# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email m.murugesu@uottawa.ca _publ_contact_author_name 'Muralee Murugesu' _publ_author_name 'Muralee Murugesu' data_p-1 _database_code_depnum_ccdc_archive 'CCDC 815193' #TrackingRef '4432_web_deposit_cif_file_0_MuraleeMURUGESU_1298934407.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H130 Fe3 N24 O40 S6' _chemical_formula_weight 2740.25 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 14.5077(7) _cell_length_b 15.0789(7) _cell_length_c 16.3192(13) _cell_angle_alpha 107.611(3) _cell_angle_beta 100.282(3) _cell_angle_gamma 110.437(2) _cell_volume 3022.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9870 _cell_measurement_theta_min 2.407 _cell_measurement_theta_max 30.543 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8786 _exptl_absorpt_correction_T_max 0.9571 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _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 APEXII CCD' _diffrn_measurement_method ' \f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60055 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.61 _reflns_number_total 18545 _reflns_number_gt 14220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _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. ; _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^)+(0.0523P)^2^+0.6178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18545 _refine_ls_number_parameters 1057 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.007 _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 0.871068(17) 0.645338(16) -0.097450(15) 0.00945(5) Uani 1 1 d . . . Fe2 Fe 1.0000 0.5000 0.0000 0.00805(6) Uani 1 2 d S . . O1 O 1.14875(11) 1.17380(10) 0.52785(9) 0.0274(3) Uani 1 1 d . . . O2 O 1.15378(16) 1.07087(12) 0.59447(10) 0.0439(4) Uani 1 1 d . . . O3 O 0.60875(12) 0.43154(12) 0.44245(10) 0.0325(3) Uani 1 1 d . . . O4 O 0.58167(10) 0.27162(10) 0.40100(9) 0.0241(3) Uani 1 1 d . . . O5 O 0.21132(10) 0.03408(10) -0.23566(9) 0.0253(3) Uani 1 1 d . . . O6 O 0.28000(11) -0.07360(10) -0.25611(12) 0.0364(4) Uani 1 1 d . . . O7 O 0.95618(9) 0.79702(9) -0.08737(8) 0.0152(2) Uani 1 1 d . . . O8 O 0.75481(9) 0.67870(9) -0.05614(8) 0.0146(2) Uani 1 1 d . . . O9 O 0.78954(10) 0.59672(10) -0.23432(8) 0.0166(2) Uani 1 1 d . . . N1 N 1.00119(10) 0.63328(9) 0.07517(9) 0.0104(2) Uani 1 1 d . . . N2 N 0.95923(10) 0.68915(10) 0.04012(9) 0.0112(2) Uani 1 1 d . . . N3 N 1.02338(10) 0.77075(10) 0.18709(9) 0.0115(2) Uani 1 1 d . . . N4 N 1.13974(13) 1.08945(12) 0.52666(10) 0.0229(3) Uani 1 1 d . . . N5 N 1.01529(10) 0.40285(10) 0.13628(9) 0.0112(2) Uani 1 1 d . . . N6 N 0.96431(10) 0.44790(9) 0.09481(9) 0.0100(2) Uani 1 1 d . . . N7 N 0.89413(10) 0.41298(10) 0.19548(9) 0.0110(2) Uani 1 1 d . . . N8 N 0.62495(11) 0.35848(12) 0.40257(10) 0.0188(3) Uani 1 1 d . . . N9 N 0.79716(10) 0.49396(10) -0.09860(9) 0.0112(2) Uani 1 1 d . . . N10 N 0.84677(10) 0.44242(9) -0.06472(8) 0.0099(2) Uani 1 1 d . . . N11 N 0.68027(10) 0.34198(10) -0.12438(9) 0.0114(2) Uani 1 1 d . . . N12 N 0.28572(11) 0.01418(11) -0.23473(10) 0.0190(3) Uani 1 1 d . . . C1 C 0.97366(12) 0.77000(12) 0.10874(11) 0.0127(3) Uani 1 1 d . . . C2 C 1.03888(12) 0.68371(11) 0.16369(11) 0.0116(3) Uani 1 1 d . . . C3 C 1.05435(12) 0.85071(12) 0.27452(10) 0.0131(3) Uani 1 1 d . . . C4 C 1.08477(14) 0.95121(12) 0.27981(12) 0.0167(3) Uani 1 1 d . . . C5 C 1.11076(14) 1.03011(13) 0.36290(12) 0.0185(3) Uani 1 1 d . . . C6 C 1.10999(13) 1.00581(13) 0.43792(11) 0.0173(3) Uani 1 1 d . . . C7 C 1.08251(14) 0.90669(13) 0.43362(12) 0.0188(3) Uani 1 1 d . . . C8 C 1.05257(13) 0.82717(13) 0.34994(11) 0.0163(3) Uani 1 1 d . . . C9 C 0.89218(12) 0.45340(12) 0.13172(10) 0.0117(3) Uani 1 1 d . . . C10 C 0.97209(12) 0.38297(12) 0.19610(11) 0.0125(3) Uani 1 1 d . . . C11 C 0.82796(12) 0.40121(12) 0.24998(10) 0.0124(3) Uani 1 1 d . . . C12 C 0.79288(13) 0.31005(13) 0.26368(11) 0.0154(3) Uani 1 1 d . . . C13 C 0.72680(13) 0.29673(13) 0.31532(12) 0.0164(3) Uani 1 1 d . . . C14 C 0.69843(13) 0.37497(13) 0.35108(11) 0.0155(3) Uani 1 1 d . . . C15 C 0.73250(13) 0.46567(13) 0.33770(12) 0.0171(3) Uani 1 1 d . . . C16 C 0.79899(13) 0.47920(12) 0.28637(11) 0.0146(3) Uani 1 1 d . . . C17 C 0.69887(12) 0.43256(12) -0.13318(11) 0.0130(3) Uani 1 1 d . . . C18 C 0.77444(12) 0.35135(11) -0.08101(10) 0.0111(3) Uani 1 1 d . . . C19 C 0.58053(12) 0.25810(11) -0.15119(10) 0.0120(3) Uani 1 1 d . . . C20 C 0.57032(13) 0.15758(12) -0.18536(11) 0.0141(3) Uani 1 1 d . . . C21 C 0.47282(13) 0.07707(12) -0.21254(11) 0.0156(3) Uani 1 1 d . . . C22 C 0.38950(12) 0.09980(12) -0.20585(11) 0.0146(3) Uani 1 1 d . . . C23 C 0.39887(13) 0.19938(13) -0.17151(12) 0.0158(3) Uani 1 1 d . . . C24 C 0.49676(13) 0.28041(12) -0.14252(12) 0.0153(3) Uani 1 1 d . . . C25 C 0.72484(14) 0.75799(13) -0.06399(12) 0.0171(3) Uani 1 1 d . . . C26 C 0.78959(16) 0.85931(14) 0.01602(13) 0.0223(4) Uani 1 1 d . . . C27 C 0.94718(14) 0.86006(13) -0.13665(12) 0.0169(3) Uani 1 1 d . . . C28 C 1.02772(16) 0.87796(16) -0.18396(14) 0.0240(4) Uani 1 1 d . . . S1 S 0.20611(3) -0.10992(3) 0.07224(3) 0.01437(8) Uani 1 1 d . . . S2 S 0.70110(3) 0.57064(3) 0.10801(3) 0.01338(8) Uani 1 1 d . . . S3 S 0.19274(3) 0.64089(3) 0.37316(3) 0.01538(8) Uani 1 1 d . . . O10 O 0.22628(9) -0.11769(10) 0.15973(9) 0.0194(2) Uani 1 1 d . . . O11 O 0.12384(9) -0.07563(9) 0.05637(9) 0.0185(2) Uani 1 1 d . . . O12 O 0.18830(10) -0.20216(9) -0.00303(9) 0.0202(3) Uani 1 1 d . . . O13 O 0.67340(10) 0.46388(9) 0.05354(9) 0.0214(3) Uani 1 1 d . . . O14 O 0.81053(9) 0.62842(10) 0.15994(9) 0.0210(3) Uani 1 1 d . . . O15 O 0.66408(11) 0.62195(11) 0.05543(9) 0.0250(3) Uani 1 1 d . . . O16 O 0.24750(11) 0.59978(10) 0.31688(10) 0.0281(3) Uani 1 1 d . . . O17 O 0.19428(10) 0.61386(10) 0.45164(8) 0.0226(3) Uani 1 1 d . . . O18 O 0.08866(10) 0.61688(9) 0.32061(9) 0.0226(3) Uani 1 1 d . . . C29 C 0.31919(12) -0.01022(12) 0.07682(11) 0.0137(3) Uani 1 1 d . . . C30 C 0.37452(14) 0.07834(13) 0.15589(12) 0.0176(3) Uani 1 1 d . . . C31 C 0.45731(14) 0.15986(13) 0.15607(12) 0.0198(3) Uani 1 1 d . . . C32 C 0.48724(13) 0.15487(13) 0.07899(12) 0.0176(3) Uani 1 1 d . . . C33 C 0.43223(14) 0.06440(13) 0.00108(12) 0.0181(3) Uani 1 1 d . . . C34 C 0.34836(13) -0.01812(13) -0.00071(12) 0.0165(3) Uani 1 1 d . . . C35 C 0.57543(16) 0.24434(15) 0.07839(15) 0.0250(4) Uani 1 1 d . . . C36 C 0.63405(12) 0.57073(12) 0.18836(11) 0.0123(3) Uani 1 1 d . . . C37 C 0.53827(13) 0.48989(12) 0.16783(11) 0.0146(3) Uani 1 1 d . . . C38 C 0.48715(13) 0.49176(13) 0.23251(11) 0.0162(3) Uani 1 1 d . . . C39 C 0.52916(13) 0.57373(13) 0.31681(11) 0.0170(3) Uani 1 1 d . . . C40 C 0.62448(14) 0.65473(13) 0.33516(12) 0.0174(3) Uani 1 1 d . . . C41 C 0.67737(13) 0.65373(12) 0.27225(11) 0.0154(3) Uani 1 1 d . . . C42 C 0.47479(15) 0.57477(16) 0.38746(13) 0.0240(4) Uani 1 1 d . . . H62A H 0.4002 0.5493 0.3584 0.036 Uiso 1 1 calc R . . H62B H 0.5022 0.6454 0.4327 0.036 Uiso 1 1 calc R . . H62C H 0.4866 0.5304 0.4172 0.036 Uiso 1 1 calc R . . C43 C 0.26302(13) 0.77675(12) 0.41480(11) 0.0157(3) Uani 1 1 d . . . C44 C 0.28930(15) 0.83846(14) 0.50514(12) 0.0204(3) Uani 1 1 d . . . C45 C 0.33945(15) 0.94504(14) 0.53451(13) 0.0236(4) Uani 1 1 d . . . C46 C 0.36398(14) 0.99160(13) 0.47471(13) 0.0218(4) Uani 1 1 d . . . C47 C 0.33647(15) 0.92804(14) 0.38371(13) 0.0224(4) Uani 1 1 d . . . C48 C 0.28679(14) 0.82163(13) 0.35368(12) 0.0194(3) Uani 1 1 d . . . C49 C 0.41825(19) 1.10690(15) 0.50701(17) 0.0314(5) Uani 1 1 d . . . O19 O 0.07961(12) 0.40483(11) 0.41016(10) 0.0276(3) Uani 1 1 d . . . O20 O 0.19060(11) 0.30369(11) 0.34794(9) 0.0236(3) Uani 1 1 d . . . C50 C 0.01339(15) 0.38470(15) 0.46407(13) 0.0226(4) Uani 1 1 d . . . C51 C -0.0236(2) 0.2738(2) 0.4512(2) 0.0402(6) Uani 1 1 d . . . C52 C 0.28483(15) 0.31685(15) 0.40613(13) 0.0234(4) Uani 1 1 d . . . C53 C 0.33339(18) 0.26161(19) 0.34840(16) 0.0323(5) Uani 1 1 d . . . H1 H 0.6459(15) 0.4470(14) -0.1630(12) 0.007(4) Uiso 1 1 d . . . H2 H 0.7883(15) 0.3042(15) -0.0629(13) 0.014(5) Uiso 1 1 d . . . H3 H 0.8478(15) 0.4815(15) 0.1181(13) 0.012(5) Uiso 1 1 d . . . H4 H 1.0709(15) 0.6656(15) 0.2065(13) 0.013(5) Uiso 1 1 d . . . H5 H 0.3450(17) 0.2132(16) -0.1667(14) 0.019(5) Uiso 1 1 d . . . H6 H 0.7324(15) 0.7633(14) -0.1198(13) 0.011(5) Uiso 1 1 d . . . H7 H 0.8211(17) 0.5376(16) 0.2740(14) 0.020(5) Uiso 1 1 d . . . H8 H 0.3568(16) 0.0842(15) 0.2078(14) 0.015(5) Uiso 1 1 d . . . H9 H 0.9948(16) 0.3567(15) 0.2349(14) 0.014(5) Uiso 1 1 d . . . H10 H 0.6276(17) 0.1441(16) -0.1915(14) 0.021(5) Uiso 1 1 d . . . H11 H 0.7022(16) 0.2338(16) 0.3235(14) 0.017(5) Uiso 1 1 d . . . H12 H 0.6542(17) 0.7093(16) 0.3909(15) 0.021(5) Uiso 1 1 d . . . H13 H 0.8755(16) 0.8228(15) -0.1822(13) 0.014(5) Uiso 1 1 d . . . H14 H 0.8162(17) 0.2577(17) 0.2371(15) 0.026(6) Uiso 1 1 d . . . H15 H 0.0499(18) 0.4306(17) 0.5267(16) 0.027(6) Uiso 1 1 d . . . H16 H 0.2695(17) 0.7796(17) 0.2909(15) 0.024(5) Uiso 1 1 d . . . H17 H 0.7425(18) 0.7082(17) 0.2880(15) 0.023(5) Uiso 1 1 d . . . H18 H 0.4200(18) 0.4356(17) 0.2195(15) 0.024(6) Uiso 1 1 d . . . H19 H 0.9479(17) 0.8150(16) 0.1032(14) 0.019(5) Uiso 1 1 d . . . H20 H 1.0825(18) 0.8931(17) 0.4865(15) 0.026(6) Uiso 1 1 d . . . H21 H 0.7062(17) 0.5164(17) 0.3600(15) 0.023(5) Uiso 1 1 d . . . H22 H -0.0473(17) 0.4006(15) 0.4457(14) 0.019(5) Uiso 1 1 d . . . H24 H 0.3562(18) 0.9558(17) 0.3418(15) 0.027(6) Uiso 1 1 d . . . H25 H 0.6501(17) 0.7344(15) -0.0704(14) 0.018(5) Uiso 1 1 d . . . H26 H 0.3602(17) 0.9869(17) 0.5993(16) 0.025(6) Uiso 1 1 d . . . H27 H 0.3075(17) -0.0819(16) -0.0575(14) 0.022(5) Uiso 1 1 d . . . H28 H 1.1314(18) 1.0997(18) 0.3697(15) 0.028(6) Uiso 1 1 d . . . H29 H 0.163(2) 0.335(2) 0.3792(18) 0.039(7) Uiso 1 1 d . . . H30 H 0.4646(17) 0.0075(17) -0.2359(15) 0.024(6) Uiso 1 1 d . . . H31 H 0.5098(16) 0.4349(16) 0.1081(14) 0.017(5) Uiso 1 1 d . . . H32 H 0.5532(19) 0.2684(19) 0.0369(17) 0.035(7) Uiso 1 1 d . . . H33 H 0.2712(17) 0.2889(16) 0.4488(15) 0.023(5) Uiso 1 1 d . . . H34 H 0.5045(17) 0.3458(17) -0.1156(14) 0.021(5) Uiso 1 1 d . . . H35 H 1.0339(18) 0.7583(18) 0.3461(15) 0.026(6) Uiso 1 1 d . . . H36 H 1.0160(19) 0.8126(19) -0.2321(16) 0.032(6) Uiso 1 1 d . . . H37 H 0.4528(16) 0.0590(15) -0.0535(14) 0.017(5) Uiso 1 1 d . . . H38 H 0.7902(19) 0.6253(19) -0.2673(17) 0.029(6) Uiso 1 1 d . . . H39 H 0.8625(19) 0.8840(17) 0.0195(15) 0.028(6) Uiso 1 1 d . . . H40 H 1.097(2) 0.9077(19) -0.1424(17) 0.036(7) Uiso 1 1 d . . . H41 H 1.024(2) 0.9241(19) -0.2157(17) 0.038(7) Uiso 1 1 d . . . H42 H 0.494(2) 0.2217(19) 0.2124(17) 0.036(6) Uiso 1 1 d . . . H43 H 0.9532(17) 0.9280(17) -0.0942(15) 0.023(5) Uiso 1 1 d . . . H44 H 0.2718(18) 0.8086(17) 0.5462(16) 0.028(6) Uiso 1 1 d . . . H45 H 1.0905(18) 0.9660(17) 0.2293(16) 0.029(6) Uiso 1 1 d . . . H47 H 0.7846(18) 0.8517(17) 0.0707(16) 0.029(6) Uiso 1 1 d . . . H48 H 0.7751(19) 0.536(2) -0.2690(17) 0.035(7) Uiso 1 1 d . . . H49 H 0.606(2) 0.299(2) 0.1359(18) 0.036(7) Uiso 1 1 d . . . H50 H 0.395(2) 0.2654(18) 0.3831(16) 0.031(6) Uiso 1 1 d . . . H51 H 0.762(2) 0.907(2) 0.0069(17) 0.041(7) Uiso 1 1 d . . . H52 H 1.013(2) 0.830(2) -0.046(2) 0.052(8) Uiso 1 1 d . . . H53 H 0.034(2) 0.265(2) 0.4745(19) 0.050(8) Uiso 1 1 d . . . H55 H -0.069(2) 0.257(2) 0.4848(18) 0.045(7) Uiso 1 1 d . . . H57 H 0.733(2) 0.660(2) -0.0154(19) 0.049(8) Uiso 1 1 d . . . H58 H 0.628(2) 0.226(2) 0.059(2) 0.055(8) Uiso 1 1 d . . . H59 H -0.064(3) 0.224(2) 0.387(2) 0.064(10) Uiso 1 1 d . . . H60 H 0.330(2) 0.395(2) 0.4392(18) 0.048(8) Uiso 1 1 d . . . H61 H 0.284(2) 0.186(2) 0.3143(19) 0.049(8) Uiso 1 1 d . . . H62 H 0.349(2) 0.293(2) 0.306(2) 0.051(8) Uiso 1 1 d . . . H63 H 0.107(2) 0.469(2) 0.424(2) 0.053(9) Uiso 1 1 d . . . H64 H 0.378(3) 1.132(2) 0.480(2) 0.064(9) Uiso 1 1 d . . . H65 H 0.426(3) 1.142(3) 0.566(2) 0.070(10) Uiso 1 1 d . . . H66 H 0.482(3) 1.128(3) 0.497(2) 0.073(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00922(10) 0.00962(10) 0.01021(10) 0.00451(8) 0.00426(8) 0.00375(8) Fe2 0.00757(13) 0.00795(13) 0.00873(14) 0.00378(11) 0.00327(11) 0.00272(10) O1 0.0306(7) 0.0164(6) 0.0237(7) -0.0012(5) 0.0069(6) 0.0061(5) O2 0.0781(13) 0.0346(8) 0.0127(7) 0.0040(6) 0.0093(7) 0.0245(9) O3 0.0393(9) 0.0355(8) 0.0376(8) 0.0164(7) 0.0304(7) 0.0217(7) O4 0.0200(6) 0.0307(7) 0.0286(7) 0.0184(6) 0.0148(6) 0.0092(5) O5 0.0124(6) 0.0259(7) 0.0320(7) 0.0100(6) 0.0071(5) 0.0033(5) O6 0.0245(7) 0.0131(6) 0.0608(11) 0.0075(6) 0.0161(7) 0.0012(5) O7 0.0136(6) 0.0126(5) 0.0175(6) 0.0089(4) 0.0023(5) 0.0025(4) O8 0.0164(6) 0.0172(5) 0.0189(6) 0.0112(5) 0.0106(5) 0.0109(5) O9 0.0206(6) 0.0167(6) 0.0120(6) 0.0053(5) 0.0030(5) 0.0089(5) N1 0.0087(6) 0.0107(6) 0.0126(6) 0.0061(5) 0.0043(5) 0.0035(5) N2 0.0109(6) 0.0107(6) 0.0142(6) 0.0065(5) 0.0043(5) 0.0055(5) N3 0.0120(6) 0.0098(6) 0.0117(6) 0.0035(5) 0.0042(5) 0.0038(5) N4 0.0243(8) 0.0207(7) 0.0147(7) -0.0004(6) 0.0049(6) 0.0066(6) N5 0.0112(6) 0.0109(6) 0.0116(6) 0.0052(5) 0.0033(5) 0.0043(5) N6 0.0096(6) 0.0091(5) 0.0110(6) 0.0040(5) 0.0031(5) 0.0037(4) N7 0.0114(6) 0.0129(6) 0.0114(6) 0.0059(5) 0.0062(5) 0.0059(5) N8 0.0164(7) 0.0265(7) 0.0178(7) 0.0116(6) 0.0102(6) 0.0092(6) N9 0.0106(6) 0.0118(6) 0.0116(6) 0.0054(5) 0.0029(5) 0.0049(5) N10 0.0111(6) 0.0101(5) 0.0101(6) 0.0049(5) 0.0045(5) 0.0049(5) N11 0.0102(6) 0.0110(6) 0.0131(6) 0.0057(5) 0.0043(5) 0.0036(5) N12 0.0158(7) 0.0157(7) 0.0197(7) 0.0058(6) 0.0067(6) 0.0009(5) C1 0.0127(7) 0.0126(7) 0.0131(7) 0.0052(6) 0.0038(6) 0.0058(6) C2 0.0102(7) 0.0113(6) 0.0133(7) 0.0050(5) 0.0046(6) 0.0039(5) C3 0.0118(7) 0.0125(7) 0.0107(7) 0.0012(5) 0.0035(6) 0.0037(5) C4 0.0208(8) 0.0139(7) 0.0142(8) 0.0058(6) 0.0064(6) 0.0056(6) C5 0.0201(8) 0.0136(7) 0.0175(8) 0.0033(6) 0.0053(7) 0.0053(6) C6 0.0167(8) 0.0161(7) 0.0125(7) 0.0000(6) 0.0037(6) 0.0051(6) C7 0.0227(9) 0.0203(8) 0.0141(8) 0.0071(6) 0.0071(7) 0.0092(7) C8 0.0188(8) 0.0164(7) 0.0146(8) 0.0061(6) 0.0069(6) 0.0080(6) C9 0.0121(7) 0.0120(7) 0.0117(7) 0.0050(5) 0.0054(6) 0.0051(5) C10 0.0119(7) 0.0134(7) 0.0142(7) 0.0064(6) 0.0054(6) 0.0060(6) C11 0.0109(7) 0.0155(7) 0.0105(7) 0.0057(6) 0.0046(5) 0.0045(6) C12 0.0164(8) 0.0175(7) 0.0166(8) 0.0091(6) 0.0087(6) 0.0084(6) C13 0.0154(8) 0.0187(8) 0.0188(8) 0.0110(6) 0.0085(6) 0.0070(6) C14 0.0135(7) 0.0222(8) 0.0132(7) 0.0090(6) 0.0079(6) 0.0068(6) C15 0.0180(8) 0.0193(8) 0.0174(8) 0.0073(6) 0.0095(6) 0.0101(6) C16 0.0154(7) 0.0150(7) 0.0154(7) 0.0074(6) 0.0075(6) 0.0061(6) C17 0.0125(7) 0.0128(7) 0.0150(7) 0.0071(6) 0.0046(6) 0.0052(6) C18 0.0115(7) 0.0111(6) 0.0110(7) 0.0044(5) 0.0043(5) 0.0046(5) C19 0.0098(7) 0.0119(7) 0.0109(7) 0.0040(5) 0.0022(5) 0.0020(5) C20 0.0131(7) 0.0139(7) 0.0157(7) 0.0059(6) 0.0061(6) 0.0054(6) C21 0.0169(8) 0.0108(7) 0.0160(8) 0.0039(6) 0.0059(6) 0.0035(6) C22 0.0120(7) 0.0134(7) 0.0142(7) 0.0059(6) 0.0041(6) 0.0005(6) C23 0.0120(7) 0.0166(7) 0.0198(8) 0.0086(6) 0.0063(6) 0.0053(6) C24 0.0139(7) 0.0119(7) 0.0193(8) 0.0055(6) 0.0056(6) 0.0050(6) C25 0.0177(8) 0.0195(8) 0.0222(8) 0.0122(7) 0.0084(7) 0.0125(6) C26 0.0276(10) 0.0187(8) 0.0245(9) 0.0086(7) 0.0098(8) 0.0134(7) C27 0.0197(8) 0.0160(7) 0.0192(8) 0.0115(6) 0.0076(7) 0.0077(6) C28 0.0238(10) 0.0262(9) 0.0246(9) 0.0156(8) 0.0106(8) 0.0075(7) S1 0.01166(17) 0.01223(17) 0.01907(19) 0.00757(14) 0.00425(15) 0.00412(14) S2 0.01456(18) 0.01512(17) 0.01581(18) 0.00856(14) 0.00950(15) 0.00788(14) S3 0.01717(19) 0.01324(17) 0.01365(18) 0.00515(14) 0.00364(15) 0.00501(14) O10 0.0160(6) 0.0238(6) 0.0234(6) 0.0150(5) 0.0083(5) 0.0082(5) O11 0.0124(5) 0.0152(5) 0.0261(6) 0.0084(5) 0.0032(5) 0.0053(4) O12 0.0203(6) 0.0115(5) 0.0250(7) 0.0057(5) 0.0055(5) 0.0048(5) O13 0.0270(7) 0.0173(6) 0.0216(6) 0.0053(5) 0.0155(5) 0.0096(5) O14 0.0133(6) 0.0238(6) 0.0257(7) 0.0095(5) 0.0101(5) 0.0059(5) O15 0.0317(7) 0.0400(8) 0.0301(7) 0.0276(6) 0.0224(6) 0.0268(6) O16 0.0321(8) 0.0182(6) 0.0328(8) 0.0049(5) 0.0185(6) 0.0099(5) O17 0.0254(7) 0.0202(6) 0.0180(6) 0.0105(5) 0.0020(5) 0.0050(5) O18 0.0202(6) 0.0179(6) 0.0227(7) 0.0088(5) -0.0015(5) 0.0040(5) C29 0.0119(7) 0.0132(7) 0.0158(7) 0.0062(6) 0.0036(6) 0.0051(6) C30 0.0182(8) 0.0169(7) 0.0151(8) 0.0050(6) 0.0061(6) 0.0054(6) C31 0.0175(8) 0.0158(8) 0.0186(8) 0.0044(6) 0.0024(7) 0.0026(6) C32 0.0133(7) 0.0184(8) 0.0238(9) 0.0124(7) 0.0050(6) 0.0066(6) C33 0.0186(8) 0.0220(8) 0.0180(8) 0.0110(7) 0.0085(7) 0.0093(7) C34 0.0160(8) 0.0160(7) 0.0163(8) 0.0054(6) 0.0045(6) 0.0068(6) C35 0.0204(9) 0.0220(9) 0.0324(11) 0.0159(8) 0.0085(8) 0.0044(7) C36 0.0115(7) 0.0142(7) 0.0139(7) 0.0071(6) 0.0063(6) 0.0061(6) C37 0.0137(7) 0.0152(7) 0.0141(7) 0.0054(6) 0.0057(6) 0.0050(6) C38 0.0110(7) 0.0198(8) 0.0175(8) 0.0085(6) 0.0051(6) 0.0048(6) C39 0.0150(8) 0.0246(8) 0.0156(8) 0.0104(7) 0.0072(6) 0.0100(6) C40 0.0181(8) 0.0181(8) 0.0134(8) 0.0038(6) 0.0047(6) 0.0073(6) C41 0.0148(7) 0.0143(7) 0.0163(8) 0.0063(6) 0.0057(6) 0.0046(6) C42 0.0190(9) 0.0350(10) 0.0188(9) 0.0099(7) 0.0112(7) 0.0104(7) C43 0.0140(7) 0.0148(7) 0.0163(8) 0.0051(6) 0.0034(6) 0.0056(6) C44 0.0262(9) 0.0202(8) 0.0149(8) 0.0075(7) 0.0061(7) 0.0097(7) C45 0.0279(10) 0.0199(8) 0.0158(8) 0.0026(7) 0.0025(7) 0.0085(7) C46 0.0189(8) 0.0172(8) 0.0251(9) 0.0054(7) 0.0057(7) 0.0065(6) C47 0.0234(9) 0.0198(8) 0.0225(9) 0.0096(7) 0.0107(7) 0.0047(7) C48 0.0214(9) 0.0173(8) 0.0151(8) 0.0042(6) 0.0068(7) 0.0050(6) C49 0.0324(12) 0.0140(8) 0.0377(12) 0.0053(8) 0.0080(10) 0.0046(8) O19 0.0335(8) 0.0212(7) 0.0355(8) 0.0153(6) 0.0213(6) 0.0114(6) O20 0.0259(7) 0.0310(7) 0.0174(6) 0.0100(5) 0.0081(5) 0.0150(6) C50 0.0239(9) 0.0258(9) 0.0200(9) 0.0090(7) 0.0100(7) 0.0113(7) C51 0.0458(14) 0.0378(13) 0.0637(18) 0.0354(13) 0.0375(14) 0.0244(11) C52 0.0221(9) 0.0253(9) 0.0176(9) 0.0097(7) 0.0023(7) 0.0053(7) C53 0.0254(10) 0.0424(13) 0.0334(12) 0.0174(10) 0.0097(9) 0.0171(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O8 2.0847(12) . ? Fe1 O9 2.0943(12) . ? Fe1 O7 2.1238(11) . ? Fe1 N5 2.1397(13) 2_765 ? Fe1 N2 2.1447(13) . ? Fe1 N9 2.1489(13) . ? Fe2 N6 2.0041(13) 2_765 ? Fe2 N6 2.0041(13) . ? Fe2 N1 2.0052(13) . ? Fe2 N1 2.0052(13) 2_765 ? Fe2 N10 2.0175(13) . ? Fe2 N10 2.0175(13) 2_765 ? O1 N4 1.226(2) . ? O2 N4 1.221(2) . ? O3 N8 1.222(2) . ? O4 N8 1.2288(19) . ? O5 N12 1.216(2) . ? O6 N12 1.2305(19) . ? O7 C27 1.4420(19) . ? O7 H52 0.84(3) . ? O8 C25 1.4391(19) . ? O8 H57 0.86(3) . ? O9 H38 0.79(3) . ? O9 H48 0.85(3) . ? N1 C2 1.314(2) . ? N1 N2 1.3902(17) . ? N2 C1 1.302(2) . ? N3 C1 1.346(2) . ? N3 C2 1.3611(19) . ? N3 C3 1.4295(19) . ? N4 C6 1.472(2) . ? N5 C10 1.304(2) . ? N5 N6 1.3846(17) . ? N5 Fe1 2.1397(13) 2_765 ? N6 C9 1.312(2) . ? N7 C10 1.356(2) . ? N7 C9 1.3565(19) . ? N7 C11 1.4231(19) . ? N8 C14 1.472(2) . ? N9 C17 1.298(2) . ? N9 N10 1.3915(17) . ? N10 C18 1.3157(19) . ? N11 C17 1.3544(19) . ? N11 C18 1.359(2) . ? N11 C19 1.4305(19) . ? N12 C22 1.475(2) . ? C1 H19 0.90(2) . ? C2 H4 0.93(2) . ? C3 C8 1.382(2) . ? C3 C4 1.392(2) . ? C4 C5 1.387(2) . ? C4 H45 0.93(2) . ? C5 C6 1.381(2) . ? C5 H28 0.95(2) . ? C6 C7 1.381(2) . ? C7 C8 1.387(2) . ? C7 H20 0.95(2) . ? C8 H35 0.96(2) . ? C9 H3 0.92(2) . ? C10 H9 0.91(2) . ? C11 C16 1.387(2) . ? C11 C12 1.392(2) . ? C12 C13 1.388(2) . ? C12 H14 0.98(2) . ? C13 C14 1.382(2) . ? C13 H11 0.95(2) . ? C14 C15 1.382(2) . ? C15 C16 1.389(2) . ? C15 H21 0.97(2) . ? C16 H7 0.92(2) . ? C17 H1 0.960(19) . ? C18 H2 0.92(2) . ? C19 C24 1.389(2) . ? C19 C20 1.390(2) . ? C20 C21 1.387(2) . ? C20 H10 0.94(2) . ? C21 C22 1.380(2) . ? C21 H30 0.96(2) . ? C22 C23 1.381(2) . ? C23 C24 1.390(2) . ? C23 H5 0.89(2) . ? C24 H34 0.91(2) . ? C25 C26 1.508(3) . ? C25 H6 0.96(2) . ? C25 H25 0.99(2) . ? C26 H39 0.98(2) . ? C26 H47 0.95(2) . ? C26 H51 0.98(3) . ? C27 C28 1.504(3) . ? C27 H13 1.01(2) . ? C27 H43 1.01(2) . ? C28 H36 0.99(2) . ? C28 H40 0.97(3) . ? C28 H41 1.00(3) . ? S1 O12 1.4533(13) . ? S1 O10 1.4538(13) . ? S1 O11 1.4698(12) . ? S1 C29 1.7673(16) . ? S2 O13 1.4484(12) . ? S2 O14 1.4507(13) . ? S2 O15 1.4665(13) . ? S2 C36 1.7666(16) . ? S3 O18 1.4541(13) . ? S3 O16 1.4556(14) . ? S3 O17 1.4557(13) . ? S3 C43 1.7747(17) . ? C29 C34 1.389(2) . ? C29 C30 1.390(2) . ? C30 C31 1.385(2) . ? C30 H8 0.92(2) . ? C31 C32 1.392(3) . ? C31 H42 0.98(3) . ? C32 C33 1.394(2) . ? C32 C35 1.505(2) . ? C33 C34 1.392(2) . ? C33 H37 0.98(2) . ? C34 H27 1.00(2) . ? C35 H32 0.92(3) . ? C35 H49 0.94(3) . ? C35 H58 0.97(3) . ? C36 C37 1.390(2) . ? C36 C41 1.394(2) . ? C37 C38 1.393(2) . ? C37 H31 0.97(2) . ? C38 C39 1.392(2) . ? C38 H18 0.98(2) . ? C39 C40 1.395(2) . ? C39 C42 1.508(2) . ? C40 C41 1.387(2) . ? C40 H12 0.92(2) . ? C41 H17 0.94(2) . ? C42 H62A 0.9800 . ? C42 H62B 0.9800 . ? C42 H62C 0.9800 . ? C43 C44 1.381(2) . ? C43 C48 1.393(2) . ? C44 C45 1.391(3) . ? C44 H44 0.94(2) . ? C45 C46 1.391(3) . ? C45 H26 0.98(2) . ? C46 C47 1.394(3) . ? C46 C49 1.504(3) . ? C47 C48 1.387(2) . ? C47 H24 0.94(2) . ? C48 H16 0.96(2) . ? C49 H64 0.92(3) . ? C49 H65 0.92(4) . ? C49 H66 0.92(4) . ? O19 C50 1.431(2) . ? O19 H63 0.84(3) . ? O20 C52 1.429(2) . ? O20 H29 0.84(3) . ? C50 C51 1.499(3) . ? C50 H15 0.96(2) . ? C50 H22 1.01(2) . ? C51 H53 0.92(3) . ? C51 H55 0.94(3) . ? C51 H59 0.99(3) . ? C52 C53 1.500(3) . ? C52 H33 0.93(2) . ? C52 H60 1.03(3) . ? C53 H50 0.95(3) . ? C53 H61 1.01(3) . ? C53 H62 0.97(3) . ? 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 O8 Fe1 O9 91.90(5) . . ? O8 Fe1 O7 93.65(5) . . ? O9 Fe1 O7 91.74(5) . . ? O8 Fe1 N5 173.92(5) . 2_765 ? O9 Fe1 N5 89.84(5) . 2_765 ? O7 Fe1 N5 92.12(5) . 2_765 ? O8 Fe1 N2 91.30(5) . . ? O9 Fe1 N2 176.46(5) . . ? O7 Fe1 N2 89.57(5) . . ? N5 Fe1 N2 86.82(5) 2_765 . ? O8 Fe1 N9 88.93(5) . . ? O9 Fe1 N9 92.70(5) . . ? O7 Fe1 N9 174.79(5) . . ? N5 Fe1 N9 85.17(5) 2_765 . ? N2 Fe1 N9 85.85(5) . . ? N6 Fe2 N6 180.000(1) 2_765 . ? N6 Fe2 N1 91.96(5) 2_765 . ? N6 Fe2 N1 88.04(5) . . ? N6 Fe2 N1 88.04(5) 2_765 2_765 ? N6 Fe2 N1 91.96(5) . 2_765 ? N1 Fe2 N1 180.00(11) . 2_765 ? N6 Fe2 N10 91.47(5) 2_765 . ? N6 Fe2 N10 88.53(5) . . ? N1 Fe2 N10 90.84(5) . . ? N1 Fe2 N10 89.16(5) 2_765 . ? N6 Fe2 N10 88.53(5) 2_765 2_765 ? N6 Fe2 N10 91.47(5) . 2_765 ? N1 Fe2 N10 89.16(5) . 2_765 ? N1 Fe2 N10 90.84(5) 2_765 2_765 ? N10 Fe2 N10 180.00(9) . 2_765 ? C27 O7 Fe1 137.71(10) . . ? C27 O7 H52 108.4(19) . . ? Fe1 O7 H52 113.7(19) . . ? C25 O8 Fe1 127.31(10) . . ? C25 O8 H57 109.0(18) . . ? Fe1 O8 H57 120.7(18) . . ? Fe1 O9 H38 132.9(18) . . ? Fe1 O9 H48 116.9(17) . . ? H38 O9 H48 103(2) . . ? C2 N1 N2 107.25(12) . . ? C2 N1 Fe2 128.39(11) . . ? N2 N1 Fe2 124.36(10) . . ? C1 N2 N1 106.86(13) . . ? C1 N2 Fe1 125.02(11) . . ? N1 N2 Fe1 127.75(9) . . ? C1 N3 C2 105.70(13) . . ? C1 N3 C3 124.84(13) . . ? C2 N3 C3 129.43(14) . . ? O2 N4 O1 123.96(16) . . ? O2 N4 C6 118.31(16) . . ? O1 N4 C6 117.73(15) . . ? C10 N5 N6 107.35(13) . . ? C10 N5 Fe1 125.54(11) . 2_765 ? N6 N5 Fe1 126.59(10) . 2_765 ? C9 N6 N5 107.25(12) . . ? C9 N6 Fe2 127.11(11) . . ? N5 N6 Fe2 125.60(10) . . ? C10 N7 C9 105.69(13) . . ? C10 N7 C11 125.96(13) . . ? C9 N7 C11 128.34(13) . . ? O3 N8 O4 123.99(15) . . ? O3 N8 C14 117.87(14) . . ? O4 N8 C14 118.11(14) . . ? C17 N9 N10 107.33(12) . . ? C17 N9 Fe1 126.59(11) . . ? N10 N9 Fe1 126.06(9) . . ? C18 N10 N9 106.84(12) . . ? C18 N10 Fe2 127.33(10) . . ? N9 N10 Fe2 125.80(9) . . ? C17 N11 C18 105.46(13) . . ? C17 N11 C19 125.90(13) . . ? C18 N11 C19 128.54(13) . . ? O5 N12 O6 123.89(15) . . ? O5 N12 C22 118.58(14) . . ? O6 N12 C22 117.53(15) . . ? N2 C1 N3 110.76(14) . . ? N2 C1 H19 123.0(13) . . ? N3 C1 H19 126.0(13) . . ? N1 C2 N3 109.42(14) . . ? N1 C2 H4 128.1(12) . . ? N3 C2 H4 122.5(12) . . ? C8 C3 C4 122.22(15) . . ? C8 C3 N3 120.24(14) . . ? C4 C3 N3 117.53(14) . . ? C5 C4 C3 119.06(16) . . ? C5 C4 H45 120.1(14) . . ? C3 C4 H45 120.8(14) . . ? C6 C5 C4 118.12(16) . . ? C6 C5 H28 119.7(14) . . ? C4 C5 H28 122.1(14) . . ? C5 C6 C7 123.11(15) . . ? C5 C6 N4 118.45(15) . . ? C7 C6 N4 118.44(16) . . ? C6 C7 C8 118.76(16) . . ? C6 C7 H20 120.6(14) . . ? C8 C7 H20 120.6(14) . . ? C3 C8 C7 118.65(16) . . ? C3 C8 H35 121.7(14) . . ? C7 C8 H35 119.6(14) . . ? N6 C9 N7 109.69(14) . . ? N6 C9 H3 125.9(12) . . ? N7 C9 H3 124.4(12) . . ? N5 C10 N7 110.03(14) . . ? N5 C10 H9 124.0(13) . . ? N7 C10 H9 125.8(13) . . ? C16 C11 C12 122.05(15) . . ? C16 C11 N7 119.61(14) . . ? C12 C11 N7 118.33(14) . . ? C13 C12 C11 118.97(15) . . ? C13 C12 H14 122.1(13) . . ? C11 C12 H14 118.9(13) . . ? C14 C13 C12 118.39(15) . . ? C14 C13 H11 123.1(13) . . ? C12 C13 H11 118.5(13) . . ? C15 C14 C13 123.15(15) . . ? C15 C14 N8 118.76(15) . . ? C13 C14 N8 118.04(14) . . ? C14 C15 C16 118.46(15) . . ? C14 C15 H21 120.4(13) . . ? C16 C15 H21 121.0(13) . . ? C11 C16 C15 118.96(15) . . ? C11 C16 H7 120.1(13) . . ? C15 C16 H7 120.9(13) . . ? N9 C17 N11 110.56(14) . . ? N9 C17 H1 125.8(11) . . ? N11 C17 H1 123.6(11) . . ? N10 C18 N11 109.81(13) . . ? N10 C18 H2 122.8(13) . . ? N11 C18 H2 127.3(13) . . ? C24 C19 C20 122.26(14) . . ? C24 C19 N11 118.39(14) . . ? C20 C19 N11 119.35(14) . . ? C21 C20 C19 118.67(15) . . ? C21 C20 H10 120.4(13) . . ? C19 C20 H10 121.0(13) . . ? C22 C21 C20 118.74(15) . . ? C22 C21 H30 121.5(13) . . ? C20 C21 H30 119.7(13) . . ? C21 C22 C23 123.05(15) . . ? C21 C22 N12 118.79(14) . . ? C23 C22 N12 118.15(15) . . ? C22 C23 C24 118.45(15) . . ? C22 C23 H5 122.4(14) . . ? C24 C23 H5 119.2(14) . . ? C19 C24 C23 118.80(15) . . ? C19 C24 H34 122.0(14) . . ? C23 C24 H34 119.1(14) . . ? O8 C25 C26 111.64(14) . . ? O8 C25 H6 106.7(11) . . ? C26 C25 H6 111.6(11) . . ? O8 C25 H25 108.4(11) . . ? C26 C25 H25 111.4(12) . . ? H6 C25 H25 107.0(17) . . ? C25 C26 H39 110.7(13) . . ? C25 C26 H47 110.5(14) . . ? H39 C26 H47 107.9(19) . . ? C25 C26 H51 106.4(15) . . ? H39 C26 H51 111(2) . . ? H47 C26 H51 111(2) . . ? O7 C27 C28 111.27(14) . . ? O7 C27 H13 107.2(11) . . ? C28 C27 H13 110.3(11) . . ? O7 C27 H43 110.1(12) . . ? C28 C27 H43 110.5(12) . . ? H13 C27 H43 107.4(17) . . ? C27 C28 H36 111.0(14) . . ? C27 C28 H40 112.1(15) . . ? H36 C28 H40 108(2) . . ? C27 C28 H41 111.3(15) . . ? H36 C28 H41 105(2) . . ? H40 C28 H41 109(2) . . ? O12 S1 O10 113.65(7) . . ? O12 S1 O11 112.46(7) . . ? O10 S1 O11 111.88(7) . . ? O12 S1 C29 106.30(8) . . ? O10 S1 C29 106.85(7) . . ? O11 S1 C29 104.99(7) . . ? O13 S2 O14 112.96(8) . . ? O13 S2 O15 112.62(8) . . ? O14 S2 O15 112.64(8) . . ? O13 S2 C36 106.92(7) . . ? O14 S2 C36 106.01(8) . . ? O15 S2 C36 104.94(7) . . ? O18 S3 O16 112.24(9) . . ? O18 S3 O17 112.60(8) . . ? O16 S3 O17 113.33(9) . . ? O18 S3 C43 105.97(7) . . ? O16 S3 C43 104.90(8) . . ? O17 S3 C43 107.07(8) . . ? C34 C29 C30 120.32(15) . . ? C34 C29 S1 119.53(12) . . ? C30 C29 S1 120.02(13) . . ? C31 C30 C29 119.46(16) . . ? C31 C30 H8 119.3(13) . . ? C29 C30 H8 121.3(13) . . ? C30 C31 C32 121.51(16) . . ? C30 C31 H42 117.5(15) . . ? C32 C31 H42 121.0(15) . . ? C31 C32 C33 118.07(15) . . ? C31 C32 C35 121.57(16) . . ? C33 C32 C35 120.35(17) . . ? C34 C33 C32 121.31(16) . . ? C34 C33 H37 119.4(12) . . ? C32 C33 H37 119.3(12) . . ? C29 C34 C33 119.31(15) . . ? C29 C34 H27 119.7(12) . . ? C33 C34 H27 121.0(12) . . ? C32 C35 H32 111.4(16) . . ? C32 C35 H49 110.7(15) . . ? H32 C35 H49 108(2) . . ? C32 C35 H58 113.1(17) . . ? H32 C35 H58 104(2) . . ? H49 C35 H58 109(2) . . ? C37 C36 C41 120.17(15) . . ? C37 C36 S2 120.54(12) . . ? C41 C36 S2 119.27(12) . . ? C36 C37 C38 119.38(15) . . ? C36 C37 H31 117.6(12) . . ? C38 C37 H31 123.0(12) . . ? C39 C38 C37 121.38(15) . . ? C39 C38 H18 118.0(13) . . ? C37 C38 H18 120.6(13) . . ? C38 C39 C40 118.13(15) . . ? C38 C39 C42 121.36(16) . . ? C40 C39 C42 120.50(16) . . ? C41 C40 C39 121.43(16) . . ? C41 C40 H12 119.0(14) . . ? C39 C40 H12 119.5(14) . . ? C40 C41 C36 119.50(15) . . ? C40 C41 H17 118.9(14) . . ? C36 C41 H17 121.6(14) . . ? C39 C42 H62A 109.5 . . ? C39 C42 H62B 109.5 . . ? H62A C42 H62B 109.5 . . ? C39 C42 H62C 109.5 . . ? H62A C42 H62C 109.5 . . ? H62B C42 H62C 109.5 . . ? C44 C43 C48 119.79(16) . . ? C44 C43 S3 121.31(13) . . ? C48 C43 S3 118.81(13) . . ? C43 C44 C45 119.76(17) . . ? C43 C44 H44 120.0(14) . . ? C45 C44 H44 120.2(14) . . ? C44 C45 C46 121.48(17) . . ? C44 C45 H26 118.2(13) . . ? C46 C45 H26 120.3(13) . . ? C45 C46 C47 117.93(16) . . ? C45 C46 C49 121.15(18) . . ? C47 C46 C49 120.92(18) . . ? C48 C47 C46 121.12(17) . . ? C48 C47 H24 117.9(14) . . ? C46 C47 H24 120.8(14) . . ? C47 C48 C43 119.93(16) . . ? C47 C48 H16 119.5(13) . . ? C43 C48 H16 120.6(13) . . ? C46 C49 H64 112(2) . . ? C46 C49 H65 114(2) . . ? H64 C49 H65 99(3) . . ? C46 C49 H66 112(2) . . ? H64 C49 H66 110(3) . . ? H65 C49 H66 110(3) . . ? C50 O19 H63 108(2) . . ? C52 O20 H29 109.1(18) . . ? O19 C50 C51 108.87(17) . . ? O19 C50 H15 110.0(14) . . ? C51 C50 H15 111.9(13) . . ? O19 C50 H22 109.9(12) . . ? C51 C50 H22 110.6(12) . . ? H15 C50 H22 105.6(18) . . ? C50 C51 H53 107.4(18) . . ? C50 C51 H55 111.7(16) . . ? H53 C51 H55 106(2) . . ? C50 C51 H59 113.8(18) . . ? H53 C51 H59 113(3) . . ? H55 C51 H59 105(2) . . ? O20 C52 C53 107.89(16) . . ? O20 C52 H33 110.4(14) . . ? C53 C52 H33 109.3(13) . . ? O20 C52 H60 106.9(15) . . ? C53 C52 H60 113.1(15) . . ? H33 C52 H60 109(2) . . ? C52 C53 H50 112.4(15) . . ? C52 C53 H61 110.2(16) . . ? H50 C53 H61 107(2) . . ? C52 C53 H62 108.5(17) . . ? H50 C53 H62 109(2) . . ? H61 C53 H62 110(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.61 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.865 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.075 # Attachment '4433_web_deposit_cif_file_1_MuraleeMURUGESU_1298934407.cif' data_mm108_0m _database_code_depnum_ccdc_archive 'CCDC 815194' #TrackingRef '4433_web_deposit_cif_file_1_MuraleeMURUGESU_1298934407.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H130 Fe3 N24 O40 S6' _chemical_formula_weight 2740.25 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 14.6130(7) _cell_length_b 15.1960(7) _cell_length_c 16.3954(8) _cell_angle_alpha 107.505(2) _cell_angle_beta 99.989(3) _cell_angle_gamma 110.731(2) _cell_volume 3083.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 181(1) _cell_measurement_reflns_used 9875 _cell_measurement_theta_min 2.387 _cell_measurement_theta_max 28.945 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8808 _exptl_absorpt_correction_T_max 0.9579 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 181(1) _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 APEXII CCD' _diffrn_measurement_method ' \f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 98389 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 30.64 _reflns_number_total 18802 _reflns_number_gt 13071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _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. ; _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^)+(0.0426P)^2^+0.8804P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18802 _refine_ls_number_parameters 1024 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Fe1 Fe 0.870775(17) 0.644792(17) -0.097201(15) 0.01475(6) Uani 1 1 d . . . Fe2 Fe 1.0000 0.5000 0.0000 0.01322(7) Uani 1 2 d S . . O1 O 1.15016(13) 1.17476(11) 0.52975(10) 0.0480(4) Uani 1 1 d . . . O2 O 1.15649(18) 1.07206(14) 0.59341(11) 0.0720(6) Uani 1 1 d . . . O3 O 0.60876(15) 0.42867(14) 0.44407(12) 0.0572(5) Uani 1 1 d . . . O4 O 0.58075(12) 0.27034(13) 0.40486(11) 0.0442(4) Uani 1 1 d . . . O5 O 0.20661(11) 0.03354(12) -0.23606(11) 0.0448(4) Uani 1 1 d . . . O6 O 0.27462(13) -0.07229(11) -0.26062(14) 0.0621(5) Uani 1 1 d . . . O7 O 0.95753(10) 0.79684(9) -0.08521(9) 0.0247(3) Uani 1 1 d . . . O8 O 0.75426(10) 0.67812(9) -0.05618(9) 0.0223(3) Uani 1 1 d . . . O9 O 0.78805(10) 0.59436(11) -0.23316(9) 0.0254(3) Uani 1 1 d . . . N1 N 0.99897(10) 0.64057(10) 0.07886(9) 0.0171(3) Uani 1 1 d . . . N2 N 0.95562(11) 0.69345(10) 0.04260(9) 0.0179(3) Uani 1 1 d . . . N3 N 1.01988(11) 0.77740(10) 0.18822(9) 0.0193(3) Uani 1 1 d . . . N4 N 1.14119(14) 1.09106(14) 0.52694(11) 0.0388(4) Uani 1 1 d . . . N5 N 1.01418(10) 0.39829(10) 0.14000(9) 0.0177(3) Uani 1 1 d . . . N6 N 0.96250(10) 0.44272(10) 0.09994(9) 0.0177(3) Uani 1 1 d . . . N7 N 0.89442(11) 0.40698(10) 0.20066(9) 0.0185(3) Uani 1 1 d . . . N8 N 0.62422(13) 0.35601(14) 0.40544(11) 0.0341(4) Uani 1 1 d . . . N9 N 0.78981(10) 0.49272(10) -0.10109(9) 0.0175(3) Uani 1 1 d . . . N10 N 0.83656(11) 0.43926(10) -0.06909(9) 0.0182(3) Uani 1 1 d . . . N11 N 0.67111(10) 0.34207(10) -0.12752(9) 0.0183(3) Uani 1 1 d . . . N12 N 0.28031(13) 0.01429(12) -0.23722(11) 0.0333(4) Uani 1 1 d . . . C1 C 0.96978(13) 0.77443(13) 0.10944(11) 0.0200(3) Uani 1 1 d . . . C2 C 1.03579(13) 0.69185(12) 0.16590(11) 0.0194(3) Uani 1 1 d . . . C3 C 1.05083(13) 0.85643(13) 0.27489(11) 0.0213(3) Uani 1 1 d . . . C4 C 1.08183(16) 0.95613(14) 0.28149(13) 0.0296(4) Uani 1 1 d . . . C5 C 1.10928(16) 1.03370(15) 0.36453(13) 0.0326(4) Uani 1 1 d . . . C6 C 1.10928(15) 1.00822(14) 0.43827(12) 0.0294(4) Uani 1 1 d . . . C7 C 1.08156(16) 0.90986(15) 0.43284(13) 0.0319(4) Uani 1 1 d . . . C8 C 1.05000(15) 0.83176(15) 0.34924(12) 0.0274(4) Uani 1 1 d . . . C9 C 0.89175(13) 0.44725(13) 0.13747(11) 0.0197(3) Uani 1 1 d . . . C10 C 0.97226(13) 0.37820(13) 0.19980(12) 0.0200(3) Uani 1 1 d . . . C11 C 0.82835(13) 0.39557(13) 0.25500(11) 0.0197(3) Uani 1 1 d . . . C12 C 0.79239(15) 0.30586(14) 0.26929(13) 0.0256(4) Uani 1 1 d . . . C13 C 0.72594(15) 0.29340(15) 0.32001(13) 0.0276(4) Uani 1 1 d . . . C14 C 0.69787(14) 0.37104(15) 0.35418(12) 0.0253(4) Uani 1 1 d . . . C15 C 0.73300(16) 0.46034(15) 0.34029(13) 0.0290(4) Uani 1 1 d . . . C16 C 0.79981(15) 0.47346(14) 0.28992(12) 0.0251(4) Uani 1 1 d . . . C17 C 0.69154(13) 0.43314(12) -0.13513(12) 0.0204(3) Uani 1 1 d . . . C18 C 0.76387(13) 0.34978(13) -0.08564(11) 0.0200(3) Uani 1 1 d . . . C19 C 0.57189(13) 0.25866(12) -0.15467(11) 0.0198(3) Uani 1 1 d . . . C20 C 0.56250(15) 0.15924(13) -0.18799(12) 0.0240(4) Uani 1 1 d . . . C21 C 0.46617(15) 0.07861(14) -0.21495(12) 0.0262(4) Uani 1 1 d . . . C22 C 0.38315(14) 0.09998(13) -0.20871(12) 0.0243(4) Uani 1 1 d . . . C23 C 0.39181(15) 0.19827(14) -0.17459(13) 0.0276(4) Uani 1 1 d . . . C24 C 0.48879(14) 0.27928(14) -0.14635(13) 0.0262(4) Uani 1 1 d . . . C25 C 0.72199(16) 0.75448(15) -0.06564(14) 0.0275(4) Uani 1 1 d . . . C26 C 0.78468(19) 0.85654(16) 0.01164(16) 0.0352(5) Uani 1 1 d . . . C27 C 0.94909(16) 0.86047(15) -0.13302(14) 0.0287(4) Uani 1 1 d . . . C28 C 1.0288(2) 0.87974(19) -0.17987(18) 0.0419(5) Uani 1 1 d . . . S1 S 0.20878(3) -0.11203(3) 0.07266(3) 0.02520(10) Uani 1 1 d . . . S2 S 0.70548(4) 0.57002(3) 0.11101(3) 0.02354(10) Uani 1 1 d . . . S3 S 0.18890(4) 0.64081(3) 0.37019(3) 0.02585(10) Uani 1 1 d . . . O10 O 0.22988(10) -0.11981(11) 0.15896(9) 0.0339(3) Uani 1 1 d . . . O11 O 0.12654(10) -0.07977(10) 0.05694(10) 0.0328(3) Uani 1 1 d . . . O12 O 0.19212(11) -0.20313(10) -0.00167(10) 0.0370(3) Uani 1 1 d . . . O13 O 0.67517(12) 0.46461(11) 0.05501(10) 0.0400(4) Uani 1 1 d . . . O14 O 0.81334(11) 0.62273(11) 0.16330(10) 0.0381(3) Uani 1 1 d . . . O15 O 0.67437(13) 0.62596(13) 0.06223(11) 0.0462(4) Uani 1 1 d . . . O16 O 0.24322(13) 0.59965(11) 0.31515(11) 0.0474(4) Uani 1 1 d . . . O17 O 0.18887(12) 0.61375(10) 0.44759(9) 0.0382(3) Uani 1 1 d . . . O18 O 0.08670(11) 0.61820(10) 0.31824(10) 0.0384(4) Uani 1 1 d . . . C29 C 0.32034(13) -0.01194(13) 0.07631(12) 0.0221(4) Uani 1 1 d . . . C30 C 0.37592(16) 0.07515(15) 0.15441(14) 0.0303(4) Uani 1 1 d . . . C31 C 0.45832(16) 0.15619(15) 0.15445(14) 0.0344(5) Uani 1 1 d . . . C32 C 0.48712(14) 0.15219(14) 0.07808(14) 0.0291(4) Uani 1 1 d . . . C33 C 0.43120(15) 0.06356(15) 0.00072(14) 0.0299(4) Uani 1 1 d . . . C34 C 0.34876(15) -0.01807(14) -0.00073(13) 0.0269(4) Uani 1 1 d . . . C35 C 0.57546(17) 0.24144(17) 0.07752(17) 0.0444(6) Uani 1 1 d . . . H35A H 0.6053 0.2974 0.1372 0.067 Uiso 1 1 calc R . . H35B H 0.5502 0.2649 0.0327 0.067 Uiso 1 1 calc R . . H35C H 0.6283 0.2200 0.0623 0.067 Uiso 1 1 calc R . . C36 C 0.63728(13) 0.56966(13) 0.19022(11) 0.0198(3) Uani 1 1 d . . . C37 C 0.54214(14) 0.48993(14) 0.16971(12) 0.0243(4) Uani 1 1 d . . . C38 C 0.49016(14) 0.49149(15) 0.23315(12) 0.0261(4) Uani 1 1 d . . . C39 C 0.53092(14) 0.57244(15) 0.31623(12) 0.0267(4) Uani 1 1 d . . . C40 C 0.62587(15) 0.65192(15) 0.33496(13) 0.0284(4) Uani 1 1 d . . . C41 C 0.67941(15) 0.65103(14) 0.27319(12) 0.0253(4) Uani 1 1 d . . . C42 C 0.47477(17) 0.57400(19) 0.38531(14) 0.0410(5) Uani 1 1 d . . . H62A H 0.4008 0.5313 0.3549 0.062 Uiso 1 1 calc R . . H62B H 0.4865 0.6444 0.4189 0.062 Uiso 1 1 calc R . . H62C H 0.5005 0.5473 0.4271 0.062 Uiso 1 1 calc R . . C43 C 0.25967(14) 0.77565(13) 0.41184(12) 0.0240(4) Uani 1 1 d . . . C44 C 0.28459(18) 0.83667(16) 0.50098(13) 0.0354(5) Uani 1 1 d . . . C45 C 0.33503(19) 0.94204(16) 0.53014(15) 0.0408(5) Uani 1 1 d . . . C46 C 0.36131(16) 0.98894(15) 0.47203(15) 0.0366(5) Uani 1 1 d . . . C47 C 0.33492(18) 0.92634(16) 0.38196(15) 0.0393(5) Uani 1 1 d . . . C48 C 0.28525(17) 0.82115(15) 0.35228(14) 0.0338(5) Uani 1 1 d . . . C49 C 0.4162(2) 1.10400(17) 0.50452(19) 0.0551(7) Uani 1 1 d . . . H49A H 0.3742 1.1282 0.4720 0.083 Uiso 1 1 calc R . . H49B H 0.4829 1.1232 0.4934 0.083 Uiso 1 1 calc R . . H49C H 0.4271 1.1353 0.5692 0.083 Uiso 1 1 calc R . . O19 O 0.08475(14) 0.40645(14) 0.41209(12) 0.0497(4) Uani 1 1 d . . . O20 O 0.19393(13) 0.30694(13) 0.34662(10) 0.0401(4) Uani 1 1 d . . . C50 C 0.01886(19) 0.38646(18) 0.46540(16) 0.0399(5) Uani 1 1 d . . . C51 C -0.0139(3) 0.2790(2) 0.4570(2) 0.0740(9) Uani 1 1 d . . . H51A H -0.0476 0.2326 0.3934 0.111 Uiso 1 1 calc R . . H51B H -0.0622 0.2637 0.4910 0.111 Uiso 1 1 calc R . . H51C H 0.0466 0.2696 0.4812 0.111 Uiso 1 1 calc R . . C52 C 0.28550(18) 0.31740(19) 0.40359(15) 0.0400(5) Uani 1 1 d . . . C53 C 0.3328(2) 0.2618(3) 0.3469(2) 0.0561(7) Uani 1 1 d . . . H1 H 0.6383(15) 0.4485(14) -0.1627(13) 0.024(5) Uiso 1 1 d . . . H2 H 0.7748(14) 0.3004(15) -0.0697(12) 0.024(5) Uiso 1 1 d . . . H3 H 0.8457(16) 0.4728(15) 0.1228(13) 0.030(5) Uiso 1 1 d . . . H4 H 1.0667(14) 0.6744(14) 0.2068(12) 0.020(5) Uiso 1 1 d . . . H5 H 0.3372(16) 0.2115(15) -0.1708(13) 0.029(5) Uiso 1 1 d . . . H6 H 0.7279(15) 0.7571(15) -0.1217(14) 0.028(5) Uiso 1 1 d . . . H7 H 0.8216(16) 0.5287(16) 0.2790(14) 0.032(6) Uiso 1 1 d . . . H8 H 0.3602(17) 0.0795(16) 0.2052(15) 0.035(6) Uiso 1 1 d . . . H9 H 0.9960(14) 0.3541(14) 0.2386(13) 0.022(5) Uiso 1 1 d . . . H10 H 0.6178(15) 0.1473(14) -0.1911(12) 0.022(5) Uiso 1 1 d . . . H11 H 0.6991(16) 0.2332(16) 0.3287(14) 0.035(6) Uiso 1 1 d . . . H12 H 0.6538(16) 0.7046(17) 0.3907(15) 0.036(6) Uiso 1 1 d . . . H13 H 0.8817(17) 0.8250(16) -0.1749(14) 0.034(6) Uiso 1 1 d . . . H14 H 0.8136(15) 0.2529(15) 0.2446(13) 0.025(5) Uiso 1 1 d . . . H16 H 0.2686(17) 0.7797(18) 0.2897(16) 0.044(6) Uiso 1 1 d . . . H17 H 0.7436(17) 0.7028(16) 0.2875(14) 0.033(6) Uiso 1 1 d . . . H18 H 0.4235(17) 0.4356(17) 0.2186(14) 0.037(6) Uiso 1 1 d . . . H19 H 0.9461(14) 0.8212(14) 0.1038(12) 0.020(5) Uiso 1 1 d . . . H20 H 1.0815(17) 0.8942(17) 0.4841(16) 0.043(6) Uiso 1 1 d . . . H21 H 0.7107(15) 0.5080(15) 0.3610(13) 0.025(5) Uiso 1 1 d . . . H22 H -0.0456(19) 0.3995(18) 0.4430(16) 0.049(7) Uiso 1 1 d . . . H24 H 0.353(2) 0.9556(19) 0.3398(17) 0.057(7) Uiso 1 1 d . . . H25 H 0.6494(17) 0.7308(15) -0.0710(13) 0.029(5) Uiso 1 1 d . . . H26 H 0.3522(17) 0.9812(17) 0.5900(15) 0.037(6) Uiso 1 1 d . . . H27 H 0.3076(17) -0.0792(17) -0.0555(14) 0.036(6) Uiso 1 1 d . . . H28 H 1.1276(17) 1.1025(18) 0.3718(15) 0.043(6) Uiso 1 1 d . . . H29 H 0.164(2) 0.338(2) 0.3761(19) 0.061(9) Uiso 1 1 d . . . H30 H 0.4586(15) 0.0108(16) -0.2392(14) 0.031(5) Uiso 1 1 d . . . H31 H 0.5124(16) 0.4356(16) 0.1141(14) 0.032(6) Uiso 1 1 d . . . H33 H 0.2689(18) 0.2903(18) 0.4449(16) 0.046(7) Uiso 1 1 d . . . H34 H 0.4955(15) 0.3461(16) -0.1182(13) 0.030(5) Uiso 1 1 d . . . H35 H 1.0302(15) 0.7657(15) 0.3430(13) 0.025(5) Uiso 1 1 d . . . H36 H 1.017(2) 0.816(2) -0.2301(18) 0.059(8) Uiso 1 1 d . . . H37 H 0.4514(16) 0.0581(16) -0.0519(14) 0.034(6) Uiso 1 1 d . . . H38 H 0.7902(18) 0.6246(19) -0.2668(16) 0.043(7) Uiso 1 1 d . . . H39 H 0.8585(18) 0.8833(15) 0.0153(14) 0.031(6) Uiso 1 1 d . . . H40 H 1.095(2) 0.905(2) -0.1373(18) 0.058(8) Uiso 1 1 d . . . H41 H 1.025(2) 0.928(2) -0.2083(18) 0.061(8) Uiso 1 1 d . . . H42 H 0.4935(18) 0.2137(18) 0.2086(16) 0.043(6) Uiso 1 1 d . . . H43 H 0.9552(16) 0.9282(17) -0.0924(14) 0.034(6) Uiso 1 1 d . . . H44 H 0.2661(18) 0.8051(17) 0.5397(16) 0.044(6) Uiso 1 1 d . . . H45 H 1.0860(16) 0.9706(15) 0.2307(14) 0.031(5) Uiso 1 1 d . . . H47 H 0.7783(18) 0.8497(18) 0.0662(17) 0.048(7) Uiso 1 1 d . . . H48 H 0.7793(19) 0.533(2) -0.2653(17) 0.053(7) Uiso 1 1 d . . . H50 H 0.394(2) 0.265(2) 0.3803(19) 0.065(8) Uiso 1 1 d . . . H51 H 0.7586(18) 0.9045(18) 0.0006(16) 0.050(7) Uiso 1 1 d . . . H52 H 1.017(2) 0.827(2) -0.044(2) 0.073(9) Uiso 1 1 d . . . H57 H 0.7337(17) 0.6608(17) -0.0183(15) 0.037(6) Uiso 1 1 d . . . H60 H 0.332(2) 0.393(2) 0.4342(18) 0.064(8) Uiso 1 1 d . . . H61 H 0.283(2) 0.185(2) 0.3153(19) 0.072(9) Uiso 1 1 d . . . H62 H 0.351(2) 0.297(2) 0.305(2) 0.075(9) Uiso 1 1 d . . . H70 H 0.111(2) 0.468(2) 0.426(2) 0.077(10) Uiso 1 1 d . . . H71 H 0.051(2) 0.434(2) 0.5265(18) 0.056(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01511(12) 0.01482(11) 0.01633(11) 0.00766(9) 0.00639(9) 0.00670(9) Fe2 0.01310(16) 0.01313(15) 0.01464(15) 0.00662(12) 0.00538(12) 0.00552(12) O1 0.0553(11) 0.0294(8) 0.0386(9) -0.0038(7) 0.0106(8) 0.0122(7) O2 0.1226(18) 0.0575(12) 0.0219(8) 0.0046(8) 0.0119(10) 0.0380(12) O3 0.0728(13) 0.0630(11) 0.0673(12) 0.0320(9) 0.0572(10) 0.0417(10) O4 0.0380(9) 0.0574(10) 0.0530(10) 0.0357(8) 0.0294(8) 0.0189(8) O5 0.0219(8) 0.0448(9) 0.0583(10) 0.0190(8) 0.0135(7) 0.0050(7) O6 0.0406(10) 0.0204(8) 0.1040(15) 0.0121(9) 0.0258(10) -0.0009(7) O7 0.0221(7) 0.0194(6) 0.0309(7) 0.0149(5) 0.0046(6) 0.0047(5) O8 0.0261(7) 0.0258(6) 0.0286(7) 0.0173(6) 0.0162(6) 0.0169(5) O9 0.0314(8) 0.0256(7) 0.0200(6) 0.0087(6) 0.0053(5) 0.0146(6) N1 0.0160(7) 0.0168(6) 0.0188(7) 0.0093(5) 0.0052(5) 0.0057(5) N2 0.0192(7) 0.0167(6) 0.0192(7) 0.0091(5) 0.0055(6) 0.0077(5) N3 0.0204(7) 0.0177(7) 0.0177(7) 0.0064(5) 0.0064(6) 0.0064(6) N4 0.0414(11) 0.0341(10) 0.0260(9) -0.0007(7) 0.0078(8) 0.0120(8) N5 0.0173(7) 0.0190(7) 0.0195(7) 0.0097(6) 0.0067(6) 0.0086(6) N6 0.0168(7) 0.0186(7) 0.0208(7) 0.0097(6) 0.0070(6) 0.0088(5) N7 0.0174(7) 0.0206(7) 0.0199(7) 0.0091(6) 0.0089(6) 0.0085(6) N8 0.0313(9) 0.0506(11) 0.0317(9) 0.0219(8) 0.0202(8) 0.0203(8) N9 0.0182(7) 0.0166(6) 0.0202(7) 0.0092(5) 0.0067(6) 0.0082(5) N10 0.0200(7) 0.0167(7) 0.0206(7) 0.0095(6) 0.0081(6) 0.0083(6) N11 0.0162(7) 0.0162(6) 0.0217(7) 0.0082(6) 0.0065(6) 0.0052(5) N12 0.0270(9) 0.0285(9) 0.0342(9) 0.0118(7) 0.0110(7) 0.0010(7) C1 0.0215(9) 0.0194(8) 0.0198(8) 0.0086(7) 0.0056(7) 0.0091(7) C2 0.0181(8) 0.0193(8) 0.0192(8) 0.0082(7) 0.0043(7) 0.0067(7) C3 0.0202(9) 0.0203(8) 0.0181(8) 0.0035(7) 0.0044(7) 0.0071(7) C4 0.0385(12) 0.0219(9) 0.0216(9) 0.0068(7) 0.0074(8) 0.0083(8) C5 0.0384(12) 0.0194(9) 0.0305(10) 0.0046(8) 0.0086(9) 0.0075(8) C6 0.0271(10) 0.0284(10) 0.0215(9) -0.0003(7) 0.0054(8) 0.0093(8) C7 0.0408(12) 0.0354(11) 0.0202(9) 0.0103(8) 0.0110(8) 0.0169(9) C8 0.0332(11) 0.0244(9) 0.0252(9) 0.0109(8) 0.0109(8) 0.0114(8) C9 0.0195(9) 0.0224(8) 0.0218(8) 0.0104(7) 0.0087(7) 0.0114(7) C10 0.0187(9) 0.0232(8) 0.0229(8) 0.0123(7) 0.0090(7) 0.0107(7) C11 0.0167(8) 0.0261(9) 0.0176(8) 0.0098(7) 0.0074(7) 0.0087(7) C12 0.0276(10) 0.0283(9) 0.0306(10) 0.0163(8) 0.0156(8) 0.0155(8) C13 0.0277(10) 0.0328(10) 0.0320(10) 0.0216(8) 0.0158(8) 0.0133(8) C14 0.0231(9) 0.0375(10) 0.0216(9) 0.0155(8) 0.0131(7) 0.0137(8) C15 0.0325(11) 0.0332(10) 0.0298(10) 0.0128(8) 0.0171(8) 0.0197(9) C16 0.0277(10) 0.0254(9) 0.0278(9) 0.0134(8) 0.0152(8) 0.0121(8) C17 0.0190(9) 0.0183(8) 0.0256(9) 0.0115(7) 0.0069(7) 0.0074(7) C18 0.0211(9) 0.0180(8) 0.0231(8) 0.0098(7) 0.0080(7) 0.0088(7) C19 0.0173(8) 0.0173(8) 0.0205(8) 0.0077(6) 0.0049(7) 0.0033(6) C20 0.0218(9) 0.0218(9) 0.0287(9) 0.0092(7) 0.0101(8) 0.0095(7) C21 0.0279(10) 0.0174(8) 0.0288(10) 0.0067(7) 0.0098(8) 0.0065(7) C22 0.0207(9) 0.0212(8) 0.0243(9) 0.0097(7) 0.0063(7) 0.0015(7) C23 0.0212(10) 0.0276(9) 0.0374(11) 0.0160(8) 0.0123(8) 0.0100(8) C24 0.0245(10) 0.0183(9) 0.0365(10) 0.0107(8) 0.0115(8) 0.0092(7) C25 0.0279(11) 0.0307(10) 0.0351(11) 0.0177(8) 0.0122(9) 0.0195(8) C26 0.0394(13) 0.0288(10) 0.0434(13) 0.0140(9) 0.0136(10) 0.0209(9) C27 0.0334(11) 0.0251(9) 0.0339(10) 0.0193(8) 0.0114(9) 0.0128(8) C28 0.0430(14) 0.0405(13) 0.0471(14) 0.0276(12) 0.0193(12) 0.0124(11) S1 0.0199(2) 0.0212(2) 0.0343(2) 0.01427(19) 0.00581(19) 0.00722(17) S2 0.0281(2) 0.0261(2) 0.0298(2) 0.01692(18) 0.01928(19) 0.01643(19) S3 0.0308(3) 0.0213(2) 0.0226(2) 0.00849(17) 0.00561(19) 0.00969(18) O10 0.0282(7) 0.0417(8) 0.0419(8) 0.0284(7) 0.0138(6) 0.0146(6) O11 0.0210(7) 0.0268(7) 0.0495(9) 0.0189(6) 0.0049(6) 0.0087(5) O12 0.0368(8) 0.0201(7) 0.0453(9) 0.0097(6) 0.0092(7) 0.0071(6) O13 0.0521(10) 0.0312(8) 0.0403(8) 0.0095(6) 0.0312(7) 0.0177(7) O14 0.0250(8) 0.0451(9) 0.0476(9) 0.0192(7) 0.0207(7) 0.0137(6) O15 0.0652(11) 0.0737(11) 0.0579(10) 0.0537(9) 0.0486(9) 0.0560(10) O16 0.0568(10) 0.0273(8) 0.0565(10) 0.0075(7) 0.0311(8) 0.0177(7) O17 0.0462(9) 0.0319(8) 0.0308(7) 0.0180(6) 0.0042(7) 0.0096(6) O18 0.0336(8) 0.0275(7) 0.0411(8) 0.0150(6) -0.0054(6) 0.0058(6) C29 0.0201(9) 0.0203(8) 0.0271(9) 0.0115(7) 0.0059(7) 0.0091(7) C30 0.0306(11) 0.0307(10) 0.0251(10) 0.0104(8) 0.0096(8) 0.0085(8) C31 0.0293(11) 0.0250(10) 0.0321(11) 0.0048(8) 0.0026(9) 0.0021(8) C32 0.0212(9) 0.0301(10) 0.0411(11) 0.0218(9) 0.0092(8) 0.0104(8) C33 0.0294(11) 0.0371(11) 0.0311(10) 0.0189(9) 0.0146(9) 0.0161(9) C34 0.0282(10) 0.0246(9) 0.0253(9) 0.0080(8) 0.0058(8) 0.0114(8) C35 0.0317(12) 0.0392(12) 0.0617(15) 0.0300(11) 0.0139(11) 0.0065(9) C36 0.0209(9) 0.0213(8) 0.0239(8) 0.0124(7) 0.0112(7) 0.0114(7) C37 0.0247(10) 0.0231(9) 0.0227(9) 0.0073(7) 0.0082(7) 0.0089(7) C38 0.0188(9) 0.0305(10) 0.0282(9) 0.0133(8) 0.0093(8) 0.0075(8) C39 0.0237(10) 0.0378(10) 0.0249(9) 0.0151(8) 0.0123(8) 0.0154(8) C40 0.0283(10) 0.0309(10) 0.0222(9) 0.0058(8) 0.0093(8) 0.0117(8) C41 0.0210(9) 0.0245(9) 0.0286(9) 0.0103(8) 0.0094(8) 0.0073(8) C42 0.0335(12) 0.0615(15) 0.0310(11) 0.0189(10) 0.0197(9) 0.0187(11) C43 0.0229(9) 0.0211(8) 0.0242(9) 0.0068(7) 0.0051(7) 0.0084(7) C44 0.0483(13) 0.0304(10) 0.0232(9) 0.0106(8) 0.0073(9) 0.0142(9) C45 0.0520(14) 0.0304(11) 0.0257(11) 0.0016(9) 0.0044(10) 0.0141(10) C46 0.0347(12) 0.0240(10) 0.0428(12) 0.0078(9) 0.0085(9) 0.0099(8) C47 0.0422(13) 0.0316(11) 0.0406(12) 0.0173(10) 0.0180(10) 0.0073(9) C48 0.0400(12) 0.0294(10) 0.0259(10) 0.0086(8) 0.0142(9) 0.0084(9) C49 0.0579(16) 0.0261(11) 0.0646(17) 0.0097(11) 0.0139(13) 0.0095(11) O19 0.0653(12) 0.0373(9) 0.0612(11) 0.0270(8) 0.0386(9) 0.0229(8) O20 0.0458(10) 0.0526(10) 0.0294(8) 0.0184(7) 0.0134(7) 0.0267(8) C50 0.0438(14) 0.0423(13) 0.0369(12) 0.0170(10) 0.0156(11) 0.0196(11) C51 0.095(2) 0.0665(19) 0.118(3) 0.0673(19) 0.077(2) 0.0501(18) C52 0.0412(13) 0.0412(13) 0.0302(11) 0.0179(10) 0.0048(10) 0.0096(10) C53 0.0437(16) 0.073(2) 0.0603(17) 0.0315(16) 0.0152(14) 0.0310(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O9 2.0975(13) . ? Fe1 O8 2.1002(12) . ? Fe1 O7 2.1333(12) . ? Fe1 N5 2.1586(14) 2_765 ? Fe1 N2 2.1641(13) . ? Fe1 N9 2.1665(13) . ? Fe2 N6 2.1388(13) 2_765 ? Fe2 N6 2.1388(13) . ? Fe2 N1 2.1455(13) 2_765 ? Fe2 N1 2.1455(13) . ? Fe2 N10 2.1705(14) 2_765 ? Fe2 N10 2.1705(14) . ? O1 N4 1.217(2) . ? O2 N4 1.213(2) . ? O3 N8 1.215(2) . ? O4 N8 1.226(2) . ? O5 N12 1.213(2) . ? O6 N12 1.222(2) . ? O7 C27 1.439(2) . ? O7 H52 0.86(3) . ? O8 C25 1.436(2) . ? O8 H57 0.81(2) . ? O9 H38 0.82(3) . ? O9 H48 0.87(3) . ? N1 C2 1.304(2) . ? N1 N2 1.3846(17) . ? N2 C1 1.299(2) . ? N3 C1 1.349(2) . ? N3 C2 1.355(2) . ? N3 C3 1.425(2) . ? N4 C6 1.471(2) . ? N5 C10 1.298(2) . ? N5 N6 1.3832(18) . ? N5 Fe1 2.1586(14) 2_765 ? N6 C9 1.303(2) . ? N7 C9 1.354(2) . ? N7 C10 1.356(2) . ? N7 C11 1.424(2) . ? N8 C14 1.474(2) . ? N9 C17 1.300(2) . ? N9 N10 1.3882(18) . ? N10 C18 1.306(2) . ? N11 C18 1.356(2) . ? N11 C17 1.358(2) . ? N11 C19 1.429(2) . ? N12 C22 1.476(2) . ? C1 H19 0.915(19) . ? C2 H4 0.900(19) . ? C3 C8 1.380(2) . ? C3 C4 1.382(2) . ? C4 C5 1.384(3) . ? C4 H45 0.93(2) . ? C5 C6 1.376(3) . ? C5 H28 0.95(2) . ? C6 C7 1.373(3) . ? C7 C8 1.384(3) . ? C7 H20 0.94(2) . ? C8 H35 0.91(2) . ? C9 H3 0.92(2) . ? C10 H9 0.901(19) . ? C11 C12 1.385(2) . ? C11 C16 1.388(2) . ? C12 C13 1.384(3) . ? C12 H14 0.966(19) . ? C13 C14 1.378(3) . ? C13 H11 0.93(2) . ? C14 C15 1.375(3) . ? C15 C16 1.384(3) . ? C15 H21 0.90(2) . ? C16 H7 0.87(2) . ? C17 H1 0.967(19) . ? C18 H2 0.919(19) . ? C19 C24 1.376(2) . ? C19 C20 1.389(2) . ? C20 C21 1.384(3) . ? C20 H10 0.90(2) . ? C21 C22 1.375(3) . ? C21 H30 0.94(2) . ? C22 C23 1.378(3) . ? C23 C24 1.390(3) . ? C23 H5 0.90(2) . ? C24 H34 0.94(2) . ? C25 C26 1.503(3) . ? C25 H6 0.95(2) . ? C25 H25 0.97(2) . ? C26 H39 0.99(2) . ? C26 H47 0.95(2) . ? C26 H51 0.98(2) . ? C27 C28 1.496(3) . ? C27 H13 0.95(2) . ? C27 H43 1.01(2) . ? C28 H36 1.00(3) . ? C28 H40 0.95(3) . ? C28 H41 0.99(3) . ? S1 O10 1.4445(14) . ? S1 O12 1.4507(14) . ? S1 O11 1.4617(13) . ? S1 C29 1.7693(18) . ? S2 O13 1.4412(14) . ? S2 O14 1.4440(15) . ? S2 O15 1.4578(13) . ? S2 C36 1.7691(17) . ? S3 O18 1.4468(14) . ? S3 O17 1.4470(14) . ? S3 O16 1.4477(16) . ? S3 C43 1.7741(18) . ? C29 C30 1.382(3) . ? C29 C34 1.384(3) . ? C30 C31 1.384(3) . ? C30 H8 0.89(2) . ? C31 C32 1.380(3) . ? C31 H42 0.93(2) . ? C32 C33 1.387(3) . ? C32 C35 1.509(3) . ? C33 C34 1.380(3) . ? C33 H37 0.95(2) . ? C34 H27 0.97(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.384(2) . ? C36 C41 1.385(2) . ? C37 C38 1.390(3) . ? C37 H31 0.93(2) . ? C38 C39 1.384(3) . ? C38 H18 0.97(2) . ? C39 C40 1.386(3) . ? C39 C42 1.509(3) . ? C40 C41 1.383(3) . ? C40 H12 0.92(2) . ? C41 H17 0.92(2) . ? C42 H62A 0.9800 . ? C42 H62B 0.9800 . ? C42 H62C 0.9800 . ? C43 C44 1.375(3) . ? C43 C48 1.386(3) . ? C44 C45 1.385(3) . ? C44 H44 0.93(2) . ? C45 C46 1.380(3) . ? C45 H26 0.91(2) . ? C46 C47 1.390(3) . ? C46 C49 1.511(3) . ? C47 C48 1.381(3) . ? C47 H24 0.95(3) . ? C48 H16 0.96(2) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? O19 C50 1.424(3) . ? O19 H70 0.81(3) . ? O20 C52 1.419(3) . ? O20 H29 0.85(3) . ? C50 C51 1.485(3) . ? C50 H22 1.06(2) . ? C50 H71 0.95(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.489(4) . ? C52 H33 0.92(2) . ? C52 H60 1.01(3) . ? C53 H50 0.94(3) . ? C53 H61 1.03(3) . ? C53 H62 1.00(3) . ? 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 O9 Fe1 O8 91.26(5) . . ? O9 Fe1 O7 93.63(5) . . ? O8 Fe1 O7 93.56(5) . . ? O9 Fe1 N5 88.58(5) . 2_765 ? O8 Fe1 N5 176.73(5) . 2_765 ? O7 Fe1 N5 89.72(5) . 2_765 ? O9 Fe1 N2 178.75(5) . . ? O8 Fe1 N2 89.22(5) . . ? O7 Fe1 N2 87.49(5) . . ? N5 Fe1 N2 90.87(5) 2_765 . ? O9 Fe1 N9 90.02(5) . . ? O8 Fe1 N9 87.27(5) . . ? O7 Fe1 N9 176.24(5) . . ? N5 Fe1 N9 89.46(5) 2_765 . ? N2 Fe1 N9 88.86(5) . . ? N6 Fe2 N6 180.0 2_765 . ? N6 Fe2 N1 88.88(5) 2_765 2_765 ? N6 Fe2 N1 91.12(5) . 2_765 ? N6 Fe2 N1 91.12(5) 2_765 . ? N6 Fe2 N1 88.88(5) . . ? N1 Fe2 N1 180.00(10) 2_765 . ? N6 Fe2 N10 89.13(5) 2_765 2_765 ? N6 Fe2 N10 90.87(5) . 2_765 ? N1 Fe2 N10 89.75(5) 2_765 2_765 ? N1 Fe2 N10 90.25(5) . 2_765 ? N6 Fe2 N10 90.87(5) 2_765 . ? N6 Fe2 N10 89.13(5) . . ? N1 Fe2 N10 90.25(5) 2_765 . ? N1 Fe2 N10 89.75(5) . . ? N10 Fe2 N10 180.00(7) 2_765 . ? C27 O7 Fe1 137.25(12) . . ? C27 O7 H52 110.2(19) . . ? Fe1 O7 H52 112.3(19) . . ? C25 O8 Fe1 128.27(12) . . ? C25 O8 H57 108.5(16) . . ? Fe1 O8 H57 120.8(16) . . ? Fe1 O9 H38 131.0(17) . . ? Fe1 O9 H48 112.6(16) . . ? H38 O9 H48 107(2) . . ? C2 N1 N2 107.22(13) . . ? C2 N1 Fe2 129.02(11) . . ? N2 N1 Fe2 123.76(10) . . ? C1 N2 N1 106.82(13) . . ? C1 N2 Fe1 126.54(11) . . ? N1 N2 Fe1 126.50(10) . . ? C1 N3 C2 105.11(14) . . ? C1 N3 C3 126.16(14) . . ? C2 N3 C3 128.70(14) . . ? O2 N4 O1 123.47(18) . . ? O2 N4 C6 118.16(18) . . ? O1 N4 C6 118.37(18) . . ? C10 N5 N6 106.95(13) . . ? C10 N5 Fe1 127.61(11) . 2_765 ? N6 N5 Fe1 125.05(10) . 2_765 ? C9 N6 N5 107.43(13) . . ? C9 N6 Fe2 127.30(11) . . ? N5 N6 Fe2 125.18(10) . . ? C9 N7 C10 105.13(14) . . ? C9 N7 C11 127.35(14) . . ? C10 N7 C11 127.51(14) . . ? O3 N8 O4 124.09(17) . . ? O3 N8 C14 118.02(17) . . ? O4 N8 C14 117.87(17) . . ? C17 N9 N10 107.04(13) . . ? C17 N9 Fe1 128.07(11) . . ? N10 N9 Fe1 124.85(10) . . ? C18 N10 N9 107.23(13) . . ? C18 N10 Fe2 127.94(11) . . ? N9 N10 Fe2 124.79(10) . . ? C18 N11 C17 105.20(14) . . ? C18 N11 C19 128.12(14) . . ? C17 N11 C19 126.62(14) . . ? O5 N12 O6 123.84(17) . . ? O5 N12 C22 118.48(16) . . ? O6 N12 C22 117.67(17) . . ? N2 C1 N3 110.78(14) . . ? N2 C1 H19 124.3(12) . . ? N3 C1 H19 124.9(12) . . ? N1 C2 N3 110.07(14) . . ? N1 C2 H4 126.7(12) . . ? N3 C2 H4 123.3(12) . . ? C8 C3 C4 122.11(16) . . ? C8 C3 N3 119.52(15) . . ? C4 C3 N3 118.36(15) . . ? C3 C4 C5 119.35(18) . . ? C3 C4 H45 119.9(13) . . ? C5 C4 H45 120.7(13) . . ? C6 C5 C4 117.88(18) . . ? C6 C5 H28 119.8(14) . . ? C4 C5 H28 122.3(14) . . ? C7 C6 C5 123.18(17) . . ? C7 C6 N4 118.91(18) . . ? C5 C6 N4 117.91(18) . . ? C6 C7 C8 118.87(18) . . ? C6 C7 H20 121.6(14) . . ? C8 C7 H20 119.5(14) . . ? C3 C8 C7 118.52(18) . . ? C3 C8 H35 120.2(12) . . ? C7 C8 H35 121.2(12) . . ? N6 C9 N7 110.00(14) . . ? N6 C9 H3 125.4(13) . . ? N7 C9 H3 124.6(13) . . ? N5 C10 N7 110.49(14) . . ? N5 C10 H9 124.1(12) . . ? N7 C10 H9 125.1(12) . . ? C12 C11 C16 122.07(16) . . ? C12 C11 N7 118.88(15) . . ? C16 C11 N7 119.03(15) . . ? C13 C12 C11 119.01(17) . . ? C13 C12 H14 120.4(12) . . ? C11 C12 H14 120.6(12) . . ? C14 C13 C12 118.48(17) . . ? C14 C13 H11 121.0(13) . . ? C12 C13 H11 120.4(13) . . ? C15 C14 C13 122.99(17) . . ? C15 C14 N8 118.64(17) . . ? C13 C14 N8 118.34(16) . . ? C14 C15 C16 118.82(18) . . ? C14 C15 H21 120.8(13) . . ? C16 C15 H21 120.3(13) . . ? C15 C16 C11 118.63(17) . . ? C15 C16 H7 120.3(14) . . ? C11 C16 H7 121.0(14) . . ? N9 C17 N11 110.44(15) . . ? N9 C17 H1 127.0(11) . . ? N11 C17 H1 122.6(11) . . ? N10 C18 N11 110.09(14) . . ? N10 C18 H2 124.2(12) . . ? N11 C18 H2 125.7(12) . . ? C24 C19 C20 122.03(16) . . ? C24 C19 N11 119.00(15) . . ? C20 C19 N11 118.96(15) . . ? C21 C20 C19 118.83(17) . . ? C21 C20 H10 120.4(12) . . ? C19 C20 H10 120.8(12) . . ? C22 C21 C20 118.68(17) . . ? C22 C21 H30 121.7(12) . . ? C20 C21 H30 119.5(12) . . ? C21 C22 C23 122.95(17) . . ? C21 C22 N12 118.89(16) . . ? C23 C22 N12 118.13(17) . . ? C22 C23 C24 118.36(18) . . ? C22 C23 H5 122.4(13) . . ? C24 C23 H5 119.3(13) . . ? C19 C24 C23 119.11(17) . . ? C19 C24 H34 122.6(12) . . ? C23 C24 H34 118.2(12) . . ? O8 C25 C26 112.09(16) . . ? O8 C25 H6 105.7(12) . . ? C26 C25 H6 112.4(12) . . ? O8 C25 H25 108.8(12) . . ? C26 C25 H25 110.8(12) . . ? H6 C25 H25 106.8(17) . . ? C25 C26 H39 111.3(12) . . ? C25 C26 H47 109.4(15) . . ? H39 C26 H47 109.2(19) . . ? C25 C26 H51 107.5(14) . . ? H39 C26 H51 108.1(18) . . ? H47 C26 H51 111(2) . . ? O7 C27 C28 111.53(17) . . ? O7 C27 H13 106.0(13) . . ? C28 C27 H13 111.0(13) . . ? O7 C27 H43 112.4(12) . . ? C28 C27 H43 108.7(12) . . ? H13 C27 H43 107.1(17) . . ? C27 C28 H36 112.0(15) . . ? C27 C28 H40 108.9(16) . . ? H36 C28 H40 109(2) . . ? C27 C28 H41 110.1(15) . . ? H36 C28 H41 105(2) . . ? H40 C28 H41 112(2) . . ? O10 S1 O12 113.16(8) . . ? O10 S1 O11 112.44(9) . . ? O12 S1 O11 112.49(8) . . ? O10 S1 C29 106.80(8) . . ? O12 S1 C29 106.20(8) . . ? O11 S1 C29 105.03(8) . . ? O13 S2 O14 112.55(9) . . ? O13 S2 O15 113.41(10) . . ? O14 S2 O15 112.54(10) . . ? O13 S2 C36 106.94(8) . . ? O14 S2 C36 105.77(8) . . ? O15 S2 C36 104.84(8) . . ? O18 S3 O17 112.53(9) . . ? O18 S3 O16 112.63(10) . . ? O17 S3 O16 113.06(10) . . ? O18 S3 C43 105.73(8) . . ? O17 S3 C43 107.01(8) . . ? O16 S3 C43 105.14(9) . . ? C30 C29 C34 119.67(17) . . ? C30 C29 S1 120.27(15) . . ? C34 C29 S1 119.95(14) . . ? C29 C30 C31 119.72(19) . . ? C29 C30 H8 120.9(14) . . ? C31 C30 H8 119.4(14) . . ? C32 C31 C30 121.54(19) . . ? C32 C31 H42 121.6(14) . . ? C30 C31 H42 116.8(14) . . ? C31 C32 C33 117.83(18) . . ? C31 C32 C35 121.55(19) . . ? C33 C32 C35 120.61(19) . . ? C34 C33 C32 121.53(19) . . ? C34 C33 H37 119.2(13) . . ? C32 C33 H37 119.2(13) . . ? C33 C34 C29 119.69(17) . . ? C33 C34 H27 121.8(13) . . ? C29 C34 H27 118.5(13) . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C41 119.88(16) . . ? C37 C36 S2 120.80(13) . . ? C41 C36 S2 119.32(13) . . ? C36 C37 C38 119.66(17) . . ? C36 C37 H31 120.9(13) . . ? C38 C37 H31 119.5(13) . . ? C39 C38 C37 121.22(17) . . ? C39 C38 H18 119.3(13) . . ? C37 C38 H18 119.5(13) . . ? C38 C39 C40 118.10(17) . . ? C38 C39 C42 121.26(18) . . ? C40 C39 C42 120.63(18) . . ? C41 C40 C39 121.51(18) . . ? C41 C40 H12 120.3(14) . . ? C39 C40 H12 118.1(14) . . ? C40 C41 C36 119.63(17) . . ? C40 C41 H17 120.6(13) . . ? C36 C41 H17 119.8(13) . . ? C39 C42 H62A 109.5 . . ? C39 C42 H62B 109.5 . . ? H62A C42 H62B 109.5 . . ? C39 C42 H62C 109.5 . . ? H62A C42 H62C 109.5 . . ? H62B C42 H62C 109.5 . . ? C44 C43 C48 119.10(18) . . ? C44 C43 S3 121.50(15) . . ? C48 C43 S3 119.29(14) . . ? C43 C44 C45 119.9(2) . . ? C43 C44 H44 118.0(14) . . ? C45 C44 H44 122.1(14) . . ? C46 C45 C44 122.0(2) . . ? C46 C45 H26 119.5(14) . . ? C44 C45 H26 118.6(14) . . ? C45 C46 C47 117.51(19) . . ? C45 C46 C49 121.5(2) . . ? C47 C46 C49 120.9(2) . . ? C48 C47 C46 121.0(2) . . ? C48 C47 H24 118.8(16) . . ? C46 C47 H24 120.2(16) . . ? C47 C48 C43 120.51(19) . . ? C47 C48 H16 119.3(14) . . ? C43 C48 H16 120.2(14) . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C50 O19 H70 107(2) . . ? C52 O20 H29 112.0(19) . . ? O19 C50 C51 109.2(2) . . ? O19 C50 H22 108.9(13) . . ? C51 C50 H22 110.9(13) . . ? O19 C50 H71 111.4(16) . . ? C51 C50 H71 111.9(16) . . ? H22 C50 H71 104(2) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O20 C52 C53 108.4(2) . . ? O20 C52 H33 108.7(15) . . ? C53 C52 H33 110.8(15) . . ? O20 C52 H60 106.2(15) . . ? C53 C52 H60 111.4(15) . . ? H33 C52 H60 111(2) . . ? C52 C53 H50 113.2(17) . . ? C52 C53 H61 110.0(16) . . ? H50 C53 H61 105(2) . . ? C52 C53 H62 106.5(17) . . ? H50 C53 H62 107(2) . . ? H61 C53 H62 115(2) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.64 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.653 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.068 # Attachment '4434_web_deposit_cif_file_2_MuraleeMURUGESU_1298934407.cif' data_ds2506 _database_code_depnum_ccdc_archive 'CCDC 815195' #TrackingRef '4434_web_deposit_cif_file_2_MuraleeMURUGESU_1298934407.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H130 Co3 N24 O40 S6' _chemical_formula_weight 2749.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.677(5) _cell_length_b 15.268(5) _cell_length_c 16.480(5) _cell_angle_alpha 107.590(4) _cell_angle_beta 99.874(4) _cell_angle_gamma 110.825(4) _cell_volume 3124.9(17) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8023 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 24.66 _exptl_crystal_description block _exptl_crystal_colour lt_brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1431 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8919 _exptl_absorpt_correction_T_max 0.9713 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 30243 _diffrn_reflns_av_R_equivalents 0.1048 _diffrn_reflns_av_sigmaI/netI 0.1403 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 24.70 _reflns_number_total 10538 _reflns_number_gt 5941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^]' _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 10538 _refine_ls_number_parameters 808 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1396 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 1.0000 0.5000 0.0169(3) Uani 1 2 d S . . Co2 Co 0.62919(5) 0.85715(5) 0.59705(5) 0.0186(2) Uani 1 1 d . . . S1 S 0.79282(12) 0.92990(11) 0.38845(11) 0.0296(4) Uani 1 1 d . . . S3 S 0.68896(12) 0.14017(11) 0.86846(11) 0.0312(4) Uani 1 1 d . . . S2 S 0.29183(12) 0.61354(11) 0.42803(11) 0.0309(4) Uani 1 1 d . . . N1 N 0.5464(3) 0.8089(3) 0.4598(3) 0.0198(11) Uani 1 1 d . . . N2 N 0.5027(3) 0.8614(3) 0.4235(3) 0.0189(11) Uani 1 1 d . . . N3 N 0.4827(3) 0.7250(3) 0.3151(3) 0.0215(11) Uani 1 1 d . . . N4 N 0.3594(4) 0.4108(4) -0.0250(4) 0.0434(15) Uani 1 1 d . . . N5 N 0.4644(3) 0.9427(3) 0.5993(3) 0.0193(11) Uani 1 1 d . . . N6 N 0.5152(3) 0.8969(3) 0.6375(3) 0.0182(11) Uani 1 1 d . . . N7 N 0.3960(3) 0.9051(3) 0.6992(3) 0.0211(11) Uani 1 1 d . . . N8 N 0.1240(4) 0.8538(5) 0.9051(4) 0.0409(14) Uani 1 1 d . . . N9 N 0.7085(3) 1.0059(3) 0.5998(3) 0.0189(11) Uani 1 1 d . . . N10 N 0.6619(3) 1.0591(3) 0.5686(3) 0.0204(11) Uani 1 1 d . . . N11 N 0.8276(3) 1.1559(3) 0.6273(3) 0.0194(11) Uani 1 1 d . . . N12 N 1.2192(4) 1.4844(4) 0.7367(3) 0.0371(14) Uani 1 1 d . . . O1 O 0.3506(4) 0.3273(4) -0.0278(3) 0.0594(15) Uani 1 1 d . . . O2 O 0.3438(5) 0.4294(4) -0.0917(3) 0.0795(19) Uani 1 1 d . . . O3 O 0.1098(4) 0.9272(4) 0.9429(4) 0.0669(16) Uani 1 1 d . . . O4 O 0.0807(3) 0.7687(4) 0.9039(3) 0.0540(14) Uani 1 1 d . . . O5 O 1.2935(3) 1.4652(3) 0.7356(3) 0.0524(13) Uani 1 1 d . . . O6 O 1.2251(4) 1.5701(4) 0.7597(4) 0.0733(18) Uani 1 1 d . . . O7 O 0.7431(3) 0.8219(3) 0.5573(3) 0.0261(9) Uani 1 1 d . . . H7A H 0.7658 0.8419 0.5115 0.039 Uiso 1 1 d R . . O8 O 0.5436(3) 0.7054(3) 0.5860(3) 0.0282(10) Uani 1 1 d . . . H8A H 0.4782 0.6645 0.5382 0.042 Uiso 1 1 d R . . O9 O 0.7135(3) 0.9056(3) 0.7299(2) 0.0301(10) Uani 1 1 d . . . H9A H 0.7040 0.8714 0.7638 0.045 Uiso 1 1 d R . . H9B H 0.7178 0.9611 0.7709 0.045 Uiso 1 1 d R . . O10 O 0.6854(3) 0.8790(3) 0.3361(3) 0.0446(12) Uani 1 1 d . . . O11 O 0.8216(4) 0.8724(4) 0.4360(3) 0.0534(14) Uani 1 1 d . . . O12 O 0.8251(3) 1.0348(3) 0.4453(3) 0.0506(13) Uani 1 1 d . . . O13 O 0.3080(3) 0.7044(3) 0.5030(3) 0.0458(12) Uani 1 1 d . . . O14 O 0.3741(3) 0.5821(3) 0.4434(3) 0.0388(11) Uani 1 1 d . . . O15 O 0.2699(3) 0.6213(3) 0.3419(3) 0.0412(11) Uani 1 1 d . . . O16 O 0.7430(4) 0.0988(3) 0.8143(3) 0.0526(13) Uani 1 1 d . . . O17 O 0.5873(3) 0.1173(3) 0.8158(3) 0.0460(12) Uani 1 1 d . . . O18 O 0.6879(3) 0.1133(3) 0.9456(3) 0.0464(12) Uani 1 1 d . . . O19 O 0.6940(3) 0.8116(3) 0.8467(3) 0.0502(13) Uani 1 1 d . . . H19A H 0.6526 0.7507 0.8188 0.075 Uiso 1 1 calc R . . O20 O 0.4894(7) 0.7782(6) 0.9574(7) 0.170(4) Uani 1 1 d . . . H20A H 0.4512 0.7664 0.9883 0.256 Uiso 1 1 calc R . . C1 C 0.5335(4) 0.7290(4) 0.3932(4) 0.0212(13) Uani 1 1 d . . . H1A H 0.5566 0.6804 0.3988 0.025 Uiso 1 1 calc R . . C2 C 0.4650(4) 0.8092(4) 0.3365(4) 0.0189(13) Uani 1 1 d . . . H2A H 0.4310 0.8274 0.2953 0.023 Uiso 1 1 calc R . . C3 C 0.4504(4) 0.6459(4) 0.2274(4) 0.0223(13) Uani 1 1 d . . . C4 C 0.4507(4) 0.6690(4) 0.1537(4) 0.0313(15) Uani 1 1 d . . . H4A H 0.4722 0.7372 0.1599 0.038 Uiso 1 1 calc R . . C5 C 0.4192(5) 0.5921(4) 0.0694(4) 0.0337(16) Uani 1 1 d . . . H5A H 0.4171 0.6069 0.0179 0.040 Uiso 1 1 calc R . . C6 C 0.3910(5) 0.4927(4) 0.0633(4) 0.0316(15) Uani 1 1 d . . . C7 C 0.3928(5) 0.4698(5) 0.1375(4) 0.0406(17) Uani 1 1 d . . . H7B H 0.3759 0.4024 0.1320 0.049 Uiso 1 1 calc R . . C8 C 0.4194(5) 0.5456(4) 0.2202(4) 0.0368(16) Uani 1 1 d . . . H8B H 0.4166 0.5300 0.2710 0.044 Uiso 1 1 calc R . . C10 C 0.3933(4) 0.9469(4) 0.6372(4) 0.0221(13) Uani 1 1 d . . . H10A H 0.3477 0.9745 0.6235 0.027 Uiso 1 1 calc R . . C11 C 0.4737(4) 0.8770(4) 0.6976(4) 0.0230(14) Uani 1 1 d . . . H11A H 0.4948 0.8472 0.7348 0.028 Uiso 1 1 calc R . . C12 C 0.3297(4) 0.8940(4) 0.7542(4) 0.0231(14) Uani 1 1 d . . . C13 C 0.2934(4) 0.8049(4) 0.7683(4) 0.0285(15) Uani 1 1 d . . . H13A H 0.3136 0.7533 0.7442 0.034 Uiso 1 1 calc R . . C14 C 0.2264(4) 0.7929(5) 0.8190(4) 0.0346(16) Uani 1 1 d . . . H14A H 0.2010 0.7332 0.8301 0.042 Uiso 1 1 calc R . . C15 C 0.1983(4) 0.8693(5) 0.8523(4) 0.0289(15) Uani 1 1 d . . . C16 C 0.2337(5) 0.9581(4) 0.8387(4) 0.0326(15) Uani 1 1 d . . . H16A H 0.2134 1.0095 0.8633 0.039 Uiso 1 1 calc R . . C17 C 0.3001(4) 0.9707(4) 0.7880(4) 0.0312(15) Uani 1 1 d . . . H17A H 0.3245 1.0303 0.7768 0.037 Uiso 1 1 calc R . . C19 C 0.8062(4) 1.0655(4) 0.6342(4) 0.0221(13) Uani 1 1 d . . . H19B H 0.8555 1.0479 0.6604 0.027 Uiso 1 1 calc R . . C20 C 0.7353(4) 1.1486(4) 0.5850(4) 0.0217(13) Uani 1 1 d . . . H20B H 0.7255 1.1998 0.5697 0.026 Uiso 1 1 calc R . . C21 C 0.9280(4) 1.2402(4) 0.6546(4) 0.0200(13) Uani 1 1 d . . . C22 C 1.0108(4) 1.2190(4) 0.6466(4) 0.0306(15) Uani 1 1 d . . . H22A H 1.0022 1.1513 0.6222 0.037 Uiso 1 1 calc R . . C23 C 1.1070(4) 1.3001(4) 0.6756(4) 0.0334(16) Uani 1 1 d . . . H23A H 1.1652 1.2882 0.6730 0.040 Uiso 1 1 calc R . . C24 C 1.1162(4) 1.3980(4) 0.7081(4) 0.0268(15) Uani 1 1 d . . . C25 C 1.0338(5) 1.4192(4) 0.7141(4) 0.0302(15) Uani 1 1 d . . . H25A H 1.0422 1.4870 0.7354 0.036 Uiso 1 1 calc R . . C26 C 0.9373(4) 1.3384(4) 0.6880(4) 0.0251(14) Uani 1 1 d . . . H26A H 0.8797 1.3506 0.6931 0.030 Uiso 1 1 calc R . . C28 C 0.7766(4) 0.7468(4) 0.5672(4) 0.0320(15) Uani 1 1 d . . . H28A H 0.7698 0.7393 0.6231 0.038 Uiso 1 1 calc R . . H28B H 0.8493 0.7706 0.5713 0.038 Uiso 1 1 calc R . . C29 C 0.7162(5) 0.6449(4) 0.4906(5) 0.0451(18) Uani 1 1 d . . . H29A H 0.7409 0.5968 0.5004 0.068 Uiso 1 1 calc R . . H29B H 0.7243 0.6515 0.4352 0.068 Uiso 1 1 calc R . . H29C H 0.6442 0.6207 0.4865 0.068 Uiso 1 1 calc R . . C30 C 0.5504(5) 0.6405(5) 0.6327(4) 0.0386(17) Uani 1 1 d . . . H30A H 0.6185 0.6731 0.6773 0.046 Uiso 1 1 calc R . . H30B H 0.5424 0.5756 0.5898 0.046 Uiso 1 1 calc R . . C31 C 0.4702(6) 0.6202(5) 0.6785(5) 0.060(2) Uani 1 1 d . . . H31A H 0.4791 0.5789 0.7111 0.090 Uiso 1 1 calc R . . H31B H 0.4026 0.5841 0.6341 0.090 Uiso 1 1 calc R . . H31C H 0.4768 0.6844 0.7200 0.090 Uiso 1 1 calc R . . C32 C 0.8618(4) 0.9299(4) 0.3090(4) 0.0230(14) Uani 1 1 d . . . C33 C 0.9571(4) 1.0085(4) 0.3292(4) 0.0325(15) Uani 1 1 d . . . H33A H 0.9867 1.0629 0.3858 0.039 Uiso 1 1 calc R . . C34 C 1.0093(4) 1.0075(4) 0.2666(4) 0.0291(15) Uani 1 1 d . . . H34A H 1.0734 1.0621 0.2807 0.035 Uiso 1 1 calc R . . C35 C 0.9684(5) 0.9273(4) 0.1835(4) 0.0309(15) Uani 1 1 d . . . C36 C 0.8726(4) 0.8482(4) 0.1646(4) 0.0333(16) Uani 1 1 d . . . H36A H 0.8435 0.7927 0.1088 0.040 Uiso 1 1 calc R . . C37 C 0.8200(4) 0.8500(4) 0.2265(4) 0.0307(15) Uani 1 1 d . . . H37A H 0.7552 0.7964 0.2122 0.037 Uiso 1 1 calc R . . C38 C 1.0234(5) 0.9239(5) 0.1132(5) 0.053(2) Uani 1 1 d . . . H38A H 0.9822 0.8617 0.0601 0.080 Uiso 1 1 calc R . . H38B H 1.0894 0.9253 0.1369 0.080 Uiso 1 1 calc R . . H38C H 1.0337 0.9824 0.0977 0.080 Uiso 1 1 calc R . . C39 C 0.1796(4) 0.5121(4) 0.4232(4) 0.0242(14) Uani 1 1 d . . . C40 C 0.1521(4) 0.5187(4) 0.5008(4) 0.0292(15) Uani 1 1 d . . . H40A H 0.1889 0.5780 0.5536 0.035 Uiso 1 1 calc R . . C41 C 0.0685(4) 0.4357(5) 0.4995(4) 0.0340(16) Uani 1 1 d . . . H41A H 0.0497 0.4400 0.5518 0.041 Uiso 1 1 calc R . . C42 C 0.0137(4) 0.3480(5) 0.4223(5) 0.0341(16) Uani 1 1 d . . . C43 C 0.0435(5) 0.3447(5) 0.3460(5) 0.0443(18) Uani 1 1 d . . . H43A H 0.0072 0.2857 0.2930 0.053 Uiso 1 1 calc R . . C44 C 0.1249(5) 0.4260(4) 0.3461(4) 0.0379(17) Uani 1 1 d . . . H44A H 0.1427 0.4221 0.2935 0.045 Uiso 1 1 calc R . . C45 C -0.0746(5) 0.2582(5) 0.4233(5) 0.0493(19) Uani 1 1 d . . . H45A H -0.0827 0.2755 0.4825 0.074 Uiso 1 1 calc R . . H45B H -0.0599 0.1992 0.4087 0.074 Uiso 1 1 calc R . . H45C H -0.1373 0.2427 0.3795 0.074 Uiso 1 1 calc R . . C46 C 0.7600(4) 0.2761(4) 0.9110(4) 0.0269(14) Uani 1 1 d . . . C47 C 0.7857(5) 0.3210(5) 0.8514(4) 0.0413(17) Uani 1 1 d . . . H47A H 0.7706 0.2804 0.7907 0.050 Uiso 1 1 calc R . . C48 C 0.8339(5) 0.4259(5) 0.8823(4) 0.0445(18) Uani 1 1 d . . . H48A H 0.8491 0.4561 0.8413 0.053 Uiso 1 1 calc R . . C49 C 0.8605(5) 0.4881(5) 0.9715(5) 0.0421(18) Uani 1 1 d . . . C50 C 0.8346(5) 0.4409(5) 1.0296(5) 0.0486(19) Uani 1 1 d . . . H50A H 0.8516 0.4810 1.0907 0.058 Uiso 1 1 calc R . . C51 C 0.7841(5) 0.3353(5) 0.9990(4) 0.0404(17) Uani 1 1 d . . . H51A H 0.7667 0.3047 1.0392 0.048 Uiso 1 1 calc R . . C52 C 0.9156(6) 0.6036(5) 1.0056(5) 0.064(2) Uani 1 1 d . . . H52A H 0.9274 0.6334 1.0696 0.096 Uiso 1 1 calc R . . H52B H 0.8737 0.6281 0.9751 0.096 Uiso 1 1 calc R . . H52C H 0.9809 0.6231 0.9938 0.096 Uiso 1 1 calc R . . C53 C 0.7841(5) 0.8187(5) 0.9029(5) 0.0463(19) Uani 1 1 d . . . H53A H 0.7662 0.7887 0.9461 0.056 Uiso 1 1 calc R . . H53B H 0.8331 0.8904 0.9364 0.056 Uiso 1 1 calc R . . C54 C 0.8317(6) 0.7635(6) 0.8469(5) 0.065(2) Uani 1 1 d . . . H54A H 0.8936 0.7694 0.8850 0.098 Uiso 1 1 calc R . . H54B H 0.8488 0.7931 0.8039 0.098 Uiso 1 1 calc R . . H54C H 0.7837 0.6921 0.8151 0.098 Uiso 1 1 calc R . . C55 C 0.5206(6) 0.8864(5) 0.9639(5) 0.054(2) Uani 1 1 d . . . H55A H 0.4592 0.8955 0.9432 0.065 Uiso 1 1 calc R . . H55B H 0.5567 0.9341 1.0265 0.065 Uiso 1 1 calc R . . C56 C 0.5838(4) 0.9075(4) 0.9121(3) 0.0162(12) Uani 1 1 d . . . H56A H 0.6033 0.9771 0.9172 0.024 Uiso 1 1 calc R . . H56B H 0.5475 0.8610 0.8500 0.024 Uiso 1 1 calc R . . H56C H 0.6449 0.8991 0.9330 0.024 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 0.0169(6) 0.0174(6) 0.0185(6) 0.0089(5) 0.0083(5) 0.0070(5) Co2 0.0184(4) 0.0192(4) 0.0200(5) 0.0097(3) 0.0077(4) 0.0077(3) S1 0.0350(9) 0.0318(9) 0.0374(10) 0.0204(8) 0.0252(8) 0.0190(8) S3 0.0366(10) 0.0261(9) 0.0268(10) 0.0095(7) 0.0080(8) 0.0108(7) S2 0.0256(9) 0.0258(9) 0.0413(11) 0.0173(8) 0.0087(8) 0.0088(7) N1 0.019(3) 0.021(3) 0.024(3) 0.010(2) 0.011(2) 0.010(2) N2 0.014(2) 0.014(2) 0.023(3) 0.004(2) 0.006(2) 0.003(2) N3 0.020(3) 0.020(3) 0.022(3) 0.006(2) 0.007(2) 0.007(2) N4 0.045(4) 0.038(4) 0.036(4) 0.003(3) 0.014(3) 0.014(3) N5 0.023(3) 0.022(3) 0.016(3) 0.009(2) 0.008(2) 0.010(2) N6 0.018(3) 0.020(2) 0.017(3) 0.008(2) 0.007(2) 0.007(2) N7 0.021(3) 0.023(3) 0.024(3) 0.010(2) 0.013(2) 0.010(2) N8 0.038(3) 0.063(4) 0.041(4) 0.030(3) 0.024(3) 0.030(3) N9 0.015(3) 0.022(3) 0.018(3) 0.010(2) 0.003(2) 0.007(2) N10 0.024(3) 0.021(3) 0.022(3) 0.011(2) 0.015(2) 0.011(2) N11 0.014(2) 0.018(3) 0.023(3) 0.008(2) 0.003(2) 0.005(2) N12 0.023(3) 0.039(4) 0.037(4) 0.012(3) 0.012(3) 0.001(3) O1 0.072(4) 0.033(3) 0.045(3) -0.005(2) 0.012(3) 0.013(3) O2 0.134(5) 0.065(4) 0.023(3) 0.004(3) 0.009(3) 0.044(4) O3 0.084(4) 0.076(4) 0.078(4) 0.039(3) 0.067(4) 0.050(3) O4 0.045(3) 0.062(3) 0.074(4) 0.044(3) 0.039(3) 0.019(3) O5 0.023(3) 0.054(3) 0.067(4) 0.021(3) 0.014(3) 0.004(2) O6 0.053(3) 0.022(3) 0.121(5) 0.017(3) 0.026(3) 0.000(2) O7 0.033(2) 0.031(2) 0.033(3) 0.022(2) 0.021(2) 0.0217(19) O8 0.025(2) 0.026(2) 0.032(3) 0.0174(19) 0.0063(19) 0.0069(18) O9 0.031(2) 0.033(2) 0.024(2) 0.0093(19) 0.006(2) 0.0151(19) O10 0.027(3) 0.051(3) 0.057(3) 0.022(2) 0.022(2) 0.014(2) O11 0.070(3) 0.083(4) 0.068(4) 0.058(3) 0.056(3) 0.059(3) O12 0.064(3) 0.034(3) 0.050(3) 0.008(2) 0.038(3) 0.016(2) O13 0.045(3) 0.025(2) 0.056(3) 0.012(2) 0.014(2) 0.006(2) O14 0.022(2) 0.029(2) 0.061(3) 0.022(2) 0.007(2) 0.0052(19) O15 0.030(2) 0.050(3) 0.053(3) 0.035(2) 0.016(2) 0.014(2) O16 0.066(3) 0.032(3) 0.062(3) 0.011(2) 0.036(3) 0.022(2) O17 0.045(3) 0.034(3) 0.043(3) 0.017(2) -0.009(2) 0.009(2) O18 0.059(3) 0.035(3) 0.037(3) 0.019(2) 0.005(2) 0.012(2) O19 0.051(3) 0.050(3) 0.045(3) 0.022(2) 0.007(3) 0.018(2) O20 0.215(10) 0.146(7) 0.249(11) 0.139(7) 0.157(9) 0.095(7) C1 0.024(3) 0.021(3) 0.020(3) 0.007(3) 0.008(3) 0.010(3) C2 0.018(3) 0.018(3) 0.022(4) 0.008(3) 0.005(3) 0.011(3) C3 0.023(3) 0.020(3) 0.023(4) 0.007(3) 0.007(3) 0.008(3) C4 0.040(4) 0.023(3) 0.030(4) 0.010(3) 0.009(3) 0.014(3) C5 0.048(4) 0.038(4) 0.024(4) 0.015(3) 0.019(3) 0.022(3) C6 0.034(4) 0.033(4) 0.019(4) 0.002(3) 0.006(3) 0.013(3) C7 0.047(4) 0.027(4) 0.040(5) 0.005(3) 0.013(4) 0.015(3) C8 0.045(4) 0.033(4) 0.024(4) 0.006(3) 0.010(3) 0.012(3) C10 0.019(3) 0.021(3) 0.029(4) 0.014(3) 0.007(3) 0.010(3) C11 0.022(3) 0.023(3) 0.028(4) 0.014(3) 0.009(3) 0.012(3) C12 0.016(3) 0.033(3) 0.024(4) 0.013(3) 0.009(3) 0.012(3) C13 0.025(3) 0.034(4) 0.038(4) 0.019(3) 0.016(3) 0.018(3) C14 0.035(4) 0.044(4) 0.039(4) 0.028(3) 0.020(3) 0.018(3) C15 0.026(3) 0.042(4) 0.024(4) 0.016(3) 0.014(3) 0.015(3) C16 0.040(4) 0.031(4) 0.034(4) 0.010(3) 0.024(3) 0.020(3) C17 0.035(4) 0.027(3) 0.034(4) 0.018(3) 0.013(3) 0.010(3) C19 0.023(3) 0.017(3) 0.023(3) 0.006(3) 0.004(3) 0.008(3) C20 0.020(3) 0.017(3) 0.026(4) 0.007(3) 0.006(3) 0.007(3) C21 0.013(3) 0.017(3) 0.021(3) 0.005(3) 0.003(3) 0.001(2) C22 0.030(4) 0.019(3) 0.047(4) 0.015(3) 0.015(3) 0.012(3) C23 0.020(3) 0.035(4) 0.053(5) 0.024(3) 0.018(3) 0.012(3) C24 0.019(3) 0.025(3) 0.022(4) 0.007(3) 0.004(3) -0.003(3) C25 0.039(4) 0.022(3) 0.026(4) 0.009(3) 0.015(3) 0.007(3) C26 0.019(3) 0.031(3) 0.023(4) 0.008(3) 0.014(3) 0.008(3) C28 0.034(4) 0.035(4) 0.040(4) 0.022(3) 0.016(3) 0.021(3) C29 0.049(4) 0.033(4) 0.056(5) 0.014(4) 0.016(4) 0.023(3) C30 0.039(4) 0.040(4) 0.042(4) 0.027(3) 0.016(3) 0.013(3) C31 0.072(6) 0.043(4) 0.061(6) 0.028(4) 0.022(5) 0.011(4) C32 0.019(3) 0.029(3) 0.023(4) 0.015(3) 0.007(3) 0.009(3) C33 0.027(4) 0.033(4) 0.033(4) 0.007(3) 0.007(3) 0.013(3) C34 0.021(3) 0.033(4) 0.036(4) 0.014(3) 0.013(3) 0.011(3) C35 0.036(4) 0.035(4) 0.030(4) 0.016(3) 0.016(3) 0.020(3) C36 0.029(4) 0.038(4) 0.025(4) 0.002(3) 0.010(3) 0.015(3) C37 0.024(3) 0.030(4) 0.032(4) 0.012(3) 0.006(3) 0.006(3) C38 0.056(5) 0.072(5) 0.045(5) 0.025(4) 0.033(4) 0.032(4) C39 0.029(3) 0.018(3) 0.029(4) 0.012(3) 0.007(3) 0.013(3) C40 0.030(4) 0.024(3) 0.025(4) 0.004(3) 0.003(3) 0.010(3) C41 0.031(4) 0.044(4) 0.034(4) 0.021(3) 0.019(3) 0.017(3) C42 0.022(3) 0.033(4) 0.049(5) 0.020(3) 0.007(3) 0.012(3) C43 0.047(4) 0.029(4) 0.033(4) 0.002(3) 0.003(4) 0.004(3) C44 0.035(4) 0.034(4) 0.039(4) 0.015(3) 0.018(3) 0.006(3) C45 0.043(4) 0.039(4) 0.062(5) 0.023(4) 0.019(4) 0.010(3) C46 0.030(3) 0.029(3) 0.020(4) 0.009(3) 0.005(3) 0.012(3) C47 0.050(4) 0.039(4) 0.026(4) 0.010(3) 0.013(3) 0.010(3) C48 0.051(4) 0.036(4) 0.034(4) 0.017(3) 0.012(4) 0.005(3) C49 0.038(4) 0.033(4) 0.044(5) 0.010(4) 0.009(4) 0.008(3) C50 0.062(5) 0.036(4) 0.031(4) 0.000(3) 0.005(4) 0.018(4) C51 0.060(5) 0.031(4) 0.022(4) 0.012(3) 0.004(3) 0.014(3) C52 0.065(5) 0.035(4) 0.076(6) 0.011(4) 0.019(5) 0.015(4) C53 0.054(5) 0.042(4) 0.038(5) 0.019(4) 0.013(4) 0.013(4) C54 0.047(5) 0.089(6) 0.067(6) 0.038(5) 0.014(4) 0.033(5) C55 0.064(5) 0.039(4) 0.054(5) 0.018(4) 0.010(4) 0.021(4) C56 0.030(3) 0.013(3) 0.021(3) 0.013(2) 0.021(3) 0.014(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 Co1 N2 2.129(4) . ? Co1 N2 2.129(4) 2_676 ? Co1 N5 2.133(4) . ? Co1 N5 2.133(4) 2_676 ? Co1 N10 2.162(4) 2_676 ? Co1 N10 2.162(4) . ? Co2 O7 2.077(4) . ? Co2 O9 2.077(4) . ? Co2 N6 2.115(4) . ? Co2 N1 2.133(5) . ? Co2 N9 2.133(4) . ? Co2 O8 2.140(4) . ? S1 O12 1.438(4) . ? S1 O10 1.446(4) . ? S1 O11 1.459(4) . ? S1 C32 1.787(6) . ? S3 O16 1.444(4) . ? S3 O18 1.449(4) . ? S3 O17 1.450(4) . ? S3 C46 1.794(6) . ? S2 O15 1.451(4) . ? S2 O14 1.461(4) . ? S2 O13 1.462(4) . ? S2 C39 1.784(6) . ? N1 C1 1.298(6) . ? N1 N2 1.391(6) . ? N2 C2 1.312(6) . ? N3 C1 1.344(7) . ? N3 C2 1.356(6) . ? N3 C3 1.441(7) . ? N4 O2 1.221(7) . ? N4 O1 1.221(7) . ? N4 C6 1.467(8) . ? N5 C10 1.315(6) . ? N5 N6 1.384(6) . ? N6 C11 1.304(7) . ? N7 C11 1.355(7) . ? N7 C10 1.360(7) . ? N7 C12 1.441(6) . ? N8 O3 1.215(6) . ? N8 O4 1.218(6) . ? N8 C15 1.506(7) . ? N9 C19 1.299(6) . ? N9 N10 1.386(6) . ? N10 C20 1.316(6) . ? N11 C19 1.348(6) . ? N11 C20 1.362(7) . ? N11 C21 1.451(6) . ? N12 O6 1.212(6) . ? N12 O5 1.227(6) . ? N12 C24 1.486(7) . ? O7 C28 1.439(6) . ? O8 C30 1.444(6) . ? O19 C53 1.427(8) . ? O20 C55 1.514(9) . ? C3 C4 1.364(8) . ? C3 C8 1.394(8) . ? C4 C5 1.390(8) . ? C5 C6 1.390(8) . ? C6 C7 1.369(9) . ? C7 C8 1.375(8) . ? C12 C13 1.382(7) . ? C12 C17 1.386(8) . ? C13 C14 1.395(8) . ? C14 C15 1.365(8) . ? C15 C16 1.371(8) . ? C16 C17 1.388(8) . ? C21 C26 1.378(7) . ? C21 C22 1.382(7) . ? C22 C23 1.386(7) . ? C23 C24 1.374(8) . ? C24 C25 1.370(8) . ? C25 C26 1.393(7) . ? C28 C29 1.499(8) . ? C30 C31 1.497(9) . ? C32 C37 1.376(8) . ? C32 C33 1.383(7) . ? C33 C34 1.387(8) . ? C34 C35 1.384(8) . ? C35 C36 1.395(8) . ? C35 C38 1.521(8) . ? C36 C37 1.381(8) . ? C39 C44 1.369(8) . ? C39 C40 1.393(8) . ? C40 C41 1.406(8) . ? C41 C42 1.383(8) . ? C42 C43 1.393(9) . ? C42 C45 1.522(8) . ? C43 C44 1.382(8) . ? C46 C51 1.359(8) . ? C46 C47 1.389(8) . ? C47 C48 1.380(8) . ? C48 C49 1.383(9) . ? C49 C50 1.388(9) . ? C49 C52 1.521(8) . ? C50 C51 1.391(8) . ? C53 C54 1.490(9) . ? C55 C56 1.383(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N2 179.998(1) . 2_676 ? N2 Co1 N5 90.30(17) . . ? N2 Co1 N5 89.70(16) 2_676 . ? N2 Co1 N5 89.70(16) . 2_676 ? N2 Co1 N5 90.30(17) 2_676 2_676 ? N5 Co1 N5 179.999(1) . 2_676 ? N2 Co1 N10 91.35(16) . 2_676 ? N2 Co1 N10 88.65(16) 2_676 2_676 ? N5 Co1 N10 90.19(16) . 2_676 ? N5 Co1 N10 89.81(16) 2_676 2_676 ? N2 Co1 N10 88.65(16) . . ? N2 Co1 N10 91.35(16) 2_676 . ? N5 Co1 N10 89.81(16) . . ? N5 Co1 N10 90.19(16) 2_676 . ? N10 Co1 N10 180.000(1) 2_676 . ? O7 Co2 O9 89.36(15) . . ? O7 Co2 N6 178.48(15) . . ? O9 Co2 N6 90.67(16) . . ? O7 Co2 N1 89.36(16) . . ? O9 Co2 N1 178.46(16) . . ? N6 Co2 N1 90.59(17) . . ? O7 Co2 N9 88.16(15) . . ? O9 Co2 N9 90.58(16) . . ? N6 Co2 N9 90.32(16) . . ? N1 Co2 N9 88.51(16) . . ? O7 Co2 O8 92.25(14) . . ? O9 Co2 O8 92.98(15) . . ? N6 Co2 O8 89.26(15) . . ? N1 Co2 O8 87.93(15) . . ? N9 Co2 O8 176.42(16) . . ? O12 S1 O10 112.9(3) . . ? O12 S1 O11 113.2(3) . . ? O10 S1 O11 112.4(3) . . ? O12 S1 C32 106.9(3) . . ? O10 S1 C32 105.7(3) . . ? O11 S1 C32 104.9(3) . . ? O16 S3 O18 113.0(3) . . ? O16 S3 O17 112.3(3) . . ? O18 S3 O17 112.5(3) . . ? O16 S3 C46 105.8(3) . . ? O18 S3 C46 106.7(3) . . ? O17 S3 C46 105.7(3) . . ? O15 S2 O14 112.7(3) . . ? O15 S2 O13 113.4(3) . . ? O14 S2 O13 112.4(3) . . ? O15 S2 C39 106.0(3) . . ? O14 S2 C39 105.3(2) . . ? O13 S2 C39 106.3(3) . . ? C1 N1 N2 106.7(4) . . ? C1 N1 Co2 126.7(4) . . ? N2 N1 Co2 126.4(3) . . ? C2 N2 N1 107.1(4) . . ? C2 N2 Co1 128.5(4) . . ? N1 N2 Co1 124.4(3) . . ? C1 N3 C2 105.6(4) . . ? C1 N3 C3 127.2(5) . . ? C2 N3 C3 127.1(5) . . ? O2 N4 O1 123.3(6) . . ? O2 N4 C6 118.7(6) . . ? O1 N4 C6 118.0(6) . . ? C10 N5 N6 107.7(4) . . ? C10 N5 Co1 126.8(4) . . ? N6 N5 Co1 125.5(3) . . ? C11 N6 N5 106.7(4) . . ? C11 N6 Co2 127.5(4) . . ? N5 N6 Co2 125.7(3) . . ? C11 N7 C10 105.3(4) . . ? C11 N7 C12 128.1(5) . . ? C10 N7 C12 126.6(5) . . ? O3 N8 O4 125.6(6) . . ? O3 N8 C15 116.6(6) . . ? O4 N8 C15 117.8(6) . . ? C19 N9 N10 107.2(4) . . ? C19 N9 Co2 127.9(4) . . ? N10 N9 Co2 124.8(3) . . ? C20 N10 N9 106.8(4) . . ? C20 N10 Co1 127.7(4) . . ? N9 N10 Co1 125.5(3) . . ? C19 N11 C20 105.0(4) . . ? C19 N11 C21 127.2(5) . . ? C20 N11 C21 127.7(4) . . ? O6 N12 O5 123.6(5) . . ? O6 N12 C24 118.1(5) . . ? O5 N12 C24 118.3(5) . . ? C28 O7 Co2 129.9(3) . . ? C30 O8 Co2 138.7(4) . . ? N1 C1 N3 110.9(5) . . ? N2 C2 N3 109.6(5) . . ? C4 C3 C8 121.2(5) . . ? C4 C3 N3 120.7(5) . . ? C8 C3 N3 118.2(5) . . ? C3 C4 C5 120.2(5) . . ? C6 C5 C4 118.1(6) . . ? C5 C6 C7 121.7(6) . . ? C5 C6 N4 118.9(6) . . ? C7 C6 N4 119.5(6) . . ? C8 C7 C6 119.9(6) . . ? C7 C8 C3 118.9(6) . . ? N5 C10 N7 109.5(5) . . ? N6 C11 N7 110.8(5) . . ? C13 C12 C17 121.6(5) . . ? C13 C12 N7 119.0(5) . . ? C17 C12 N7 119.4(5) . . ? C12 C13 C14 118.9(5) . . ? C15 C14 C13 118.8(6) . . ? C16 C15 C14 122.9(5) . . ? C16 C15 N8 119.1(5) . . ? C14 C15 N8 117.9(5) . . ? C15 C16 C17 118.8(5) . . ? C12 C17 C16 119.0(5) . . ? N9 C19 N11 111.1(5) . . ? N10 C20 N11 109.9(5) . . ? C26 C21 C22 122.5(5) . . ? C26 C21 N11 118.8(5) . . ? C22 C21 N11 118.8(5) . . ? C23 C22 C21 118.3(5) . . ? C24 C23 C22 119.3(5) . . ? C25 C24 C23 122.5(5) . . ? C25 C24 N12 118.6(5) . . ? C23 C24 N12 118.9(5) . . ? C24 C25 C26 118.7(5) . . ? C21 C26 C25 118.7(5) . . ? O7 C28 C29 112.4(5) . . ? O8 C30 C31 111.9(5) . . ? C37 C32 C33 119.2(5) . . ? C37 C32 S1 119.6(4) . . ? C33 C32 S1 121.2(4) . . ? C34 C33 C32 120.4(6) . . ? C33 C34 C35 120.9(5) . . ? C36 C35 C34 117.9(5) . . ? C36 C35 C38 119.7(6) . . ? C34 C35 C38 122.3(6) . . ? C37 C36 C35 121.1(6) . . ? C32 C37 C36 120.4(5) . . ? C44 C39 C40 120.1(5) . . ? C44 C39 S2 120.8(5) . . ? C40 C39 S2 118.9(4) . . ? C41 C40 C39 119.4(5) . . ? C42 C41 C40 120.9(6) . . ? C43 C42 C41 117.9(5) . . ? C43 C42 C45 122.2(6) . . ? C41 C42 C45 119.9(6) . . ? C42 C43 C44 121.8(6) . . ? C39 C44 C43 119.9(6) . . ? C51 C46 C47 120.1(6) . . ? C51 C46 S3 121.2(5) . . ? C47 C46 S3 118.7(5) . . ? C48 C47 C46 119.1(6) . . ? C49 C48 C47 122.1(6) . . ? C50 C49 C48 117.4(6) . . ? C50 C49 C52 120.7(6) . . ? C48 C49 C52 121.9(6) . . ? C49 C50 C51 121.1(6) . . ? C46 C51 C50 120.2(6) . . ? O19 C53 C54 109.5(6) . . ? C56 C55 O20 110.5(6) . . ? 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 O7 Co2 N1 C1 42.1(4) . . . . ? O9 Co2 N1 C1 76(6) . . . . ? N6 Co2 N1 C1 -139.4(4) . . . . ? N9 Co2 N1 C1 130.3(4) . . . . ? O8 Co2 N1 C1 -50.1(4) . . . . ? O7 Co2 N1 N2 -132.4(4) . . . . ? O9 Co2 N1 N2 -98(6) . . . . ? N6 Co2 N1 N2 46.0(4) . . . . ? N9 Co2 N1 N2 -44.3(4) . . . . ? O8 Co2 N1 N2 135.3(4) . . . . ? C1 N1 N2 C2 0.5(5) . . . . ? Co2 N1 N2 C2 176.0(3) . . . . ? C1 N1 N2 Co1 -179.9(3) . . . . ? Co2 N1 N2 Co1 -4.4(5) . . . . ? N2 Co1 N2 C2 -25(12) 2_676 . . . ? N5 Co1 N2 C2 138.0(4) . . . . ? N5 Co1 N2 C2 -42.0(4) 2_676 . . . ? N10 Co1 N2 C2 47.8(4) 2_676 . . . ? N10 Co1 N2 C2 -132.2(4) . . . . ? N2 Co1 N2 N1 155(12) 2_676 . . . ? N5 Co1 N2 N1 -41.5(4) . . . . ? N5 Co1 N2 N1 138.5(4) 2_676 . . . ? N10 Co1 N2 N1 -131.7(4) 2_676 . . . ? N10 Co1 N2 N1 48.3(4) . . . . ? N2 Co1 N5 C10 -133.6(4) . . . . ? N2 Co1 N5 C10 46.4(4) 2_676 . . . ? N5 Co1 N5 C10 -173(19) 2_676 . . . ? N10 Co1 N5 C10 -42.3(4) 2_676 . . . ? N10 Co1 N5 C10 137.7(4) . . . . ? N2 Co1 N5 N6 48.6(4) . . . . ? N2 Co1 N5 N6 -131.4(4) 2_676 . . . ? N5 Co1 N5 N6 9(19) 2_676 . . . ? N10 Co1 N5 N6 139.9(4) 2_676 . . . ? N10 Co1 N5 N6 -40.1(4) . . . . ? C10 N5 N6 C11 -1.0(5) . . . . ? Co1 N5 N6 C11 177.2(3) . . . . ? C10 N5 N6 Co2 174.5(3) . . . . ? Co1 N5 N6 Co2 -7.4(5) . . . . ? O7 Co2 N6 C11 -137(6) . . . . ? O9 Co2 N6 C11 -45.7(4) . . . . ? N1 Co2 N6 C11 135.2(4) . . . . ? N9 Co2 N6 C11 -136.3(4) . . . . ? O8 Co2 N6 C11 47.3(4) . . . . ? O7 Co2 N6 N5 49(6) . . . . ? O9 Co2 N6 N5 139.9(4) . . . . ? N1 Co2 N6 N5 -39.2(4) . . . . ? N9 Co2 N6 N5 49.3(4) . . . . ? O8 Co2 N6 N5 -127.2(4) . . . . ? O7 Co2 N9 C19 -45.7(5) . . . . ? O9 Co2 N9 C19 43.7(5) . . . . ? N6 Co2 N9 C19 134.4(5) . . . . ? N1 Co2 N9 C19 -135.1(5) . . . . ? O8 Co2 N9 C19 -142(2) . . . . ? O7 Co2 N9 N10 138.3(4) . . . . ? O9 Co2 N9 N10 -132.3(4) . . . . ? N6 Co2 N9 N10 -41.7(4) . . . . ? N1 Co2 N9 N10 48.9(4) . . . . ? O8 Co2 N9 N10 42(3) . . . . ? C19 N9 N10 C20 0.9(6) . . . . ? Co2 N9 N10 C20 177.6(3) . . . . ? C19 N9 N10 Co1 177.9(3) . . . . ? Co2 N9 N10 Co1 -5.4(6) . . . . ? N2 Co1 N10 C20 133.0(4) . . . . ? N2 Co1 N10 C20 -47.0(4) 2_676 . . . ? N5 Co1 N10 C20 -136.7(4) . . . . ? N5 Co1 N10 C20 43.3(4) 2_676 . . . ? N10 Co1 N10 C20 -93(100) 2_676 . . . ? N2 Co1 N10 N9 -43.3(4) . . . . ? N2 Co1 N10 N9 136.7(4) 2_676 . . . ? N5 Co1 N10 N9 47.0(4) . . . . ? N5 Co1 N10 N9 -133.0(4) 2_676 . . . ? N10 Co1 N10 N9 91(100) 2_676 . . . ? O9 Co2 O7 C28 64.9(4) . . . . ? N6 Co2 O7 C28 156(6) . . . . ? N1 Co2 O7 C28 -116.0(4) . . . . ? N9 Co2 O7 C28 155.5(4) . . . . ? O8 Co2 O7 C28 -28.1(4) . . . . ? O7 Co2 O8 C30 71.9(5) . . . . ? O9 Co2 O8 C30 -17.5(5) . . . . ? N6 Co2 O8 C30 -108.2(5) . . . . ? N1 Co2 O8 C30 161.2(5) . . . . ? N9 Co2 O8 C30 168(2) . . . . ? N2 N1 C1 N3 -0.8(5) . . . . ? Co2 N1 C1 N3 -176.2(3) . . . . ? C2 N3 C1 N1 0.7(6) . . . . ? C3 N3 C1 N1 -177.2(5) . . . . ? N1 N2 C2 N3 -0.1(5) . . . . ? Co1 N2 C2 N3 -179.6(3) . . . . ? C1 N3 C2 N2 -0.4(6) . . . . ? C3 N3 C2 N2 177.5(5) . . . . ? C1 N3 C3 C4 -144.8(6) . . . . ? C2 N3 C3 C4 37.6(8) . . . . ? C1 N3 C3 C8 34.9(8) . . . . ? C2 N3 C3 C8 -142.6(5) . . . . ? C8 C3 C4 C5 0.3(9) . . . . ? N3 C3 C4 C5 -179.9(5) . . . . ? C3 C4 C5 C6 -2.0(9) . . . . ? C4 C5 C6 C7 0.6(9) . . . . ? C4 C5 C6 N4 -178.9(5) . . . . ? O2 N4 C6 C5 -11.0(9) . . . . ? O1 N4 C6 C5 168.6(6) . . . . ? O2 N4 C6 C7 169.5(6) . . . . ? O1 N4 C6 C7 -10.9(9) . . . . ? C5 C6 C7 C8 2.5(10) . . . . ? N4 C6 C7 C8 -178.0(6) . . . . ? C6 C7 C8 C3 -4.1(9) . . . . ? C4 C3 C8 C7 2.7(9) . . . . ? N3 C3 C8 C7 -177.0(5) . . . . ? N6 N5 C10 N7 0.0(6) . . . . ? Co1 N5 C10 N7 -178.1(3) . . . . ? C11 N7 C10 N5 0.9(6) . . . . ? C12 N7 C10 N5 -179.1(5) . . . . ? N5 N6 C11 N7 1.6(6) . . . . ? Co2 N6 C11 N7 -173.7(3) . . . . ? C10 N7 C11 N6 -1.6(6) . . . . ? C12 N7 C11 N6 178.5(5) . . . . ? C11 N7 C12 C13 -41.0(8) . . . . ? C10 N7 C12 C13 139.1(6) . . . . ? C11 N7 C12 C17 142.0(6) . . . . ? C10 N7 C12 C17 -37.9(8) . . . . ? C17 C12 C13 C14 -0.9(9) . . . . ? N7 C12 C13 C14 -177.8(5) . . . . ? C12 C13 C14 C15 0.5(9) . . . . ? C13 C14 C15 C16 -0.5(9) . . . . ? C13 C14 C15 N8 178.7(5) . . . . ? O3 N8 C15 C16 -9.3(8) . . . . ? O4 N8 C15 C16 168.1(6) . . . . ? O3 N8 C15 C14 171.5(6) . . . . ? O4 N8 C15 C14 -11.1(8) . . . . ? C14 C15 C16 C17 0.8(9) . . . . ? N8 C15 C16 C17 -178.3(5) . . . . ? C13 C12 C17 C16 1.2(9) . . . . ? N7 C12 C17 C16 178.1(5) . . . . ? C15 C16 C17 C12 -1.1(9) . . . . ? N10 N9 C19 N11 -0.3(6) . . . . ? Co2 N9 C19 N11 -176.8(3) . . . . ? C20 N11 C19 N9 -0.5(6) . . . . ? C21 N11 C19 N9 -177.3(5) . . . . ? N9 N10 C20 N11 -1.2(6) . . . . ? Co1 N10 C20 N11 -178.1(3) . . . . ? C19 N11 C20 N10 1.0(6) . . . . ? C21 N11 C20 N10 177.9(5) . . . . ? C19 N11 C21 C26 -145.6(5) . . . . ? C20 N11 C21 C26 38.2(8) . . . . ? C19 N11 C21 C22 34.1(8) . . . . ? C20 N11 C21 C22 -142.1(6) . . . . ? C26 C21 C22 C23 1.7(9) . . . . ? N11 C21 C22 C23 -178.0(5) . . . . ? C21 C22 C23 C24 -2.2(9) . . . . ? C22 C23 C24 C25 0.7(9) . . . . ? C22 C23 C24 N12 -178.4(5) . . . . ? O6 N12 C24 C25 -3.9(8) . . . . ? O5 N12 C24 C25 176.2(6) . . . . ? O6 N12 C24 C23 175.3(6) . . . . ? O5 N12 C24 C23 -4.6(8) . . . . ? C23 C24 C25 C26 1.4(9) . . . . ? N12 C24 C25 C26 -179.5(5) . . . . ? C22 C21 C26 C25 0.4(8) . . . . ? N11 C21 C26 C25 -179.9(5) . . . . ? C24 C25 C26 C21 -1.9(8) . . . . ? Co2 O7 C28 C29 88.0(6) . . . . ? Co2 O8 C30 C31 110.7(6) . . . . ? O12 S1 C32 C37 -153.0(5) . . . . ? O10 S1 C32 C37 -32.5(5) . . . . ? O11 S1 C32 C37 86.5(5) . . . . ? O12 S1 C32 C33 27.6(6) . . . . ? O10 S1 C32 C33 148.1(5) . . . . ? O11 S1 C32 C33 -92.9(5) . . . . ? C37 C32 C33 C34 0.9(9) . . . . ? S1 C32 C33 C34 -179.7(5) . . . . ? C32 C33 C34 C35 -1.3(9) . . . . ? C33 C34 C35 C36 0.7(9) . . . . ? C33 C34 C35 C38 179.9(6) . . . . ? C34 C35 C36 C37 0.4(9) . . . . ? C38 C35 C36 C37 -178.9(6) . . . . ? C33 C32 C37 C36 0.1(9) . . . . ? S1 C32 C37 C36 -179.3(5) . . . . ? C35 C36 C37 C32 -0.8(9) . . . . ? O15 S2 C39 C44 38.4(6) . . . . ? O14 S2 C39 C44 -81.2(5) . . . . ? O13 S2 C39 C44 159.3(5) . . . . ? O15 S2 C39 C40 -145.8(5) . . . . ? O14 S2 C39 C40 94.5(5) . . . . ? O13 S2 C39 C40 -24.9(5) . . . . ? C44 C39 C40 C41 0.7(9) . . . . ? S2 C39 C40 C41 -175.0(4) . . . . ? C39 C40 C41 C42 0.1(9) . . . . ? C40 C41 C42 C43 -0.4(9) . . . . ? C40 C41 C42 C45 178.4(6) . . . . ? C41 C42 C43 C44 -0.1(10) . . . . ? C45 C42 C43 C44 -178.8(6) . . . . ? C40 C39 C44 C43 -1.3(9) . . . . ? S2 C39 C44 C43 174.4(5) . . . . ? C42 C43 C44 C39 0.9(10) . . . . ? O16 S3 C46 C51 -133.1(5) . . . . ? O18 S3 C46 C51 -12.5(6) . . . . ? O17 S3 C46 C51 107.6(6) . . . . ? O16 S3 C46 C47 50.1(6) . . . . ? O18 S3 C46 C47 170.7(5) . . . . ? O17 S3 C46 C47 -69.3(6) . . . . ? C51 C46 C47 C48 -1.4(10) . . . . ? S3 C46 C47 C48 175.4(5) . . . . ? C46 C47 C48 C49 2.2(10) . . . . ? C47 C48 C49 C50 -1.5(11) . . . . ? C47 C48 C49 C52 178.7(7) . . . . ? C48 C49 C50 C51 0.1(11) . . . . ? C52 C49 C50 C51 179.9(6) . . . . ? C47 C46 C51 C50 0.1(10) . . . . ? S3 C46 C51 C50 -176.7(5) . . . . ? C49 C50 C51 C46 0.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.657 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.089 # Attachment '4435_web_deposit_cif_file_3_MuraleeMURUGESU_1298934407.cif' data_ds2508 _database_code_depnum_ccdc_archive 'CCDC 815196' #TrackingRef '4435_web_deposit_cif_file_3_MuraleeMURUGESU_1298934407.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H114 Co3 N24 O40 S6' _chemical_formula_weight 2637.28 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5049(16) _cell_length_b 14.7832(18) _cell_length_c 17.414(2) _cell_angle_alpha 65.672(2) _cell_angle_beta 69.922(2) _cell_angle_gamma 83.052(2) _cell_volume 2974.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5777 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 24.71 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1367 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9414 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 16150 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.1498 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 21.97 _reflns_number_total 7232 _reflns_number_gt 3854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+1.1610P] 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 7232 _refine_ls_number_parameters 766 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1494 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.82857(8) 0.31134(9) 0.49784(7) 0.0305(4) Uani 1 1 d . . . Co2 Co 1.0000 0.5000 0.5000 0.0277(4) Uani 1 2 d S . . S1 S 0.81750(19) 0.7104(2) 0.68450(17) 0.0452(7) Uani 1 1 d . . . S2 S 0.3147(2) 0.3670(2) 0.67163(17) 0.0522(7) Uani 1 1 d . . . S3 S 0.19945(19) 0.8057(2) 1.19852(16) 0.0458(7) Uani 1 1 d . . . N1 N 0.7736(5) 0.3990(5) 0.5738(4) 0.0300(17) Uani 1 1 d . . . N2 N 0.8390(5) 0.4615(5) 0.5766(4) 0.0264(17) Uani 1 1 d . . . N3 N 0.6819(5) 0.4581(5) 0.6722(4) 0.0297(17) Uani 1 1 d . . . N4 N 0.3463(7) 0.5480(6) 0.9263(6) 0.057(2) Uani 1 1 d . . . N5 N 0.9134(5) 0.4324(5) 0.3886(4) 0.0271(17) Uani 1 1 d . . . N6 N 0.9699(5) 0.5080(5) 0.3841(5) 0.0279(17) Uani 1 1 d . . . N7 N 0.9747(5) 0.5375(5) 0.2482(5) 0.0288(17) Uani 1 1 d . . . N8 N 1.0701(7) 0.6857(6) -0.1216(5) 0.051(2) Uani 1 1 d . . . N9 N 0.9600(5) 0.2761(5) 0.5440(4) 0.0308(17) Uani 1 1 d . . . N10 N 1.0288(5) 0.3450(5) 0.5343(4) 0.0339(18) Uani 1 1 d . . . N11 N 1.0926(5) 0.1964(5) 0.5837(4) 0.0337(18) Uani 1 1 d . . . N12 N 1.3712(8) -0.1128(11) 0.6954(10) 0.120(5) Uani 1 1 d . . . O1 O 0.2576(5) 0.5298(5) 0.9322(5) 0.073(2) Uani 1 1 d . . . O2 O 0.3646(5) 0.5814(6) 0.9735(5) 0.073(2) Uani 1 1 d . . . O3 O 1.0135(6) 0.6628(6) -0.1518(4) 0.078(2) Uani 1 1 d . . . O4 O 1.1493(7) 0.7340(6) -0.1686(5) 0.098(3) Uani 1 1 d . . . O5 O 1.3551(11) -0.1618(11) 0.7641(8) 0.197(5) Uani 1 1 d . . . O6 O 1.4539(11) -0.1004(9) 0.6355(7) 0.197(5) Uani 1 1 d . . . O7 O 0.8952(4) 0.2249(4) 0.4233(4) 0.0494(17) Uani 1 1 d . . . H7B H 0.9703 0.2194 0.4093 0.074 Uiso 1 1 d R . . O8 O 0.7401(5) 0.1917(4) 0.6030(4) 0.0491(17) Uani 1 1 d . . . H8B H 0.7345 0.1910 0.6597 0.074 Uiso 1 1 d R . . O9 O 0.7065(4) 0.3498(4) 0.4435(4) 0.0461(17) Uani 1 1 d . . . H9B H 0.7152 0.3167 0.4044 0.069 Uiso 1 1 d R . . H9C H 0.6403 0.3293 0.4907 0.069 Uiso 1 1 d R . . O10 O 0.8948(5) 0.7916(5) 0.6440(4) 0.074(2) Uani 1 1 d . . . O11 O 0.8641(4) 0.6137(4) 0.7179(4) 0.0480(17) Uani 1 1 d . . . O12 O 0.7568(5) 0.7165(5) 0.6284(4) 0.0564(18) Uani 1 1 d . . . O13 O 0.2996(5) 0.4627(5) 0.6790(4) 0.0568(18) Uani 1 1 d . . . O14 O 0.4224(4) 0.3358(5) 0.6590(4) 0.0538(18) Uani 1 1 d . . . O15 O 0.2722(5) 0.3633(5) 0.6081(4) 0.078(2) Uani 1 1 d . . . O16 O 0.0899(5) 0.8304(5) 1.2236(4) 0.075(2) Uani 1 1 d . . . O17 O 0.2589(6) 0.8280(5) 1.2435(4) 0.076(2) Uani 1 1 d . . . O18 O 0.2131(5) 0.7053(5) 1.2037(4) 0.0613(19) Uani 1 1 d . . . O19 O 0.5113(5) 0.2745(6) 0.5168(5) 0.088(3) Uani 1 1 d . . . H19A H 0.4654 0.2662 0.5654 0.133 Uiso 1 1 calc R . . O20 O 0.9007(7) 0.9641(6) 0.6650(7) 0.116(3) Uani 1 1 d . . . H20B H 0.8919 1.0242 0.6389 0.175 Uiso 1 1 calc R . . C1 C 0.6811(6) 0.3971(6) 0.6321(5) 0.035(2) Uani 1 1 d . . . H1A H 0.6225 0.3589 0.6444 0.042 Uiso 1 1 calc R . . C2 C 0.7797(6) 0.4948(6) 0.6366(5) 0.031(2) Uani 1 1 d . . . H2A H 0.8039 0.5395 0.6524 0.037 Uiso 1 1 calc R . . C3 C 0.5962(6) 0.4793(6) 0.7389(6) 0.036(2) Uani 1 1 d . . . C4 C 0.4956(7) 0.4751(7) 0.7394(6) 0.053(3) Uani 1 1 d . . . H4A H 0.4829 0.4573 0.6976 0.064 Uiso 1 1 calc R . . C5 C 0.4127(7) 0.4972(7) 0.8016(6) 0.056(3) Uani 1 1 d . . . H5A H 0.3426 0.4940 0.8038 0.068 Uiso 1 1 calc R . . C6 C 0.4365(7) 0.5241(7) 0.8604(6) 0.043(2) Uani 1 1 d . . . C7 C 0.5352(7) 0.5277(6) 0.8612(5) 0.041(2) Uani 1 1 d . . . H7A H 0.5478 0.5454 0.9031 0.050 Uiso 1 1 calc R . . C8 C 0.6179(6) 0.5048(6) 0.7989(5) 0.038(2) Uani 1 1 d . . . H8A H 0.6877 0.5066 0.7977 0.046 Uiso 1 1 calc R . . C9 C 0.9193(6) 0.4518(6) 0.3069(6) 0.031(2) Uani 1 1 d . . . H9A H 0.8888 0.4114 0.2907 0.038 Uiso 1 1 calc R . . C10 C 1.0059(6) 0.5685(6) 0.3003(6) 0.029(2) Uani 1 1 d . . . H10A H 1.0477 0.6258 0.2788 0.035 Uiso 1 1 calc R . . C11 C 0.9983(7) 0.5780(6) 0.1544(6) 0.034(2) Uani 1 1 d . . . C12 C 1.0940(6) 0.6275(6) 0.0994(6) 0.036(2) Uani 1 1 d . . . H12A H 1.1432 0.6350 0.1237 0.043 Uiso 1 1 calc R . . C13 C 1.1157(7) 0.6657(6) 0.0078(6) 0.040(2) Uani 1 1 d . . . H13A H 1.1786 0.7019 -0.0313 0.048 Uiso 1 1 calc R . . C14 C 1.0427(7) 0.6494(6) -0.0241(6) 0.033(2) Uani 1 1 d . . . C15 C 0.9496(7) 0.6031(6) 0.0281(6) 0.037(2) Uani 1 1 d . . . H15A H 0.9013 0.5948 0.0033 0.044 Uiso 1 1 calc R . . C16 C 0.9260(7) 0.5680(6) 0.1189(6) 0.036(2) Uani 1 1 d . . . H16A H 0.8601 0.5370 0.1568 0.043 Uiso 1 1 calc R . . C17 C 1.0009(7) 0.1903(7) 0.5730(5) 0.036(2) Uani 1 1 d . . . H17A H 0.9696 0.1304 0.5852 0.043 Uiso 1 1 calc R . . C18 C 1.1076(6) 0.2950(7) 0.5582(5) 0.033(2) Uani 1 1 d . . . H18A H 1.1665 0.3235 0.5577 0.040 Uiso 1 1 calc R . . C19 C 1.1650(7) 0.1189(7) 0.6103(6) 0.035(2) Uani 1 1 d . . . C20 C 1.1374(7) 0.0474(7) 0.6915(7) 0.049(3) Uani 1 1 d . . . H20A H 1.0705 0.0474 0.7325 0.059 Uiso 1 1 calc R . . C21 C 1.2078(9) -0.0284(7) 0.7164(7) 0.058(3) Uani 1 1 d . . . H21A H 1.1889 -0.0806 0.7731 0.069 Uiso 1 1 calc R . . C22 C 1.3010(9) -0.0233(10) 0.6571(9) 0.076(4) Uani 1 1 d . . . C23 C 1.3336(11) 0.0496(13) 0.5750(9) 0.178(10) Uani 1 1 d . . . H23A H 1.4027 0.0535 0.5359 0.213 Uiso 1 1 calc R . . C24 C 1.2585(10) 0.1188(11) 0.5518(8) 0.142(7) Uani 1 1 d . . . H24A H 1.2745 0.1667 0.4930 0.170 Uiso 1 1 calc R . . C25 C 0.8508(8) 0.1730(8) 0.3903(7) 0.069(3) Uani 1 1 d . . . H25A H 0.9061 0.1405 0.3587 0.103 Uiso 1 1 calc R . . H25B H 0.8157 0.2193 0.3499 0.103 Uiso 1 1 calc R . . H25C H 0.8000 0.1236 0.4395 0.103 Uiso 1 1 calc R . . C26 C 0.6825(10) 0.1061(10) 0.6126(8) 0.126(6) Uani 1 1 d . . . H26A H 0.6493 0.0660 0.6753 0.189 Uiso 1 1 calc R . . H26B H 0.7317 0.0662 0.5850 0.189 Uiso 1 1 calc R . . H26C H 0.6290 0.1303 0.5838 0.189 Uiso 1 1 calc R . . C27 C 0.7267(6) 0.7244(6) 0.7792(6) 0.036(2) Uani 1 1 d . . . C28 C 0.6339(7) 0.7727(7) 0.7762(6) 0.051(3) Uani 1 1 d . . . H28A H 0.6189 0.8002 0.7222 0.061 Uiso 1 1 calc R . . C29 C 0.5612(7) 0.7817(7) 0.8523(7) 0.056(3) Uani 1 1 d . . . H29A H 0.4976 0.8145 0.8492 0.068 Uiso 1 1 calc R . . C30 C 0.5821(7) 0.7430(7) 0.9313(7) 0.042(2) Uani 1 1 d . . . C31 C 0.6758(7) 0.6948(6) 0.9344(6) 0.044(2) Uani 1 1 d . . . H31A H 0.6910 0.6678 0.9883 0.052 Uiso 1 1 calc R . . C32 C 0.7475(7) 0.6860(7) 0.8591(7) 0.045(3) Uani 1 1 d . . . H32A H 0.8112 0.6535 0.8622 0.054 Uiso 1 1 calc R . . C33 C 0.5023(8) 0.7515(7) 1.0141(6) 0.068(3) Uani 1 1 d . . . H33A H 0.5296 0.7207 1.0636 0.102 Uiso 1 1 calc R . . H33B H 0.4367 0.7183 1.0283 0.102 Uiso 1 1 calc R . . H33C H 0.4896 0.8211 1.0032 0.102 Uiso 1 1 calc R . . C34 C 0.2412(7) 0.2811(6) 0.7775(6) 0.042(2) Uani 1 1 d . . . C35 C 0.1517(7) 0.2353(7) 0.7890(7) 0.047(3) Uani 1 1 d . . . H35A H 0.1324 0.2455 0.7391 0.056 Uiso 1 1 calc R . . C36 C 0.0892(8) 0.1741(7) 0.8734(8) 0.055(3) Uani 1 1 d . . . H36A H 0.0274 0.1442 0.8801 0.066 Uiso 1 1 calc R . . C37 C 0.1171(8) 0.1568(7) 0.9481(7) 0.050(3) Uani 1 1 d . . . C38 C 0.2069(8) 0.2021(8) 0.9367(7) 0.055(3) Uani 1 1 d . . . H38A H 0.2262 0.1918 0.9867 0.065 Uiso 1 1 calc R . . C39 C 0.2696(8) 0.2629(8) 0.8526(7) 0.056(3) Uani 1 1 d . . . H39A H 0.3317 0.2923 0.8459 0.067 Uiso 1 1 calc R . . C40 C 0.0478(8) 0.0918(7) 1.0399(7) 0.070(3) Uani 1 1 d . . . H40A H 0.0788 0.0878 1.0838 0.106 Uiso 1 1 calc R . . H40B H 0.0415 0.0259 1.0425 0.106 Uiso 1 1 calc R . . H40C H -0.0216 0.1202 1.0522 0.106 Uiso 1 1 calc R . . C41 C 0.2590(7) 0.8843(6) 1.0850(6) 0.036(2) Uani 1 1 d . . . C42 C 0.3317(7) 0.9556(7) 1.0603(7) 0.044(3) Uani 1 1 d . . . H42A H 0.3495 0.9662 1.1036 0.053 Uiso 1 1 calc R . . C43 C 0.3793(8) 1.0126(7) 0.9704(8) 0.057(3) Uani 1 1 d . . . H43A H 0.4291 1.0622 0.9535 0.069 Uiso 1 1 calc R . . C44 C 0.3557(9) 0.9983(8) 0.9056(7) 0.057(3) Uani 1 1 d . . . C45 C 0.2824(9) 0.9272(8) 0.9324(7) 0.062(3) Uani 1 1 d . . . H45A H 0.2659 0.9150 0.8892 0.074 Uiso 1 1 calc R . . C46 C 0.2323(7) 0.8732(7) 1.0199(7) 0.053(3) Uani 1 1 d . . . H46A H 0.1785 0.8275 1.0363 0.063 Uiso 1 1 calc R . . C47 C 0.4128(9) 1.0603(8) 0.8078(7) 0.083(4) Uani 1 1 d . . . H47A H 0.3872 1.0410 0.7709 0.124 Uiso 1 1 calc R . . H47B H 0.4879 1.0493 0.7947 0.124 Uiso 1 1 calc R . . H47C H 0.3994 1.1301 0.7954 0.124 Uiso 1 1 calc R . . C48 C 0.8615(11) 0.9375(9) 0.7577(8) 0.101(5) Uani 1 1 d . . . H48A H 0.8990 0.8806 0.7867 0.151 Uiso 1 1 calc R . . H48B H 0.7869 0.9207 0.7796 0.151 Uiso 1 1 calc R . . H48C H 0.8716 0.9928 0.7707 0.151 Uiso 1 1 calc R . . C49 C 0.4684(11) 0.3131(15) 0.4529(10) 0.176(9) Uani 1 1 d . . . H49A H 0.3937 0.2963 0.4776 0.263 Uiso 1 1 calc R . . H49B H 0.5019 0.2867 0.4078 0.263 Uiso 1 1 calc R . . H49C H 0.4782 0.3847 0.4263 0.263 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 0.0244(7) 0.0409(8) 0.0308(7) -0.0201(6) -0.0056(6) -0.0037(6) Co2 0.0205(9) 0.0383(11) 0.0284(10) -0.0196(9) -0.0037(8) -0.0026(8) S1 0.0388(15) 0.0504(18) 0.0486(17) -0.0324(14) 0.0010(13) -0.0051(14) S2 0.0408(16) 0.073(2) 0.0555(19) -0.0305(16) -0.0228(14) -0.0032(15) S3 0.0436(16) 0.0587(19) 0.0369(16) -0.0208(14) -0.0092(13) -0.0093(14) N1 0.028(4) 0.041(5) 0.025(4) -0.019(4) -0.004(4) -0.004(4) N2 0.022(4) 0.039(5) 0.025(4) -0.022(4) -0.003(3) -0.005(3) N3 0.022(4) 0.039(5) 0.035(5) -0.025(4) -0.003(4) -0.005(4) N4 0.036(6) 0.079(7) 0.060(6) -0.045(5) 0.000(5) 0.002(5) N5 0.021(4) 0.038(5) 0.029(5) -0.021(4) -0.006(3) 0.000(3) N6 0.020(4) 0.035(5) 0.032(5) -0.016(4) -0.004(3) -0.010(3) N7 0.022(4) 0.041(5) 0.033(5) -0.024(4) -0.008(4) -0.003(4) N8 0.061(6) 0.056(6) 0.026(6) -0.011(5) -0.009(5) 0.004(5) N9 0.031(4) 0.034(5) 0.036(5) -0.019(4) -0.017(4) 0.007(4) N10 0.025(4) 0.050(5) 0.033(4) -0.022(4) -0.005(4) -0.014(4) N11 0.032(5) 0.030(5) 0.038(5) -0.015(4) -0.009(4) 0.003(4) N12 0.034(6) 0.210(16) 0.178(14) -0.151(13) -0.031(9) 0.050(8) O1 0.024(4) 0.108(6) 0.096(6) -0.074(5) 0.012(4) -0.009(4) O2 0.056(5) 0.114(7) 0.077(6) -0.077(5) -0.008(4) 0.006(4) O3 0.089(6) 0.112(7) 0.042(5) -0.027(5) -0.027(4) -0.022(5) O4 0.090(6) 0.141(8) 0.029(5) 0.004(5) -0.004(4) -0.062(6) O5 0.193(9) 0.223(9) 0.112(7) -0.021(6) -0.078(7) 0.142(8) O6 0.193(9) 0.223(9) 0.112(7) -0.021(6) -0.078(7) 0.142(8) O7 0.043(4) 0.070(5) 0.058(4) -0.050(4) -0.011(3) -0.004(3) O8 0.059(4) 0.060(4) 0.028(4) -0.015(3) -0.009(3) -0.026(4) O9 0.029(3) 0.076(5) 0.043(4) -0.037(4) -0.003(3) -0.009(3) O10 0.059(5) 0.070(5) 0.082(5) -0.053(4) 0.026(4) -0.028(4) O11 0.042(4) 0.058(4) 0.058(4) -0.038(4) -0.016(3) 0.010(3) O12 0.065(5) 0.073(5) 0.041(4) -0.033(4) -0.017(4) 0.009(4) O13 0.053(4) 0.053(5) 0.066(5) -0.020(4) -0.028(4) 0.004(4) O14 0.039(4) 0.076(5) 0.061(5) -0.040(4) -0.019(3) 0.003(3) O15 0.067(5) 0.124(7) 0.056(5) -0.031(5) -0.031(4) -0.034(5) O16 0.048(5) 0.108(6) 0.056(5) -0.036(4) 0.002(4) 0.010(4) O17 0.103(6) 0.092(6) 0.041(4) -0.013(4) -0.034(4) -0.041(5) O18 0.071(5) 0.044(4) 0.056(5) -0.010(4) -0.014(4) -0.010(4) O19 0.049(5) 0.131(7) 0.081(6) -0.050(6) -0.003(4) -0.007(5) O20 0.130(8) 0.062(6) 0.134(9) -0.040(6) -0.011(7) -0.008(5) C1 0.022(5) 0.052(6) 0.040(6) -0.025(5) -0.008(5) -0.008(4) C2 0.026(5) 0.032(6) 0.043(6) -0.022(5) -0.008(5) -0.007(4) C3 0.028(5) 0.049(6) 0.040(6) -0.036(5) 0.000(5) 0.000(4) C4 0.035(6) 0.091(8) 0.058(7) -0.050(6) -0.021(5) 0.011(6) C5 0.028(6) 0.085(8) 0.072(8) -0.057(7) -0.008(5) 0.014(5) C6 0.027(6) 0.063(7) 0.047(6) -0.042(6) 0.005(5) -0.006(5) C7 0.032(6) 0.064(7) 0.034(6) -0.034(5) 0.001(5) -0.003(5) C8 0.023(5) 0.058(7) 0.038(6) -0.031(5) 0.002(5) -0.009(5) C9 0.027(5) 0.034(6) 0.043(7) -0.023(5) -0.015(5) 0.007(4) C10 0.017(5) 0.033(6) 0.038(6) -0.020(5) -0.003(5) -0.004(4) C11 0.034(6) 0.046(6) 0.031(6) -0.023(5) -0.012(5) 0.003(5) C12 0.027(5) 0.044(6) 0.038(6) -0.016(5) -0.010(5) -0.007(5) C13 0.036(6) 0.051(6) 0.031(6) -0.020(5) -0.003(5) 0.002(5) C14 0.030(5) 0.038(6) 0.026(6) -0.017(5) -0.003(5) 0.009(5) C15 0.038(6) 0.053(6) 0.021(6) -0.019(5) -0.011(5) 0.009(5) C16 0.031(5) 0.045(6) 0.036(6) -0.020(5) -0.009(5) -0.003(4) C17 0.031(6) 0.045(7) 0.026(6) -0.013(5) -0.001(4) -0.013(5) C18 0.022(5) 0.050(7) 0.035(6) -0.019(5) -0.014(4) 0.001(5) C19 0.035(6) 0.046(7) 0.028(6) -0.019(5) -0.013(5) 0.010(5) C20 0.033(6) 0.052(7) 0.053(8) -0.014(6) -0.006(5) -0.013(5) C21 0.064(8) 0.047(7) 0.064(8) -0.006(6) -0.044(7) 0.003(6) C22 0.053(8) 0.109(11) 0.070(9) -0.049(9) -0.026(7) 0.053(8) C23 0.101(12) 0.25(2) 0.034(9) 0.024(11) 0.014(8) 0.104(13) C24 0.065(9) 0.187(16) 0.061(9) 0.021(9) 0.000(8) 0.077(10) C25 0.069(8) 0.076(8) 0.074(8) -0.048(7) -0.010(6) -0.014(6) C26 0.111(11) 0.161(14) 0.081(10) -0.012(10) -0.018(8) -0.080(11) C27 0.026(5) 0.045(6) 0.046(7) -0.025(5) -0.015(5) 0.004(5) C28 0.050(7) 0.068(8) 0.039(7) -0.026(6) -0.015(5) 0.006(6) C29 0.044(6) 0.067(8) 0.055(8) -0.026(6) -0.020(6) 0.027(6) C30 0.041(6) 0.038(6) 0.050(7) -0.026(5) -0.008(5) 0.000(5) C31 0.051(7) 0.043(6) 0.043(7) -0.024(5) -0.015(5) 0.005(5) C32 0.026(5) 0.064(7) 0.056(7) -0.036(6) -0.012(5) 0.007(5) C33 0.058(7) 0.072(8) 0.065(8) -0.045(6) 0.006(6) 0.016(6) C34 0.033(6) 0.043(6) 0.055(7) -0.025(5) -0.016(5) 0.006(5) C35 0.046(6) 0.053(7) 0.051(7) -0.031(6) -0.015(6) 0.006(6) C36 0.042(6) 0.054(7) 0.074(9) -0.031(7) -0.017(6) 0.000(5) C37 0.064(8) 0.037(7) 0.060(8) -0.031(6) -0.025(7) 0.014(6) C38 0.065(8) 0.059(7) 0.052(8) -0.029(6) -0.030(7) 0.017(6) C39 0.042(6) 0.076(8) 0.061(8) -0.033(7) -0.021(6) -0.005(6) C40 0.084(8) 0.050(7) 0.057(8) -0.012(6) -0.007(6) -0.006(6) C41 0.039(6) 0.036(6) 0.038(6) -0.019(5) -0.015(5) 0.006(5) C42 0.041(6) 0.043(6) 0.053(7) -0.027(6) -0.009(5) -0.003(5) C43 0.051(7) 0.052(7) 0.056(8) -0.011(7) -0.013(6) -0.005(6) C44 0.065(8) 0.057(8) 0.036(7) -0.013(6) -0.010(6) 0.014(6) C45 0.086(9) 0.070(8) 0.030(7) -0.023(6) -0.017(6) -0.001(7) C46 0.053(7) 0.070(8) 0.045(7) -0.028(6) -0.019(6) -0.008(6) C47 0.094(9) 0.063(8) 0.054(8) -0.008(7) 0.002(7) -0.004(7) C48 0.145(13) 0.087(10) 0.081(10) -0.052(9) -0.021(10) -0.012(9) C49 0.086(11) 0.34(3) 0.099(13) -0.083(15) -0.047(10) 0.065(14) _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 O8 2.062(6) . ? Co1 O9 2.083(5) . ? Co1 N5 2.080(7) . ? Co1 O7 2.101(6) . ? Co1 N9 2.116(6) . ? Co1 N1 2.118(6) . ? Co2 N2 2.125(6) . ? Co2 N2 2.125(6) 2_766 ? Co2 N10 2.138(7) . ? Co2 N10 2.138(7) 2_766 ? Co2 N6 2.147(6) . ? Co2 N6 2.147(6) 2_766 ? S1 O12 1.447(6) . ? S1 O11 1.458(6) . ? S1 O10 1.459(6) . ? S1 C27 1.760(9) . ? S2 O15 1.432(6) . ? S2 O14 1.443(6) . ? S2 O13 1.456(6) . ? S2 C34 1.765(9) . ? S3 O16 1.439(6) . ? S3 O18 1.441(6) . ? S3 O17 1.441(6) . ? S3 C41 1.774(9) . ? N1 C1 1.306(9) . ? N1 N2 1.379(8) . ? N2 C2 1.315(9) . ? N3 C2 1.326(9) . ? N3 C1 1.352(9) . ? N3 C3 1.440(9) . ? N4 O2 1.219(9) . ? N4 O1 1.220(9) . ? N4 C6 1.482(11) . ? N5 C9 1.306(9) . ? N5 N6 1.389(8) . ? N6 C10 1.308(9) . ? N7 C9 1.360(9) . ? N7 C10 1.365(9) . ? N7 C11 1.417(10) . ? N8 O4 1.194(9) . ? N8 O3 1.207(9) . ? N8 C14 1.474(11) . ? N9 C17 1.288(10) . ? N9 N10 1.382(8) . ? N10 C18 1.309(9) . ? N11 C17 1.333(10) . ? N11 C18 1.356(10) . ? N11 C19 1.445(10) . ? N12 O5 1.073(15) . ? N12 O6 1.209(14) . ? N12 C22 1.580(16) . ? O7 C25 1.411(9) . ? O8 C26 1.484(12) . ? O19 C49 1.317(13) . ? O20 C48 1.408(12) . ? C3 C4 1.365(11) . ? C3 C8 1.371(10) . ? C4 C5 1.380(11) . ? C5 C6 1.379(11) . ? C6 C7 1.347(11) . ? C7 C8 1.385(10) . ? C11 C16 1.372(10) . ? C11 C12 1.387(11) . ? C12 C13 1.389(11) . ? C13 C14 1.373(11) . ? C14 C15 1.337(11) . ? C15 C16 1.374(10) . ? C19 C24 1.323(13) . ? C19 C20 1.326(11) . ? C20 C21 1.403(12) . ? C21 C22 1.313(13) . ? C22 C23 1.346(16) . ? C23 C24 1.388(15) . ? C27 C28 1.372(11) . ? C27 C32 1.385(11) . ? C28 C29 1.399(12) . ? C29 C30 1.371(11) . ? C30 C31 1.382(11) . ? C30 C33 1.519(12) . ? C31 C32 1.384(11) . ? C34 C35 1.369(11) . ? C34 C39 1.402(12) . ? C35 C36 1.388(12) . ? C36 C37 1.393(12) . ? C37 C38 1.372(13) . ? C37 C40 1.509(13) . ? C38 C39 1.384(12) . ? C41 C42 1.359(11) . ? C41 C46 1.375(11) . ? C42 C43 1.388(12) . ? C43 C44 1.371(13) . ? C44 C45 1.354(13) . ? C44 C47 1.523(13) . ? C45 C46 1.356(12) . ? 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 O8 Co1 O9 90.3(2) . . ? O8 Co1 N5 177.4(2) . . ? O9 Co1 N5 87.2(2) . . ? O8 Co1 O7 91.6(2) . . ? O9 Co1 O7 90.4(2) . . ? N5 Co1 O7 87.7(2) . . ? O8 Co1 N9 93.0(2) . . ? O9 Co1 N9 176.0(2) . . ? N5 Co1 N9 89.4(3) . . ? O7 Co1 N9 87.4(2) . . ? O8 Co1 N1 90.1(2) . . ? O9 Co1 N1 93.9(2) . . ? N5 Co1 N1 90.8(3) . . ? O7 Co1 N1 175.4(2) . . ? N9 Co1 N1 88.2(2) . . ? N2 Co2 N2 180.000(2) . 2_766 ? N2 Co2 N10 87.9(2) . . ? N2 Co2 N10 92.1(2) 2_766 . ? N2 Co2 N10 92.1(2) . 2_766 ? N2 Co2 N10 87.9(2) 2_766 2_766 ? N10 Co2 N10 180.000(1) . 2_766 ? N2 Co2 N6 90.2(2) . . ? N2 Co2 N6 89.8(2) 2_766 . ? N10 Co2 N6 89.2(2) . . ? N10 Co2 N6 90.8(2) 2_766 . ? N2 Co2 N6 89.8(2) . 2_766 ? N2 Co2 N6 90.2(2) 2_766 2_766 ? N10 Co2 N6 90.8(2) . 2_766 ? N10 Co2 N6 89.2(2) 2_766 2_766 ? N6 Co2 N6 180.000(1) . 2_766 ? O12 S1 O11 113.6(4) . . ? O12 S1 O10 113.1(4) . . ? O11 S1 O10 112.0(4) . . ? O12 S1 C27 105.8(4) . . ? O11 S1 C27 105.6(4) . . ? O10 S1 C27 105.9(4) . . ? O15 S2 O14 113.9(4) . . ? O15 S2 O13 112.4(4) . . ? O14 S2 O13 112.1(4) . . ? O15 S2 C34 107.3(4) . . ? O14 S2 C34 105.3(4) . . ? O13 S2 C34 105.0(4) . . ? O16 S3 O18 111.9(4) . . ? O16 S3 O17 114.1(5) . . ? O18 S3 O17 112.7(4) . . ? O16 S3 C41 107.4(4) . . ? O18 S3 C41 106.4(4) . . ? O17 S3 C41 103.5(4) . . ? C1 N1 N2 107.8(6) . . ? C1 N1 Co1 129.0(6) . . ? N2 N1 Co1 122.8(5) . . ? C2 N2 N1 105.2(6) . . ? C2 N2 Co2 126.4(5) . . ? N1 N2 Co2 128.4(5) . . ? C2 N3 C1 104.8(6) . . ? C2 N3 C3 127.1(7) . . ? C1 N3 C3 128.2(7) . . ? O2 N4 O1 123.7(8) . . ? O2 N4 C6 118.5(8) . . ? O1 N4 C6 117.8(8) . . ? C9 N5 N6 106.3(6) . . ? C9 N5 Co1 123.1(6) . . ? N6 N5 Co1 130.6(5) . . ? C10 N6 N5 107.3(6) . . ? C10 N6 Co2 131.7(5) . . ? N5 N6 Co2 120.5(5) . . ? C9 N7 C10 103.7(7) . . ? C9 N7 C11 126.0(7) . . ? C10 N7 C11 130.1(7) . . ? O4 N8 O3 121.7(8) . . ? O4 N8 C14 119.3(9) . . ? O3 N8 C14 118.9(9) . . ? C17 N9 N10 106.6(7) . . ? C17 N9 Co1 127.8(6) . . ? N10 N9 Co1 124.8(5) . . ? C18 N10 N9 106.4(7) . . ? C18 N10 Co2 128.1(6) . . ? N9 N10 Co2 125.3(5) . . ? C17 N11 C18 104.1(7) . . ? C17 N11 C19 129.4(8) . . ? C18 N11 C19 126.4(7) . . ? O5 N12 O6 127.4(16) . . ? O5 N12 C22 125.8(13) . . ? O6 N12 C22 105.1(14) . . ? C25 O7 Co1 132.4(6) . . ? C26 O8 Co1 135.7(6) . . ? N1 C1 N3 110.1(7) . . ? N2 C2 N3 112.2(7) . . ? C4 C3 C8 121.9(8) . . ? C4 C3 N3 118.7(8) . . ? C8 C3 N3 119.4(7) . . ? C3 C4 C5 119.6(8) . . ? C6 C5 C4 117.5(8) . . ? C7 C6 C5 123.5(8) . . ? C7 C6 N4 119.9(8) . . ? C5 C6 N4 116.6(8) . . ? C6 C7 C8 118.5(8) . . ? C3 C8 C7 118.9(8) . . ? N5 C9 N7 111.8(7) . . ? N6 C10 N7 110.9(7) . . ? C16 C11 C12 120.6(8) . . ? C16 C11 N7 119.6(8) . . ? C12 C11 N7 119.8(7) . . ? C11 C12 C13 118.8(8) . . ? C14 C13 C12 118.1(8) . . ? C15 C14 C13 123.6(8) . . ? C15 C14 N8 119.2(9) . . ? C13 C14 N8 117.2(8) . . ? C14 C15 C16 118.5(8) . . ? C11 C16 C15 120.3(8) . . ? N9 C17 N11 112.3(8) . . ? N10 C18 N11 110.6(7) . . ? C24 C19 C20 120.3(10) . . ? C24 C19 N11 119.1(9) . . ? C20 C19 N11 120.6(8) . . ? C19 C20 C21 120.2(9) . . ? C22 C21 C20 117.2(10) . . ? C21 C22 C23 124.5(11) . . ? C21 C22 N12 111.1(11) . . ? C23 C22 N12 124.3(11) . . ? C22 C23 C24 115.7(11) . . ? C19 C24 C23 121.6(11) . . ? C28 C27 C32 118.4(8) . . ? C28 C27 S1 121.3(7) . . ? C32 C27 S1 120.3(7) . . ? C27 C28 C29 120.9(9) . . ? C30 C29 C28 120.4(9) . . ? C29 C30 C31 118.9(8) . . ? C29 C30 C33 120.2(9) . . ? C31 C30 C33 120.8(9) . . ? C30 C31 C32 120.6(9) . . ? C27 C32 C31 120.8(9) . . ? C35 C34 C39 118.5(9) . . ? C35 C34 S2 121.0(8) . . ? C39 C34 S2 120.4(7) . . ? C34 C35 C36 121.0(9) . . ? C37 C36 C35 120.5(9) . . ? C38 C37 C36 118.7(10) . . ? C38 C37 C40 120.9(10) . . ? C36 C37 C40 120.4(10) . . ? C37 C38 C39 120.9(10) . . ? C34 C39 C38 120.5(9) . . ? C42 C41 C46 118.6(9) . . ? C42 C41 S3 121.4(7) . . ? C46 C41 S3 119.9(7) . . ? C41 C42 C43 119.3(9) . . ? C44 C43 C42 121.8(10) . . ? C45 C44 C43 117.5(10) . . ? C45 C44 C47 122.6(11) . . ? C43 C44 C47 119.9(11) . . ? C44 C45 C46 121.6(10) . . ? C45 C46 C41 121.1(9) . . ? 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 O8 Co1 N1 C1 -35.0(7) . . . . ? O9 Co1 N1 C1 55.3(7) . . . . ? N5 Co1 N1 C1 142.6(7) . . . . ? O7 Co1 N1 C1 -146(3) . . . . ? N9 Co1 N1 C1 -128.0(7) . . . . ? O8 Co1 N1 N2 136.2(6) . . . . ? O9 Co1 N1 N2 -133.5(5) . . . . ? N5 Co1 N1 N2 -46.2(6) . . . . ? O7 Co1 N1 N2 25(3) . . . . ? N9 Co1 N1 N2 43.2(6) . . . . ? C1 N1 N2 C2 -1.0(8) . . . . ? Co1 N1 N2 C2 -173.8(5) . . . . ? C1 N1 N2 Co2 -179.9(5) . . . . ? Co1 N1 N2 Co2 7.3(8) . . . . ? N2 Co2 N2 C2 -105(100) 2_766 . . . ? N10 Co2 N2 C2 132.2(7) . . . . ? N10 Co2 N2 C2 -47.8(7) 2_766 . . . ? N6 Co2 N2 C2 -138.6(7) . . . . ? N6 Co2 N2 C2 41.4(7) 2_766 . . . ? N2 Co2 N2 N1 73(100) 2_766 . . . ? N10 Co2 N2 N1 -49.1(6) . . . . ? N10 Co2 N2 N1 130.9(6) 2_766 . . . ? N6 Co2 N2 N1 40.1(6) . . . . ? N6 Co2 N2 N1 -139.9(6) 2_766 . . . ? O8 Co1 N5 C9 -28(6) . . . . ? O9 Co1 N5 C9 -45.7(6) . . . . ? O7 Co1 N5 C9 44.8(6) . . . . ? N9 Co1 N5 C9 132.2(6) . . . . ? N1 Co1 N5 C9 -139.6(6) . . . . ? O8 Co1 N5 N6 150(5) . . . . ? O9 Co1 N5 N6 131.9(6) . . . . ? O7 Co1 N5 N6 -137.6(6) . . . . ? N9 Co1 N5 N6 -50.2(6) . . . . ? N1 Co1 N5 N6 38.0(6) . . . . ? C9 N5 N6 C10 0.3(8) . . . . ? Co1 N5 N6 C10 -177.7(5) . . . . ? C9 N5 N6 Co2 -172.4(5) . . . . ? Co1 N5 N6 Co2 9.7(8) . . . . ? N2 Co2 N6 C10 141.8(7) . . . . ? N2 Co2 N6 C10 -38.2(7) 2_766 . . . ? N10 Co2 N6 C10 -130.3(7) . . . . ? N10 Co2 N6 C10 49.7(7) 2_766 . . . ? N6 Co2 N6 C10 103(100) 2_766 . . . ? N2 Co2 N6 N5 -47.7(5) . . . . ? N2 Co2 N6 N5 132.3(5) 2_766 . . . ? N10 Co2 N6 N5 40.2(5) . . . . ? N10 Co2 N6 N5 -139.8(5) 2_766 . . . ? N6 Co2 N6 N5 -86(100) 2_766 . . . ? O8 Co1 N9 C17 45.4(7) . . . . ? O9 Co1 N9 C17 -102(4) . . . . ? N5 Co1 N9 C17 -133.7(7) . . . . ? O7 Co1 N9 C17 -46.0(7) . . . . ? N1 Co1 N9 C17 135.4(7) . . . . ? O8 Co1 N9 N10 -146.1(6) . . . . ? O9 Co1 N9 N10 67(4) . . . . ? N5 Co1 N9 N10 34.8(6) . . . . ? O7 Co1 N9 N10 122.5(6) . . . . ? N1 Co1 N9 N10 -56.0(6) . . . . ? C17 N9 N10 C18 0.3(8) . . . . ? Co1 N9 N10 C18 -170.2(5) . . . . ? C17 N9 N10 Co2 -174.0(5) . . . . ? Co1 N9 N10 Co2 15.4(8) . . . . ? N2 Co2 N10 C18 -137.3(7) . . . . ? N2 Co2 N10 C18 42.7(7) 2_766 . . . ? N10 Co2 N10 C18 -147(100) 2_766 . . . ? N6 Co2 N10 C18 132.4(7) . . . . ? N6 Co2 N10 C18 -47.6(7) 2_766 . . . ? N2 Co2 N10 N9 35.8(6) . . . . ? N2 Co2 N10 N9 -144.2(6) 2_766 . . . ? N10 Co2 N10 N9 26(100) 2_766 . . . ? N6 Co2 N10 N9 -54.5(6) . . . . ? N6 Co2 N10 N9 125.5(6) 2_766 . . . ? O8 Co1 O7 C25 61.8(8) . . . . ? O9 Co1 O7 C25 -28.6(8) . . . . ? N5 Co1 O7 C25 -115.7(8) . . . . ? N9 Co1 O7 C25 154.7(8) . . . . ? N1 Co1 O7 C25 173(3) . . . . ? O9 Co1 O8 C26 52.9(10) . . . . ? N5 Co1 O8 C26 35(6) . . . . ? O7 Co1 O8 C26 -37.5(10) . . . . ? N9 Co1 O8 C26 -125.0(10) . . . . ? N1 Co1 O8 C26 146.8(10) . . . . ? N2 N1 C1 N3 1.5(9) . . . . ? Co1 N1 C1 N3 173.7(5) . . . . ? C2 N3 C1 N1 -1.4(9) . . . . ? C3 N3 C1 N1 178.7(8) . . . . ? N1 N2 C2 N3 0.1(9) . . . . ? Co2 N2 C2 N3 179.0(5) . . . . ? C1 N3 C2 N2 0.7(9) . . . . ? C3 N3 C2 N2 -179.3(7) . . . . ? C2 N3 C3 C4 150.2(9) . . . . ? C1 N3 C3 C4 -29.9(13) . . . . ? C2 N3 C3 C8 -28.7(13) . . . . ? C1 N3 C3 C8 151.3(9) . . . . ? C8 C3 C4 C5 0.2(15) . . . . ? N3 C3 C4 C5 -178.6(8) . . . . ? C3 C4 C5 C6 0.8(15) . . . . ? C4 C5 C6 C7 -1.4(15) . . . . ? C4 C5 C6 N4 179.7(9) . . . . ? O2 N4 C6 C7 8.3(14) . . . . ? O1 N4 C6 C7 -169.4(9) . . . . ? O2 N4 C6 C5 -172.9(9) . . . . ? O1 N4 C6 C5 9.5(13) . . . . ? C5 C6 C7 C8 1.0(15) . . . . ? N4 C6 C7 C8 179.8(8) . . . . ? C4 C3 C8 C7 -0.6(14) . . . . ? N3 C3 C8 C7 178.2(8) . . . . ? C6 C7 C8 C3 0.0(13) . . . . ? N6 N5 C9 N7 -1.3(8) . . . . ? Co1 N5 C9 N7 176.8(5) . . . . ? C10 N7 C9 N5 1.8(8) . . . . ? C11 N7 C9 N5 177.9(7) . . . . ? N5 N6 C10 N7 0.9(8) . . . . ? Co2 N6 C10 N7 172.4(5) . . . . ? C9 N7 C10 N6 -1.6(8) . . . . ? C11 N7 C10 N6 -177.5(7) . . . . ? C9 N7 C11 C16 35.5(11) . . . . ? C10 N7 C11 C16 -149.4(8) . . . . ? C9 N7 C11 C12 -144.6(8) . . . . ? C10 N7 C11 C12 30.5(12) . . . . ? C16 C11 C12 C13 -0.7(12) . . . . ? N7 C11 C12 C13 179.5(7) . . . . ? C11 C12 C13 C14 -2.4(12) . . . . ? C12 C13 C14 C15 3.6(13) . . . . ? C12 C13 C14 N8 -176.6(7) . . . . ? O4 N8 C14 C15 174.0(9) . . . . ? O3 N8 C14 C15 -8.6(12) . . . . ? O4 N8 C14 C13 -5.9(12) . . . . ? O3 N8 C14 C13 171.6(9) . . . . ? C13 C14 C15 C16 -1.4(13) . . . . ? N8 C14 C15 C16 178.8(7) . . . . ? C12 C11 C16 C15 2.9(13) . . . . ? N7 C11 C16 C15 -177.2(7) . . . . ? C14 C15 C16 C11 -1.9(12) . . . . ? N10 N9 C17 N11 0.0(9) . . . . ? Co1 N9 C17 N11 170.2(5) . . . . ? C18 N11 C17 N9 -0.3(9) . . . . ? C19 N11 C17 N9 -176.6(7) . . . . ? N9 N10 C18 N11 -0.6(9) . . . . ? Co2 N10 C18 N11 173.6(5) . . . . ? C17 N11 C18 N10 0.6(9) . . . . ? C19 N11 C18 N10 177.0(7) . . . . ? C17 N11 C19 C24 112.3(13) . . . . ? C18 N11 C19 C24 -63.1(14) . . . . ? C17 N11 C19 C20 -66.0(12) . . . . ? C18 N11 C19 C20 118.6(10) . . . . ? C24 C19 C20 C21 0.8(16) . . . . ? N11 C19 C20 C21 179.1(8) . . . . ? C19 C20 C21 C22 1.7(15) . . . . ? C20 C21 C22 C23 1(2) . . . . ? C20 C21 C22 N12 179.3(8) . . . . ? O5 N12 C22 C21 -14(2) . . . . ? O6 N12 C22 C21 179.8(13) . . . . ? O5 N12 C22 C23 165(2) . . . . ? O6 N12 C22 C23 -1(2) . . . . ? C21 C22 C23 C24 -5(3) . . . . ? N12 C22 C23 C24 176.6(14) . . . . ? C20 C19 C24 C23 -5(2) . . . . ? N11 C19 C24 C23 176.3(15) . . . . ? C22 C23 C24 C19 7(3) . . . . ? O12 S1 C27 C28 -24.4(8) . . . . ? O11 S1 C27 C28 -145.1(7) . . . . ? O10 S1 C27 C28 95.9(8) . . . . ? O12 S1 C27 C32 155.3(7) . . . . ? O11 S1 C27 C32 34.6(8) . . . . ? O10 S1 C27 C32 -84.4(8) . . . . ? C32 C27 C28 C29 -1.0(14) . . . . ? S1 C27 C28 C29 178.7(7) . . . . ? C27 C28 C29 C30 0.6(15) . . . . ? C28 C29 C30 C31 -0.2(14) . . . . ? C28 C29 C30 C33 -179.1(9) . . . . ? C29 C30 C31 C32 0.1(13) . . . . ? C33 C30 C31 C32 179.1(8) . . . . ? C28 C27 C32 C31 1.0(13) . . . . ? S1 C27 C32 C31 -178.7(7) . . . . ? C30 C31 C32 C27 -0.5(13) . . . . ? O15 S2 C34 C35 -8.7(9) . . . . ? O14 S2 C34 C35 -130.4(7) . . . . ? O13 S2 C34 C35 111.1(8) . . . . ? O15 S2 C34 C39 175.4(7) . . . . ? O14 S2 C34 C39 53.7(8) . . . . ? O13 S2 C34 C39 -64.8(8) . . . . ? C39 C34 C35 C36 1.4(13) . . . . ? S2 C34 C35 C36 -174.6(7) . . . . ? C34 C35 C36 C37 -1.0(14) . . . . ? C35 C36 C37 C38 0.7(14) . . . . ? C35 C36 C37 C40 178.8(8) . . . . ? C36 C37 C38 C39 -0.9(14) . . . . ? C40 C37 C38 C39 -179.0(9) . . . . ? C35 C34 C39 C38 -1.6(14) . . . . ? S2 C34 C39 C38 174.4(7) . . . . ? C37 C38 C39 C34 1.4(15) . . . . ? O16 S3 C41 C42 112.3(8) . . . . ? O18 S3 C41 C42 -127.7(7) . . . . ? O17 S3 C41 C42 -8.8(8) . . . . ? O16 S3 C41 C46 -68.2(8) . . . . ? O18 S3 C41 C46 51.8(8) . . . . ? O17 S3 C41 C46 170.7(7) . . . . ? C46 C41 C42 C43 -2.2(13) . . . . ? S3 C41 C42 C43 177.4(7) . . . . ? C41 C42 C43 C44 -0.6(14) . . . . ? C42 C43 C44 C45 1.0(15) . . . . ? C42 C43 C44 C47 -177.9(9) . . . . ? C43 C44 C45 C46 1.4(16) . . . . ? C47 C44 C45 C46 -179.7(9) . . . . ? C44 C45 C46 C41 -4.3(16) . . . . ? C42 C41 C46 C45 4.6(14) . . . . ? S3 C41 C46 C45 -175.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.765 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.081 # Attachment '4436_web_deposit_cif_file_4_MuraleeMURUGESU_1298934407.cif' data_ds2720 _database_code_depnum_ccdc_archive 'CCDC 815197' #TrackingRef '4436_web_deposit_cif_file_4_MuraleeMURUGESU_1298934407.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96.32 H109.28 N24 Ni3 O39.32 S6' _chemical_formula_weight 2600.81 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' Ni Ni 0.3393 1.1124 '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 15.056(2) _cell_length_b 16.698(2) _cell_length_c 16.718(2) _cell_angle_alpha 103.588(2) _cell_angle_beta 109.528(2) _cell_angle_gamma 111.430(2) _cell_volume 3368.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7514 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1350 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7776 _exptl_absorpt_correction_T_max 0.8668 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 29317 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 23.26 _reflns_number_total 9465 _reflns_number_gt 6704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+9.4018P] 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 9465 _refine_ls_number_parameters 787 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2361 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.0000 0.5000 0.0249(3) Uani 1 2 d S . . Ni2 Ni 0.36661(6) 0.15004(5) 0.52427(6) 0.0296(3) Uani 1 1 d . A . N1 N 0.4449(4) 0.0234(3) 0.5990(3) 0.0277(11) Uani 1 1 d . . . N2 N 0.4001(4) 0.0822(3) 0.6099(4) 0.0301(12) Uani 1 1 d . . . N3 N 0.4074(4) 0.0250(3) 0.7143(4) 0.0321(12) Uani 1 1 d . . . N4 N 0.3361(6) -0.0631(6) 1.0003(5) 0.0617(19) Uani 1 1 d . . . N5 N 0.5692(4) 0.1444(3) 0.5292(3) 0.0278(11) Uani 1 1 d . . . N6 N 0.5188(4) 0.1986(3) 0.5376(4) 0.0322(12) Uani 1 1 d . . . N7 N 0.6838(4) 0.2892(3) 0.5686(4) 0.0293(12) Uani 1 1 d . . . N8 N 1.0719(5) 0.6092(4) 0.6754(5) 0.0543(17) Uani 1 1 d . . . N9 N 0.3564(4) -0.0229(3) 0.3959(4) 0.0294(12) Uani 1 1 d . . . N10 N 0.3087(4) 0.0324(3) 0.4076(4) 0.0296(12) Uani 1 1 d . . . N11 N 0.2122(4) -0.0773(4) 0.2663(4) 0.0311(12) Uani 1 1 d . . . N12 N -0.1287(6) -0.2956(5) -0.0969(5) 0.0600(18) Uani 1 1 d . . . C2 C 0.3789(5) 0.0822(4) 0.6787(5) 0.0340(15) Uani 1 1 d . . . H2A H 0.3480 0.1169 0.7010 0.041 Uiso 1 1 calc R . . C3 C 0.3916(5) 0.0029(4) 0.7880(5) 0.0346(15) Uani 1 1 d . . . C4 C 0.3337(6) -0.0894(5) 0.7716(5) 0.0469(18) Uani 1 1 d . . . H4A H 0.3063 -0.1380 0.7129 0.056 Uiso 1 1 calc R . . C5 C 0.3155(6) -0.1111(5) 0.8421(5) 0.0507(19) Uani 1 1 d . . . H5A H 0.2761 -0.1746 0.8328 0.061 Uiso 1 1 calc R . . C6 C 0.3554(6) -0.0393(5) 0.9242(5) 0.0432(17) Uani 1 1 d . . . C7 C 0.4134(7) 0.0544(5) 0.9436(5) 0.0522(19) Uani 1 1 d . . . H7A H 0.4403 0.1024 1.0026 0.063 Uiso 1 1 calc R . . C8 C 0.4308(6) 0.0758(5) 0.8720(5) 0.0489(19) Uani 1 1 d . . . H8A H 0.4690 0.1394 0.8810 0.059 Uiso 1 1 calc R . . C9 C 0.6670(5) 0.2005(4) 0.5481(4) 0.0289(14) Uani 1 1 d . . . H9A H 0.7191 0.1816 0.5474 0.035 Uiso 1 1 calc R . . C10 C 0.5890(5) 0.2850(4) 0.5613(4) 0.0303(14) Uani 1 1 d . . . H10A H 0.5762 0.3373 0.5719 0.036 Uiso 1 1 calc R . . C11 C 0.7807(5) 0.3715(4) 0.5940(4) 0.0293(14) Uani 1 1 d . . . C12 C 0.8435(5) 0.3639(4) 0.5513(5) 0.0349(15) Uani 1 1 d . . . H12A H 0.8209 0.3059 0.5038 0.042 Uiso 1 1 calc R . . C13 C 0.9392(5) 0.4419(5) 0.5791(5) 0.0392(16) Uani 1 1 d . . . H13A H 0.9852 0.4383 0.5526 0.047 Uiso 1 1 calc R . . C14 C 0.9670(5) 0.5248(5) 0.6454(5) 0.0386(16) Uani 1 1 d . . . C15 C 0.9046(6) 0.5343(5) 0.6863(5) 0.0437(17) Uani 1 1 d . . . H15A H 0.9259 0.5937 0.7308 0.052 Uiso 1 1 calc R . . C16 C 0.8090(5) 0.4551(4) 0.6617(5) 0.0387(16) Uani 1 1 d . . . H16A H 0.7649 0.4585 0.6904 0.046 Uiso 1 1 calc R . . C17 C 0.2967(5) -0.0879(4) 0.3106(4) 0.0320(14) Uani 1 1 d . . . H17A H 0.3114 -0.1355 0.2841 0.038 Uiso 1 1 calc R . . C18 C 0.2214(5) -0.0013(4) 0.3297(5) 0.0341(15) Uani 1 1 d . . . H18A H 0.1723 0.0227 0.3188 0.041 Uiso 1 1 calc R . . C19 C 0.1248(5) -0.1336(4) 0.1736(4) 0.0337(15) Uani 1 1 d . . . C20 C 0.1459(5) -0.1708(5) 0.1032(5) 0.0416(17) Uani 1 1 d . . . H20A H 0.2165 -0.1605 0.1160 0.050 Uiso 1 1 calc R . . C21 C 0.0624(6) -0.2228(5) 0.0145(5) 0.0475(18) Uani 1 1 d . . . H21A H 0.0745 -0.2492 -0.0351 0.057 Uiso 1 1 calc R . . C22 C -0.0386(6) -0.2363(5) -0.0018(5) 0.0436(17) Uani 1 1 d . . . C23 C -0.0589(6) -0.2010(6) 0.0675(5) 0.054(2) Uani 1 1 d . . . H23A H -0.1298 -0.2120 0.0542 0.065 Uiso 1 1 calc R . . C24 C 0.0238(5) -0.1487(5) 0.1578(5) 0.0443(18) Uani 1 1 d . . . H24A H 0.0106 -0.1242 0.2073 0.053 Uiso 1 1 calc R . . C25 C 0.1750(14) 0.1531(12) 0.5598(15) 0.057(4) Uani 0.50 1 d P A 1 H25A H 0.0991 0.1126 0.5413 0.086 Uiso 0.50 1 calc PR A 1 H25B H 0.1827 0.2076 0.5444 0.086 Uiso 0.50 1 calc PR A 1 H25C H 0.2180 0.1748 0.6269 0.086 Uiso 0.50 1 calc PR A 1 C26 C 0.318(2) 0.2973(17) 0.452(2) 0.088(7) Uani 0.50 1 d P B 1 H26A H 0.3060 0.3115 0.3968 0.132 Uiso 0.50 1 calc PR B 1 H26B H 0.3807 0.3519 0.5063 0.132 Uiso 0.50 1 calc PR B 1 H26C H 0.2540 0.2831 0.4618 0.132 Uiso 0.50 1 calc PR B 1 C25' C 0.1330(13) 0.1249(13) 0.4846(17) 0.059(5) Uani 0.50 1 d P A 2 H25D H 0.0702 0.0821 0.4875 0.089 Uiso 0.50 1 calc PR A 2 H25E H 0.1123 0.1202 0.4208 0.089 Uiso 0.50 1 calc PR A 2 H25F H 0.1596 0.1897 0.5264 0.089 Uiso 0.50 1 calc PR A 2 C26' C 0.2517(19) 0.2398(19) 0.3991(18) 0.088(7) Uani 0.50 1 d P B 2 H26D H 0.2679 0.2736 0.3608 0.133 Uiso 0.50 1 calc PR B 2 H26E H 0.2453 0.2788 0.4484 0.133 Uiso 0.50 1 calc PR B 2 H26F H 0.1836 0.1807 0.3602 0.133 Uiso 0.50 1 calc PR B 2 C27 C 0.4465(5) -0.0106(4) 0.6615(4) 0.0304(14) Uani 1 1 d . . . H27A H 0.4716 -0.0543 0.6691 0.036 Uiso 1 1 calc R . . C28 C 0.0016(5) 0.2488(5) 0.5508(5) 0.0376(16) Uani 1 1 d . . . C29 C 0.0034(6) 0.2575(5) 0.4708(5) 0.0432(17) Uani 1 1 d . . . H29A H -0.0542 0.2121 0.4115 0.052 Uiso 1 1 calc R . . C30 C 0.0898(6) 0.3332(5) 0.4781(6) 0.0468(18) Uani 1 1 d . . . H30A H 0.0917 0.3382 0.4232 0.056 Uiso 1 1 calc R . . C31 C 0.1725(6) 0.4008(5) 0.5631(6) 0.051(2) Uani 1 1 d . . . C32 C 0.1701(6) 0.3922(5) 0.6417(6) 0.054(2) Uani 1 1 d . . . H32A H 0.2264 0.4393 0.7009 0.065 Uiso 1 1 calc R . . C33 C 0.0857(6) 0.3149(5) 0.6360(6) 0.053(2) Uani 1 1 d . . . H33A H 0.0865 0.3081 0.6911 0.064 Uiso 1 1 calc R . . C34 C 0.2665(7) 0.4849(6) 0.5696(8) 0.073(3) Uani 1 1 d . . . H34A H 0.3180 0.5261 0.6350 0.110 Uiso 1 1 calc R . . H34B H 0.2389 0.5204 0.5393 0.110 Uiso 1 1 calc R . . H34C H 0.3027 0.4620 0.5385 0.110 Uiso 1 1 calc R . . C35 C 0.2327(7) 0.6177(5) 1.0748(5) 0.0522(19) Uani 1 1 d . . . C36 C 0.2071(6) 0.6335(6) 0.9952(6) 0.055(2) Uani 1 1 d . . . H36A H 0.2450 0.6946 0.9981 0.066 Uiso 1 1 calc R . . C37 C 0.1264(7) 0.5607(6) 0.9111(6) 0.063(2) Uani 1 1 d . . . H37A H 0.1103 0.5727 0.8567 0.075 Uiso 1 1 calc R . . C38 C 0.0684(7) 0.4709(5) 0.9036(5) 0.058(2) Uani 1 1 d . . . C39 C 0.0880(10) 0.4598(7) 0.9850(7) 0.103(4) Uani 1 1 d . . . H39A H 0.0433 0.4013 0.9833 0.123 Uiso 1 1 calc R . . C40 C 0.1709(10) 0.5312(7) 1.0705(7) 0.092(4) Uani 1 1 d . . . H40A H 0.1846 0.5200 1.1254 0.110 Uiso 1 1 calc R . . C41 C -0.0201(8) 0.3899(7) 0.8111(6) 0.079(3) Uani 1 1 d . . . H41A H -0.0501 0.3325 0.8211 0.118 Uiso 1 1 calc R . . H41B H 0.0101 0.3799 0.7684 0.118 Uiso 1 1 calc R . . H41C H -0.0771 0.4053 0.7844 0.118 Uiso 1 1 calc R . . C42 C 0.5058(6) 0.2583(5) 0.2264(5) 0.0498(19) Uani 1 1 d . . . C43 C 0.4241(8) 0.2645(8) 0.1663(8) 0.086(3) Uani 1 1 d . . . H43A H 0.3611 0.2527 0.1733 0.103 Uiso 1 1 calc R . . C44 C 0.4344(10) 0.2885(10) 0.0937(9) 0.103(4) Uani 1 1 d . . . H44A H 0.3743 0.2847 0.0465 0.123 Uiso 1 1 calc R . . C45 C 0.5290(9) 0.3172(9) 0.0900(8) 0.085(3) Uani 1 1 d . . . C46 C 0.5430(13) 0.3503(13) 0.0132(11) 0.138(6) Uani 1 1 d . . . H46A H 0.6159 0.3675 0.0210 0.207 Uiso 1 1 calc R . . H46B H 0.5317 0.4051 0.0184 0.207 Uiso 1 1 calc R . . H46C H 0.4901 0.2991 -0.0481 0.207 Uiso 1 1 calc R . . C47 C 0.6116(8) 0.3133(7) 0.1524(7) 0.071(3) Uani 1 1 d . . . H47A H 0.6770 0.3311 0.1485 0.085 Uiso 1 1 calc R . . C48 C 0.6021(6) 0.2843(6) 0.2205(6) 0.057(2) Uani 1 1 d . . . H48A H 0.6602 0.2818 0.2634 0.069 Uiso 1 1 calc R . . O1 O 0.2802(6) -0.1472(5) 0.9805(5) 0.087(2) Uani 1 1 d . . . O2 O 0.3783(6) 0.0002(5) 1.0766(5) 0.085(2) Uani 1 1 d . . . O3 O 1.1243(4) 0.6024(4) 0.6359(5) 0.0692(17) Uani 1 1 d . . . O4 O 1.0969(5) 0.6805(4) 0.7384(5) 0.090(2) Uani 1 1 d . . . O5 O -0.1151(6) -0.3377(6) -0.1543(5) 0.107(3) Uani 1 1 d . . . O6 O -0.2139(6) -0.2991(6) -0.1102(5) 0.112(3) Uani 1 1 d . . . O7 O 0.4203(4) 0.2697(3) 0.6385(3) 0.0471(12) Uani 1 1 d . . . H7B H 0.4426 0.2584 0.6937 0.071 Uiso 1 1 d R . . H7C H 0.3630 0.2845 0.6320 0.071 Uiso 1 1 d R . . O8 O 0.3350(4) 0.2201(3) 0.4388(4) 0.0479(12) Uani 1 1 d . . . H8B H 0.2813 0.1769 0.3880 0.072 Uiso 0.50 1 d PR B 1 H8C H 0.3350 0.1907 0.3899 0.072 Uiso 0.50 1 d PR B 2 O9 O 0.2122(4) 0.1007(3) 0.5111(3) 0.0447(12) Uani 1 1 d . . . H9B H 0.1998 0.0538 0.5258 0.067 Uiso 0.50 1 d PR A 1 H9C H 0.1801 0.0429 0.4747 0.067 Uiso 0.50 1 d PR A 2 S1 S -0.10797(14) 0.15127(12) 0.54133(15) 0.0492(5) Uani 1 1 d . . . S2 S 0.33911(17) 0.70790(15) 1.18228(14) 0.0577(6) Uani 1 1 d . . . S3 S 0.49219(18) 0.22144(17) 0.31456(16) 0.0590(6) Uani 1 1 d . . . O10 O -0.2004(4) 0.1290(4) 0.4586(4) 0.0643(15) Uani 1 1 d . . . O11 O -0.0791(5) 0.0763(4) 0.5341(6) 0.086(2) Uani 1 1 d . . . O12 O -0.1179(4) 0.1823(4) 0.6246(4) 0.0581(14) Uani 1 1 d . . . O13 O 0.4212(8) 0.6839(8) 1.2020(6) 0.187(7) Uani 1 1 d . . . O14 O 0.3670(5) 0.7957(4) 1.1731(5) 0.088(2) Uani 1 1 d . . . O15 O 0.2970(6) 0.7120(5) 1.2463(5) 0.101(2) Uani 1 1 d . . . O16 O 0.5838(5) 0.2133(4) 0.3616(4) 0.0705(17) Uani 1 1 d . . . O17 O 0.3980(6) 0.1258(6) 0.2658(6) 0.115(3) Uani 1 1 d . . . O18 O 0.4750(9) 0.2860(7) 0.3696(6) 0.123(3) Uani 1 1 d . . . O19 O 0.3918(17) 0.4548(16) 0.3446(15) 0.157(8) Uiso 0.50 1 d PD . . H19 H 0.4150 0.4696 0.3081 0.235 Uiso 0.50 1 calc PR . . C49 C 0.4762(14) 0.4497(13) 0.4199(12) 0.069(5) Uiso 0.50 1 d PD . . H49A H 0.5458 0.4810 0.4206 0.103 Uiso 0.50 1 calc PR . . H49B H 0.4559 0.3836 0.4079 0.103 Uiso 0.50 1 calc PR . . H49C H 0.4819 0.4811 0.4802 0.103 Uiso 0.50 1 calc PR . . O20 O 0.1914(9) 0.0777(8) 0.1550(7) 0.029(3) Uiso 0.33 1 d PD . . H20 H 0.1742 0.1196 0.1686 0.044 Uiso 0.33 1 calc PR . . C50 C 0.1630(15) 0.0443(12) 0.0576(10) 0.029(4) Uiso 0.33 1 d PD . . H50A H 0.1254 0.0748 0.0284 0.043 Uiso 0.33 1 calc PR . . H50B H 0.1157 -0.0241 0.0278 0.043 Uiso 0.33 1 calc PR . . H50C H 0.2285 0.0594 0.0505 0.043 Uiso 0.33 1 calc PR . . O21 O 0.0438(12) 0.0648(10) 0.2139(10) 0.045(3) Uiso 0.33 1 d PD . . H21 H 0.1068 0.0923 0.2577 0.068 Uiso 0.33 1 calc PR . . C51 C 0.002(2) 0.1344(19) 0.210(2) 0.077(8) Uiso 0.33 1 d PD . . H51A H 0.0615 0.1982 0.2529 0.116 Uiso 0.33 1 calc PR . . H51B H -0.0550 0.1192 0.2286 0.116 Uiso 0.33 1 calc PR . . H51C H -0.0260 0.1309 0.1468 0.116 Uiso 0.33 1 calc PR . . O22 O 0.576(3) 0.482(2) -0.115(2) 0.096(9) Uiso 0.25 1 d P . . H22A H 0.4922 0.4536 -0.1448 0.144 Uiso 0.25 1 d PR . . H22B H 0.6183 0.5116 -0.1439 0.144 Uiso 0.25 1 d PR . . O23 O 0.285(2) 0.1804(18) 0.7988(17) 0.071(6) Uiso 0.25 1 d P . . H23B H 0.2240 0.1177 0.7706 0.106 Uiso 0.25 1 d PR . . H23C H 0.2855 0.2274 0.8492 0.106 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0208(6) 0.0203(6) 0.0361(6) 0.0113(5) 0.0164(5) 0.0095(5) Ni2 0.0253(4) 0.0253(4) 0.0442(5) 0.0142(4) 0.0201(4) 0.0144(4) N1 0.024(3) 0.022(3) 0.038(3) 0.013(2) 0.018(2) 0.009(2) N2 0.028(3) 0.025(3) 0.043(3) 0.014(2) 0.022(3) 0.015(2) N3 0.029(3) 0.028(3) 0.039(3) 0.012(2) 0.020(2) 0.012(2) N4 0.066(5) 0.081(6) 0.069(5) 0.045(5) 0.048(4) 0.041(4) N5 0.026(3) 0.024(3) 0.036(3) 0.013(2) 0.016(2) 0.012(2) N6 0.030(3) 0.024(3) 0.046(3) 0.014(2) 0.019(3) 0.015(2) N7 0.024(3) 0.023(3) 0.040(3) 0.014(2) 0.018(2) 0.008(2) N8 0.041(4) 0.038(4) 0.061(4) 0.021(3) 0.016(3) 0.003(3) N9 0.023(3) 0.026(3) 0.037(3) 0.011(2) 0.015(2) 0.010(2) N10 0.026(3) 0.030(3) 0.042(3) 0.017(2) 0.019(3) 0.019(2) N11 0.025(3) 0.033(3) 0.038(3) 0.017(2) 0.016(2) 0.013(2) N12 0.050(4) 0.070(5) 0.043(4) 0.009(3) 0.011(3) 0.032(4) C2 0.033(4) 0.035(4) 0.043(4) 0.015(3) 0.024(3) 0.020(3) C3 0.038(4) 0.033(4) 0.041(4) 0.016(3) 0.027(3) 0.017(3) C4 0.053(5) 0.036(4) 0.044(4) 0.013(3) 0.026(4) 0.013(4) C5 0.050(5) 0.038(4) 0.058(5) 0.021(4) 0.032(4) 0.009(4) C6 0.046(4) 0.048(4) 0.047(4) 0.024(4) 0.032(4) 0.022(4) C7 0.066(5) 0.040(4) 0.049(4) 0.012(4) 0.036(4) 0.019(4) C8 0.055(5) 0.032(4) 0.052(5) 0.012(3) 0.033(4) 0.011(3) C9 0.026(3) 0.026(3) 0.037(4) 0.012(3) 0.017(3) 0.014(3) C10 0.024(3) 0.025(3) 0.043(4) 0.011(3) 0.016(3) 0.013(3) C11 0.021(3) 0.023(3) 0.036(4) 0.010(3) 0.012(3) 0.006(3) C12 0.033(4) 0.028(3) 0.041(4) 0.011(3) 0.019(3) 0.012(3) C13 0.026(4) 0.042(4) 0.051(4) 0.022(3) 0.021(3) 0.013(3) C14 0.025(3) 0.031(4) 0.041(4) 0.012(3) 0.010(3) 0.002(3) C15 0.044(4) 0.027(4) 0.048(4) 0.010(3) 0.024(4) 0.007(3) C16 0.035(4) 0.033(4) 0.042(4) 0.010(3) 0.020(3) 0.012(3) C17 0.027(3) 0.029(3) 0.041(4) 0.014(3) 0.017(3) 0.014(3) C18 0.028(4) 0.037(4) 0.042(4) 0.018(3) 0.018(3) 0.017(3) C19 0.031(4) 0.030(3) 0.038(4) 0.017(3) 0.015(3) 0.012(3) C20 0.033(4) 0.056(4) 0.040(4) 0.016(4) 0.020(3) 0.025(4) C21 0.047(5) 0.057(5) 0.040(4) 0.017(4) 0.020(4) 0.029(4) C22 0.042(4) 0.044(4) 0.037(4) 0.013(3) 0.012(3) 0.021(3) C23 0.038(4) 0.068(5) 0.055(5) 0.019(4) 0.021(4) 0.029(4) C24 0.026(4) 0.052(4) 0.039(4) 0.004(3) 0.013(3) 0.015(3) C25 0.045(10) 0.052(10) 0.073(12) 0.018(10) 0.030(10) 0.025(9) C26 0.103(19) 0.072(15) 0.14(2) 0.072(16) 0.074(18) 0.063(15) C25' 0.034(9) 0.059(11) 0.117(17) 0.057(12) 0.042(11) 0.035(9) C26' 0.072(16) 0.084(17) 0.099(18) 0.041(14) 0.025(13) 0.039(13) C27 0.026(3) 0.027(3) 0.042(4) 0.013(3) 0.018(3) 0.014(3) C28 0.031(4) 0.034(4) 0.056(5) 0.019(3) 0.025(4) 0.019(3) C29 0.035(4) 0.037(4) 0.057(5) 0.013(3) 0.021(4) 0.021(3) C30 0.050(5) 0.047(4) 0.062(5) 0.031(4) 0.034(4) 0.029(4) C31 0.042(4) 0.041(4) 0.089(6) 0.032(4) 0.039(5) 0.028(4) C32 0.032(4) 0.044(4) 0.071(6) 0.016(4) 0.018(4) 0.012(4) C33 0.043(5) 0.055(5) 0.065(5) 0.027(4) 0.029(4) 0.023(4) C34 0.056(5) 0.046(5) 0.130(9) 0.039(5) 0.059(6) 0.020(4) C35 0.066(5) 0.041(4) 0.043(4) 0.012(4) 0.028(4) 0.019(4) C36 0.055(5) 0.045(4) 0.055(5) 0.020(4) 0.024(4) 0.014(4) C37 0.070(6) 0.066(6) 0.048(5) 0.025(4) 0.025(5) 0.030(5) C38 0.074(6) 0.038(4) 0.046(5) 0.011(4) 0.020(4) 0.024(4) C39 0.129(10) 0.037(5) 0.065(7) 0.019(5) 0.007(6) 0.003(6) C40 0.137(10) 0.065(6) 0.051(6) 0.030(5) 0.031(6) 0.036(7) C41 0.091(7) 0.062(6) 0.044(5) 0.008(4) 0.006(5) 0.031(5) C42 0.050(5) 0.057(5) 0.054(5) 0.028(4) 0.027(4) 0.031(4) C43 0.071(6) 0.140(10) 0.109(8) 0.092(8) 0.063(6) 0.067(7) C44 0.100(9) 0.167(12) 0.108(9) 0.102(9) 0.061(7) 0.087(9) C45 0.092(8) 0.125(9) 0.107(8) 0.084(8) 0.074(7) 0.073(7) C46 0.155(13) 0.224(17) 0.172(14) 0.159(14) 0.126(12) 0.130(13) C47 0.072(6) 0.083(7) 0.101(7) 0.054(6) 0.066(6) 0.045(5) C48 0.047(5) 0.064(5) 0.065(5) 0.028(4) 0.030(4) 0.028(4) O1 0.106(5) 0.074(5) 0.092(5) 0.050(4) 0.069(4) 0.024(4) O2 0.123(6) 0.090(5) 0.056(4) 0.031(4) 0.062(4) 0.048(4) O3 0.038(3) 0.059(4) 0.099(5) 0.027(3) 0.041(3) 0.007(3) O4 0.070(4) 0.039(3) 0.093(5) -0.007(3) 0.037(4) -0.019(3) O5 0.075(5) 0.144(7) 0.053(4) -0.016(4) 0.014(4) 0.055(5) O6 0.057(4) 0.163(8) 0.062(4) -0.008(4) -0.003(3) 0.061(5) O7 0.046(3) 0.040(3) 0.059(3) 0.012(2) 0.024(2) 0.030(2) O8 0.053(3) 0.046(3) 0.068(3) 0.034(3) 0.036(3) 0.034(3) O9 0.036(3) 0.042(3) 0.070(3) 0.023(2) 0.031(3) 0.026(2) S1 0.0361(10) 0.0345(10) 0.0845(15) 0.0229(10) 0.0373(11) 0.0169(8) S2 0.0584(13) 0.0525(12) 0.0434(11) 0.0058(9) 0.0172(10) 0.0231(10) S3 0.0654(14) 0.0745(15) 0.0645(13) 0.0410(12) 0.0417(12) 0.0420(12) O10 0.037(3) 0.055(3) 0.069(4) 0.008(3) 0.020(3) 0.006(3) O11 0.060(4) 0.047(3) 0.180(7) 0.049(4) 0.079(5) 0.031(3) O12 0.046(3) 0.062(3) 0.070(4) 0.032(3) 0.036(3) 0.019(3) O13 0.149(8) 0.175(9) 0.103(6) -0.075(6) -0.055(6) 0.132(8) O14 0.066(4) 0.050(4) 0.097(5) 0.011(3) 0.019(4) 0.007(3) O15 0.109(6) 0.083(5) 0.063(4) -0.003(4) 0.047(4) 0.014(4) O16 0.097(5) 0.082(4) 0.073(4) 0.045(3) 0.047(4) 0.067(4) O17 0.086(5) 0.124(7) 0.099(6) 0.063(5) 0.035(5) 0.012(5) O18 0.239(10) 0.156(8) 0.136(7) 0.109(6) 0.147(8) 0.168(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N9 2.102(5) . ? Ni1 N9 2.102(5) 2_656 ? Ni1 N5 2.100(5) . ? Ni1 N5 2.100(5) 2_656 ? Ni1 N1 2.105(5) . ? Ni1 N1 2.105(5) 2_656 ? Ni2 N10 2.058(5) . ? Ni2 N6 2.044(5) . ? Ni2 N2 2.069(5) . ? Ni2 O9 2.075(4) . ? Ni2 O7 2.071(5) . ? Ni2 O8 2.091(5) . ? N1 C27 1.299(8) . ? N1 N2 1.390(6) . ? N2 C2 1.292(8) . ? N3 C27 1.355(8) . ? N3 C2 1.359(8) . ? N3 C3 1.434(8) . ? N4 O2 1.218(9) . ? N4 O1 1.234(9) . ? N4 C6 1.504(10) . ? N5 C9 1.299(8) . ? N5 N6 1.387(6) . ? N6 C10 1.301(8) . ? N7 C9 1.342(7) . ? N7 C10 1.366(7) . ? N7 C11 1.429(8) . ? N8 O3 1.204(8) . ? N8 O4 1.219(9) . ? N8 C14 1.498(9) . ? N9 C17 1.313(8) . ? N9 N10 1.378(6) . ? N10 C18 1.307(8) . ? N11 C17 1.341(8) . ? N11 C18 1.376(8) . ? N11 C19 1.437(8) . ? N12 O5 1.174(9) . ? N12 O6 1.203(9) . ? N12 C22 1.478(10) . ? C3 C4 1.367(9) . ? C3 C8 1.385(9) . ? C4 C5 1.393(10) . ? C5 C6 1.352(10) . ? C6 C7 1.375(10) . ? C7 C8 1.404(11) . ? C11 C12 1.385(9) . ? C11 C16 1.382(9) . ? C12 C13 1.373(9) . ? C13 C14 1.366(9) . ? C14 C15 1.365(10) . ? C15 C16 1.396(9) . ? C19 C24 1.366(9) . ? C19 C20 1.386(9) . ? C20 C21 1.372(10) . ? C21 C22 1.371(10) . ? C22 C23 1.354(10) . ? C23 C24 1.386(10) . ? C25 O9 1.438(16) . ? C26 O8 1.390(19) . ? C25' O9 1.366(14) . ? C26' O8 1.40(2) . ? C28 C33 1.373(11) . ? C28 C29 1.387(10) . ? C28 S1 1.772(7) . ? C29 C30 1.387(10) . ? C30 C31 1.372(11) . ? C31 C32 1.366(12) . ? C31 C34 1.537(11) . ? C32 C33 1.398(11) . ? C35 C40 1.371(13) . ? C35 C36 1.372(11) . ? C35 S2 1.763(8) . ? C36 C37 1.381(11) . ? C37 C38 1.381(12) . ? C38 C39 1.365(13) . ? C38 C41 1.522(11) . ? C39 C40 1.393(14) . ? C42 C43 1.359(12) . ? C42 C48 1.399(11) . ? C42 S3 1.769(8) . ? C43 C44 1.402(14) . ? C44 C45 1.356(14) . ? C45 C47 1.364(13) . ? C45 C46 1.558(15) . ? C47 C48 1.367(12) . ? S1 O12 1.444(6) . ? S1 O10 1.443(6) . ? S1 O11 1.460(6) . ? S2 O13 1.396(8) . ? S2 O15 1.416(7) . ? S2 O14 1.431(7) . ? S3 O16 1.414(6) . ? S3 O18 1.404(7) . ? S3 O17 1.478(8) . ? O19 C49 1.506(17) . ? O20 C50 1.441(15) . ? O21 C51 1.509(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N9 Ni1 N9 180.000(2) . 2_656 ? N9 Ni1 N5 89.83(19) . . ? N9 Ni1 N5 90.17(19) 2_656 . ? N9 Ni1 N5 90.17(19) . 2_656 ? N9 Ni1 N5 89.83(19) 2_656 2_656 ? N5 Ni1 N5 179.999(2) . 2_656 ? N9 Ni1 N1 90.23(19) . . ? N9 Ni1 N1 89.77(19) 2_656 . ? N5 Ni1 N1 89.40(18) . . ? N5 Ni1 N1 90.60(18) 2_656 . ? N9 Ni1 N1 89.77(19) . 2_656 ? N9 Ni1 N1 90.23(19) 2_656 2_656 ? N5 Ni1 N1 90.60(18) . 2_656 ? N5 Ni1 N1 89.40(18) 2_656 2_656 ? N1 Ni1 N1 180.000(1) . 2_656 ? N10 Ni2 N6 91.18(19) . . ? N10 Ni2 N2 91.60(19) . . ? N6 Ni2 N2 89.9(2) . . ? N10 Ni2 O9 88.88(19) . . ? N6 Ni2 O9 179.8(2) . . ? N2 Ni2 O9 89.93(19) . . ? N10 Ni2 O7 177.62(19) . . ? N6 Ni2 O7 90.11(19) . . ? N2 Ni2 O7 90.4(2) . . ? O9 Ni2 O7 89.84(18) . . ? N10 Ni2 O8 88.9(2) . . ? N6 Ni2 O8 89.5(2) . . ? N2 Ni2 O8 179.2(2) . . ? O9 Ni2 O8 90.71(19) . . ? O7 Ni2 O8 89.1(2) . . ? C27 N1 N2 106.6(5) . . ? C27 N1 Ni1 128.8(4) . . ? N2 N1 Ni1 124.7(4) . . ? C2 N2 N1 107.9(5) . . ? C2 N2 Ni2 127.2(4) . . ? N1 N2 Ni2 124.7(4) . . ? C27 N3 C2 105.4(5) . . ? C27 N3 C3 128.0(5) . . ? C2 N3 C3 126.5(5) . . ? O2 N4 O1 124.8(7) . . ? O2 N4 C6 118.7(7) . . ? O1 N4 C6 116.4(7) . . ? C9 N5 N6 107.4(5) . . ? C9 N5 Ni1 127.4(4) . . ? N6 N5 Ni1 125.1(4) . . ? C10 N6 N5 107.1(5) . . ? C10 N6 Ni2 127.6(4) . . ? N5 N6 Ni2 125.1(4) . . ? C9 N7 C10 105.6(5) . . ? C9 N7 C11 127.7(5) . . ? C10 N7 C11 126.7(5) . . ? O3 N8 O4 125.1(7) . . ? O3 N8 C14 118.5(7) . . ? O4 N8 C14 116.4(7) . . ? C17 N9 N10 107.5(5) . . ? C17 N9 Ni1 128.8(4) . . ? N10 N9 Ni1 123.7(4) . . ? C18 N10 N9 107.7(5) . . ? C18 N10 Ni2 125.8(4) . . ? N9 N10 Ni2 126.5(4) . . ? C17 N11 C18 105.9(5) . . ? C17 N11 C19 129.3(5) . . ? C18 N11 C19 124.7(5) . . ? O5 N12 O6 123.5(7) . . ? O5 N12 C22 119.6(7) . . ? O6 N12 C22 116.8(7) . . ? N2 C2 N3 109.7(5) . . ? C4 C3 C8 122.0(6) . . ? C4 C3 N3 118.9(6) . . ? C8 C3 N3 119.0(6) . . ? C3 C4 C5 119.1(7) . . ? C6 C5 C4 118.2(7) . . ? C5 C6 C7 124.7(7) . . ? C5 C6 N4 118.1(7) . . ? C7 C6 N4 117.2(7) . . ? C6 C7 C8 116.7(7) . . ? C7 C8 C3 119.2(7) . . ? N5 C9 N7 110.3(5) . . ? N6 C10 N7 109.6(5) . . ? C12 C11 C16 122.7(6) . . ? C12 C11 N7 118.7(5) . . ? C16 C11 N7 118.6(5) . . ? C13 C12 C11 118.7(6) . . ? C12 C13 C14 118.8(6) . . ? C13 C14 C15 123.3(6) . . ? C13 C14 N8 118.3(6) . . ? C15 C14 N8 118.4(6) . . ? C14 C15 C16 118.9(6) . . ? C15 C16 C11 117.6(6) . . ? N11 C17 N9 110.0(5) . . ? N10 C18 N11 109.0(5) . . ? C24 C19 C20 122.2(6) . . ? C24 C19 N11 118.9(6) . . ? C20 C19 N11 118.9(6) . . ? C21 C20 C19 118.5(6) . . ? C22 C21 C20 119.4(7) . . ? C21 C22 C23 121.8(7) . . ? C21 C22 N12 118.9(7) . . ? C23 C22 N12 119.2(7) . . ? C22 C23 C24 120.0(7) . . ? C19 C24 C23 118.1(7) . . ? N1 C27 N3 110.4(5) . . ? C33 C28 C29 119.5(7) . . ? C33 C28 S1 121.1(6) . . ? C29 C28 S1 119.4(5) . . ? C30 C29 C28 119.5(7) . . ? C29 C30 C31 121.2(7) . . ? C32 C31 C30 119.0(7) . . ? C32 C31 C34 120.6(8) . . ? C30 C31 C34 120.3(8) . . ? C31 C32 C33 120.7(8) . . ? C32 C33 C28 119.9(8) . . ? C40 C35 C36 119.0(8) . . ? C40 C35 S2 119.9(7) . . ? C36 C35 S2 121.1(6) . . ? C35 C36 C37 120.0(8) . . ? C38 C37 C36 122.2(8) . . ? C37 C38 C39 116.3(8) . . ? C37 C38 C41 122.6(8) . . ? C39 C38 C41 120.9(8) . . ? C38 C39 C40 122.5(9) . . ? C35 C40 C39 119.5(9) . . ? C43 C42 C48 119.9(8) . . ? C43 C42 S3 120.1(6) . . ? C48 C42 S3 120.0(6) . . ? C44 C43 C42 119.0(9) . . ? C45 C44 C43 120.9(10) . . ? C44 C45 C47 119.2(9) . . ? C44 C45 C46 121.0(10) . . ? C47 C45 C46 119.8(9) . . ? C48 C47 C45 121.4(8) . . ? C47 C48 C42 119.2(8) . . ? C26' O8 C26 42.1(12) . . ? C26' O8 Ni2 136.1(12) . . ? C26 O8 Ni2 131.9(12) . . ? C25' O9 C25 45.4(10) . . ? C25' O9 Ni2 135.6(7) . . ? C25 O9 Ni2 126.4(8) . . ? O12 S1 O10 112.5(3) . . ? O12 S1 O11 112.8(4) . . ? O10 S1 O11 113.0(4) . . ? O12 S1 C28 106.3(3) . . ? O10 S1 C28 105.7(3) . . ? O11 S1 C28 105.9(3) . . ? O13 S2 O15 115.8(7) . . ? O13 S2 O14 114.5(7) . . ? O15 S2 O14 105.8(5) . . ? O13 S2 C35 105.5(4) . . ? O15 S2 C35 106.8(4) . . ? O14 S2 C35 108.1(4) . . ? O16 S3 O18 115.7(5) . . ? O16 S3 O17 107.5(5) . . ? O18 S3 O17 112.0(6) . . ? O16 S3 C42 108.6(4) . . ? O18 S3 C42 106.8(4) . . ? O17 S3 C42 105.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N9 Ni1 N1 C27 133.3(5) . . . . ? N9 Ni1 N1 C27 -46.7(5) 2_656 . . . ? N5 Ni1 N1 C27 -136.8(5) . . . . ? N5 Ni1 N1 C27 43.2(5) 2_656 . . . ? N1 Ni1 N1 C27 -107(32) 2_656 . . . ? N9 Ni1 N1 N2 -47.9(4) . . . . ? N9 Ni1 N1 N2 132.1(4) 2_656 . . . ? N5 Ni1 N1 N2 41.9(4) . . . . ? N5 Ni1 N1 N2 -138.1(4) 2_656 . . . ? N1 Ni1 N1 N2 72(32) 2_656 . . . ? C27 N1 N2 C2 1.1(6) . . . . ? Ni1 N1 N2 C2 -177.9(4) . . . . ? C27 N1 N2 Ni2 -175.6(4) . . . . ? Ni1 N1 N2 Ni2 5.4(6) . . . . ? N10 Ni2 N2 C2 -134.8(5) . . . . ? N6 Ni2 N2 C2 134.0(5) . . . . ? O9 Ni2 N2 C2 -46.0(5) . . . . ? O7 Ni2 N2 C2 43.9(5) . . . . ? O8 Ni2 N2 C2 99(14) . . . . ? N10 Ni2 N2 N1 41.3(4) . . . . ? N6 Ni2 N2 N1 -49.9(4) . . . . ? O9 Ni2 N2 N1 130.2(4) . . . . ? O7 Ni2 N2 N1 -140.0(4) . . . . ? O8 Ni2 N2 N1 -85(14) . . . . ? N9 Ni1 N5 C9 -139.7(5) . . . . ? N9 Ni1 N5 C9 40.3(5) 2_656 . . . ? N5 Ni1 N5 C9 143(20) 2_656 . . . ? N1 Ni1 N5 C9 130.1(5) . . . . ? N1 Ni1 N5 C9 -49.9(5) 2_656 . . . ? N9 Ni1 N5 N6 44.7(5) . . . . ? N9 Ni1 N5 N6 -135.3(5) 2_656 . . . ? N5 Ni1 N5 N6 -32(20) 2_656 . . . ? N1 Ni1 N5 N6 -45.6(5) . . . . ? N1 Ni1 N5 N6 134.4(5) 2_656 . . . ? C9 N5 N6 C10 -0.2(7) . . . . ? Ni1 N5 N6 C10 176.2(4) . . . . ? C9 N5 N6 Ni2 -175.8(4) . . . . ? Ni1 N5 N6 Ni2 0.5(7) . . . . ? N10 Ni2 N6 C10 140.2(6) . . . . ? N2 Ni2 N6 C10 -128.2(6) . . . . ? O9 Ni2 N6 C10 -110(100) . . . . ? O7 Ni2 N6 C10 -37.8(6) . . . . ? O8 Ni2 N6 C10 51.4(6) . . . . ? N10 Ni2 N6 N5 -45.0(5) . . . . ? N2 Ni2 N6 N5 46.6(5) . . . . ? O9 Ni2 N6 N5 64(100) . . . . ? O7 Ni2 N6 N5 137.0(5) . . . . ? O8 Ni2 N6 N5 -133.8(5) . . . . ? N9 Ni1 N9 C17 -17(40) 2_656 . . . ? N5 Ni1 N9 C17 133.3(5) . . . . ? N5 Ni1 N9 C17 -46.7(5) 2_656 . . . ? N1 Ni1 N9 C17 -137.3(5) . . . . ? N1 Ni1 N9 C17 42.7(5) 2_656 . . . ? N9 Ni1 N9 N10 164(39) 2_656 . . . ? N5 Ni1 N9 N10 -45.6(4) . . . . ? N5 Ni1 N9 N10 134.4(4) 2_656 . . . ? N1 Ni1 N9 N10 43.8(4) . . . . ? N1 Ni1 N9 N10 -136.2(4) 2_656 . . . ? C17 N9 N10 C18 0.8(6) . . . . ? Ni1 N9 N10 C18 180.0(4) . . . . ? C17 N9 N10 Ni2 -177.1(4) . . . . ? Ni1 N9 N10 Ni2 2.1(6) . . . . ? N6 Ni2 N10 C18 -133.6(5) . . . . ? N2 Ni2 N10 C18 136.5(5) . . . . ? O9 Ni2 N10 C18 46.6(5) . . . . ? O7 Ni2 N10 C18 -11(5) . . . . ? O8 Ni2 N10 C18 -44.1(5) . . . . ? N6 Ni2 N10 N9 44.0(5) . . . . ? N2 Ni2 N10 N9 -46.0(5) . . . . ? O9 Ni2 N10 N9 -135.9(5) . . . . ? O7 Ni2 N10 N9 167(5) . . . . ? O8 Ni2 N10 N9 133.4(5) . . . . ? N1 N2 C2 N3 -0.3(7) . . . . ? Ni2 N2 C2 N3 176.4(4) . . . . ? C27 N3 C2 N2 -0.6(7) . . . . ? C3 N3 C2 N2 -176.7(6) . . . . ? C27 N3 C3 C4 -52.5(9) . . . . ? C2 N3 C3 C4 122.6(7) . . . . ? C27 N3 C3 C8 130.6(7) . . . . ? C2 N3 C3 C8 -54.2(9) . . . . ? C8 C3 C4 C5 -1.5(11) . . . . ? N3 C3 C4 C5 -178.2(6) . . . . ? C3 C4 C5 C6 0.6(11) . . . . ? C4 C5 C6 C7 -0.1(12) . . . . ? C4 C5 C6 N4 -179.7(7) . . . . ? O2 N4 C6 C5 174.6(8) . . . . ? O1 N4 C6 C5 -3.3(10) . . . . ? O2 N4 C6 C7 -5.0(11) . . . . ? O1 N4 C6 C7 177.0(8) . . . . ? C5 C6 C7 C8 0.5(12) . . . . ? N4 C6 C7 C8 -179.9(7) . . . . ? C6 C7 C8 C3 -1.3(11) . . . . ? C4 C3 C8 C7 1.9(11) . . . . ? N3 C3 C8 C7 178.6(7) . . . . ? N6 N5 C9 N7 0.1(7) . . . . ? Ni1 N5 C9 N7 -176.2(4) . . . . ? C10 N7 C9 N5 0.0(7) . . . . ? C11 N7 C9 N5 179.3(6) . . . . ? N5 N6 C10 N7 0.1(7) . . . . ? Ni2 N6 C10 N7 175.7(4) . . . . ? C9 N7 C10 N6 -0.1(7) . . . . ? C11 N7 C10 N6 -179.4(6) . . . . ? C9 N7 C11 C12 37.2(9) . . . . ? C10 N7 C11 C12 -143.7(6) . . . . ? C9 N7 C11 C16 -141.5(6) . . . . ? C10 N7 C11 C16 37.7(9) . . . . ? C16 C11 C12 C13 1.7(10) . . . . ? N7 C11 C12 C13 -176.9(6) . . . . ? C11 C12 C13 C14 -2.2(10) . . . . ? C12 C13 C14 C15 0.3(11) . . . . ? C12 C13 C14 N8 179.6(6) . . . . ? O3 N8 C14 C13 4.7(10) . . . . ? O4 N8 C14 C13 -176.0(7) . . . . ? O3 N8 C14 C15 -176.0(7) . . . . ? O4 N8 C14 C15 3.3(10) . . . . ? C13 C14 C15 C16 2.0(11) . . . . ? N8 C14 C15 C16 -177.2(6) . . . . ? C14 C15 C16 C11 -2.4(10) . . . . ? C12 C11 C16 C15 0.6(10) . . . . ? N7 C11 C16 C15 179.2(6) . . . . ? C18 N11 C17 N9 -0.5(7) . . . . ? C19 N11 C17 N9 -177.9(5) . . . . ? N10 N9 C17 N11 -0.2(7) . . . . ? Ni1 N9 C17 N11 -179.2(4) . . . . ? N9 N10 C18 N11 -1.2(7) . . . . ? Ni2 N10 C18 N11 176.8(4) . . . . ? C17 N11 C18 N10 1.1(7) . . . . ? C19 N11 C18 N10 178.6(5) . . . . ? C17 N11 C19 C24 142.6(7) . . . . ? C18 N11 C19 C24 -34.4(9) . . . . ? C17 N11 C19 C20 -37.3(9) . . . . ? C18 N11 C19 C20 145.8(6) . . . . ? C24 C19 C20 C21 1.5(11) . . . . ? N11 C19 C20 C21 -178.7(6) . . . . ? C19 C20 C21 C22 0.1(11) . . . . ? C20 C21 C22 C23 -1.1(12) . . . . ? C20 C21 C22 N12 -177.6(7) . . . . ? O5 N12 C22 C21 7.8(12) . . . . ? O6 N12 C22 C21 -173.7(9) . . . . ? O5 N12 C22 C23 -168.8(9) . . . . ? O6 N12 C22 C23 9.7(12) . . . . ? C21 C22 C23 C24 0.6(12) . . . . ? N12 C22 C23 C24 177.1(7) . . . . ? C20 C19 C24 C23 -1.9(11) . . . . ? N11 C19 C24 C23 178.2(6) . . . . ? C22 C23 C24 C19 0.9(12) . . . . ? N2 N1 C27 N3 -1.5(6) . . . . ? Ni1 N1 C27 N3 177.4(4) . . . . ? C2 N3 C27 N1 1.4(7) . . . . ? C3 N3 C27 N1 177.3(6) . . . . ? C33 C28 C29 C30 -0.3(10) . . . . ? S1 C28 C29 C30 -179.2(5) . . . . ? C28 C29 C30 C31 -1.6(10) . . . . ? C29 C30 C31 C32 1.1(10) . . . . ? C29 C30 C31 C34 -179.0(6) . . . . ? C30 C31 C32 C33 1.1(11) . . . . ? C34 C31 C32 C33 -178.8(7) . . . . ? C31 C32 C33 C28 -2.9(11) . . . . ? C29 C28 C33 C32 2.5(10) . . . . ? S1 C28 C33 C32 -178.6(5) . . . . ? C40 C35 C36 C37 -5.6(13) . . . . ? S2 C35 C36 C37 177.2(7) . . . . ? C35 C36 C37 C38 0.7(13) . . . . ? C36 C37 C38 C39 6.0(14) . . . . ? C36 C37 C38 C41 -179.5(9) . . . . ? C37 C38 C39 C40 -8.0(18) . . . . ? C41 C38 C39 C40 177.4(11) . . . . ? C36 C35 C40 C39 3.7(16) . . . . ? S2 C35 C40 C39 -179.1(10) . . . . ? C38 C39 C40 C35 3(2) . . . . ? C48 C42 C43 C44 5.9(16) . . . . ? S3 C42 C43 C44 -176.3(9) . . . . ? C42 C43 C44 C45 -9(2) . . . . ? C43 C44 C45 C47 7(2) . . . . ? C43 C44 C45 C46 -175.9(13) . . . . ? C44 C45 C47 C48 -2.3(17) . . . . ? C46 C45 C47 C48 -179.8(11) . . . . ? C45 C47 C48 C42 -0.1(14) . . . . ? C43 C42 C48 C47 -1.7(13) . . . . ? S3 C42 C48 C47 -179.5(7) . . . . ? N10 Ni2 O8 C26' 97.5(17) . . . . ? N6 Ni2 O8 C26' -171.3(17) . . . . ? N2 Ni2 O8 C26' -136(14) . . . . ? O9 Ni2 O8 C26' 8.6(17) . . . . ? O7 Ni2 O8 C26' -81.2(17) . . . . ? N10 Ni2 O8 C26 157.1(16) . . . . ? N6 Ni2 O8 C26 -111.7(16) . . . . ? N2 Ni2 O8 C26 -77(14) . . . . ? O9 Ni2 O8 C26 68.2(16) . . . . ? O7 Ni2 O8 C26 -21.6(16) . . . . ? N10 Ni2 O9 C25' -107.2(16) . . . . ? N6 Ni2 O9 C25' 143(100) . . . . ? N2 Ni2 O9 C25' 161.2(16) . . . . ? O7 Ni2 O9 C25' 70.8(16) . . . . ? O8 Ni2 O9 C25' -18.4(16) . . . . ? N10 Ni2 O9 C25 -167.6(11) . . . . ? N6 Ni2 O9 C25 83(100) . . . . ? N2 Ni2 O9 C25 100.8(11) . . . . ? O7 Ni2 O9 C25 10.4(11) . . . . ? O8 Ni2 O9 C25 -78.7(12) . . . . ? C33 C28 S1 O12 29.3(7) . . . . ? C29 C28 S1 O12 -151.8(5) . . . . ? C33 C28 S1 O10 149.1(6) . . . . ? C29 C28 S1 O10 -32.0(6) . . . . ? C33 C28 S1 O11 -90.8(7) . . . . ? C29 C28 S1 O11 88.1(6) . . . . ? C40 C35 S2 O13 75.0(11) . . . . ? C36 C35 S2 O13 -107.9(10) . . . . ? C40 C35 S2 O15 -48.7(10) . . . . ? C36 C35 S2 O15 128.4(8) . . . . ? C40 C35 S2 O14 -162.1(8) . . . . ? C36 C35 S2 O14 15.1(8) . . . . ? C43 C42 S3 O16 175.0(8) . . . . ? C48 C42 S3 O16 -7.2(8) . . . . ? C43 C42 S3 O18 -59.7(10) . . . . ? C48 C42 S3 O18 118.1(8) . . . . ? C43 C42 S3 O17 59.8(9) . . . . ? C48 C42 S3 O17 -122.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.420 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.114