.0010(13) C29 0.0221(15) 0.0206(16) 0.0361(19) -0.0012(14) 0.0172(14) -0.0017(13) C30 0.0377(19) 0.0331(19) 0.039(2) 0.0083(16) 0.0149(16) -0.0005(16) S1 0.0229(4) 0.0203(4) 0.0198(4) 0.0053(3) 0.0104(3) 0.0051(3) S2 0.0244(4) 0.0188(3) 0.0211(4) 0.0050(3) 0.0124(3) 0.0048(3) S3 0.0186(3) 0.0191(4) 0.0217(4) 0.0038(3) 0.0080(3) 0.0028(3) S4 0.0244(4) 0.0206(4) 0.0247(4) 0.0037(3) 0.0141(3) 0.0038(3) C31 0.0226(15) 0.0153(15) 0.0230(16) 0.0020(12) 0.0086(13) 0.0031(12) C32 0.0186(15) 0.0210(15) 0.0251(16) 0.0005(13) 0.0074(12) 0.0019(12) C33 0.0204(15) 0.0157(14) 0.0184(15) -0.0034(12) 0.0087(12) 0.0003(12) C34 0.0204(15) 0.0147(14) 0.0218(15) -0.0004(12) 0.0095(13) -0.0013(12) C35 0.0168(15) 0.0185(15) 0.0291(17) -0.0013(13) 0.0059(13) 0.0030(12) C36 0.0202(15) 0.0176(15) 0.0354(18) 0.0011(14) 0.0135(14) 0.0032(13) O9 0.0477(15) 0.0326(13) 0.0382(14) 0.0054(11) 0.0216(12) 0.0104(11) O10 0.0622(18) 0.0578(18) 0.063(2) 0.0256(16) 0.0419(16) 0.0114(15) C37 0.051(2) 0.040(2) 0.048(2) -0.0015(19) 0.015(2) 0.0098(19) C38 0.0359(19) 0.0267(18) 0.047(2) 0.0126(16) 0.0086(17) -0.0019(15) C39 0.0321(19) 0.041(2) 0.039(2) 0.0003(18) 0.0148(17) -0.0008(16) C40 0.038(2) 0.0319(19) 0.044(2) -0.0034(17) 0.0110(17) 0.0049(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 1.848(2) . ? Co1 N2 1.856(2) . ? Co1 N4 1.963(2) . ? Co1 N1 1.964(2) . ? Co1 N6 1.978(2) . ? Co1 N3 1.980(2) . ? N1 C5 1.330(3) . ? N1 C3 1.476(3) . ? C1 O1 1.398(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O1 C2 1.421(3) . ? O2 C5 1.252(3) . ? N2 C10 1.334(3) . ? N2 C6 1.347(3) . ? C2 C3 1.509(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C11 1.255(3) . ? N3 C11 1.338(3) . ? N3 C12 1.476(3) . ? C3 C4 1.527(4) . ? C3 H3A 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O4 C14 1.412(4) . ? O4 C15 1.421(4) . ? C5 C6 1.507(4) . ? C6 C7 1.379(4) . ? C7 C8 1.394(4) . ? C7 H7A 0.9500 . ? C8 C9 1.395(4) . ? C8 H8A 0.9500 . ? C9 C10 1.380(4) . ? C9 H9A 0.9500 . ? C10 C11 1.504(4) . ? C12 C14 1.524(4) . ? C12 C13 1.524(4) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N4 C20 1.341(3) . ? N4 C18 1.471(3) . ? N5 C25 1.345(3) . ? N5 C21 1.347(3) . ? O5 C17 1.414(3) . ? O5 C16 1.432(4) . ? O6 C20 1.238(3) . ? N6 C26 1.340(3) . ? N6 C27 1.473(3) . ? O7 C26 1.247(3) . ? O8 C30 1.417(4) . ? O8 C29 1.417(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.532(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.530(4) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.509(4) . ? C21 C22 1.382(4) . ? C22 C23 1.394(4) . ? C22 H22A 0.9500 . ? C23 C24 1.384(4) . ? C23 H23A 0.9500 . ? C24 C25 1.389(4) . ? C24 H24A 0.9500 . ? C25 C26 1.499(4) . ? C27 C29 1.530(4) . ? C27 C28 1.534(4) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? S1 C33 1.723(3) . ? S1 C31 1.723(3) . ? S2 C33 1.716(3) . ? S2 C32 1.718(3) . ? S3 C35 1.722(3) . ? S3 C34 1.723(3) . ? S4 C36 1.721(3) . ? S4 C34 1.722(3) . ? C31 C32 1.340(4) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.395(4) . ? C35 C36 1.339(4) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? O9 C39 1.327(4) . ? O9 C38 1.470(4) . ? O10 C39 1.200(4) . ? C37 C38 1.443(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.492(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Co1 N2 176.49(9) . . ? N5 Co1 N4 81.70(9) . . ? N2 Co1 N4 100.33(9) . . ? N5 Co1 N1 101.29(9) . . ? N2 Co1 N1 81.71(9) . . ? N4 Co1 N1 87.79(9) . . ? N5 Co1 N6 81.61(9) . . ? N2 Co1 N6 96.49(9) . . ? N4 Co1 N6 163.06(9) . . ? N1 Co1 N6 92.66(10) . . ? N5 Co1 N3 95.62(9) . . ? N2 Co1 N3 81.48(9) . . ? N4 Co1 N3 91.97(9) . . ? N1 Co1 N3 162.87(9) . . ? N6 Co1 N3 92.51(9) . . ? C5 N1 C3 120.0(2) . . ? C5 N1 Co1 116.04(18) . . ? C3 N1 Co1 123.76(18) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 O1 C2 113.4(3) . . ? C10 N2 C6 122.2(2) . . ? C10 N2 Co1 119.18(18) . . ? C6 N2 Co1 118.56(18) . . ? O1 C2 C3 113.0(2) . . ? O1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? O1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C11 N3 C12 117.6(2) . . ? C11 N3 Co1 115.27(18) . . ? C12 N3 Co1 127.17(16) . . ? N1 C3 C2 110.0(2) . . ? N1 C3 C4 115.6(2) . . ? C2 C3 C4 112.6(2) . . ? N1 C3 H3A 106.0 . . ? C2 C3 H3A 106.0 . . ? C4 C3 H3A 106.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C14 O4 C15 110.2(2) . . ? O2 C5 N1 129.8(3) . . ? O2 C5 C6 118.9(2) . . ? N1 C5 C6 111.3(2) . . ? N2 C6 C7 120.3(2) . . ? N2 C6 C5 112.2(2) . . ? C7 C6 C5 127.5(2) . . ? C6 C7 C8 118.2(3) . . ? C6 C7 H7A 120.9 . . ? C8 C7 H7A 120.9 . . ? C7 C8 C9 120.6(2) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C10 C9 C8 118.0(3) . . ? C10 C9 H9A 121.0 . . ? C8 C9 H9A 121.0 . . ? N2 C10 C9 120.7(2) . . ? N2 C10 C11 112.5(2) . . ? C9 C10 C11 126.8(2) . . ? O3 C11 N3 129.5(3) . . ? O3 C11 C10 119.0(2) . . ? N3 C11 C10 111.5(2) . . ? N3 C12 C14 111.1(2) . . ? N3 C12 C13 112.4(2) . . ? C14 C12 C13 112.8(2) . . ? N3 C12 H12A 106.7 . . ? C14 C12 H12A 106.7 . . ? C13 C12 H12A 106.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 C14 C12 109.7(2) . . ? O4 C14 H14A 109.7 . . ? C12 C14 H14A 109.7 . . ? O4 C14 H14B 109.7 . . ? C12 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? O4 C15 H15A 109.5 . . ? O4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C20 N4 C18 119.7(2) . . ? C20 N4 Co1 115.87(19) . . ? C18 N4 Co1 124.40(17) . . ? C25 N5 C21 122.0(2) . . ? C25 N5 Co1 118.87(18) . . ? C21 N5 Co1 118.85(18) . . ? C17 O5 C16 113.2(2) . . ? C26 N6 C27 118.2(2) . . ? C26 N6 Co1 115.34(17) . . ? C27 N6 Co1 126.02(18) . . ? C30 O8 C29 113.0(2) . . ? O5 C16 H16A 109.5 . . ? O5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 C18 114.0(2) . . ? O5 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? O5 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N4 C18 C19 115.5(2) . . ? N4 C18 C17 108.9(2) . . ? C19 C18 C17 111.1(2) . . ? N4 C18 H18A 107.0 . . ? C19 C18 H18A 107.0 . . ? C17 C18 H18A 107.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 N4 129.7(3) . . ? O6 C20 C21 119.5(2) . . ? N4 C20 C21 110.7(2) . . ? N5 C21 C22 120.6(2) . . ? N5 C21 C20 112.2(2) . . ? C22 C21 C20 127.2(2) . . ? C21 C22 C23 118.1(3) . . ? C21 C22 H22A 120.9 . . ? C23 C22 H22A 120.9 . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 118.6(3) . . ? C23 C24 H24A 120.7 . . ? C25 C24 H24A 120.7 . . ? N5 C25 C24 119.9(2) . . ? N5 C25 C26 112.6(2) . . ? C24 C25 C26 127.4(2) . . ? O7 C26 N6 129.5(3) . . ? O7 C26 C25 119.2(2) . . ? N6 C26 C25 111.2(2) . . ? N6 C27 C29 115.5(2) . . ? N6 C27 C28 111.1(2) . . ? C29 C27 C28 107.3(2) . . ? N6 C27 H27A 107.5 . . ? C29 C27 H27A 107.5 . . ? C28 C27 H27A 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O8 C29 C27 115.8(2) . . ? O8 C29 H29A 108.3 . . ? C27 C29 H29A 108.3 . . ? O8 C29 H29B 108.3 . . ? C27 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? O8 C30 H30A 109.5 . . ? O8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 S1 C31 95.20(14) . . ? C33 S2 C32 95.65(14) . . ? C35 S3 C34 95.35(14) . . ? C36 S4 C34 95.10(14) . . ? C32 C31 S1 117.1(2) . . ? C32 C31 H31A 121.4 . . ? S1 C31 H31A 121.4 . . ? C31 C32 S2 116.9(2) . . ? C31 C32 H32A 121.6 . . ? S2 C32 H32A 121.6 . . ? C34 C33 S2 122.1(2) . . ? C34 C33 S1 122.8(2) . . ? S2 C33 S1 115.15(16) . . ? C33 C34 S4 122.0(2) . . ? C33 C34 S3 122.7(2) . . ? S4 C34 S3 115.25(16) . . ? C36 C35 S3 116.9(2) . . ? C36 C35 H35A 121.6 . . ? S3 C35 H35A 121.6 . . ? C35 C36 S4 117.4(2) . . ? C35 C36 H36A 121.3 . . ? S4 C36 H36A 121.3 . . ? C39 O9 C38 117.9(3) . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C37 C38 O9 108.7(3) . . ? C37 C38 H38A 110.0 . . ? O9 C38 H38A 110.0 . . ? C37 C38 H38B 110.0 . . ? O9 C38 H38B 110.0 . . ? H38A C38 H38B 108.3 . . ? O10 C39 O9 121.7(4) . . ? O10 C39 C40 125.4(4) . . ? O9 C39 C40 113.0(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C35 H35A O6 0.95 2.26 2.985(3) 132.5 2_746 C32 H32A O8 0.95 2.29 3.193(4) 159.4 . C31 H31A O7 0.95 2.53 3.165(3) 124.3 . C31 H31A O2 0.95 2.39 2.941(3) 117.0 1_554 C36 H36A O10 0.95 2.51 2.955(4) 108.9 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 61.94 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.477 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.049