# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sally Brooker' _publ_contact_author_email SBROOKER@CHEMISTRY.OTAGO.AC.NZ _publ_section_title ; Towards Langmuir-Blodgett films of magnetically interesting materials: solution high spin/low spin equilibrium in ambiphilic iron(II) complexes of a triazole-containing ligand ; loop_ _publ_author_name 'Sally Brooker' 'Martin Albrecht' 'Humphrey L. C. Feltham' 'Claudio Gandolfi' 'Nicholas G White' # Attachment 'nw454.cif' data_nw454 _database_code_depnum_ccdc_archive 'CCDC 741107' #TrackingRef 'nw454.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H86 Fe N12 O6 S2' _chemical_formula_weight 1143.34 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0978(6) _cell_length_b 14.2697(10) _cell_length_c 22.0872(15) _cell_angle_alpha 102.047(3) _cell_angle_beta 97.982(3) _cell_angle_gamma 104.035(3) _cell_volume 2958.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 92(2) _cell_measurement_reflns_used 7109 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 26.24 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8048 _exptl_absorpt_correction_T_max 0.9924 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 92(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62470 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.38 _reflns_number_total 12032 _reflns_number_gt 9921 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains one whole Fe(II)-containing complex only. No solvent is present. This complex consists of one Fe(II) ion bound to two adpt ligands and two, trans, hexadecane sulfonate anions. No disorder is present in the structure. All non-H atoms are ANIS. Amino protons were found in the map and AFIX 01'ed with temperature factors equal to 1.2 times that of the nitrogen atom to which they were attached. One of these protons had its N-H distance HIMPed to be 0.95 A, the same length as the other proton bound to the same nitrogen atom. One reflection [0 0 1] was omitted as it was behind the beamstop. ; _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^)+(0.0424P)^2^+6.9371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12032 _refine_ls_number_parameters 696 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1552 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 Fe1 Fe 0.21516(5) 0.76258(3) 0.49125(2) 0.01291(12) Uani 1 1 d . . . S1 S 0.07928(8) 0.74755(6) 0.62156(4) 0.01482(17) Uani 1 1 d . . . O11 O 0.1031(2) 0.78051(16) 0.56386(10) 0.0167(5) Uani 1 1 d . . . O12 O -0.0416(2) 0.77318(17) 0.64130(11) 0.0202(5) Uani 1 1 d . . . O13 O 0.0779(3) 0.64405(16) 0.61563(12) 0.0225(5) Uani 1 1 d . . . S2 S 0.43190(8) 0.71871(6) 0.39030(4) 0.01798(18) Uani 1 1 d . . . O21 O 0.3216(2) 0.75560(16) 0.41593(11) 0.0172(5) Uani 1 1 d . . . O22 O 0.4679(3) 0.76163(18) 0.33890(13) 0.0310(6) Uani 1 1 d . . . O23 O 0.5510(2) 0.72937(17) 0.43877(13) 0.0267(6) Uani 1 1 d . . . N1 N 0.2634(3) 0.62783(19) 0.50963(12) 0.0144(5) Uani 1 1 d . . . N2 N 0.4054(3) 0.81825(19) 0.55862(13) 0.0150(6) Uani 1 1 d . . . N3 N 0.4898(3) 0.9103(2) 0.59197(13) 0.0169(6) Uani 1 1 d . . . N4 N 0.7970(3) 0.9506(2) 0.71085(14) 0.0258(7) Uani 1 1 d . . . N5 N 0.5801(3) 0.79446(19) 0.61808(13) 0.0145(6) Uani 1 1 d . . . N6 N 0.6678(3) 0.7448(2) 0.64650(15) 0.0241(7) Uani 1 1 d . . . H6X H 0.7396 0.7483 0.6225 0.029 Uiso 1 1 d . . . H6Y H 0.7110 0.7897 0.6866 0.029 Uiso 1 1 d . . . N21 N 0.1681(3) 0.89686(19) 0.47114(12) 0.0145(6) Uani 1 1 d . . . N22 N 0.0259(3) 0.70679(19) 0.42228(13) 0.0161(6) Uani 1 1 d . . . N23 N -0.0574(3) 0.61448(19) 0.38869(13) 0.0160(6) Uani 1 1 d . . . N24 N -0.3528(3) 0.5760(2) 0.26403(13) 0.0204(6) Uani 1 1 d . . . N25 N -0.1452(3) 0.73035(19) 0.36131(13) 0.0150(6) Uani 1 1 d . . . N26 N -0.2320(3) 0.7811(2) 0.33315(15) 0.0245(7) Uani 1 1 d . . . H26X H -0.2795 0.7330 0.2969 0.029 Uiso 1 1 d . . . H26Y H -0.2982 0.7869 0.3575 0.029 Uiso 1 1 d . . . C1 C 0.1823(3) 0.5337(2) 0.48452(16) 0.0168(7) Uani 1 1 d . . . H1 H 0.0959 0.5230 0.4571 0.020 Uiso 1 1 calc R . . C2 C 0.2207(4) 0.4515(2) 0.49743(16) 0.0200(7) Uani 1 1 d . . . H2 H 0.1612 0.3859 0.4791 0.024 Uiso 1 1 calc R . . C3 C 0.3460(4) 0.4662(2) 0.53706(17) 0.0208(7) Uani 1 1 d . . . H3 H 0.3741 0.4109 0.5461 0.025 Uiso 1 1 calc R . . C4 C 0.4315(3) 0.5635(2) 0.56391(16) 0.0180(7) Uani 1 1 d . . . H4 H 0.5185 0.5758 0.5913 0.022 Uiso 1 1 calc R . . C5 C 0.3852(3) 0.6418(2) 0.54921(15) 0.0142(6) Uani 1 1 d . . . C6 C 0.4594(3) 0.7486(2) 0.57525(15) 0.0149(6) Uani 1 1 d . . . C7 C 0.5948(3) 0.8961(2) 0.62752(15) 0.0152(7) Uani 1 1 d . . . C8 C 0.7082(3) 0.9766(3) 0.67091(16) 0.0189(7) Uani 1 1 d . . . C9 C 0.7170(4) 1.0750(3) 0.66808(17) 0.0231(8) Uani 1 1 d . . . H9 H 0.6500 1.0899 0.6397 0.028 Uiso 1 1 calc R . . C10 C 0.8273(4) 1.1496(3) 0.70832(18) 0.0309(9) Uani 1 1 d . . . H10 H 0.8372 1.2176 0.7084 0.037 Uiso 1 1 calc R . . C11 C 0.9231(4) 1.1243(3) 0.74844(19) 0.0372(10) Uani 1 1 d . . . H11 H 1.0009 1.1743 0.7754 0.045 Uiso 1 1 calc R . . C12 C 0.9035(4) 1.0245(3) 0.74856(19) 0.0356(10) Uani 1 1 d . . . H12 H 0.9688 1.0078 0.7767 0.043 Uiso 1 1 calc R . . C21 C 0.2490(3) 0.9908(2) 0.49625(16) 0.0170(7) Uani 1 1 d . . . H21 H 0.3333 1.0018 0.5253 0.020 Uiso 1 1 calc R . . C22 C 0.2134(4) 1.0725(2) 0.48118(16) 0.0195(7) Uani 1 1 d . . . H22 H 0.2725 1.1382 0.4995 0.023 Uiso 1 1 calc R . . C23 C 0.0908(3) 1.0566(2) 0.43918(16) 0.0192(7) Uani 1 1 d . . . H23 H 0.0648 1.1116 0.4284 0.023 Uiso 1 1 calc R . . C24 C 0.0053(3) 0.9603(2) 0.41272(16) 0.0177(7) Uani 1 1 d . . . H24 H -0.0798 0.9479 0.3839 0.021 Uiso 1 1 calc R . . C25 C 0.0485(3) 0.8827(2) 0.42991(15) 0.0136(6) Uani 1 1 d . . . C26 C -0.0257(3) 0.7760(2) 0.40472(15) 0.0146(6) Uani 1 1 d . . . C27 C -0.1604(3) 0.6295(2) 0.35206(15) 0.0142(6) Uani 1 1 d . . . C28 C -0.2718(3) 0.5492(2) 0.30688(15) 0.0170(7) Uani 1 1 d . . . C29 C -0.2867(3) 0.4504(2) 0.30972(16) 0.0205(7) Uani 1 1 d . . . H29 H -0.2259 0.4342 0.3402 0.025 Uiso 1 1 calc R . . C30 C -0.3937(4) 0.3769(3) 0.26636(17) 0.0245(8) Uani 1 1 d . . . H30 H -0.4076 0.3087 0.2667 0.029 Uiso 1 1 calc R . . C31 C -0.4793(4) 0.4034(3) 0.22300(17) 0.0242(8) Uani 1 1 d . . . H31 H -0.5538 0.3541 0.1934 0.029 Uiso 1 1 calc R . . C32 C -0.4550(4) 0.5028(3) 0.22318(17) 0.0255(8) Uani 1 1 d . . . H32 H -0.5139 0.5204 0.1927 0.031 Uiso 1 1 calc R . . C41 C 0.2265(3) 0.8198(2) 0.68165(15) 0.0167(7) Uani 1 1 d . . . H41A H 0.2154 0.7995 0.7213 0.020 Uiso 1 1 calc R . . H41B H 0.3107 0.8039 0.6694 0.020 Uiso 1 1 calc R . . C42 C 0.2503(3) 0.9329(2) 0.69485(16) 0.0185(7) Uani 1 1 d . . . H42A H 0.1674 0.9500 0.7079 0.022 Uiso 1 1 calc R . . H42B H 0.2625 0.9544 0.6557 0.022 Uiso 1 1 calc R . . C43 C 0.3792(3) 0.9888(2) 0.74690(16) 0.0182(7) Uani 1 1 d . . . H43A H 0.3666 0.9668 0.7859 0.022 Uiso 1 1 calc R . . H43B H 0.4616 0.9711 0.7337 0.022 Uiso 1 1 calc R . . C44 C 0.4064(3) 1.1020(2) 0.76133(16) 0.0199(7) Uani 1 1 d . . . H44A H 0.4134 1.1232 0.7217 0.024 Uiso 1 1 calc R . . H44B H 0.3256 1.1197 0.7765 0.024 Uiso 1 1 calc R . . C45 C 0.5377(3) 1.1598(2) 0.81032(16) 0.0191(7) Uani 1 1 d . . . H45A H 0.6184 1.1416 0.7955 0.023 Uiso 1 1 calc R . . H45B H 0.5302 1.1395 0.8502 0.023 Uiso 1 1 calc R . . C46 C 0.5646(4) 1.2728(2) 0.82358(16) 0.0209(7) Uani 1 1 d . . . H46A H 0.4852 1.2910 0.8398 0.025 Uiso 1 1 calc R . . H46B H 0.5683 1.2926 0.7833 0.025 Uiso 1 1 calc R . . C47 C 0.6990(4) 1.3320(2) 0.87100(17) 0.0218(7) Uani 1 1 d . . . H47A H 0.7788 1.3145 0.8548 0.026 Uiso 1 1 calc R . . H47B H 0.6958 1.3125 0.9114 0.026 Uiso 1 1 calc R . . C48 C 0.7228(3) 1.4450(2) 0.88353(16) 0.0204(7) Uani 1 1 d . . . H48A H 0.7289 1.4642 0.8432 0.024 Uiso 1 1 calc R . . H48B H 0.6407 1.4615 0.8978 0.024 Uiso 1 1 calc R . . C49 C 0.8526(4) 1.5074(2) 0.93232(17) 0.0221(7) Uani 1 1 d . . . H49A H 0.9358 1.4942 0.9172 0.027 Uiso 1 1 calc R . . H49B H 0.8492 1.4868 0.9723 0.027 Uiso 1 1 calc R . . C50 C 0.8674(4) 1.6195(2) 0.94522(17) 0.0217(7) Uani 1 1 d . . . H50A H 0.8733 1.6403 0.9054 0.026 Uiso 1 1 calc R . . H50B H 0.7829 1.6324 0.9591 0.026 Uiso 1 1 calc R . . C51 C 0.9951(4) 1.6829(2) 0.99539(17) 0.0217(7) Uani 1 1 d . . . H51A H 1.0798 1.6739 0.9799 0.026 Uiso 1 1 calc R . . H51B H 0.9930 1.6581 1.0340 0.026 Uiso 1 1 calc R . . C52 C 1.0060(4) 1.7941(2) 1.01283(17) 0.0236(8) Uani 1 1 d . . . H52A H 1.0067 1.8192 0.9743 0.028 Uiso 1 1 calc R . . H52B H 0.9229 1.8038 1.0295 0.028 Uiso 1 1 calc R . . C53 C 1.1365(4) 1.8548(2) 1.06198(17) 0.0228(8) Uani 1 1 d . . . H53A H 1.2191 1.8437 1.0454 0.027 Uiso 1 1 calc R . . H53B H 1.1348 1.8296 1.1005 0.027 Uiso 1 1 calc R . . C54 C 1.1529(4) 1.9671(2) 1.08036(18) 0.0234(8) Uani 1 1 d . . . H54A H 1.1506 1.9924 1.0419 0.028 Uiso 1 1 calc R . . H54B H 1.0735 1.9792 1.0994 0.028 Uiso 1 1 calc R . . C55 C 1.2884(4) 2.0243(3) 1.12696(18) 0.0263(8) Uani 1 1 d . . . H55A H 1.3675 2.0134 1.1073 0.032 Uiso 1 1 calc R . . H55B H 1.2917 1.9972 1.1647 0.032 Uiso 1 1 calc R . . C56 C 1.3061(5) 2.1362(3) 1.1478(2) 0.0406(11) Uani 1 1 d . . . H56A H 1.3966 2.1690 1.1763 0.049 Uiso 1 1 calc R . . H56B H 1.2315 2.1479 1.1698 0.049 Uiso 1 1 calc R . . H56C H 1.3015 2.1635 1.1106 0.049 Uiso 1 1 calc R . . C61 C 0.3593(3) 0.5881(2) 0.35822(16) 0.0179(7) Uani 1 1 d . . . H61A H 0.4293 0.5612 0.3387 0.021 Uiso 1 1 calc R . . H61B H 0.3414 0.5566 0.3933 0.021 Uiso 1 1 calc R . . C62 C 0.2247(3) 0.5572(2) 0.30914(17) 0.0209(7) Uani 1 1 d . . . H62A H 0.2395 0.5897 0.2742 0.025 Uiso 1 1 calc R . . H62B H 0.1511 0.5790 0.3286 0.025 Uiso 1 1 calc R . . C63 C 0.1787(4) 0.4438(2) 0.28322(17) 0.0226(8) Uani 1 1 d . . . H63A H 0.2537 0.4234 0.2641 0.027 Uiso 1 1 calc R . . H63B H 0.1679 0.4126 0.3190 0.027 Uiso 1 1 calc R . . C64 C 0.0442(4) 0.4029(3) 0.23449(17) 0.0235(8) Uani 1 1 d . . . H64A H 0.0506 0.4372 0.2000 0.028 Uiso 1 1 calc R . . H64B H -0.0338 0.4161 0.2543 0.028 Uiso 1 1 calc R . . C65 C 0.0155(4) 0.2911(2) 0.20745(16) 0.0209(7) Uani 1 1 d . . . H65A H 0.0933 0.2797 0.1868 0.025 Uiso 1 1 calc R . . H65B H 0.0160 0.2587 0.2430 0.025 Uiso 1 1 calc R . . C66 C -0.1204(3) 0.2394(2) 0.15994(16) 0.0207(7) Uani 1 1 d . . . H66A H -0.1194 0.2670 0.1224 0.025 Uiso 1 1 calc R . . H66B H -0.1992 0.2528 0.1791 0.025 Uiso 1 1 calc R . . C67 C -0.1417(3) 0.1269(2) 0.13960(17) 0.0215(7) Uani 1 1 d . . . H67A H -0.0608 0.1148 0.1217 0.026 Uiso 1 1 calc R . . H67B H -0.1424 0.1005 0.1776 0.026 Uiso 1 1 calc R . . C68 C -0.2745(3) 0.0680(2) 0.09118(17) 0.0209(7) Uani 1 1 d . . . H68A H -0.3559 0.0807 0.1082 0.025 Uiso 1 1 calc R . . H68B H -0.2729 0.0919 0.0522 0.025 Uiso 1 1 calc R . . C69 C -0.2910(3) -0.0437(2) 0.07471(17) 0.0214(7) Uani 1 1 d . . . H69A H -0.2083 -0.0556 0.0586 0.026 Uiso 1 1 calc R . . H69B H -0.2927 -0.0670 0.1139 0.026 Uiso 1 1 calc R . . C70 C -0.4208(3) -0.1060(2) 0.02607(16) 0.0205(7) Uani 1 1 d . . . H70A H -0.4177 -0.0848 -0.0138 0.025 Uiso 1 1 calc R . . H70B H -0.5037 -0.0928 0.0414 0.025 Uiso 1 1 calc R . . C71 C -0.4366(4) -0.2178(3) 0.01237(18) 0.0243(8) Uani 1 1 d . . . H71A H -0.3542 -0.2308 -0.0036 0.029 Uiso 1 1 calc R . . H71B H -0.4375 -0.2384 0.0525 0.029 Uiso 1 1 calc R . . C72 C -0.5670(4) -0.2819(3) -0.03519(17) 0.0234(8) Uani 1 1 d . . . H72A H -0.5644 -0.2642 -0.0761 0.028 Uiso 1 1 calc R . . H72B H -0.6496 -0.2674 -0.0203 0.028 Uiso 1 1 calc R . . C73 C -0.5816(4) -0.3934(3) -0.04520(19) 0.0285(8) Uani 1 1 d . . . H73A H -0.4992 -0.4074 -0.0607 0.034 Uiso 1 1 calc R . . H73B H -0.5809 -0.4100 -0.0038 0.034 Uiso 1 1 calc R . . C74 C -0.7115(4) -0.4615(3) -0.0911(2) 0.0327(9) Uani 1 1 d . . . H74A H -0.7113 -0.4480 -0.1333 0.039 Uiso 1 1 calc R . . H74B H -0.7949 -0.4475 -0.0767 0.039 Uiso 1 1 calc R . . C75 C -0.7189(5) -0.5714(3) -0.0961(2) 0.0458(12) Uani 1 1 d . . . H75A H -0.6321 -0.5836 -0.1076 0.055 Uiso 1 1 calc R . . H75B H -0.7241 -0.5850 -0.0542 0.055 Uiso 1 1 calc R . . C76 C -0.8424(6) -0.6439(4) -0.1444(3) 0.0642(17) Uani 1 1 d . . . H76A H -0.9287 -0.6299 -0.1350 0.077 Uiso 1 1 calc R . . H76B H -0.8453 -0.7124 -0.1427 0.077 Uiso 1 1 calc R . . H76C H -0.8329 -0.6362 -0.1868 0.077 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 0.0127(2) 0.0076(2) 0.0175(2) 0.00222(17) 0.00051(17) 0.00356(17) S1 0.0143(4) 0.0103(4) 0.0190(4) 0.0039(3) 0.0010(3) 0.0030(3) O11 0.0212(12) 0.0138(11) 0.0163(11) 0.0038(9) 0.0041(9) 0.0070(9) O12 0.0153(11) 0.0201(12) 0.0269(13) 0.0090(10) 0.0062(10) 0.0046(10) O13 0.0292(13) 0.0066(11) 0.0312(14) 0.0073(10) -0.0006(11) 0.0056(10) S2 0.0158(4) 0.0094(4) 0.0281(5) 0.0025(3) 0.0062(3) 0.0033(3) O21 0.0176(11) 0.0116(11) 0.0242(12) 0.0047(9) 0.0067(9) 0.0055(9) O22 0.0411(16) 0.0176(13) 0.0430(16) 0.0109(12) 0.0284(13) 0.0099(12) O23 0.0174(12) 0.0124(12) 0.0431(16) -0.0023(11) -0.0030(11) 0.0036(10) N1 0.0156(13) 0.0091(13) 0.0194(14) 0.0041(11) 0.0036(11) 0.0045(11) N2 0.0157(13) 0.0073(12) 0.0214(14) 0.0028(11) 0.0024(11) 0.0035(10) N3 0.0158(14) 0.0109(13) 0.0211(15) 0.0007(11) 0.0018(11) 0.0021(11) N4 0.0191(15) 0.0302(17) 0.0225(16) 0.0019(13) -0.0014(12) 0.0038(13) N5 0.0121(13) 0.0102(13) 0.0203(14) 0.0034(11) 0.0006(11) 0.0033(10) N6 0.0183(15) 0.0211(15) 0.0333(17) 0.0098(13) -0.0025(13) 0.0083(12) N21 0.0142(13) 0.0106(13) 0.0196(14) 0.0039(11) 0.0045(11) 0.0043(11) N22 0.0170(14) 0.0062(12) 0.0226(15) 0.0014(11) 0.0005(11) 0.0025(10) N23 0.0151(13) 0.0091(13) 0.0205(14) 0.0008(11) -0.0004(11) 0.0019(10) N24 0.0188(14) 0.0176(15) 0.0217(15) 0.0037(12) -0.0032(12) 0.0046(12) N25 0.0130(13) 0.0115(13) 0.0217(14) 0.0063(11) 0.0015(11) 0.0050(11) N26 0.0190(15) 0.0163(15) 0.0374(18) 0.0077(13) -0.0050(13) 0.0087(12) C1 0.0158(16) 0.0093(15) 0.0244(18) 0.0050(13) 0.0041(13) 0.0010(12) C2 0.0257(18) 0.0108(15) 0.0236(18) 0.0044(13) 0.0070(14) 0.0040(14) C3 0.0224(17) 0.0133(16) 0.0308(19) 0.0083(14) 0.0087(15) 0.0080(14) C4 0.0173(16) 0.0144(16) 0.0250(18) 0.0069(13) 0.0044(14) 0.0076(13) C5 0.0130(15) 0.0112(15) 0.0182(16) 0.0033(12) 0.0031(12) 0.0031(12) C6 0.0150(15) 0.0124(15) 0.0170(16) 0.0027(12) 0.0037(13) 0.0041(12) C7 0.0156(16) 0.0103(15) 0.0195(16) 0.0026(12) 0.0060(13) 0.0027(12) C8 0.0147(16) 0.0214(18) 0.0177(17) 0.0002(13) 0.0047(13) 0.0030(14) C9 0.0190(17) 0.0206(18) 0.0261(19) -0.0006(14) 0.0068(14) 0.0029(14) C10 0.029(2) 0.0187(19) 0.034(2) -0.0059(16) 0.0094(17) -0.0044(16) C11 0.029(2) 0.033(2) 0.031(2) -0.0088(18) 0.0007(17) -0.0096(18) C12 0.0219(19) 0.046(3) 0.027(2) 0.0008(18) -0.0069(16) 0.0015(18) C21 0.0168(16) 0.0090(15) 0.0240(17) 0.0025(13) 0.0037(13) 0.0028(12) C22 0.0239(18) 0.0085(15) 0.0273(19) 0.0048(13) 0.0084(14) 0.0047(13) C23 0.0242(18) 0.0121(16) 0.0268(18) 0.0085(13) 0.0098(14) 0.0094(14) C24 0.0170(16) 0.0161(16) 0.0223(17) 0.0068(13) 0.0039(13) 0.0071(13) C25 0.0138(15) 0.0106(15) 0.0178(16) 0.0043(12) 0.0053(12) 0.0042(12) C26 0.0132(15) 0.0126(15) 0.0179(16) 0.0026(12) 0.0043(12) 0.0040(12) C27 0.0159(15) 0.0099(15) 0.0172(16) 0.0044(12) 0.0026(13) 0.0037(12) C28 0.0143(16) 0.0175(17) 0.0187(17) 0.0053(13) 0.0043(13) 0.0027(13) C29 0.0207(17) 0.0160(17) 0.0232(18) 0.0054(14) -0.0004(14) 0.0048(14) C30 0.0248(18) 0.0161(17) 0.030(2) 0.0043(15) 0.0010(15) 0.0037(14) C31 0.0201(17) 0.0198(18) 0.0255(19) -0.0008(14) -0.0023(14) 0.0015(14) C32 0.0248(19) 0.0245(19) 0.0235(19) 0.0052(15) -0.0045(15) 0.0061(15) C41 0.0180(16) 0.0140(16) 0.0171(16) 0.0039(13) 0.0008(13) 0.0040(13) C42 0.0199(17) 0.0129(16) 0.0216(17) 0.0037(13) 0.0026(14) 0.0038(13) C43 0.0208(17) 0.0119(16) 0.0190(17) 0.0026(13) 0.0015(13) 0.0019(13) C44 0.0220(17) 0.0118(16) 0.0237(18) 0.0045(13) 0.0001(14) 0.0028(13) C45 0.0197(17) 0.0119(16) 0.0223(18) 0.0027(13) 0.0024(14) 0.0002(13) C46 0.0225(17) 0.0118(16) 0.0237(18) 0.0013(13) -0.0030(14) 0.0028(13) C47 0.0206(17) 0.0156(17) 0.0268(19) 0.0045(14) 0.0000(14) 0.0043(14) C48 0.0185(17) 0.0168(17) 0.0230(18) 0.0033(14) -0.0021(14) 0.0046(14) C49 0.0198(17) 0.0166(17) 0.0275(19) 0.0030(14) -0.0002(14) 0.0054(14) C50 0.0202(17) 0.0154(17) 0.0273(19) 0.0029(14) 0.0005(14) 0.0058(14) C51 0.0216(17) 0.0143(17) 0.0266(19) 0.0028(14) 0.0006(14) 0.0045(14) C52 0.0236(18) 0.0137(17) 0.031(2) 0.0016(14) 0.0017(15) 0.0069(14) C53 0.0228(18) 0.0151(17) 0.0253(19) -0.0009(14) 0.0010(15) 0.0030(14) C54 0.0246(18) 0.0118(16) 0.032(2) 0.0026(14) 0.0037(15) 0.0056(14) C55 0.0243(19) 0.0141(17) 0.034(2) -0.0033(15) 0.0033(16) 0.0027(14) C56 0.042(2) 0.017(2) 0.053(3) -0.0035(18) 0.000(2) 0.0070(18) C61 0.0206(17) 0.0054(14) 0.0266(18) 0.0019(13) 0.0070(14) 0.0023(12) C62 0.0204(17) 0.0130(16) 0.0272(19) 0.0030(14) 0.0030(14) 0.0034(14) C63 0.0230(18) 0.0141(17) 0.0272(19) 0.0002(14) 0.0025(15) 0.0044(14) C64 0.0222(18) 0.0162(17) 0.029(2) 0.0008(14) 0.0046(15) 0.0037(14) C65 0.0230(18) 0.0152(17) 0.0213(18) 0.0027(14) 0.0020(14) 0.0028(14) C66 0.0202(17) 0.0164(17) 0.0241(18) 0.0037(14) 0.0029(14) 0.0051(14) C67 0.0202(17) 0.0150(17) 0.0254(19) 0.0021(14) 0.0003(14) 0.0028(14) C68 0.0178(17) 0.0175(17) 0.0250(18) 0.0036(14) 0.0021(14) 0.0030(14) C69 0.0187(17) 0.0160(17) 0.0262(19) 0.0034(14) 0.0007(14) 0.0026(14) C70 0.0219(17) 0.0149(16) 0.0230(18) 0.0028(14) 0.0023(14) 0.0051(14) C71 0.0195(17) 0.0187(18) 0.031(2) 0.0023(15) 0.0026(15) 0.0039(14) C72 0.0216(18) 0.0171(17) 0.0280(19) -0.0002(14) 0.0032(15) 0.0048(14) C73 0.0250(19) 0.0183(18) 0.040(2) 0.0000(16) 0.0085(17) 0.0063(15) C74 0.029(2) 0.0204(19) 0.039(2) -0.0061(16) 0.0113(17) -0.0018(16) C75 0.048(3) 0.021(2) 0.056(3) -0.008(2) 0.024(2) -0.0056(19) C76 0.064(3) 0.038(3) 0.061(3) -0.019(2) 0.028(3) -0.021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O11 2.096(2) . y Fe1 O21 2.101(2) . y Fe1 N2 2.123(3) . y Fe1 N22 2.134(3) . y Fe1 N1 2.197(3) . y Fe1 N21 2.198(3) . y S1 O13 1.452(2) . ? S1 O12 1.453(2) . ? S1 O11 1.478(2) . ? S1 C41 1.781(3) . ? S2 O22 1.447(3) . ? S2 O23 1.449(3) . ? S2 O21 1.474(2) . ? S2 C61 1.776(3) . ? N1 C1 1.346(4) . ? N1 C5 1.351(4) . ? N2 C6 1.335(4) . ? N2 N3 1.369(4) . ? N3 C7 1.312(4) . ? N4 C12 1.340(5) . ? N4 C8 1.341(4) . ? N5 C6 1.357(4) . ? N5 C7 1.389(4) . ? N5 N6 1.420(4) . ? N6 H6X 0.9538 . ? N6 H6Y 0.9514 . ? N21 C21 1.343(4) . ? N21 C25 1.352(4) . ? N22 C26 1.323(4) . ? N22 N23 1.369(4) . ? N23 C27 1.315(4) . ? N24 C32 1.340(4) . ? N24 C28 1.342(4) . ? N25 C26 1.355(4) . ? N25 C27 1.377(4) . ? N25 N26 1.422(4) . ? N26 H26X 0.9197 . ? N26 H26Y 0.9227 . ? C1 C2 1.392(4) . ? C1 H1 0.9500 . ? C2 C3 1.378(5) . ? C2 H2 0.9500 . ? C3 C4 1.399(5) . ? C3 H3 0.9500 . ? C4 C5 1.391(4) . ? C4 H4 0.9500 . ? C5 C6 1.475(4) . ? C7 C8 1.465(4) . ? C8 C9 1.400(5) . ? C9 C10 1.386(5) . ? C9 H9 0.9500 . ? C10 C11 1.385(6) . ? C10 H10 0.9500 . ? C11 C12 1.390(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C21 C22 1.390(4) . ? C21 H21 0.9500 . ? C22 C23 1.379(5) . ? C22 H22 0.9500 . ? C23 C24 1.388(5) . ? C23 H23 0.9500 . ? C24 C25 1.387(4) . ? C24 H24 0.9500 . ? C25 C26 1.472(4) . ? C27 C28 1.470(4) . ? C28 C29 1.396(5) . ? C29 C30 1.389(5) . ? C29 H29 0.9500 . ? C30 C31 1.374(5) . ? C30 H30 0.9500 . ? C31 C32 1.379(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C41 C42 1.530(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.533(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.528(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.519(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.527(4) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.528(5) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.530(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.521(5) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.531(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.526(5) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.526(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.523(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.531(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.521(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.524(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C61 C62 1.522(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.529(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.514(5) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.522(4) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.522(5) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.527(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.526(4) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.522(5) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.519(4) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.525(5) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.518(5) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.527(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.514(5) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.531(6) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.519(6) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 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 O11 Fe1 O21 174.64(9) . . y O11 Fe1 N2 90.33(10) . . y O21 Fe1 N2 91.57(10) . . y O11 Fe1 N22 90.63(10) . . y O21 Fe1 N22 87.47(10) . . y N2 Fe1 N22 179.03(11) . . y O11 Fe1 N1 94.66(9) . . y O21 Fe1 N1 90.66(9) . . y N2 Fe1 N1 75.91(10) . . y N22 Fe1 N1 104.20(10) . . y O11 Fe1 N21 86.40(9) . . y O21 Fe1 N21 88.27(9) . . y N2 Fe1 N21 104.35(10) . . y N22 Fe1 N21 75.52(10) . . y N1 Fe1 N21 178.91(10) . . y O13 S1 O12 115.07(15) . . ? O13 S1 O11 112.52(14) . . ? O12 S1 O11 110.01(13) . . ? O13 S1 C41 106.06(15) . . ? O12 S1 C41 106.73(15) . . ? O11 S1 C41 105.79(15) . . ? S1 O11 Fe1 141.51(14) . . ? O22 S2 O23 113.68(17) . . ? O22 S2 O21 110.83(14) . . ? O23 S2 O21 112.85(14) . . ? O22 S2 C61 107.23(16) . . ? O23 S2 C61 105.48(15) . . ? O21 S2 C61 106.17(14) . . ? S2 O21 Fe1 143.93(15) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Fe1 125.3(2) . . ? C5 N1 Fe1 116.5(2) . . ? C6 N2 N3 108.7(3) . . ? C6 N2 Fe1 115.1(2) . . ? N3 N2 Fe1 136.3(2) . . ? C7 N3 N2 107.4(3) . . ? C12 N4 C8 116.9(3) . . ? C6 N5 C7 105.6(3) . . ? C6 N5 N6 125.1(3) . . ? C7 N5 N6 129.3(3) . . ? N5 N6 H6X 103.0 . . ? N5 N6 H6Y 103.9 . . ? H6X N6 H6Y 104.9 . . ? C21 N21 C25 118.1(3) . . ? C21 N21 Fe1 125.1(2) . . ? C25 N21 Fe1 116.8(2) . . ? C26 N22 N23 109.1(3) . . ? C26 N22 Fe1 115.0(2) . . ? N23 N22 Fe1 135.8(2) . . ? C27 N23 N22 106.5(3) . . ? C32 N24 C28 116.9(3) . . ? C26 N25 C27 105.6(2) . . ? C26 N25 N26 124.7(3) . . ? C27 N25 N26 129.7(3) . . ? N25 N26 H26X 101.2 . . ? N25 N26 H26Y 107.0 . . ? H26X N26 H26Y 104.8 . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 117.9(3) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 123.1(3) . . ? N1 C5 C6 112.0(3) . . ? C4 C5 C6 124.9(3) . . ? N2 C6 N5 108.7(3) . . ? N2 C6 C5 120.3(3) . . ? N5 C6 C5 130.9(3) . . ? N3 C7 N5 109.7(3) . . ? N3 C7 C8 124.2(3) . . ? N5 C7 C8 126.1(3) . . ? N4 C8 C9 124.3(3) . . ? N4 C8 C7 117.4(3) . . ? C9 C8 C7 118.3(3) . . ? C10 C9 C8 117.3(4) . . ? C10 C9 H9 121.4 . . ? C8 C9 H9 121.4 . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 118.9(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? N4 C12 C11 123.2(4) . . ? N4 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? N21 C21 C22 122.2(3) . . ? N21 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 118.9(3) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 117.6(3) . . ? C25 C24 H24 121.2 . . ? C23 C24 H24 121.2 . . ? N21 C25 C24 123.2(3) . . ? N21 C25 C26 111.7(3) . . ? C24 C25 C26 125.1(3) . . ? N22 C26 N25 108.7(3) . . ? N22 C26 C25 120.9(3) . . ? N25 C26 C25 130.4(3) . . ? N23 C27 N25 110.0(3) . . ? N23 C27 C28 124.0(3) . . ? N25 C27 C28 126.0(3) . . ? N24 C28 C29 123.7(3) . . ? N24 C28 C27 117.0(3) . . ? C29 C28 C27 119.4(3) . . ? C30 C29 C28 117.5(3) . . ? C30 C29 H29 121.2 . . ? C28 C29 H29 121.2 . . ? C31 C30 C29 119.5(3) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 118.8(3) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N24 C32 C31 123.6(3) . . ? N24 C32 H32 118.2 . . ? C31 C32 H32 118.2 . . ? C42 C41 S1 115.0(2) . . ? C42 C41 H41A 108.5 . . ? S1 C41 H41A 108.5 . . ? C42 C41 H41B 108.5 . . ? S1 C41 H41B 108.5 . . ? H41A C41 H41B 107.5 . . ? C41 C42 C43 111.3(3) . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C44 C43 C42 112.8(3) . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? C42 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C45 C44 C43 114.0(3) . . ? C45 C44 H44A 108.7 . . ? C43 C44 H44A 108.7 . . ? C45 C44 H44B 108.7 . . ? C43 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? C44 C45 C46 113.5(3) . . ? C44 C45 H45A 108.9 . . ? C46 C45 H45A 108.9 . . ? C44 C45 H45B 108.9 . . ? C46 C45 H45B 108.9 . . ? H45A C45 H45B 107.7 . . ? C45 C46 C47 114.1(3) . . ? C45 C46 H46A 108.7 . . ? C47 C46 H46A 108.7 . . ? C45 C46 H46B 108.7 . . ? C47 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? C46 C47 C48 112.9(3) . . ? C46 C47 H47A 109.0 . . ? C48 C47 H47A 109.0 . . ? C46 C47 H47B 109.0 . . ? C48 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? C49 C48 C47 115.0(3) . . ? C49 C48 H48A 108.5 . . ? C47 C48 H48A 108.5 . . ? C49 C48 H48B 108.5 . . ? C47 C48 H48B 108.5 . . ? H48A C48 H48B 107.5 . . ? C48 C49 C50 112.7(3) . . ? C48 C49 H49A 109.0 . . ? C50 C49 H49A 109.0 . . ? C48 C49 H49B 109.0 . . ? C50 C49 H49B 109.0 . . ? H49A C49 H49B 107.8 . . ? C51 C50 C49 113.3(3) . . ? C51 C50 H50A 108.9 . . ? C49 C50 H50A 108.9 . . ? C51 C50 H50B 108.9 . . ? C49 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C50 C51 C52 114.3(3) . . ? C50 C51 H51A 108.7 . . ? C52 C51 H51A 108.7 . . ? C50 C51 H51B 108.7 . . ? C52 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C53 C52 C51 112.5(3) . . ? C53 C52 H52A 109.1 . . ? C51 C52 H52A 109.1 . . ? C53 C52 H52B 109.1 . . ? C51 C52 H52B 109.1 . . ? H52A C52 H52B 107.8 . . ? C52 C53 C54 114.4(3) . . ? C52 C53 H53A 108.7 . . ? C54 C53 H53A 108.7 . . ? C52 C53 H53B 108.7 . . ? C54 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C55 C54 C53 112.0(3) . . ? C55 C54 H54A 109.2 . . ? C53 C54 H54A 109.2 . . ? C55 C54 H54B 109.2 . . ? C53 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? C54 C55 C56 113.4(3) . . ? C54 C55 H55A 108.9 . . ? C56 C55 H55A 108.9 . . ? C54 C55 H55B 108.9 . . ? C56 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C62 C61 S2 115.5(2) . . ? C62 C61 H61A 108.4 . . ? S2 C61 H61A 108.4 . . ? C62 C61 H61B 108.4 . . ? S2 C61 H61B 108.4 . . ? H61A C61 H61B 107.5 . . ? C61 C62 C63 109.7(3) . . ? C61 C62 H62A 109.7 . . ? C63 C62 H62A 109.7 . . ? C61 C62 H62B 109.7 . . ? C63 C62 H62B 109.7 . . ? H62A C62 H62B 108.2 . . ? C64 C63 C62 115.1(3) . . ? C64 C63 H63A 108.5 . . ? C62 C63 H63A 108.5 . . ? C64 C63 H63B 108.5 . . ? C62 C63 H63B 108.5 . . ? H63A C63 H63B 107.5 . . ? C63 C64 C65 110.6(3) . . ? C63 C64 H64A 109.5 . . ? C65 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? C66 C65 C64 116.1(3) . . ? C66 C65 H65A 108.3 . . ? C64 C65 H65A 108.3 . . ? C66 C65 H65B 108.3 . . ? C64 C65 H65B 108.3 . . ? H65A C65 H65B 107.4 . . ? C65 C66 C67 111.1(3) . . ? C65 C66 H66A 109.4 . . ? C67 C66 H66A 109.4 . . ? C65 C66 H66B 109.4 . . ? C67 C66 H66B 109.4 . . ? H66A C66 H66B 108.0 . . ? C68 C67 C66 115.3(3) . . ? C68 C67 H67A 108.4 . . ? C66 C67 H67A 108.4 . . ? C68 C67 H67B 108.4 . . ? C66 C67 H67B 108.4 . . ? H67A C67 H67B 107.5 . . ? C69 C68 C67 112.5(3) . . ? C69 C68 H68A 109.1 . . ? C67 C68 H68A 109.1 . . ? C69 C68 H68B 109.1 . . ? C67 C68 H68B 109.1 . . ? H68A C68 H68B 107.8 . . ? C70 C69 C68 114.8(3) . . ? C70 C69 H69A 108.6 . . ? C68 C69 H69A 108.6 . . ? C70 C69 H69B 108.6 . . ? C68 C69 H69B 108.6 . . ? H69A C69 H69B 107.6 . . ? C69 C70 C71 113.4(3) . . ? C69 C70 H70A 108.9 . . ? C71 C70 H70A 108.9 . . ? C69 C70 H70B 108.9 . . ? C71 C70 H70B 108.9 . . ? H70A C70 H70B 107.7 . . ? C72 C71 C70 114.4(3) . . ? C72 C71 H71A 108.7 . . ? C70 C71 H71A 108.7 . . ? C72 C71 H71B 108.7 . . ? C70 C71 H71B 108.7 . . ? H71A C71 H71B 107.6 . . ? C71 C72 C73 112.5(3) . . ? C71 C72 H72A 109.1 . . ? C73 C72 H72A 109.1 . . ? C71 C72 H72B 109.1 . . ? C73 C72 H72B 109.1 . . ? H72A C72 H72B 107.8 . . ? C74 C73 C72 115.1(3) . . ? C74 C73 H73A 108.5 . . ? C72 C73 H73A 108.5 . . ? C74 C73 H73B 108.5 . . ? C72 C73 H73B 108.5 . . ? H73A C73 H73B 107.5 . . ? C73 C74 C75 111.1(4) . . ? C73 C74 H74A 109.4 . . ? C75 C74 H74A 109.4 . . ? C73 C74 H74B 109.4 . . ? C75 C74 H74B 109.4 . . ? H74A C74 H74B 108.0 . . ? C76 C75 C74 113.8(4) . . ? C76 C75 H75A 108.8 . . ? C74 C75 H75A 108.8 . . ? C76 C75 H75B 108.8 . . ? C74 C75 H75B 108.8 . . ? H75A C75 H75B 107.7 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 S1 O11 Fe1 -36.5(3) . . . . ? O12 S1 O11 Fe1 -166.2(2) . . . . ? C41 S1 O11 Fe1 78.8(2) . . . . ? O21 Fe1 O11 S1 -170.4(8) . . . . ? N2 Fe1 O11 S1 -59.7(2) . . . . ? N22 Fe1 O11 S1 120.5(2) . . . . ? N1 Fe1 O11 S1 16.2(2) . . . . ? N21 Fe1 O11 S1 -164.1(2) . . . . ? O22 S2 O21 Fe1 -168.2(2) . . . . ? O23 S2 O21 Fe1 -39.4(3) . . . . ? C61 S2 O21 Fe1 75.7(3) . . . . ? O11 Fe1 O21 S2 161.7(8) . . . . ? N2 Fe1 O21 S2 51.1(2) . . . . ? N22 Fe1 O21 S2 -129.0(2) . . . . ? N1 Fe1 O21 S2 -24.8(2) . . . . ? N21 Fe1 O21 S2 155.4(2) . . . . ? O11 Fe1 N1 C1 87.9(3) . . . . ? O21 Fe1 N1 C1 -91.5(3) . . . . ? N2 Fe1 N1 C1 177.1(3) . . . . ? N22 Fe1 N1 C1 -3.9(3) . . . . ? N21 Fe1 N1 C1 -79(5) . . . . ? O11 Fe1 N1 C5 -92.4(2) . . . . ? O21 Fe1 N1 C5 88.2(2) . . . . ? N2 Fe1 N1 C5 -3.3(2) . . . . ? N22 Fe1 N1 C5 175.7(2) . . . . ? N21 Fe1 N1 C5 101(5) . . . . ? O11 Fe1 N2 C6 97.6(2) . . . . ? O21 Fe1 N2 C6 -87.4(2) . . . . ? N22 Fe1 N2 C6 -94(6) . . . . ? N1 Fe1 N2 C6 2.9(2) . . . . ? N21 Fe1 N2 C6 -176.1(2) . . . . ? O11 Fe1 N2 N3 -80.8(3) . . . . ? O21 Fe1 N2 N3 94.2(3) . . . . ? N22 Fe1 N2 N3 88(6) . . . . ? N1 Fe1 N2 N3 -175.5(3) . . . . ? N21 Fe1 N2 N3 5.6(3) . . . . ? C6 N2 N3 C7 1.0(4) . . . . ? Fe1 N2 N3 C7 179.4(2) . . . . ? O11 Fe1 N21 C21 91.2(3) . . . . ? O21 Fe1 N21 C21 -89.4(3) . . . . ? N2 Fe1 N21 C21 1.8(3) . . . . ? N22 Fe1 N21 C21 -177.2(3) . . . . ? N1 Fe1 N21 C21 -102(5) . . . . ? O11 Fe1 N21 C25 -89.2(2) . . . . ? O21 Fe1 N21 C25 90.2(2) . . . . ? N2 Fe1 N21 C25 -178.6(2) . . . . ? N22 Fe1 N21 C25 2.4(2) . . . . ? N1 Fe1 N21 C25 78(5) . . . . ? O11 Fe1 N22 C26 83.6(2) . . . . ? O21 Fe1 N22 C26 -91.4(2) . . . . ? N2 Fe1 N22 C26 -85(6) . . . . ? N1 Fe1 N22 C26 178.5(2) . . . . ? N21 Fe1 N22 C26 -2.6(2) . . . . ? O11 Fe1 N22 N23 -98.9(3) . . . . ? O21 Fe1 N22 N23 86.1(3) . . . . ? N2 Fe1 N22 N23 92(6) . . . . ? N1 Fe1 N22 N23 -4.0(3) . . . . ? N21 Fe1 N22 N23 174.9(3) . . . . ? C26 N22 N23 C27 -1.3(4) . . . . ? Fe1 N22 N23 C27 -178.9(2) . . . . ? C5 N1 C1 C2 -0.8(5) . . . . ? Fe1 N1 C1 C2 178.8(2) . . . . ? N1 C1 C2 C3 -0.2(5) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C1 N1 C5 C4 1.5(5) . . . . ? Fe1 N1 C5 C4 -178.2(2) . . . . ? C1 N1 C5 C6 -177.3(3) . . . . ? Fe1 N1 C5 C6 3.0(3) . . . . ? C3 C4 C5 N1 -1.2(5) . . . . ? C3 C4 C5 C6 177.5(3) . . . . ? N3 N2 C6 N5 -1.4(4) . . . . ? Fe1 N2 C6 N5 179.8(2) . . . . ? N3 N2 C6 C5 176.5(3) . . . . ? Fe1 N2 C6 C5 -2.3(4) . . . . ? C7 N5 C6 N2 1.2(4) . . . . ? N6 N5 C6 N2 -179.7(3) . . . . ? C7 N5 C6 C5 -176.3(3) . . . . ? N6 N5 C6 C5 2.8(5) . . . . ? N1 C5 C6 N2 -0.5(4) . . . . ? C4 C5 C6 N2 -179.3(3) . . . . ? N1 C5 C6 N5 176.8(3) . . . . ? C4 C5 C6 N5 -2.0(6) . . . . ? N2 N3 C7 N5 -0.2(4) . . . . ? N2 N3 C7 C8 -179.5(3) . . . . ? C6 N5 C7 N3 -0.6(4) . . . . ? N6 N5 C7 N3 -179.7(3) . . . . ? C6 N5 C7 C8 178.6(3) . . . . ? N6 N5 C7 C8 -0.5(5) . . . . ? C12 N4 C8 C9 -2.6(5) . . . . ? C12 N4 C8 C7 177.4(3) . . . . ? N3 C7 C8 N4 170.4(3) . . . . ? N5 C7 C8 N4 -8.7(5) . . . . ? N3 C7 C8 C9 -9.6(5) . . . . ? N5 C7 C8 C9 171.3(3) . . . . ? N4 C8 C9 C10 1.8(5) . . . . ? C7 C8 C9 C10 -178.2(3) . . . . ? C8 C9 C10 C11 0.6(5) . . . . ? C9 C10 C11 C12 -1.9(6) . . . . ? C8 N4 C12 C11 1.1(6) . . . . ? C10 C11 C12 N4 1.1(6) . . . . ? C25 N21 C21 C22 0.0(5) . . . . ? Fe1 N21 C21 C22 179.6(2) . . . . ? N21 C21 C22 C23 0.2(5) . . . . ? C21 C22 C23 C24 0.0(5) . . . . ? C22 C23 C24 C25 -0.3(5) . . . . ? C21 N21 C25 C24 -0.4(5) . . . . ? Fe1 N21 C25 C24 180.0(2) . . . . ? C21 N21 C25 C26 177.8(3) . . . . ? Fe1 N21 C25 C26 -1.8(3) . . . . ? C23 C24 C25 N21 0.6(5) . . . . ? C23 C24 C25 C26 -177.4(3) . . . . ? N23 N22 C26 N25 2.1(4) . . . . ? Fe1 N22 C26 N25 -179.8(2) . . . . ? N23 N22 C26 C25 -175.5(3) . . . . ? Fe1 N22 C26 C25 2.6(4) . . . . ? C27 N25 C26 N22 -2.0(4) . . . . ? N26 N25 C26 N22 178.0(3) . . . . ? C27 N25 C26 C25 175.3(3) . . . . ? N26 N25 C26 C25 -4.7(5) . . . . ? N21 C25 C26 N22 -0.5(4) . . . . ? C24 C25 C26 N22 177.7(3) . . . . ? N21 C25 C26 N25 -177.6(3) . . . . ? C24 C25 C26 N25 0.6(6) . . . . ? N22 N23 C27 N25 0.1(4) . . . . ? N22 N23 C27 C28 178.4(3) . . . . ? C26 N25 C27 N23 1.2(4) . . . . ? N26 N25 C27 N23 -178.8(3) . . . . ? C26 N25 C27 C28 -177.1(3) . . . . ? N26 N25 C27 C28 3.0(5) . . . . ? C32 N24 C28 C29 1.6(5) . . . . ? C32 N24 C28 C27 -179.5(3) . . . . ? N23 C27 C28 N24 -166.8(3) . . . . ? N25 C27 C28 N24 11.3(5) . . . . ? N23 C27 C28 C29 12.1(5) . . . . ? N25 C27 C28 C29 -169.8(3) . . . . ? N24 C28 C29 C30 -1.4(5) . . . . ? C27 C28 C29 C30 179.7(3) . . . . ? C28 C29 C30 C31 0.1(5) . . . . ? C29 C30 C31 C32 1.0(6) . . . . ? C28 N24 C32 C31 -0.4(5) . . . . ? C30 C31 C32 N24 -0.8(6) . . . . ? O13 S1 C41 C42 178.6(2) . . . . ? O12 S1 C41 C42 -58.2(3) . . . . ? O11 S1 C41 C42 58.9(3) . . . . ? S1 C41 C42 C43 -179.8(2) . . . . ? C41 C42 C43 C44 179.9(3) . . . . ? C42 C43 C44 C45 -177.0(3) . . . . ? C43 C44 C45 C46 179.2(3) . . . . ? C44 C45 C46 C47 -177.9(3) . . . . ? C45 C46 C47 C48 -179.8(3) . . . . ? C46 C47 C48 C49 177.8(3) . . . . ? C47 C48 C49 C50 -177.3(3) . . . . ? C48 C49 C50 C51 178.4(3) . . . . ? C49 C50 C51 C52 -175.4(3) . . . . ? C50 C51 C52 C53 -178.8(3) . . . . ? C51 C52 C53 C54 179.3(3) . . . . ? C52 C53 C54 C55 -177.1(3) . . . . ? C53 C54 C55 C56 -178.3(3) . . . . ? O22 S2 C61 C62 -63.0(3) . . . . ? O23 S2 C61 C62 175.5(3) . . . . ? O21 S2 C61 C62 55.5(3) . . . . ? S2 C61 C62 C63 177.0(2) . . . . ? C61 C62 C63 C64 179.0(3) . . . . ? C62 C63 C64 C65 174.6(3) . . . . ? C63 C64 C65 C66 177.3(3) . . . . ? C64 C65 C66 C67 -176.3(3) . . . . ? C65 C66 C67 C68 -179.2(3) . . . . ? C66 C67 C68 C69 -178.2(3) . . . . ? C67 C68 C69 C70 -179.3(3) . . . . ? C68 C69 C70 C71 -178.0(3) . . . . ? C69 C70 C71 C72 178.9(3) . . . . ? C70 C71 C72 C73 -177.5(3) . . . . ? C71 C72 C73 C74 178.7(3) . . . . ? C72 C73 C74 C75 -178.1(3) . . . . ? C73 C74 C75 C76 -176.5(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 N6 H6X O12 0.95 2.12 2.885(4) 136.6 1_655 N6 H6Y N4 0.95 2.17 2.870(4) 129.5 . N26 H26X N24 0.92 2.11 2.875(4) 139.6 . N26 H26Y O22 0.92 2.27 2.998(4) 136.0 1_455 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.494 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.084 # Attachment 'nw646.cif' data_nw646 _database_code_depnum_ccdc_archive 'CCDC 741108' #TrackingRef 'nw646.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59.33 H99.33 Co N12 O9.33 S2' _chemical_formula_weight 1253.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.467(6) _cell_length_b 15.060(4) _cell_length_c 26.051(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.714(12) _cell_angle_gamma 90.00 _cell_volume 9901(4) _cell_formula_units_Z 6 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8288 _cell_measurement_theta_min 2.324 _cell_measurement_theta_max 26.649 _exptl_crystal_description block _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4038 _exptl_absorpt_coefficient_mu 0.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.877 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 234885 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.81 _diffrn_reflns_theta_max 26.63 _reflns_number_total 20632 _reflns_number_gt 14306 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. One and a half [CoII(adpt)2(CH3OH)2](C16SO3)2 complexes and two methanol solvents of crystallisation in the asymmetric unit. All non-H ANIS. All H's calc and ride with U = 1.2 times attached atom except N-H and O-H's, which were found in the map and AFIX01'ed. No disorder present, no restraints used. ; _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^)+(0.0481P)^2^+5.3528P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20632 _refine_ls_number_parameters 1140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.152891(9) 0.496969(16) 0.524316(9) 0.01421(7) Uani 1 1 d . . . N1 N -0.08392(6) 0.57214(10) 0.51226(6) 0.0166(3) Uani 1 1 d . . . C1 C -0.03716(7) 0.56994(12) 0.54254(7) 0.0198(4) Uani 1 1 d . . . H1 H -0.0343 0.5373 0.5740 0.024 Uiso 1 1 calc R . . C2 C 0.00735(7) 0.61362(13) 0.52971(8) 0.0221(4) Uani 1 1 d . . . H2 H 0.0399 0.6119 0.5522 0.027 Uiso 1 1 calc R . . C3 C 0.00319(7) 0.65967(13) 0.48349(8) 0.0234(4) Uani 1 1 d . . . H3 H 0.0334 0.6882 0.4733 0.028 Uiso 1 1 calc R . . C4 C -0.04510(7) 0.66419(13) 0.45201(8) 0.0216(4) Uani 1 1 d . . . H4 H -0.0487 0.6962 0.4203 0.026 Uiso 1 1 calc R . . C5 C -0.08820(7) 0.62060(12) 0.46798(7) 0.0164(4) Uani 1 1 d . . . C6 C -0.14275(7) 0.62068(12) 0.44115(7) 0.0148(4) Uani 1 1 d . . . N2 N -0.18057(6) 0.57933(10) 0.46188(6) 0.0157(3) Uani 1 1 d . . . N3 N -0.22735(6) 0.58721(10) 0.42913(6) 0.0165(3) Uani 1 1 d . . . C7 C -0.21613(7) 0.63242(12) 0.38865(7) 0.0153(4) Uani 1 1 d . . . C8 C -0.25459(7) 0.65381(12) 0.34327(7) 0.0166(4) Uani 1 1 d . . . C9 C -0.30253(7) 0.60822(12) 0.33507(7) 0.0189(4) Uani 1 1 d . . . H9 H -0.3107 0.5639 0.3587 0.023 Uiso 1 1 calc R . . C10 C -0.33797(7) 0.62893(13) 0.29168(8) 0.0231(4) Uani 1 1 d . . . H12 H -0.3710 0.5989 0.2847 0.028 Uiso 1 1 calc R . . C11 C -0.32424(8) 0.69460(13) 0.25852(7) 0.0234(4) Uani 1 1 d . . . H11 H -0.3477 0.7100 0.2283 0.028 Uiso 1 1 calc R . . C12 C -0.27594(7) 0.73738(13) 0.26999(7) 0.0220(4) Uani 1 1 d . . . H10 H -0.2671 0.7825 0.2471 0.026 Uiso 1 1 calc R . . N4 N -0.24108(6) 0.71831(10) 0.31178(6) 0.0187(3) Uani 1 1 d . . . N5 N -0.16351(6) 0.65616(10) 0.39543(6) 0.0155(3) Uani 1 1 d . . . N6 N -0.13407(6) 0.70337(11) 0.36155(6) 0.0210(4) Uani 1 1 d . . . H6X H -0.1615 0.7348 0.3389 0.025 Uiso 1 1 d . . . H6Y H -0.1231 0.6597 0.3420 0.025 Uiso 1 1 d . . . N21 N -0.22115(6) 0.42159(10) 0.53877(6) 0.0158(3) Uani 1 1 d . . . C21 C -0.26871(7) 0.42268(12) 0.50981(7) 0.0185(4) Uani 1 1 d . . . H21 H -0.2733 0.4574 0.4791 0.022 Uiso 1 1 calc R . . C22 C -0.31161(7) 0.37512(13) 0.52293(7) 0.0213(4) Uani 1 1 d . . . H22 H -0.3448 0.3768 0.5014 0.026 Uiso 1 1 calc R . . C23 C -0.30520(7) 0.32518(13) 0.56788(7) 0.0216(4) Uani 1 1 d . . . H23 H -0.3341 0.2924 0.5777 0.026 Uiso 1 1 calc R . . C24 C -0.25619(7) 0.32321(12) 0.59853(7) 0.0195(4) Uani 1 1 d . . . H24 H -0.2510 0.2895 0.6296 0.023 Uiso 1 1 calc R . . C25 C -0.21500(7) 0.37173(12) 0.58253(7) 0.0165(4) Uani 1 1 d . . . C26 C -0.16020(7) 0.37405(12) 0.60844(7) 0.0151(4) Uani 1 1 d . . . N22 N -0.12279(6) 0.41403(10) 0.58632(6) 0.0164(3) Uani 1 1 d . . . N23 N -0.07535(6) 0.40552(10) 0.61802(6) 0.0178(3) Uani 1 1 d . . . C27 C -0.08558(7) 0.36122(12) 0.65925(7) 0.0158(4) Uani 1 1 d . . . C28 C -0.04583(7) 0.33631(13) 0.70314(7) 0.0189(4) Uani 1 1 d . . . C29 C 0.00169(7) 0.38275(14) 0.71259(7) 0.0233(4) Uani 1 1 d . . . H29 H 0.0088 0.4317 0.6916 0.028 Uiso 1 1 calc R . . C30 C 0.03836(8) 0.35521(15) 0.75375(8) 0.0281(5) Uani 1 1 d . . . H30 H 0.0713 0.3851 0.7615 0.034 Uiso 1 1 calc R . . C31 C 0.02644(8) 0.28374(15) 0.78344(8) 0.0272(5) Uani 1 1 d . . . H31 H 0.0511 0.2638 0.8117 0.033 Uiso 1 1 calc R . . C32 C -0.02204(8) 0.24167(14) 0.77138(7) 0.0254(4) Uani 1 1 d . . . H32 H -0.0301 0.1930 0.7922 0.030 Uiso 1 1 calc R . . N24 N -0.05808(6) 0.26654(11) 0.73181(6) 0.0215(4) Uani 1 1 d . . . N25 N -0.13845(6) 0.33984(10) 0.65422(6) 0.0157(3) Uani 1 1 d . . . N26 N -0.16745(6) 0.29838(11) 0.69070(6) 0.0224(4) Uani 1 1 d . . . H26X H -0.1783 0.3428 0.7105 0.027 Uiso 1 1 d . . . H26Y H -0.1429 0.2658 0.7106 0.027 Uiso 1 1 d . . . O71 O -0.17402(5) 0.58757(9) 0.57759(5) 0.0237(3) Uani 1 1 d . . . H71X H -0.1688 0.5747 0.6129 0.028 Uiso 1 1 d . . . C72 C -0.17494(12) 0.68124(14) 0.57329(10) 0.0477(7) Uani 1 1 d . . . H72A H -0.1387 0.7035 0.5742 0.057 Uiso 1 1 calc R . . H72B H -0.1909 0.7067 0.6022 0.057 Uiso 1 1 calc R . . H72C H -0.1959 0.6984 0.5405 0.057 Uiso 1 1 calc R . . O81 O -0.13633(5) 0.40796(8) 0.46744(5) 0.0183(3) Uani 1 1 d . . . H81X H -0.1442 0.4286 0.4345 0.022 Uiso 1 1 d . . . C82 C -0.14622(8) 0.31478(13) 0.46589(8) 0.0253(4) Uani 1 1 d . . . H82A H -0.1413 0.2910 0.5012 0.030 Uiso 1 1 calc R . . H82B H -0.1215 0.2856 0.4456 0.030 Uiso 1 1 calc R . . H82C H -0.1827 0.3037 0.4498 0.030 Uiso 1 1 calc R . . Co2 Co 0.5000 0.5000 0.5000 0.01339(8) Uani 1 2 d S . . N41 N 0.43212(6) 0.42204(10) 0.51358(6) 0.0159(3) Uani 1 1 d . . . C41 C 0.38435(7) 0.42304(12) 0.48484(7) 0.0191(4) Uani 1 1 d . . . H41 H 0.3798 0.4572 0.4539 0.023 Uiso 1 1 calc R . . C42 C 0.34121(7) 0.37639(13) 0.49823(7) 0.0208(4) Uani 1 1 d . . . H42 H 0.3079 0.3783 0.4769 0.025 Uiso 1 1 calc R . . C43 C 0.34779(7) 0.32702(13) 0.54349(7) 0.0218(4) Uani 1 1 d . . . H43 H 0.3188 0.2950 0.5537 0.026 Uiso 1 1 calc R . . C44 C 0.39692(7) 0.32450(12) 0.57385(7) 0.0185(4) Uani 1 1 d . . . H44 H 0.4022 0.2908 0.6049 0.022 Uiso 1 1 calc R . . C45 C 0.43818(7) 0.37258(12) 0.55758(7) 0.0148(4) Uani 1 1 d . . . C46 C 0.49291(7) 0.37645(12) 0.58400(7) 0.0149(4) Uani 1 1 d . . . N42 N 0.52975(6) 0.41969(10) 0.56275(6) 0.0154(3) Uani 1 1 d . . . N43 N 0.57690(6) 0.41388(10) 0.59509(6) 0.0162(3) Uani 1 1 d . . . C47 C 0.56693(7) 0.36783(12) 0.63593(7) 0.0151(4) Uani 1 1 d . . . C48 C 0.60646(7) 0.34693(12) 0.68051(7) 0.0159(4) Uani 1 1 d . . . C49 C 0.65403(7) 0.39384(12) 0.68859(7) 0.0188(4) Uani 1 1 d . . . H49 H 0.6615 0.4392 0.6653 0.023 Uiso 1 1 calc R . . C50 C 0.69018(7) 0.37268(13) 0.73153(7) 0.0217(4) Uani 1 1 d . . . H50 H 0.7230 0.4034 0.7384 0.026 Uiso 1 1 calc R . . C51 C 0.67737(7) 0.30562(13) 0.76427(7) 0.0228(4) Uani 1 1 d . . . H51 H 0.7013 0.2900 0.7941 0.027 Uiso 1 1 calc R . . C52 C 0.62942(7) 0.26167(13) 0.75307(7) 0.0206(4) Uani 1 1 d . . . H52 H 0.6213 0.2156 0.7757 0.025 Uiso 1 1 calc R . . N44 N 0.59397(6) 0.28113(10) 0.71186(6) 0.0175(3) Uani 1 1 d . . . N45 N 0.51465(6) 0.34236(10) 0.62978(6) 0.0145(3) Uani 1 1 d . . . N46 N 0.48619(6) 0.29603(11) 0.66475(6) 0.0203(3) Uani 1 1 d . . . H46X H 0.5101 0.2642 0.6844 0.024 Uiso 1 1 d . . . H46Y H 0.4723 0.3427 0.6840 0.024 Uiso 1 1 d . . . O91 O 0.47885(5) 0.58841(8) 0.55450(5) 0.0227(3) Uani 1 1 d . . . H91X H 0.4877 0.5745 0.5891 0.027 Uiso 1 1 d . . . C92 C 0.47306(11) 0.68160(14) 0.55038(9) 0.0391(6) Uani 1 1 d . . . H92A H 0.4558 0.6969 0.5156 0.047 Uiso 1 1 calc R . . H92B H 0.5080 0.7097 0.5564 0.047 Uiso 1 1 calc R . . H92C H 0.4513 0.7028 0.5762 0.047 Uiso 1 1 calc R . . S1 S -0.119071(19) 0.45444(3) 0.332015(18) 0.02088(11) Uani 1 1 d . . . O11 O -0.15496(5) 0.45759(9) 0.37181(5) 0.0250(3) Uani 1 1 d . . . O12 O -0.07174(6) 0.40332(10) 0.34830(6) 0.0368(4) Uani 1 1 d . . . O13 O -0.10894(6) 0.54230(10) 0.31295(6) 0.0301(3) Uani 1 1 d . . . C101 C -0.15570(8) 0.39810(13) 0.27874(7) 0.0223(4) Uani 1 1 d . . . H10A H -0.1350 0.3984 0.2491 0.027 Uiso 1 1 calc R . . H10B H -0.1609 0.3355 0.2885 0.027 Uiso 1 1 calc R . . C102 C -0.20948(7) 0.44051(13) 0.26206(7) 0.0209(4) Uani 1 1 d . . . H10C H -0.2043 0.5031 0.2523 0.025 Uiso 1 1 calc R . . H10D H -0.2301 0.4403 0.2917 0.025 Uiso 1 1 calc R . . C103 C -0.24087(7) 0.39239(13) 0.21653(7) 0.0226(4) Uani 1 1 d . . . H10E H -0.2431 0.3286 0.2252 0.027 Uiso 1 1 calc R . . H10F H -0.2217 0.3974 0.1860 0.027 Uiso 1 1 calc R . . C104 C -0.29680(7) 0.42903(13) 0.20248(7) 0.0225(4) Uani 1 1 d . . . H10G H -0.2946 0.4935 0.1956 0.027 Uiso 1 1 calc R . . H10H H -0.3165 0.4213 0.2324 0.027 Uiso 1 1 calc R . . C105 C -0.32760(7) 0.38414(13) 0.15522(7) 0.0216(4) Uani 1 1 d . . . H10I H -0.3084 0.3933 0.1250 0.026 Uiso 1 1 calc R . . H10J H -0.3290 0.3195 0.1617 0.026 Uiso 1 1 calc R . . C106 C -0.38397(7) 0.41913(13) 0.14219(7) 0.0230(4) Uani 1 1 d . . . H10K H -0.4031 0.4094 0.1724 0.028 Uiso 1 1 calc R . . H10L H -0.3825 0.4840 0.1362 0.028 Uiso 1 1 calc R . . C107 C -0.41516(7) 0.37579(13) 0.09474(7) 0.0218(4) Uani 1 1 d . . . H10M H -0.3963 0.3861 0.0645 0.026 Uiso 1 1 calc R . . H10N H -0.4163 0.3109 0.1005 0.026 Uiso 1 1 calc R . . C108 C -0.47169(7) 0.41025(13) 0.08221(7) 0.0227(4) Uani 1 1 d . . . H10O H -0.4907 0.3998 0.1124 0.027 Uiso 1 1 calc R . . H10P H -0.4706 0.4752 0.0765 0.027 Uiso 1 1 calc R . . C109 C -0.50254(7) 0.36681(13) 0.03475(8) 0.0224(4) Uani 1 1 d . . . H10Q H -0.5035 0.3019 0.0405 0.027 Uiso 1 1 calc R . . H10R H -0.4835 0.3774 0.0046 0.027 Uiso 1 1 calc R . . C110 C -0.55927(7) 0.40094(13) 0.02204(8) 0.0232(4) Uani 1 1 d . . . H11A H -0.5785 0.3890 0.0519 0.028 Uiso 1 1 calc R . . H11B H -0.5583 0.4661 0.0171 0.028 Uiso 1 1 calc R . . C111 C -0.58972(7) 0.35882(13) -0.02637(8) 0.0226(4) Uani 1 1 d . . . H11C H -0.5902 0.2936 -0.0217 0.027 Uiso 1 1 calc R . . H11D H -0.5708 0.3716 -0.0564 0.027 Uiso 1 1 calc R . . C112 C -0.64671(7) 0.39214(14) -0.03840(8) 0.0240(4) Uani 1 1 d . . . H11E H -0.6658 0.3786 -0.0086 0.029 Uiso 1 1 calc R . . H11F H -0.6462 0.4575 -0.0425 0.029 Uiso 1 1 calc R . . C113 C -0.67700(7) 0.35121(13) -0.08712(8) 0.0239(4) Uani 1 1 d . . . H11G H -0.6778 0.2859 -0.0828 0.029 Uiso 1 1 calc R . . H11H H -0.6577 0.3641 -0.1168 0.029 Uiso 1 1 calc R . . C114 C -0.73384(7) 0.38497(14) -0.09973(8) 0.0241(4) Uani 1 1 d . . . H11I H -0.7540 0.3678 -0.0713 0.029 Uiso 1 1 calc R . . H11J H -0.7333 0.4506 -0.1014 0.029 Uiso 1 1 calc R . . C115 C -0.76219(8) 0.34893(14) -0.15068(8) 0.0267(5) Uani 1 1 d . . . H11K H -0.7612 0.2832 -0.1496 0.032 Uiso 1 1 calc R . . H11L H -0.7429 0.3685 -0.1793 0.032 Uiso 1 1 calc R . . C116 C -0.81982(8) 0.37933(15) -0.16205(9) 0.0338(5) Uani 1 1 d . . . H11M H -0.8396 0.3577 -0.1348 0.041 Uiso 1 1 calc R . . H11N H -0.8357 0.3555 -0.1956 0.041 Uiso 1 1 calc R . . H11O H -0.8211 0.4444 -0.1631 0.041 Uiso 1 1 calc R . . S2 S -0.179777(19) 0.55213(3) 0.715631(18) 0.02238(11) Uani 1 1 d . . . O21 O -0.14706(6) 0.54356(10) 0.67366(5) 0.0288(3) Uani 1 1 d . . . O22 O -0.19088(6) 0.46651(10) 0.73719(6) 0.0323(3) Uani 1 1 d . . . O23 O -0.22663(6) 0.60618(11) 0.70062(6) 0.0397(4) Uani 1 1 d . . . C121 C -0.13991(7) 0.61127(14) 0.76538(7) 0.0231(4) Uani 1 1 d . . . H12A H -0.1353 0.6730 0.7538 0.028 Uiso 1 1 calc R . . H12B H -0.1583 0.6135 0.7965 0.028 Uiso 1 1 calc R . . C122 C -0.08560(7) 0.56870(13) 0.77959(7) 0.0227(4) Uani 1 1 d . . . H12C H -0.0669 0.5681 0.7486 0.027 Uiso 1 1 calc R . . H12D H -0.0903 0.5063 0.7901 0.027 Uiso 1 1 calc R . . C123 C -0.05137(7) 0.61735(14) 0.82350(8) 0.0233(4) Uani 1 1 d . . . H12E H -0.0490 0.6808 0.8142 0.028 Uiso 1 1 calc R . . H12F H -0.0686 0.6137 0.8553 0.028 Uiso 1 1 calc R . . C124 C 0.00424(7) 0.57874(13) 0.83436(8) 0.0245(4) Uani 1 1 d . . . H12G H 0.0214 0.5834 0.8026 0.029 Uiso 1 1 calc R . . H12H H 0.0016 0.5149 0.8427 0.029 Uiso 1 1 calc R . . C125 C 0.03928(7) 0.62454(13) 0.87869(8) 0.0229(4) Uani 1 1 d . . . H12I H 0.0402 0.6890 0.8714 0.027 Uiso 1 1 calc R . . H12J H 0.0234 0.6165 0.9110 0.027 Uiso 1 1 calc R . . C126 C 0.09580(8) 0.58917(14) 0.88682(8) 0.0248(4) Uani 1 1 d . . . H12K H 0.0949 0.5244 0.8931 0.030 Uiso 1 1 calc R . . H12L H 0.1120 0.5988 0.8548 0.030 Uiso 1 1 calc R . . C127 C 0.13040(7) 0.63291(13) 0.93194(7) 0.0217(4) Uani 1 1 d . . . H12M H 0.1130 0.6260 0.9635 0.026 Uiso 1 1 calc R . . H12N H 0.1326 0.6973 0.9248 0.026 Uiso 1 1 calc R . . C128 C 0.18668(8) 0.59555(14) 0.94280(8) 0.0246(4) Uani 1 1 d . . . H12O H 0.1847 0.5308 0.9488 0.030 Uiso 1 1 calc R . . H12P H 0.2048 0.6048 0.9119 0.030 Uiso 1 1 calc R . . C129 C 0.21942(7) 0.63822(13) 0.98943(7) 0.0213(4) Uani 1 1 d . . . H12Q H 0.2004 0.6309 1.0199 0.026 Uiso 1 1 calc R . . H12R H 0.2222 0.7027 0.9828 0.026 Uiso 1 1 calc R . . C130 C 0.27525(7) 0.60034(13) 1.00258(7) 0.0223(4) Uani 1 1 d . . . H13A H 0.2728 0.5357 1.0087 0.027 Uiso 1 1 calc R . . H13B H 0.2949 0.6090 0.9726 0.027 Uiso 1 1 calc R . . C131 C 0.30608(7) 0.64390(13) 1.05032(7) 0.0213(4) Uani 1 1 d . . . H13C H 0.3075 0.7087 1.0443 0.026 Uiso 1 1 calc R . . H13D H 0.2865 0.6343 1.0802 0.026 Uiso 1 1 calc R . . C132 C 0.36234(7) 0.60934(13) 1.06415(7) 0.0219(4) Uani 1 1 d . . . H13E H 0.3611 0.5443 1.0692 0.026 Uiso 1 1 calc R . . H13F H 0.3824 0.6209 1.0348 0.026 Uiso 1 1 calc R . . C133 C 0.39149(7) 0.65169(13) 1.11281(7) 0.0206(4) Uani 1 1 d . . . H13G H 0.3730 0.6359 1.1426 0.025 Uiso 1 1 calc R . . H13H H 0.3899 0.7171 1.1089 0.025 Uiso 1 1 calc R . . C134 C 0.44948(7) 0.62365(13) 1.12486(7) 0.0209(4) Uani 1 1 d . . . H13I H 0.4511 0.5591 1.1320 0.025 Uiso 1 1 calc R . . H13J H 0.4674 0.6347 1.0940 0.025 Uiso 1 1 calc R . . C135 C 0.47921(7) 0.67278(14) 1.17103(7) 0.0235(4) Uani 1 1 d . . . H13K H 0.4731 0.7373 1.1662 0.028 Uiso 1 1 calc R . . H13L H 0.4646 0.6548 1.2028 0.028 Uiso 1 1 calc R . . C136 C 0.53866(8) 0.65535(17) 1.17864(8) 0.0342(5) Uani 1 1 d . . . H13M H 0.5452 0.5917 1.1842 0.041 Uiso 1 1 calc R . . H13N H 0.5554 0.6885 1.2089 0.041 Uiso 1 1 calc R . . H13O H 0.5537 0.6746 1.1478 0.041 Uiso 1 1 calc R . . S3 S 0.467549(18) 0.54689(3) 0.693227(18) 0.01921(11) Uani 1 1 d . . . O31 O 0.50169(5) 0.54596(9) 0.65226(5) 0.0258(3) Uani 1 1 d . . . O32 O 0.45749(5) 0.45810(10) 0.71106(6) 0.0295(3) Uani 1 1 d . . . O33 O 0.41971(6) 0.59891(10) 0.67937(6) 0.0368(4) Uani 1 1 d . . . C141 C 0.50458(7) 0.60241(13) 0.74641(7) 0.0202(4) Uani 1 1 d . . . H14A H 0.5096 0.6651 0.7368 0.024 Uiso 1 1 calc R . . H14B H 0.4841 0.6018 0.7761 0.024 Uiso 1 1 calc R . . C142 C 0.55848(7) 0.56026(13) 0.76283(7) 0.0196(4) Uani 1 1 d . . . H14C H 0.5782 0.5579 0.7326 0.024 Uiso 1 1 calc R . . H14D H 0.5534 0.4985 0.7743 0.024 Uiso 1 1 calc R . . C143 C 0.59125(7) 0.61124(13) 0.80663(7) 0.0195(4) Uani 1 1 d . . . H14E H 0.5941 0.6740 0.7961 0.023 Uiso 1 1 calc R . . H14F H 0.5726 0.6100 0.8376 0.023 Uiso 1 1 calc R . . C144 C 0.64676(7) 0.57336(13) 0.82086(7) 0.0212(4) Uani 1 1 d . . . H14G H 0.6662 0.5785 0.7906 0.025 Uiso 1 1 calc R . . H14H H 0.6439 0.5094 0.8289 0.025 Uiso 1 1 calc R . . C145 C 0.67846(7) 0.61968(13) 0.86699(7) 0.0196(4) Uani 1 1 d . . . H14I H 0.6597 0.6128 0.8977 0.024 Uiso 1 1 calc R . . H14J H 0.6804 0.6839 0.8594 0.024 Uiso 1 1 calc R . . C146 C 0.73453(7) 0.58305(13) 0.87971(8) 0.0216(4) Uani 1 1 d . . . H14K H 0.7324 0.5185 0.8862 0.026 Uiso 1 1 calc R . . H14L H 0.7534 0.5912 0.8492 0.026 Uiso 1 1 calc R . . C147 C 0.76685(7) 0.62643(13) 0.92642(7) 0.0198(4) Uani 1 1 d . . . H14M H 0.7485 0.6172 0.9572 0.024 Uiso 1 1 calc R . . H14N H 0.7685 0.6912 0.9203 0.024 Uiso 1 1 calc R . . C148 C 0.82322(7) 0.59020(13) 0.93785(7) 0.0218(4) Uani 1 1 d . . . H14O H 0.8215 0.5254 0.9438 0.026 Uiso 1 1 calc R . . H14P H 0.8415 0.5997 0.9071 0.026 Uiso 1 1 calc R . . C149 C 0.85578(7) 0.63298(13) 0.98467(7) 0.0212(4) Uani 1 1 d . . . H14Q H 0.8379 0.6223 1.0156 0.025 Uiso 1 1 calc R . . H14R H 0.8569 0.6979 0.9791 0.025 Uiso 1 1 calc R . . C150 C 0.91248(7) 0.59789(13) 0.99522(8) 0.0227(4) Uani 1 1 d . . . H15A H 0.9113 0.5328 1.0001 0.027 Uiso 1 1 calc R . . H15B H 0.9305 0.6095 0.9645 0.027 Uiso 1 1 calc R . . C151 C 0.94502(7) 0.63914(13) 1.04257(7) 0.0219(4) Uani 1 1 d . . . H15C H 0.9282 0.6246 1.0737 0.026 Uiso 1 1 calc R . . H15D H 0.9446 0.7045 1.0386 0.026 Uiso 1 1 calc R . . C152 C 1.00248(7) 0.60712(13) 1.05084(8) 0.0230(4) Uani 1 1 d . . . H15E H 1.0029 0.5418 1.0554 0.028 Uiso 1 1 calc R . . H15F H 1.0190 0.6207 1.0195 0.028 Uiso 1 1 calc R . . C153 C 1.03550(7) 0.64936(13) 1.09760(7) 0.0209(4) Uani 1 1 d . . . H15G H 1.0193 0.6347 1.1290 0.025 Uiso 1 1 calc R . . H15H H 1.0344 0.7147 1.0934 0.025 Uiso 1 1 calc R . . C154 C 1.09325(7) 0.61945(13) 1.10563(7) 0.0210(4) Uani 1 1 d . . . H15I H 1.1090 0.6305 1.0735 0.025 Uiso 1 1 calc R . . H15J H 1.0946 0.5547 1.1123 0.025 Uiso 1 1 calc R . . C155 C 1.12631(7) 0.66732(14) 1.15057(8) 0.0237(4) Uani 1 1 d . . . H15K H 1.1208 0.7321 1.1463 0.028 Uiso 1 1 calc R . . H15L H 1.1136 0.6496 1.1834 0.028 Uiso 1 1 calc R . . C156 C 1.18535(8) 0.64766(16) 1.15456(8) 0.0329(5) Uani 1 1 d . . . H15M H 1.1914 0.5840 1.1606 0.040 Uiso 1 1 calc R . . H15N H 1.2044 0.6814 1.1834 0.040 Uiso 1 1 calc R . . H15O H 1.1983 0.6648 1.1222 0.040 Uiso 1 1 calc R . . O161 O -0.31388(6) 0.58595(11) 0.62520(6) 0.0353(4) Uani 1 1 d . . . H16X H -0.2795 0.5886 0.6431 0.042 Uiso 1 1 d . . . C162 C -0.35389(9) 0.62389(15) 0.65085(9) 0.0339(5) Uani 1 1 d . . . H16A H -0.3452 0.6149 0.6883 0.041 Uiso 1 1 calc R . . H16B H -0.3879 0.5955 0.6387 0.041 Uiso 1 1 calc R . . H16C H -0.3563 0.6876 0.6434 0.041 Uiso 1 1 calc R . . O171 O 0.33667(6) 0.58632(11) 0.60017(6) 0.0368(4) Uani 1 1 d . . . H17X H 0.3695 0.5908 0.6222 0.044 Uiso 1 1 d . . . C172 C 0.29631(8) 0.62438(15) 0.62545(8) 0.0315(5) Uani 1 1 d . . . H17A H 0.3044 0.6146 0.6629 0.038 Uiso 1 1 calc R . . H17B H 0.2623 0.5966 0.6126 0.038 Uiso 1 1 calc R . . H17C H 0.2943 0.6883 0.6184 0.038 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 0.01479(12) 0.01505(13) 0.01300(13) 0.00069(10) 0.00264(9) -0.00052(10) N1 0.0176(8) 0.0155(8) 0.0171(8) 0.0000(6) 0.0034(6) 0.0006(6) C1 0.0202(9) 0.0196(10) 0.0190(10) 0.0005(8) 0.0001(8) 0.0009(8) C2 0.0165(9) 0.0218(10) 0.0276(11) -0.0026(8) 0.0010(8) 0.0006(8) C3 0.0183(10) 0.0261(11) 0.0270(11) -0.0018(9) 0.0072(8) -0.0041(8) C4 0.0234(10) 0.0225(10) 0.0200(10) 0.0012(8) 0.0066(8) -0.0025(8) C5 0.0187(9) 0.0143(9) 0.0167(9) -0.0019(7) 0.0043(7) 0.0002(7) C6 0.0180(9) 0.0125(9) 0.0144(9) -0.0010(7) 0.0044(7) -0.0007(7) N2 0.0133(7) 0.0175(8) 0.0164(8) 0.0010(6) 0.0019(6) 0.0004(6) N3 0.0172(8) 0.0174(8) 0.0150(8) 0.0025(6) 0.0024(6) 0.0008(6) C7 0.0158(9) 0.0128(9) 0.0175(9) -0.0001(7) 0.0031(7) 0.0008(7) C8 0.0178(9) 0.0168(9) 0.0154(9) -0.0007(7) 0.0030(7) 0.0029(7) C9 0.0203(9) 0.0161(10) 0.0208(10) 0.0009(8) 0.0047(8) 0.0003(7) C10 0.0190(10) 0.0258(11) 0.0245(11) -0.0009(9) 0.0034(8) -0.0019(8) C11 0.0229(10) 0.0288(11) 0.0177(10) 0.0032(8) 0.0003(8) 0.0034(8) C12 0.0242(10) 0.0233(11) 0.0191(10) 0.0036(8) 0.0052(8) 0.0012(8) N4 0.0206(8) 0.0173(8) 0.0184(8) 0.0020(7) 0.0032(6) 0.0008(6) N5 0.0168(8) 0.0141(8) 0.0160(8) 0.0015(6) 0.0041(6) -0.0014(6) N6 0.0225(8) 0.0224(9) 0.0193(9) 0.0069(7) 0.0069(7) -0.0033(7) N21 0.0181(8) 0.0158(8) 0.0141(8) -0.0018(6) 0.0035(6) -0.0007(6) C21 0.0186(9) 0.0199(10) 0.0169(10) 0.0002(8) 0.0015(7) 0.0028(8) C22 0.0159(9) 0.0258(11) 0.0219(10) -0.0029(8) 0.0016(8) -0.0005(8) C23 0.0188(9) 0.0234(11) 0.0239(10) -0.0004(8) 0.0074(8) -0.0041(8) C24 0.0206(10) 0.0196(10) 0.0189(10) 0.0033(8) 0.0041(8) -0.0005(8) C25 0.0188(9) 0.0152(9) 0.0160(9) -0.0025(7) 0.0040(7) 0.0004(7) C26 0.0182(9) 0.0138(9) 0.0142(9) -0.0014(7) 0.0049(7) -0.0010(7) N22 0.0151(7) 0.0176(8) 0.0164(8) -0.0002(6) 0.0017(6) -0.0002(6) N23 0.0152(8) 0.0210(8) 0.0174(8) 0.0011(7) 0.0024(6) 0.0001(6) C27 0.0151(9) 0.0149(9) 0.0181(9) -0.0011(7) 0.0047(7) 0.0004(7) C28 0.0197(9) 0.0222(10) 0.0157(9) 0.0020(8) 0.0052(7) 0.0040(8) C29 0.0203(10) 0.0292(11) 0.0203(10) 0.0035(9) 0.0027(8) -0.0020(8) C30 0.0203(10) 0.0420(13) 0.0211(11) 0.0016(9) -0.0001(8) -0.0026(9) C31 0.0226(10) 0.0410(13) 0.0172(10) 0.0050(9) -0.0007(8) 0.0064(9) C32 0.0267(11) 0.0310(12) 0.0190(10) 0.0079(9) 0.0052(8) 0.0053(9) N24 0.0217(8) 0.0246(9) 0.0186(8) 0.0030(7) 0.0048(7) 0.0023(7) N25 0.0172(8) 0.0155(8) 0.0151(8) 0.0018(6) 0.0048(6) -0.0013(6) N26 0.0225(8) 0.0274(9) 0.0187(9) 0.0088(7) 0.0074(7) -0.0016(7) O71 0.0377(8) 0.0171(7) 0.0176(7) -0.0010(6) 0.0088(6) 0.0009(6) C72 0.093(2) 0.0189(12) 0.0359(14) -0.0023(10) 0.0259(14) 0.0050(13) O81 0.0244(7) 0.0150(7) 0.0159(7) -0.0001(5) 0.0045(5) -0.0005(5) C82 0.0326(11) 0.0172(10) 0.0265(11) -0.0017(8) 0.0051(9) -0.0025(8) Co2 0.01602(17) 0.01352(18) 0.01073(17) 0.00044(14) 0.00211(13) 0.00050(14) N41 0.0171(8) 0.0157(8) 0.0148(8) -0.0007(6) 0.0017(6) 0.0009(6) C41 0.0211(10) 0.0199(10) 0.0161(9) -0.0009(8) 0.0011(8) 0.0012(8) C42 0.0177(9) 0.0232(10) 0.0207(10) -0.0006(8) -0.0003(8) 0.0016(8) C43 0.0189(10) 0.0238(11) 0.0233(10) 0.0007(8) 0.0052(8) -0.0029(8) C44 0.0187(9) 0.0190(10) 0.0183(10) 0.0017(8) 0.0041(7) -0.0001(8) C45 0.0154(9) 0.0146(9) 0.0143(9) -0.0011(7) 0.0018(7) 0.0006(7) C46 0.0186(9) 0.0135(9) 0.0131(9) 0.0007(7) 0.0034(7) 0.0003(7) N42 0.0162(7) 0.0158(8) 0.0141(8) 0.0001(6) 0.0017(6) 0.0001(6) N43 0.0156(7) 0.0180(8) 0.0145(8) 0.0020(6) 0.0006(6) 0.0015(6) C47 0.0161(9) 0.0137(9) 0.0159(9) -0.0003(7) 0.0035(7) 0.0000(7) C48 0.0171(9) 0.0173(9) 0.0138(9) -0.0008(7) 0.0037(7) 0.0041(7) C49 0.0211(10) 0.0182(10) 0.0175(10) 0.0020(8) 0.0042(8) 0.0006(8) C50 0.0161(9) 0.0269(11) 0.0213(10) -0.0015(8) 0.0002(8) -0.0016(8) C51 0.0192(10) 0.0309(12) 0.0178(10) 0.0034(9) 0.0008(8) 0.0034(8) C52 0.0207(10) 0.0231(10) 0.0183(10) 0.0056(8) 0.0043(8) 0.0035(8) N44 0.0187(8) 0.0186(8) 0.0154(8) 0.0027(6) 0.0030(6) 0.0025(6) N45 0.0161(7) 0.0149(8) 0.0127(8) 0.0025(6) 0.0027(6) -0.0001(6) N46 0.0199(8) 0.0231(9) 0.0184(8) 0.0088(7) 0.0045(7) -0.0022(7) O91 0.0390(8) 0.0152(7) 0.0148(7) -0.0010(5) 0.0068(6) 0.0024(6) C92 0.0723(17) 0.0175(11) 0.0298(12) -0.0015(9) 0.0154(12) 0.0049(11) S1 0.0233(2) 0.0236(3) 0.0156(2) -0.00346(19) 0.00192(19) 0.0026(2) O11 0.0332(8) 0.0277(8) 0.0148(7) -0.0012(6) 0.0064(6) -0.0010(6) O12 0.0343(8) 0.0439(10) 0.0288(8) -0.0137(7) -0.0077(7) 0.0147(7) O13 0.0316(8) 0.0303(8) 0.0291(8) -0.0005(7) 0.0067(6) -0.0082(7) C101 0.0274(10) 0.0242(11) 0.0154(10) -0.0047(8) 0.0026(8) 0.0006(8) C102 0.0230(10) 0.0218(10) 0.0182(10) -0.0014(8) 0.0034(8) 0.0002(8) C103 0.0230(10) 0.0233(11) 0.0215(10) -0.0023(8) 0.0034(8) -0.0014(8) C104 0.0238(10) 0.0218(10) 0.0225(10) -0.0017(8) 0.0049(8) -0.0019(8) C105 0.0210(10) 0.0245(11) 0.0199(10) -0.0010(8) 0.0049(8) -0.0017(8) C106 0.0239(10) 0.0241(11) 0.0216(10) -0.0007(8) 0.0051(8) 0.0005(8) C107 0.0215(10) 0.0202(10) 0.0242(11) 0.0000(8) 0.0047(8) -0.0010(8) C108 0.0234(10) 0.0241(11) 0.0213(10) -0.0010(8) 0.0047(8) 0.0011(8) C109 0.0221(10) 0.0203(10) 0.0255(11) -0.0007(8) 0.0058(8) -0.0003(8) C110 0.0219(10) 0.0244(11) 0.0239(11) -0.0001(8) 0.0051(8) 0.0015(8) C111 0.0220(10) 0.0218(10) 0.0251(11) -0.0014(8) 0.0065(8) -0.0002(8) C112 0.0222(10) 0.0254(11) 0.0249(11) -0.0014(9) 0.0043(8) 0.0026(8) C113 0.0231(10) 0.0233(11) 0.0260(11) -0.0022(9) 0.0053(8) 0.0016(8) C114 0.0229(10) 0.0242(11) 0.0258(11) -0.0002(9) 0.0049(8) 0.0005(8) C115 0.0265(11) 0.0262(11) 0.0277(11) 0.0013(9) 0.0051(9) -0.0027(9) C116 0.0307(12) 0.0344(13) 0.0350(13) 0.0042(10) -0.0004(10) -0.0016(10) S2 0.0219(2) 0.0272(3) 0.0172(2) -0.0062(2) -0.00038(19) 0.0036(2) O21 0.0380(8) 0.0341(9) 0.0148(7) -0.0038(6) 0.0058(6) 0.0027(7) O22 0.0300(8) 0.0355(9) 0.0310(8) -0.0010(7) 0.0028(7) -0.0109(7) O23 0.0311(8) 0.0471(10) 0.0364(9) -0.0209(8) -0.0118(7) 0.0175(7) C121 0.0228(10) 0.0275(11) 0.0185(10) -0.0060(8) 0.0010(8) 0.0021(8) C122 0.0233(10) 0.0231(11) 0.0209(10) -0.0036(8) -0.0005(8) 0.0002(8) C123 0.0231(10) 0.0250(11) 0.0214(10) -0.0043(8) 0.0015(8) -0.0024(8) C124 0.0235(10) 0.0233(11) 0.0253(11) -0.0017(9) -0.0014(8) -0.0020(8) C125 0.0252(10) 0.0218(10) 0.0212(10) 0.0000(8) 0.0013(8) -0.0015(8) C126 0.0250(10) 0.0242(11) 0.0243(11) -0.0032(9) -0.0003(8) -0.0016(8) C127 0.0220(10) 0.0211(10) 0.0219(10) -0.0017(8) 0.0021(8) -0.0011(8) C128 0.0255(10) 0.0245(11) 0.0234(11) -0.0027(9) 0.0018(8) 0.0002(8) C129 0.0208(10) 0.0212(10) 0.0224(10) 0.0002(8) 0.0041(8) 0.0010(8) C130 0.0207(10) 0.0246(11) 0.0214(10) -0.0014(8) 0.0025(8) 0.0025(8) C131 0.0219(10) 0.0208(10) 0.0215(10) -0.0017(8) 0.0034(8) 0.0001(8) C132 0.0219(10) 0.0235(11) 0.0205(10) -0.0025(8) 0.0031(8) 0.0018(8) C133 0.0206(10) 0.0202(10) 0.0217(10) -0.0010(8) 0.0053(8) -0.0006(8) C134 0.0233(10) 0.0194(10) 0.0201(10) 0.0033(8) 0.0040(8) 0.0017(8) C135 0.0241(10) 0.0257(11) 0.0204(10) 0.0005(8) 0.0022(8) 0.0016(8) C136 0.0256(11) 0.0516(15) 0.0245(12) -0.0005(10) 0.0000(9) 0.0027(10) S3 0.0180(2) 0.0231(3) 0.0158(2) -0.00521(19) -0.00051(18) 0.00217(19) O31 0.0331(8) 0.0311(8) 0.0136(7) -0.0030(6) 0.0051(6) -0.0002(6) O32 0.0286(8) 0.0298(8) 0.0296(8) -0.0010(7) 0.0025(6) -0.0095(6) O33 0.0269(8) 0.0441(10) 0.0347(9) -0.0194(7) -0.0129(7) 0.0153(7) C141 0.0216(10) 0.0242(10) 0.0144(9) -0.0052(8) 0.0006(8) 0.0007(8) C142 0.0178(9) 0.0221(10) 0.0187(10) -0.0013(8) 0.0010(8) 0.0002(8) C143 0.0173(9) 0.0222(10) 0.0187(10) -0.0010(8) 0.0013(8) -0.0011(8) C144 0.0187(9) 0.0236(11) 0.0207(10) -0.0021(8) 0.0006(8) 0.0005(8) C145 0.0194(9) 0.0213(10) 0.0178(10) 0.0009(8) 0.0011(8) 0.0005(8) C146 0.0184(9) 0.0214(10) 0.0243(11) -0.0006(8) 0.0002(8) 0.0003(8) C147 0.0176(9) 0.0183(10) 0.0229(10) 0.0014(8) 0.0003(8) -0.0012(8) C148 0.0190(9) 0.0226(10) 0.0227(10) -0.0008(8) -0.0008(8) 0.0009(8) C149 0.0193(10) 0.0200(10) 0.0237(10) 0.0000(8) 0.0010(8) -0.0009(8) C150 0.0181(9) 0.0253(11) 0.0237(11) -0.0015(8) -0.0004(8) 0.0004(8) C151 0.0200(10) 0.0227(10) 0.0222(10) -0.0014(8) 0.0004(8) -0.0010(8) C152 0.0205(10) 0.0253(11) 0.0228(11) -0.0017(8) 0.0008(8) 0.0012(8) C153 0.0186(9) 0.0228(10) 0.0206(10) -0.0011(8) 0.0002(8) 0.0003(8) C154 0.0223(10) 0.0212(10) 0.0189(10) 0.0005(8) 0.0000(8) 0.0014(8) C155 0.0200(10) 0.0284(11) 0.0220(10) -0.0011(9) -0.0001(8) -0.0004(8) C156 0.0226(11) 0.0474(14) 0.0275(12) 0.0004(10) -0.0015(9) 0.0003(10) O161 0.0272(8) 0.0521(10) 0.0253(8) -0.0049(7) -0.0018(6) -0.0021(7) C162 0.0372(13) 0.0338(13) 0.0313(12) 0.0002(10) 0.0071(10) -0.0033(10) O171 0.0251(8) 0.0600(11) 0.0236(8) -0.0046(8) -0.0032(6) 0.0008(7) C172 0.0314(12) 0.0333(12) 0.0292(12) 0.0022(10) 0.0018(9) -0.0032(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O71 2.0682(13) . y Co1 O81 2.0828(13) . y Co1 N2 2.0912(15) . y Co1 N22 2.1036(16) . y Co1 N1 2.1479(15) . y Co1 N21 2.1512(15) . y N1 C1 1.338(2) . ? N1 C5 1.357(2) . ? C1 C2 1.389(3) . ? C1 H1 0.9500 . ? C2 C3 1.381(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.390(3) . ? C4 H4 0.9500 . ? C5 C6 1.469(3) . ? C6 N2 1.322(2) . ? C6 N5 1.347(2) . ? N2 N3 1.374(2) . ? N3 C7 1.318(2) . ? C7 N5 1.375(2) . ? C7 C8 1.466(3) . ? C8 N4 1.346(2) . ? C8 C9 1.392(3) . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(3) . ? C10 H12 0.9500 . ? C11 C12 1.385(3) . ? C11 H11 0.9500 . ? C12 N4 1.340(2) . ? C12 H10 0.9500 . ? N5 N6 1.423(2) . ? N6 H6X 0.9746 . ? N6 H6Y 0.8989 . ? N21 C21 1.338(2) . ? N21 C25 1.356(2) . ? C21 C22 1.387(3) . ? C21 H21 0.9500 . ? C22 C23 1.383(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.388(2) . ? C24 H24 0.9500 . ? C25 C26 1.467(2) . ? C26 N22 1.323(2) . ? C26 N25 1.348(2) . ? N22 N23 1.375(2) . ? N23 C27 1.320(2) . ? C27 N25 1.374(2) . ? C27 C28 1.470(3) . ? C28 N24 1.350(2) . ? C28 C29 1.391(3) . ? C29 C30 1.387(3) . ? C29 H29 0.9500 . ? C30 C31 1.383(3) . ? C30 H30 0.9500 . ? C31 C32 1.386(3) . ? C31 H31 0.9500 . ? C32 N24 1.338(2) . ? C32 H32 0.9500 . ? N25 N26 1.424(2) . ? N26 H26X 0.9101 . ? N26 H26Y 0.9019 . ? O71 C72 1.415(3) . ? O71 H71X 0.9321 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? O81 C82 1.425(2) . ? O81 H81X 0.9094 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? Co2 O91 2.0697(13) 3_666 y Co2 O91 2.0697(13) . y Co2 N42 2.0920(15) 3_666 y Co2 N42 2.0920(15) . y Co2 N41 2.1576(15) 3_666 y Co2 N41 2.1577(15) . y N41 C41 1.340(2) . ? N41 C45 1.358(2) . ? C41 C42 1.388(3) . ? C41 H41 0.9500 . ? C42 C43 1.385(3) . ? C42 H42 0.9500 . ? C43 C44 1.388(3) . ? C43 H43 0.9500 . ? C44 C45 1.388(2) . ? C44 H44 0.9500 . ? C45 C46 1.470(2) . ? C46 N42 1.323(2) . ? C46 N45 1.347(2) . ? N42 N43 1.374(2) . ? N43 C47 1.323(2) . ? C47 N45 1.374(2) . ? C47 C48 1.465(3) . ? C48 N44 1.349(2) . ? C48 C49 1.394(3) . ? C49 C50 1.387(3) . ? C49 H49 0.9500 . ? C50 C51 1.389(3) . ? C50 H50 0.9500 . ? C51 C52 1.385(3) . ? C51 H51 0.9500 . ? C52 N44 1.339(2) . ? C52 H52 0.9500 . ? N45 N46 1.421(2) . ? N46 H46X 0.8826 . ? N46 H46Y 0.9583 . ? O91 C92 1.414(2) . ? O91 H91X 0.9235 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? S1 O12 1.4450(15) . ? S1 O13 1.4486(15) . ? S1 O11 1.4720(14) . ? S1 C101 1.7800(19) . ? C101 C102 1.521(3) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.522(3) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.526(3) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 C105 1.526(3) . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.524(3) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 C107 1.524(3) . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.524(3) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 C109 1.521(3) . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.527(3) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 C111 1.527(3) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.528(3) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 C113 1.524(3) . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.528(3) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 C115 1.523(3) . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.528(3) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9800 . ? C116 H11N 0.9800 . ? C116 H11O 0.9800 . ? S2 O22 1.4494(16) . ? S2 O23 1.4540(15) . ? S2 O21 1.4667(14) . ? S2 C121 1.775(2) . ? C121 C122 1.524(3) . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C122 C123 1.529(3) . ? C122 H12C 0.9900 . ? C122 H12D 0.9900 . ? C123 C124 1.522(3) . ? C123 H12E 0.9900 . ? C123 H12F 0.9900 . ? C124 C125 1.526(3) . ? C124 H12G 0.9900 . ? C124 H12H 0.9900 . ? C125 C126 1.523(3) . ? C125 H12I 0.9900 . ? C125 H12J 0.9900 . ? C126 C127 1.521(3) . ? C126 H12K 0.9900 . ? C126 H12L 0.9900 . ? C127 C128 1.530(3) . ? C127 H12M 0.9900 . ? C127 H12N 0.9900 . ? C128 C129 1.520(3) . ? C128 H12O 0.9900 . ? C128 H12P 0.9900 . ? C129 C130 1.528(3) . ? C129 H12Q 0.9900 . ? C129 H12R 0.9900 . ? C130 C131 1.527(3) . ? C130 H13A 0.9900 . ? C130 H13B 0.9900 . ? C131 C132 1.521(3) . ? C131 H13C 0.9900 . ? C131 H13D 0.9900 . ? C132 C133 1.521(3) . ? C132 H13E 0.9900 . ? C132 H13F 0.9900 . ? C133 C134 1.528(3) . ? C133 H13G 0.9900 . ? C133 H13H 0.9900 . ? C134 C135 1.524(3) . ? C134 H13I 0.9900 . ? C134 H13J 0.9900 . ? C135 C136 1.523(3) . ? C135 H13K 0.9900 . ? C135 H13L 0.9900 . ? C136 H13M 0.9800 . ? C136 H13N 0.9800 . ? C136 H13O 0.9800 . ? S3 O32 1.4496(15) . ? S3 O33 1.4528(15) . ? S3 O31 1.4644(14) . ? S3 C141 1.7767(19) . ? C141 C142 1.521(3) . ? C141 H14A 0.9900 . ? C141 H14B 0.9900 . ? C142 C143 1.527(3) . ? C142 H14C 0.9900 . ? C142 H14D 0.9900 . ? C143 C144 1.523(3) . ? C143 H14E 0.9900 . ? C143 H14F 0.9900 . ? C144 C145 1.524(3) . ? C144 H14G 0.9900 . ? C144 H14H 0.9900 . ? C145 C146 1.525(3) . ? C145 H14I 0.9900 . ? C145 H14J 0.9900 . ? C146 C147 1.522(3) . ? C146 H14K 0.9900 . ? C146 H14L 0.9900 . ? C147 C148 1.527(3) . ? C147 H14M 0.9900 . ? C147 H14N 0.9900 . ? C148 C149 1.523(3) . ? C148 H14O 0.9900 . ? C148 H14P 0.9900 . ? C149 C150 1.527(3) . ? C149 H14Q 0.9900 . ? C149 H14R 0.9900 . ? C150 C151 1.523(3) . ? C150 H15A 0.9900 . ? C150 H15B 0.9900 . ? C151 C152 1.528(3) . ? C151 H15C 0.9900 . ? C151 H15D 0.9900 . ? C152 C153 1.523(3) . ? C152 H15E 0.9900 . ? C152 H15F 0.9900 . ? C153 C154 1.525(3) . ? C153 H15G 0.9900 . ? C153 H15H 0.9900 . ? C154 C155 1.528(3) . ? C154 H15I 0.9900 . ? C154 H15J 0.9900 . ? C155 C156 1.522(3) . ? C155 H15K 0.9900 . ? C155 H15L 0.9900 . ? C156 H15M 0.9800 . ? C156 H15N 0.9800 . ? C156 H15O 0.9800 . ? O161 C162 1.412(3) . ? O161 H16X 0.9360 . ? C162 H16A 0.9800 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? O171 C172 1.414(2) . ? O171 H17X 0.9507 . ? C172 H17A 0.9800 . ? C172 H17B 0.9800 . ? C172 H17C 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 O71 Co1 O81 176.11(5) . . y O71 Co1 N2 92.28(6) . . y O81 Co1 N2 84.70(6) . . y O71 Co1 N22 88.70(6) . . y O81 Co1 N22 94.38(6) . . y N2 Co1 N22 178.26(6) . . y O71 Co1 N1 92.40(6) . . y O81 Co1 N1 89.29(5) . . y N2 Co1 N1 76.73(6) . . y N22 Co1 N1 101.79(6) . . y O71 Co1 N21 86.65(6) . . y O81 Co1 N21 91.74(5) . . y N2 Co1 N21 104.67(6) . . y N22 Co1 N21 76.82(6) . . y N1 Co1 N21 178.33(6) . . y C1 N1 C5 118.57(16) . . ? C1 N1 Co1 125.55(13) . . ? C5 N1 Co1 115.71(12) . . ? N1 C1 C2 122.47(18) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.54(18) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.93(18) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 118.27(18) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 122.14(17) . . ? N1 C5 C6 111.58(15) . . ? C4 C5 C6 126.28(17) . . ? N2 C6 N5 109.09(15) . . ? N2 C6 C5 119.99(16) . . ? N5 C6 C5 130.91(16) . . ? C6 N2 N3 108.92(14) . . ? C6 N2 Co1 114.16(12) . . ? N3 N2 Co1 135.05(11) . . ? C7 N3 N2 106.16(14) . . ? N3 C7 N5 110.10(15) . . ? N3 C7 C8 124.43(16) . . ? N5 C7 C8 125.47(16) . . ? N4 C8 C9 123.58(17) . . ? N4 C8 C7 116.91(16) . . ? C9 C8 C7 119.51(17) . . ? C10 C9 C8 118.46(18) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C9 C10 C11 118.53(18) . . ? C9 C10 H12 120.7 . . ? C11 C10 H12 120.7 . . ? C12 C11 C10 119.18(18) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? N4 C12 C11 123.21(18) . . ? N4 C12 H10 118.4 . . ? C11 C12 H10 118.4 . . ? C12 N4 C8 117.02(16) . . ? C6 N5 C7 105.69(14) . . ? C6 N5 N6 124.72(15) . . ? C7 N5 N6 129.49(15) . . ? N5 N6 H6X 102.9 . . ? N5 N6 H6Y 102.4 . . ? H6X N6 H6Y 105.3 . . ? C21 N21 C25 118.30(15) . . ? C21 N21 Co1 125.89(12) . . ? C25 N21 Co1 115.75(12) . . ? N21 C21 C22 122.54(17) . . ? N21 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C23 C22 C21 118.83(18) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 119.56(17) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 118.25(17) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? N21 C25 C24 122.50(17) . . ? N21 C25 C26 111.65(15) . . ? C24 C25 C26 125.82(17) . . ? N22 C26 N25 108.96(15) . . ? N22 C26 C25 120.45(16) . . ? N25 C26 C25 130.58(16) . . ? C26 N22 N23 108.80(14) . . ? C26 N22 Co1 113.27(12) . . ? N23 N22 Co1 135.80(11) . . ? C27 N23 N22 106.41(14) . . ? N23 C27 N25 109.81(16) . . ? N23 C27 C28 124.85(16) . . ? N25 C27 C28 125.32(16) . . ? N24 C28 C29 123.64(18) . . ? N24 C28 C27 116.28(16) . . ? C29 C28 C27 120.07(17) . . ? C30 C29 C28 117.75(19) . . ? C30 C29 H29 121.1 . . ? C28 C29 H29 121.1 . . ? C31 C30 C29 119.31(19) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 119.01(18) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? N24 C32 C31 122.99(19) . . ? N24 C32 H32 118.5 . . ? C31 C32 H32 118.5 . . ? C32 N24 C28 117.29(17) . . ? C26 N25 C27 106.01(14) . . ? C26 N25 N26 124.73(14) . . ? C27 N25 N26 128.97(15) . . ? N25 N26 H26X 106.3 . . ? N25 N26 H26Y 103.9 . . ? H26X N26 H26Y 108.3 . . ? C72 O71 Co1 127.42(13) . . ? C72 O71 H71X 106.5 . . ? Co1 O71 H71X 120.6 . . ? O71 C72 H72A 109.5 . . ? O71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? O71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C82 O81 Co1 127.01(11) . . ? C82 O81 H81X 107.1 . . ? Co1 O81 H81X 114.3 . . ? O81 C82 H82A 109.5 . . ? O81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O91 Co2 O91 179.998(1) 3_666 . y O91 Co2 N42 86.35(6) 3_666 3_666 y O91 Co2 N42 93.65(6) . 3_666 y O91 Co2 N42 93.65(6) 3_666 . y O91 Co2 N42 86.35(6) . . y N42 Co2 N42 180.00(6) 3_666 . y O91 Co2 N41 87.11(6) 3_666 3_666 y O91 Co2 N41 92.89(6) . 3_666 y N42 Co2 N41 76.79(6) 3_666 3_666 y N42 Co2 N41 103.21(6) . 3_666 y O91 Co2 N41 92.89(6) 3_666 . y O91 Co2 N41 87.11(6) . . y N42 Co2 N41 103.21(6) 3_666 . y N42 Co2 N41 76.79(6) . . y N41 Co2 N41 180.0 3_666 . y C41 N41 C45 117.99(15) . . ? C41 N41 Co2 126.11(12) . . ? C45 N41 Co2 115.72(11) . . ? N41 C41 C42 122.94(17) . . ? N41 C41 H41 118.5 . . ? C42 C41 H41 118.5 . . ? C43 C42 C41 118.46(17) . . ? C43 C42 H42 120.8 . . ? C41 C42 H42 120.8 . . ? C42 C43 C44 119.77(17) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C45 118.24(17) . . ? C43 C44 H44 120.9 . . ? C45 C44 H44 120.9 . . ? N41 C45 C44 122.59(16) . . ? N41 C45 C46 111.49(15) . . ? C44 C45 C46 125.91(16) . . ? N42 C46 N45 109.13(15) . . ? N42 C46 C45 120.30(16) . . ? N45 C46 C45 130.56(16) . . ? C46 N42 N43 108.81(14) . . ? C46 N42 Co2 114.12(12) . . ? N43 N42 Co2 135.32(11) . . ? C47 N43 N42 106.29(14) . . ? N43 C47 N45 109.88(15) . . ? N43 C47 C48 124.36(16) . . ? N45 C47 C48 125.76(16) . . ? N44 C48 C49 123.48(17) . . ? N44 C48 C47 116.41(16) . . ? C49 C48 C47 120.10(16) . . ? C50 C49 C48 118.34(17) . . ? C50 C49 H49 120.8 . . ? C48 C49 H49 120.8 . . ? C49 C50 C51 118.51(18) . . ? C49 C50 H50 120.7 . . ? C51 C50 H50 120.7 . . ? C52 C51 C50 119.42(18) . . ? C52 C51 H51 120.3 . . ? C50 C51 H51 120.3 . . ? N44 C52 C51 123.02(18) . . ? N44 C52 H52 118.5 . . ? C51 C52 H52 118.5 . . ? C52 N44 C48 117.23(16) . . ? C46 N45 C47 105.87(14) . . ? C46 N45 N46 124.77(14) . . ? C47 N45 N46 129.19(14) . . ? N45 N46 H46X 105.5 . . ? N45 N46 H46Y 103.4 . . ? H46X N46 H46Y 111.7 . . ? C92 O91 Co2 128.36(12) . . ? C92 O91 H91X 108.0 . . ? Co2 O91 H91X 118.1 . . ? O91 C92 H92A 109.5 . . ? O91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? O91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? O12 S1 O13 114.03(9) . . ? O12 S1 O11 112.50(9) . . ? O13 S1 O11 111.60(8) . . ? O12 S1 C101 107.70(9) . . ? O13 S1 C101 105.47(9) . . ? O11 S1 C101 104.75(9) . . ? C102 C101 S1 112.35(13) . . ? C102 C101 H10A 109.1 . . ? S1 C101 H10A 109.1 . . ? C102 C101 H10B 109.1 . . ? S1 C101 H10B 109.1 . . ? H10A C101 H10B 107.9 . . ? C101 C102 C103 112.42(16) . . ? C101 C102 H10C 109.1 . . ? C103 C102 H10C 109.1 . . ? C101 C102 H10D 109.1 . . ? C103 C102 H10D 109.1 . . ? H10C C102 H10D 107.9 . . ? C102 C103 C104 112.99(16) . . ? C102 C103 H10E 109.0 . . ? C104 C103 H10E 109.0 . . ? C102 C103 H10F 109.0 . . ? C104 C103 H10F 109.0 . . ? H10E C103 H10F 107.8 . . ? C103 C104 C105 113.31(16) . . ? C103 C104 H10G 108.9 . . ? C105 C104 H10G 108.9 . . ? C103 C104 H10H 108.9 . . ? C105 C104 H10H 108.9 . . ? H10G C104 H10H 107.7 . . ? C106 C105 C104 113.15(16) . . ? C106 C105 H10I 108.9 . . ? C104 C105 H10I 108.9 . . ? C106 C105 H10J 108.9 . . ? C104 C105 H10J 108.9 . . ? H10I C105 H10J 107.8 . . ? C107 C106 C105 113.92(16) . . ? C107 C106 H10K 108.8 . . ? C105 C106 H10K 108.8 . . ? C107 C106 H10L 108.8 . . ? C105 C106 H10L 108.8 . . ? H10K C106 H10L 107.7 . . ? C108 C107 C106 113.75(16) . . ? C108 C107 H10M 108.8 . . ? C106 C107 H10M 108.8 . . ? C108 C107 H10N 108.8 . . ? C106 C107 H10N 108.8 . . ? H10M C107 H10N 107.7 . . ? C109 C108 C107 113.44(16) . . ? C109 C108 H10O 108.9 . . ? C107 C108 H10O 108.9 . . ? C109 C108 H10P 108.9 . . ? C107 C108 H10P 108.9 . . ? H10O C108 H10P 107.7 . . ? C108 C109 C110 113.70(16) . . ? C108 C109 H10Q 108.8 . . ? C110 C109 H10Q 108.8 . . ? C108 C109 H10R 108.8 . . ? C110 C109 H10R 108.8 . . ? H10Q C109 H10R 107.7 . . ? C111 C110 C109 113.58(16) . . ? C111 C110 H11A 108.8 . . ? C109 C110 H11A 108.8 . . ? C111 C110 H11B 108.8 . . ? C109 C110 H11B 108.8 . . ? H11A C110 H11B 107.7 . . ? C110 C111 C112 113.33(16) . . ? C110 C111 H11C 108.9 . . ? C112 C111 H11C 108.9 . . ? C110 C111 H11D 108.9 . . ? C112 C111 H11D 108.9 . . ? H11C C111 H11D 107.7 . . ? C113 C112 C111 113.49(16) . . ? C113 C112 H11E 108.9 . . ? C111 C112 H11E 108.9 . . ? C113 C112 H11F 108.9 . . ? C111 C112 H11F 108.9 . . ? H11E C112 H11F 107.7 . . ? C112 C113 C114 113.80(16) . . ? C112 C113 H11G 108.8 . . ? C114 C113 H11G 108.8 . . ? C112 C113 H11H 108.8 . . ? C114 C113 H11H 108.8 . . ? H11G C113 H11H 107.7 . . ? C115 C114 C113 113.18(16) . . ? C115 C114 H11I 108.9 . . ? C113 C114 H11I 108.9 . . ? C115 C114 H11J 108.9 . . ? C113 C114 H11J 108.9 . . ? H11I C114 H11J 107.8 . . ? C114 C115 C116 113.14(17) . . ? C114 C115 H11K 109.0 . . ? C116 C115 H11K 109.0 . . ? C114 C115 H11L 109.0 . . ? C116 C115 H11L 109.0 . . ? H11K C115 H11L 107.8 . . ? C115 C116 H11M 109.5 . . ? C115 C116 H11N 109.5 . . ? H11M C116 H11N 109.5 . . ? C115 C116 H11O 109.5 . . ? H11M C116 H11O 109.5 . . ? H11N C116 H11O 109.5 . . ? O22 S2 O23 113.99(10) . . ? O22 S2 O21 111.74(9) . . ? O23 S2 O21 112.12(9) . . ? O22 S2 C121 106.60(9) . . ? O23 S2 C121 106.48(9) . . ? O21 S2 C121 105.19(9) . . ? C122 C121 S2 112.19(14) . . ? C122 C121 H12A 109.2 . . ? S2 C121 H12A 109.2 . . ? C122 C121 H12B 109.2 . . ? S2 C121 H12B 109.2 . . ? H12A C121 H12B 107.9 . . ? C121 C122 C123 112.81(16) . . ? C121 C122 H12C 109.0 . . ? C123 C122 H12C 109.0 . . ? C121 C122 H12D 109.0 . . ? C123 C122 H12D 109.0 . . ? H12C C122 H12D 107.8 . . ? C124 C123 C122 112.26(16) . . ? C124 C123 H12E 109.2 . . ? C122 C123 H12E 109.2 . . ? C124 C123 H12F 109.2 . . ? C122 C123 H12F 109.2 . . ? H12E C123 H12F 107.9 . . ? C123 C124 C125 113.77(16) . . ? C123 C124 H12G 108.8 . . ? C125 C124 H12G 108.8 . . ? C123 C124 H12H 108.8 . . ? C125 C124 H12H 108.8 . . ? H12G C124 H12H 107.7 . . ? C126 C125 C124 113.14(16) . . ? C126 C125 H12I 109.0 . . ? C124 C125 H12I 109.0 . . ? C126 C125 H12J 109.0 . . ? C124 C125 H12J 109.0 . . ? H12I C125 H12J 107.8 . . ? C127 C126 C125 113.26(16) . . ? C127 C126 H12K 108.9 . . ? C125 C126 H12K 108.9 . . ? C127 C126 H12L 108.9 . . ? C125 C126 H12L 108.9 . . ? H12K C126 H12L 107.7 . . ? C126 C127 C128 114.50(16) . . ? C126 C127 H12M 108.6 . . ? C128 C127 H12M 108.6 . . ? C126 C127 H12N 108.6 . . ? C128 C127 H12N 108.6 . . ? H12M C127 H12N 107.6 . . ? C129 C128 C127 113.06(16) . . ? C129 C128 H12O 109.0 . . ? C127 C128 H12O 109.0 . . ? C129 C128 H12P 109.0 . . ? C127 C128 H12P 109.0 . . ? H12O C128 H12P 107.8 . . ? C128 C129 C130 114.54(16) . . ? C128 C129 H12Q 108.6 . . ? C130 C129 H12Q 108.6 . . ? C128 C129 H12R 108.6 . . ? C130 C129 H12R 108.6 . . ? H12Q C129 H12R 107.6 . . ? C131 C130 C129 112.55(16) . . ? C131 C130 H13A 109.1 . . ? C129 C130 H13A 109.1 . . ? C131 C130 H13B 109.1 . . ? C129 C130 H13B 109.1 . . ? H13A C130 H13B 107.8 . . ? C132 C131 C130 114.25(16) . . ? C132 C131 H13C 108.7 . . ? C130 C131 H13C 108.7 . . ? C132 C131 H13D 108.7 . . ? C130 C131 H13D 108.7 . . ? H13C C131 H13D 107.6 . . ? C133 C132 C131 113.12(16) . . ? C133 C132 H13E 109.0 . . ? C131 C132 H13E 109.0 . . ? C133 C132 H13F 109.0 . . ? C131 C132 H13F 109.0 . . ? H13E C132 H13F 107.8 . . ? C132 C133 C134 113.94(16) . . ? C132 C133 H13G 108.8 . . ? C134 C133 H13G 108.8 . . ? C132 C133 H13H 108.8 . . ? C134 C133 H13H 108.8 . . ? H13G C133 H13H 107.7 . . ? C135 C134 C133 113.09(16) . . ? C135 C134 H13I 109.0 . . ? C133 C134 H13I 109.0 . . ? C135 C134 H13J 109.0 . . ? C133 C134 H13J 109.0 . . ? H13I C134 H13J 107.8 . . ? C136 C135 C134 113.51(17) . . ? C136 C135 H13K 108.9 . . ? C134 C135 H13K 108.9 . . ? C136 C135 H13L 108.9 . . ? C134 C135 H13L 108.9 . . ? H13K C135 H13L 107.7 . . ? C135 C136 H13M 109.5 . . ? C135 C136 H13N 109.5 . . ? H13M C136 H13N 109.5 . . ? C135 C136 H13O 109.5 . . ? H13M C136 H13O 109.5 . . ? H13N C136 H13O 109.5 . . ? O32 S3 O33 113.50(9) . . ? O32 S3 O31 111.87(9) . . ? O33 S3 O31 112.60(9) . . ? O32 S3 C141 106.40(9) . . ? O33 S3 C141 106.24(9) . . ? O31 S3 C141 105.54(9) . . ? C142 C141 S3 112.80(13) . . ? C142 C141 H14A 109.0 . . ? S3 C141 H14A 109.0 . . ? C142 C141 H14B 109.0 . . ? S3 C141 H14B 109.0 . . ? H14A C141 H14B 107.8 . . ? C141 C142 C143 112.48(15) . . ? C141 C142 H14C 109.1 . . ? C143 C142 H14C 109.1 . . ? C141 C142 H14D 109.1 . . ? C143 C142 H14D 109.1 . . ? H14C C142 H14D 107.8 . . ? C144 C143 C142 112.94(15) . . ? C144 C143 H14E 109.0 . . ? C142 C143 H14E 109.0 . . ? C144 C143 H14F 109.0 . . ? C142 C143 H14F 109.0 . . ? H14E C143 H14F 107.8 . . ? C143 C144 C145 113.38(16) . . ? C143 C144 H14G 108.9 . . ? C145 C144 H14G 108.9 . . ? C143 C144 H14H 108.9 . . ? C145 C144 H14H 108.9 . . ? H14G C144 H14H 107.7 . . ? C144 C145 C146 112.79(16) . . ? C144 C145 H14I 109.0 . . ? C146 C145 H14I 109.0 . . ? C144 C145 H14J 109.0 . . ? C146 C145 H14J 109.0 . . ? H14I C145 H14J 107.8 . . ? C147 C146 C145 114.11(16) . . ? C147 C146 H14K 108.7 . . ? C145 C146 H14K 108.7 . . ? C147 C146 H14L 108.7 . . ? C145 C146 H14L 108.7 . . ? H14K C146 H14L 107.6 . . ? C146 C147 C148 113.32(16) . . ? C146 C147 H14M 108.9 . . ? C148 C147 H14M 108.9 . . ? C146 C147 H14N 108.9 . . ? C148 C147 H14N 108.9 . . ? H14M C147 H14N 107.7 . . ? C149 C148 C147 113.68(16) . . ? C149 C148 H14O 108.8 . . ? C147 C148 H14O 108.8 . . ? C149 C148 H14P 108.8 . . ? C147 C148 H14P 108.8 . . ? H14O C148 H14P 107.7 . . ? C148 C149 C150 113.43(16) . . ? C148 C149 H14Q 108.9 . . ? C150 C149 H14Q 108.9 . . ? C148 C149 H14R 108.9 . . ? C150 C149 H14R 108.9 . . ? H14Q C149 H14R 107.7 . . ? C151 C150 C149 113.77(16) . . ? C151 C150 H15A 108.8 . . ? C149 C150 H15A 108.8 . . ? C151 C150 H15B 108.8 . . ? C149 C150 H15B 108.8 . . ? H15A C150 H15B 107.7 . . ? C150 C151 C152 113.09(16) . . ? C150 C151 H15C 109.0 . . ? C152 C151 H15C 109.0 . . ? C150 C151 H15D 109.0 . . ? C152 C151 H15D 109.0 . . ? H15C C151 H15D 107.8 . . ? C153 C152 C151 113.35(16) . . ? C153 C152 H15E 108.9 . . ? C151 C152 H15E 108.9 . . ? C153 C152 H15F 108.9 . . ? C151 C152 H15F 108.9 . . ? H15E C152 H15F 107.7 . . ? C152 C153 C154 113.89(16) . . ? C152 C153 H15G 108.8 . . ? C154 C153 H15G 108.8 . . ? C152 C153 H15H 108.8 . . ? C154 C153 H15H 108.8 . . ? H15G C153 H15H 107.7 . . ? C153 C154 C155 112.82(16) . . ? C153 C154 H15I 109.0 . . ? C155 C154 H15I 109.0 . . ? C153 C154 H15J 109.0 . . ? C155 C154 H15J 109.0 . . ? H15I C154 H15J 107.8 . . ? C156 C155 C154 113.46(17) . . ? C156 C155 H15K 108.9 . . ? C154 C155 H15K 108.9 . . ? C156 C155 H15L 108.9 . . ? C154 C155 H15L 108.9 . . ? H15K C155 H15L 107.7 . . ? C155 C156 H15M 109.5 . . ? C155 C156 H15N 109.5 . . ? H15M C156 H15N 109.5 . . ? C155 C156 H15O 109.5 . . ? H15M C156 H15O 109.5 . . ? H15N C156 H15O 109.5 . . ? C162 O161 H16X 115.7 . . ? O161 C162 H16A 109.5 . . ? O161 C162 H16B 109.5 . . ? H16A C162 H16B 109.5 . . ? O161 C162 H16C 109.5 . . ? H16A C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C172 O171 H17X 109.0 . . ? O171 C172 H17A 109.5 . . ? O171 C172 H17B 109.5 . . ? H17A C172 H17B 109.5 . . ? O171 C172 H17C 109.5 . . ? H17A C172 H17C 109.5 . . ? H17B C172 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O71 Co1 N1 C1 82.05(15) . . . . ? O81 Co1 N1 C1 -101.45(15) . . . . ? N2 Co1 N1 C1 173.83(16) . . . . ? N22 Co1 N1 C1 -7.12(16) . . . . ? N21 Co1 N1 C1 27(2) . . . . ? O71 Co1 N1 C5 -102.77(13) . . . . ? O81 Co1 N1 C5 73.73(13) . . . . ? N2 Co1 N1 C5 -10.99(12) . . . . ? N22 Co1 N1 C5 168.06(12) . . . . ? N21 Co1 N1 C5 -158.1(19) . . . . ? C5 N1 C1 C2 -1.5(3) . . . . ? Co1 N1 C1 C2 173.51(14) . . . . ? N1 C1 C2 C3 -1.2(3) . . . . ? C1 C2 C3 C4 2.3(3) . . . . ? C2 C3 C4 C5 -0.8(3) . . . . ? C1 N1 C5 C4 3.2(3) . . . . ? Co1 N1 C5 C4 -172.37(14) . . . . ? C1 N1 C5 C6 -176.27(16) . . . . ? Co1 N1 C5 C6 8.19(19) . . . . ? C3 C4 C5 N1 -2.0(3) . . . . ? C3 C4 C5 C6 177.35(18) . . . . ? N1 C5 C6 N2 2.3(2) . . . . ? C4 C5 C6 N2 -177.08(18) . . . . ? N1 C5 C6 N5 -176.30(18) . . . . ? C4 C5 C6 N5 4.3(3) . . . . ? N5 C6 N2 N3 0.3(2) . . . . ? C5 C6 N2 N3 -178.64(15) . . . . ? N5 C6 N2 Co1 167.09(11) . . . . ? C5 C6 N2 Co1 -11.8(2) . . . . ? O71 Co1 N2 C6 103.74(13) . . . . ? O81 Co1 N2 C6 -78.71(13) . . . . ? N22 Co1 N2 C6 -20(2) . . . . ? N1 Co1 N2 C6 11.81(12) . . . . ? N21 Co1 N2 C6 -169.13(12) . . . . ? O71 Co1 N2 N3 -94.02(16) . . . . ? O81 Co1 N2 N3 83.53(16) . . . . ? N22 Co1 N2 N3 141.9(19) . . . . ? N1 Co1 N2 N3 174.04(17) . . . . ? N21 Co1 N2 N3 -6.89(17) . . . . ? C6 N2 N3 C7 1.01(19) . . . . ? Co1 N2 N3 C7 -161.87(13) . . . . ? N2 N3 C7 N5 -1.89(19) . . . . ? N2 N3 C7 C8 178.12(16) . . . . ? N3 C7 C8 N4 163.49(17) . . . . ? N5 C7 C8 N4 -16.5(3) . . . . ? N3 C7 C8 C9 -15.9(3) . . . . ? N5 C7 C8 C9 164.08(17) . . . . ? N4 C8 C9 C10 1.3(3) . . . . ? C7 C8 C9 C10 -179.34(17) . . . . ? C8 C9 C10 C11 -0.4(3) . . . . ? C9 C10 C11 C12 -0.4(3) . . . . ? C10 C11 C12 N4 0.4(3) . . . . ? C11 C12 N4 C8 0.4(3) . . . . ? C9 C8 N4 C12 -1.2(3) . . . . ? C7 C8 N4 C12 179.36(16) . . . . ? N2 C6 N5 C7 -1.4(2) . . . . ? C5 C6 N5 C7 177.37(18) . . . . ? N2 C6 N5 N6 -178.10(15) . . . . ? C5 C6 N5 N6 0.6(3) . . . . ? N3 C7 N5 C6 2.1(2) . . . . ? C8 C7 N5 C6 -177.96(17) . . . . ? N3 C7 N5 N6 178.56(16) . . . . ? C8 C7 N5 N6 -1.5(3) . . . . ? O71 Co1 N21 C21 97.61(15) . . . . ? O81 Co1 N21 C21 -78.85(15) . . . . ? N2 Co1 N21 C21 6.13(16) . . . . ? N22 Co1 N21 C21 -172.94(15) . . . . ? N1 Co1 N21 C21 153.0(19) . . . . ? O71 Co1 N21 C25 -79.60(13) . . . . ? O81 Co1 N21 C25 103.94(13) . . . . ? N2 Co1 N21 C25 -171.08(12) . . . . ? N22 Co1 N21 C25 9.85(12) . . . . ? N1 Co1 N21 C25 -24(2) . . . . ? C25 N21 C21 C22 0.1(3) . . . . ? Co1 N21 C21 C22 -177.03(14) . . . . ? N21 C21 C22 C23 0.6(3) . . . . ? C21 C22 C23 C24 -0.5(3) . . . . ? C22 C23 C24 C25 -0.3(3) . . . . ? C21 N21 C25 C24 -0.9(3) . . . . ? Co1 N21 C25 C24 176.53(14) . . . . ? C21 N21 C25 C26 177.18(15) . . . . ? Co1 N21 C25 C26 -5.39(19) . . . . ? C23 C24 C25 N21 1.0(3) . . . . ? C23 C24 C25 C26 -176.82(17) . . . . ? N21 C25 C26 N22 -6.3(2) . . . . ? C24 C25 C26 N22 171.71(18) . . . . ? N21 C25 C26 N25 174.34(17) . . . . ? C24 C25 C26 N25 -7.7(3) . . . . ? N25 C26 N22 N23 0.4(2) . . . . ? C25 C26 N22 N23 -179.11(15) . . . . ? N25 C26 N22 Co1 -165.75(11) . . . . ? C25 C26 N22 Co1 14.8(2) . . . . ? O71 Co1 N22 C26 74.17(13) . . . . ? O81 Co1 N22 C26 -103.46(13) . . . . ? N2 Co1 N22 C26 -161.7(19) . . . . ? N1 Co1 N22 C26 166.35(12) . . . . ? N21 Co1 N22 C26 -12.69(12) . . . . ? O71 Co1 N22 N23 -86.83(16) . . . . ? O81 Co1 N22 N23 95.54(16) . . . . ? N2 Co1 N22 N23 37(2) . . . . ? N1 Co1 N22 N23 5.36(17) . . . . ? N21 Co1 N22 N23 -173.69(17) . . . . ? C26 N22 N23 C27 -0.87(19) . . . . ? Co1 N22 N23 C27 160.71(14) . . . . ? N22 N23 C27 N25 1.02(19) . . . . ? N22 N23 C27 C28 179.28(17) . . . . ? N23 C27 C28 N24 -156.81(17) . . . . ? N25 C27 C28 N24 21.2(3) . . . . ? N23 C27 C28 C29 22.0(3) . . . . ? N25 C27 C28 C29 -160.04(18) . . . . ? N24 C28 C29 C30 0.2(3) . . . . ? C27 C28 C29 C30 -178.50(18) . . . . ? C28 C29 C30 C31 -0.1(3) . . . . ? C29 C30 C31 C32 -0.3(3) . . . . ? C30 C31 C32 N24 0.6(3) . . . . ? C31 C32 N24 C28 -0.5(3) . . . . ? C29 C28 N24 C32 0.1(3) . . . . ? C27 C28 N24 C32 178.80(17) . . . . ? N22 C26 N25 C27 0.2(2) . . . . ? C25 C26 N25 C27 179.66(18) . . . . ? N22 C26 N25 N26 174.65(15) . . . . ? C25 C26 N25 N26 -5.9(3) . . . . ? N23 C27 N25 C26 -0.8(2) . . . . ? C28 C27 N25 C26 -179.06(17) . . . . ? N23 C27 N25 N26 -174.90(16) . . . . ? C28 C27 N25 N26 6.9(3) . . . . ? O81 Co1 O71 C72 -70.4(8) . . . . ? N2 Co1 O71 C72 -31.43(19) . . . . ? N22 Co1 O71 C72 147.13(19) . . . . ? N1 Co1 O71 C72 45.38(19) . . . . ? N21 Co1 O71 C72 -135.99(19) . . . . ? O71 Co1 O81 C82 -97.5(8) . . . . ? N2 Co1 O81 C82 -136.58(15) . . . . ? N22 Co1 O81 C82 44.90(15) . . . . ? N1 Co1 O81 C82 146.67(15) . . . . ? N21 Co1 O81 C82 -32.01(15) . . . . ? O91 Co2 N41 C41 -82.49(15) 3_666 . . . ? O91 Co2 N41 C41 97.50(15) . . . . ? N42 Co2 N41 C41 4.43(16) 3_666 . . . ? N42 Co2 N41 C41 -175.57(16) . . . . ? N41 Co2 N41 C41 170(14) 3_666 . . . ? O91 Co2 N41 C45 102.43(12) 3_666 . . . ? O91 Co2 N41 C45 -77.57(12) . . . . ? N42 Co2 N41 C45 -170.65(12) 3_666 . . . ? N42 Co2 N41 C45 9.35(12) . . . . ? N41 Co2 N41 C45 -5(14) 3_666 . . . ? C45 N41 C41 C42 0.3(3) . . . . ? Co2 N41 C41 C42 -174.66(14) . . . . ? N41 C41 C42 C43 0.4(3) . . . . ? C41 C42 C43 C44 -0.7(3) . . . . ? C42 C43 C44 C45 0.3(3) . . . . ? C41 N41 C45 C44 -0.8(3) . . . . ? Co2 N41 C45 C44 174.74(14) . . . . ? C41 N41 C45 C46 178.54(15) . . . . ? Co2 N41 C45 C46 -5.96(18) . . . . ? C43 C44 C45 N41 0.5(3) . . . . ? C43 C44 C45 C46 -178.73(17) . . . . ? N41 C45 C46 N42 -4.1(2) . . . . ? C44 C45 C46 N42 175.18(17) . . . . ? N41 C45 C46 N45 175.14(18) . . . . ? C44 C45 C46 N45 -5.6(3) . . . . ? N45 C46 N42 N43 0.2(2) . . . . ? C45 C46 N42 N43 179.54(15) . . . . ? N45 C46 N42 Co2 -167.17(11) . . . . ? C45 C46 N42 Co2 12.2(2) . . . . ? O91 Co2 N42 C46 -103.26(13) 3_666 . . . ? O91 Co2 N42 C46 76.74(13) . . . . ? N42 Co2 N42 C46 12(3) 3_666 . . . ? N41 Co2 N42 C46 168.86(12) 3_666 . . . ? N41 Co2 N42 C46 -11.14(12) . . . . ? O91 Co2 N42 N43 93.92(16) 3_666 . . . ? O91 Co2 N42 N43 -86.08(16) . . . . ? N42 Co2 N42 N43 -151(3) 3_666 . . . ? N41 Co2 N42 N43 6.04(17) 3_666 . . . ? N41 Co2 N42 N43 -173.96(17) . . . . ? C46 N42 N43 C47 -0.96(19) . . . . ? Co2 N42 N43 C47 162.50(13) . . . . ? N42 N43 C47 N45 1.39(19) . . . . ? N42 N43 C47 C48 -179.23(16) . . . . ? N43 C47 C48 N44 -163.06(17) . . . . ? N45 C47 C48 N44 16.2(3) . . . . ? N43 C47 C48 C49 16.7(3) . . . . ? N45 C47 C48 C49 -164.03(17) . . . . ? N44 C48 C49 C50 -0.9(3) . . . . ? C47 C48 C49 C50 179.34(17) . . . . ? C48 C49 C50 C51 0.3(3) . . . . ? C49 C50 C51 C52 0.4(3) . . . . ? C50 C51 C52 N44 -0.5(3) . . . . ? C51 C52 N44 C48 -0.1(3) . . . . ? C49 C48 N44 C52 0.9(3) . . . . ? C47 C48 N44 C52 -179.40(16) . . . . ? N42 C46 N45 C47 0.7(2) . . . . ? C45 C46 N45 C47 -178.62(18) . . . . ? N42 C46 N45 N46 176.26(15) . . . . ? C45 C46 N45 N46 -3.0(3) . . . . ? N43 C47 N45 C46 -1.3(2) . . . . ? C48 C47 N45 C46 179.33(17) . . . . ? N43 C47 N45 N46 -176.63(16) . . . . ? C48 C47 N45 N46 4.0(3) . . . . ? O91 Co2 O91 C92 -80(5) 3_666 . . . ? N42 Co2 O91 C92 -27.20(18) 3_666 . . . ? N42 Co2 O91 C92 152.80(18) . . . . ? N41 Co2 O91 C92 49.73(18) 3_666 . . . ? N41 Co2 O91 C92 -130.27(18) . . . . ? O12 S1 C101 C102 173.65(14) . . . . ? O13 S1 C101 C102 -64.21(16) . . . . ? O11 S1 C101 C102 53.69(16) . . . . ? S1 C101 C102 C103 -179.96(13) . . . . ? C101 C102 C103 C104 174.85(16) . . . . ? C102 C103 C104 C105 177.19(16) . . . . ? C103 C104 C105 C106 178.41(16) . . . . ? C104 C105 C106 C107 179.36(16) . . . . ? C105 C106 C107 C108 179.36(16) . . . . ? C106 C107 C108 C109 179.90(16) . . . . ? C107 C108 C109 C110 179.90(16) . . . . ? C108 C109 C110 C111 178.62(16) . . . . ? C109 C110 C111 C112 179.09(16) . . . . ? C110 C111 C112 C113 179.19(17) . . . . ? C111 C112 C113 C114 -179.37(17) . . . . ? C112 C113 C114 C115 175.56(17) . . . . ? C113 C114 C115 C116 177.37(17) . . . . ? O22 S2 C121 C122 66.18(16) . . . . ? O23 S2 C121 C122 -171.77(15) . . . . ? O21 S2 C121 C122 -52.60(16) . . . . ? S2 C121 C122 C123 -178.33(14) . . . . ? C121 C122 C123 C124 -175.39(17) . . . . ? C122 C123 C124 C125 -178.90(17) . . . . ? C123 C124 C125 C126 -176.30(17) . . . . ? C124 C125 C126 C127 -178.40(17) . . . . ? C125 C126 C127 C128 177.12(17) . . . . ? C126 C127 C128 C129 -177.69(17) . . . . ? C127 C128 C129 C130 178.00(17) . . . . ? C128 C129 C130 C131 -178.76(16) . . . . ? C129 C130 C131 C132 -178.84(16) . . . . ? C130 C131 C132 C133 -178.13(16) . . . . ? C131 C132 C133 C134 -175.19(16) . . . . ? C132 C133 C134 C135 175.04(16) . . . . ? C133 C134 C135 C136 -171.67(17) . . . . ? O32 S3 C141 C142 63.63(16) . . . . ? O33 S3 C141 C142 -175.14(14) . . . . ? O31 S3 C141 C142 -55.38(16) . . . . ? S3 C141 C142 C143 176.93(13) . . . . ? C141 C142 C143 C144 -176.02(16) . . . . ? C142 C143 C144 C145 -175.99(16) . . . . ? C143 C144 C145 C146 -178.16(16) . . . . ? C144 C145 C146 C147 -178.63(16) . . . . ? C145 C146 C147 C148 -178.83(16) . . . . ? C146 C147 C148 C149 -179.76(16) . . . . ? C147 C148 C149 C150 -178.75(16) . . . . ? C148 C149 C150 C151 -178.95(16) . . . . ? C149 C150 C151 C152 -176.84(17) . . . . ? C150 C151 C152 C153 178.98(17) . . . . ? C151 C152 C153 C154 -178.77(16) . . . . ? C152 C153 C154 C155 176.21(17) . . . . ? C153 C154 C155 C156 -172.17(17) . . . . ? 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 N6 H6X N4 0.97 2.07 2.866(2) 137.6 . N6 H6Y O13 0.90 1.98 2.849(2) 163.4 . N26 H26X O22 0.91 2.03 2.903(2) 160.6 . N26 H26Y N24 0.90 2.16 2.887(2) 137.5 . N46 H46X N44 0.88 2.17 2.861(2) 134.3 . N46 H46Y O32 0.96 1.93 2.861(2) 162.7 . O71 H71X O21 0.93 1.67 2.591(2) 167.9 . O81 H81X O11 0.91 1.68 2.5831(19) 173.9 . O91 H91X O31 0.92 1.69 2.6144(19) 177.5 . O161 H16X O23 0.94 1.89 2.778(2) 156.7 . O171 H17X O33 0.95 1.83 2.756(2) 163.0 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.63 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.684 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.058