data_asb150 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H65 Cl2 F3 Fe2 N12 O7 S' _chemical_formula_weight 1229.81 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 11.5239(6) _cell_length_b 13.2419(7) _cell_length_c 20.3198(11) _cell_angle_alpha 85.1888(7) _cell_angle_beta 77.8930(7) _cell_angle_gamma 71.2408(6) _cell_volume 2870.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9839 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.22 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8424 _exptl_absorpt_correction_T_max 0.9066 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32646 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.10 _reflns_number_total 12521 _reflns_number_gt 10158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+3.2207P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap & geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12521 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _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 -0.02495(3) 0.82721(3) 0.257795(17) 0.01814(9) Uani 1 1 d . . . Fe2 Fe 0.11255(3) 0.46885(3) 0.268872(17) 0.01624(9) Uani 1 1 d . . . O1 O -0.03432(18) 0.80504(15) 0.16465(9) 0.0266(4) Uani 1 1 d . . . O2 O -0.49167(19) 1.04474(17) 0.22334(11) 0.0354(5) Uani 1 1 d . . . O3 O -0.04516(17) 0.47899(16) 0.24300(9) 0.0284(4) Uani 1 1 d . . . O4 O -0.01307(17) 0.52850(14) 0.36875(9) 0.0235(4) Uani 1 1 d . . . N1 N -0.0059(2) 0.90217(16) 0.34735(11) 0.0204(4) Uani 1 1 d . . . N2 N 0.0338(2) 0.95835(16) 0.21602(11) 0.0216(4) Uani 1 1 d . . . N3 N -0.2123(2) 0.88536(17) 0.31361(11) 0.0220(4) Uani 1 1 d . . . N4 N 0.10841(19) 0.70781(16) 0.29779(10) 0.0178(4) Uani 1 1 d . . . N5 N 0.1013(2) 0.89238(18) 0.10294(11) 0.0281(5) Uani 1 1 d . . . N6 N -0.3106(2) 0.90924(19) 0.22148(12) 0.0256(5) Uani 1 1 d . . . H6 H -0.246(3) 0.883(3) 0.2007(17) 0.029(9) Uiso 1 1 d . . . N7 N 0.32198(19) 0.40290(16) 0.26175(10) 0.0193(4) Uani 1 1 d . . . N8 N 0.1910(2) 0.41671(16) 0.16480(10) 0.0201(4) Uani 1 1 d . . . N9 N 0.14523(19) 0.32672(16) 0.33668(10) 0.0176(4) Uani 1 1 d . . . N10 N 0.17069(18) 0.60143(16) 0.28439(10) 0.0176(4) Uani 1 1 d . . . N11 N 0.0028(2) 0.4038(2) 0.13673(12) 0.0305(5) Uani 1 1 d . . . N12 N -0.05929(19) 0.37596(16) 0.40318(11) 0.0180(4) Uani 1 1 d . . . H12 H -0.114(3) 0.353(2) 0.4237(14) 0.015(7) Uiso 1 1 d . . . C1 C -0.0361(3) 1.0174(2) 0.33144(13) 0.0239(5) Uani 1 1 d . . . H1A H -0.0067 1.0523 0.3629 0.029 Uiso 1 1 calc R . . H1B H -0.1277 1.0502 0.3365 0.029 Uiso 1 1 calc R . . C2 C 0.0268(3) 1.0331(2) 0.26002(14) 0.0250(6) Uani 1 1 d . . . C3 C 0.0711(3) 1.1178(2) 0.24044(15) 0.0351(7) Uani 1 1 d . . . H3A H 0.0650 1.1691 0.2721 0.042 Uiso 1 1 calc R . . C4 C 0.1251(4) 1.1269(3) 0.17311(16) 0.0429(8) Uani 1 1 d . . . H4A H 0.1567 1.1847 0.1582 0.051 Uiso 1 1 calc R . . C5 C 0.1326(3) 1.0522(2) 0.12849(15) 0.0355(7) Uani 1 1 d . . . H5A H 0.1696 1.0578 0.0825 0.043 Uiso 1 1 calc R . . C6 C 0.0856(3) 0.9672(2) 0.15061(14) 0.0258(6) Uani 1 1 d . . . C7 C 0.0459(3) 0.8192(2) 0.11227(13) 0.0252(6) Uani 1 1 d . . . C8 C 0.0772(3) 0.7422(2) 0.05369(14) 0.0304(6) Uani 1 1 d . . . C9 C 0.2196(3) 0.6945(3) 0.03413(18) 0.0493(9) Uani 1 1 d . . . H9A H 0.2410 0.6502 -0.0057 0.074 Uiso 1 1 calc R . . H9B H 0.2517 0.6505 0.0716 0.074 Uiso 1 1 calc R . . H9C H 0.2570 0.7521 0.0240 0.074 Uiso 1 1 calc R . . C10 C 0.0263(3) 0.8058(2) -0.00622(14) 0.0328(6) Uani 1 1 d . . . H10A H 0.0438 0.7576 -0.0437 0.049 Uiso 1 1 calc R . . H10B H 0.0668 0.8609 -0.0203 0.049 Uiso 1 1 calc R . . H10C H -0.0641 0.8394 0.0070 0.049 Uiso 1 1 calc R . . C11 C 0.0192(4) 0.6533(2) 0.07397(16) 0.0409(8) Uani 1 1 d . . . H11A H 0.0415 0.6046 0.0363 0.061 Uiso 1 1 calc R . . H11B H -0.0718 0.6840 0.0857 0.061 Uiso 1 1 calc R . . H11C H 0.0506 0.6140 0.1130 0.061 Uiso 1 1 calc R . . C12 C -0.0976(2) 0.8768(2) 0.40298(13) 0.0230(5) Uani 1 1 d . . . H12A H -0.1136 0.9245 0.4411 0.028 Uiso 1 1 calc R . . H12B H -0.0631 0.8024 0.4187 0.028 Uiso 1 1 calc R . . C13 C -0.2189(2) 0.89001(19) 0.38076(13) 0.0212(5) Uani 1 1 d . . . C14 C -0.3299(2) 0.9063(2) 0.42660(13) 0.0239(5) Uani 1 1 d . . . H14A H -0.3323 0.9118 0.4732 0.029 Uiso 1 1 calc R . . C15 C -0.4370(3) 0.9144(2) 0.40373(14) 0.0257(6) Uani 1 1 d . . . H15A H -0.5133 0.9214 0.4347 0.031 Uiso 1 1 calc R . . C16 C -0.4327(3) 0.9123(2) 0.33524(14) 0.0270(6) Uani 1 1 d . . . H16A H -0.5056 0.9179 0.3185 0.032 Uiso 1 1 calc R . . C17 C -0.3196(2) 0.9017(2) 0.29162(13) 0.0233(5) Uani 1 1 d . . . C18 C -0.3972(3) 0.9857(2) 0.19087(14) 0.0264(6) Uani 1 1 d . . . C19 C -0.3637(3) 0.9916(2) 0.11378(14) 0.0293(6) Uani 1 1 d . . . C20 C -0.2562(3) 1.0403(3) 0.09411(16) 0.0372(7) Uani 1 1 d . . . H20A H -0.1817 0.9924 0.1092 0.056 Uiso 1 1 calc R . . H20B H -0.2808 1.1096 0.1155 0.056 Uiso 1 1 calc R . . H20C H -0.2376 1.0497 0.0451 0.056 Uiso 1 1 calc R . . C21 C -0.4786(3) 1.0654(3) 0.08800(17) 0.0439(8) Uani 1 1 d . . . H21A H -0.5479 1.0357 0.1013 0.066 Uiso 1 1 calc R . . H21B H -0.4586 1.0715 0.0388 0.066 Uiso 1 1 calc R . . H21C H -0.5027 1.1362 0.1075 0.066 Uiso 1 1 calc R . . C22 C -0.3254(3) 0.8812(2) 0.08329(15) 0.0336(6) Uani 1 1 d . . . H22A H -0.3931 0.8498 0.0980 0.050 Uiso 1 1 calc R . . H22B H -0.2498 0.8352 0.0982 0.050 Uiso 1 1 calc R . . H22C H -0.3087 0.8877 0.0341 0.050 Uiso 1 1 calc R . . C23 C 0.1232(2) 0.8547(2) 0.35836(13) 0.0218(5) Uani 1 1 d . . . H23A H 0.1255 0.8595 0.4064 0.026 Uiso 1 1 calc R . . H23B H 0.1775 0.8938 0.3312 0.026 Uiso 1 1 calc R . . C24 C 0.1693(2) 0.73986(19) 0.33805(12) 0.0197(5) Uani 1 1 d . . . C25 C 0.2715(2) 0.6566(2) 0.35129(13) 0.0213(5) Uani 1 1 d . . . H25A H 0.3301 0.6572 0.3778 0.026 Uiso 1 1 calc R . . C26 C 0.2676(2) 0.57214(19) 0.31653(12) 0.0190(5) Uani 1 1 d . . . C27 C 0.3490(2) 0.4575(2) 0.31412(13) 0.0218(5) Uani 1 1 d . . . H27A H 0.4381 0.4538 0.3039 0.026 Uiso 1 1 calc R . . H27B H 0.3322 0.4221 0.3584 0.026 Uiso 1 1 calc R . . C28 C 0.3777(2) 0.4311(2) 0.19360(13) 0.0231(5) Uani 1 1 d . . . H28A H 0.4680 0.3911 0.1837 0.028 Uiso 1 1 calc R . . H28B H 0.3681 0.5083 0.1908 0.028 Uiso 1 1 calc R . . C29 C 0.3144(2) 0.4045(2) 0.14309(13) 0.0233(5) Uani 1 1 d . . . C30 C 0.3784(3) 0.3710(2) 0.07964(14) 0.0307(6) Uani 1 1 d . . . H30A H 0.4646 0.3639 0.0662 0.037 Uiso 1 1 calc R . . C31 C 0.3127(3) 0.3474(3) 0.03533(15) 0.0389(7) Uani 1 1 d . . . H31A H 0.3540 0.3239 -0.0089 0.047 Uiso 1 1 calc R . . C32 C 0.1892(3) 0.3586(2) 0.05627(14) 0.0326(6) Uani 1 1 d . . . H32A H 0.1444 0.3420 0.0267 0.039 Uiso 1 1 calc R . . C33 C 0.1271(3) 0.3947(2) 0.12160(13) 0.0245(5) Uani 1 1 d . . . C34 C -0.0713(3) 0.4442(3) 0.19266(14) 0.0312(6) Uani 1 1 d . . . C35 C -0.2105(3) 0.4556(4) 0.20000(18) 0.0593(12) Uani 1 1 d . . . C36 C -0.2848(4) 0.5803(5) 0.2124(3) 0.0945(19) Uani 1 1 d . . . H36A H -0.3747 0.5906 0.2246 0.142 Uiso 1 1 calc R . . H36B H -0.2673 0.6212 0.1711 0.142 Uiso 1 1 calc R . . H36C H -0.2576 0.6049 0.2489 0.142 Uiso 1 1 calc R . . C37 C -0.2513(5) 0.4034(6) 0.2626(3) 0.107(2) Uani 1 1 d . . . H37A H -0.2199 0.3259 0.2572 0.160 Uiso 1 1 calc R . . H37B H -0.3428 0.4267 0.2739 0.160 Uiso 1 1 calc R . . H37C H -0.2186 0.4226 0.2990 0.160 Uiso 1 1 calc R . . C38 C -0.2424(4) 0.4361(5) 0.1364(2) 0.0851(18) Uani 1 1 d . . . H38A H -0.2065 0.3600 0.1261 0.128 Uiso 1 1 calc R . . H38B H -0.2083 0.4778 0.0998 0.128 Uiso 1 1 calc R . . H38C H -0.3334 0.4574 0.1412 0.128 Uiso 1 1 calc R . . C39 C 0.3579(2) 0.28697(19) 0.27192(13) 0.0221(5) Uani 1 1 d . . . H39A H 0.4394 0.2615 0.2864 0.027 Uiso 1 1 calc R . . H39B H 0.3674 0.2527 0.2288 0.027 Uiso 1 1 calc R . . C40 C 0.2613(2) 0.25505(19) 0.32432(12) 0.0191(5) Uani 1 1 d . . . C41 C 0.2919(2) 0.1561(2) 0.35587(13) 0.0223(5) Uani 1 1 d . . . H41A H 0.3746 0.1081 0.3461 0.027 Uiso 1 1 calc R . . C42 C 0.2000(2) 0.1282(2) 0.40193(13) 0.0221(5) Uani 1 1 d . . . H42A H 0.2177 0.0596 0.4230 0.027 Uiso 1 1 calc R . . C43 C 0.0821(2) 0.20136(19) 0.41691(12) 0.0206(5) Uani 1 1 d . . . H43A H 0.0179 0.1843 0.4489 0.025 Uiso 1 1 calc R . . C44 C 0.0588(2) 0.30069(19) 0.38419(12) 0.0173(5) Uani 1 1 d . . . C45 C -0.0864(2) 0.48371(19) 0.40077(12) 0.0178(5) Uani 1 1 d . . . C46 C -0.2114(2) 0.55027(19) 0.44227(13) 0.0205(5) Uani 1 1 d . . . C47 C -0.1768(3) 0.6052(3) 0.49571(15) 0.0337(7) Uani 1 1 d . . . H47A H -0.2523 0.6569 0.5199 0.051 Uiso 1 1 calc R . . H47B H -0.1173 0.6422 0.4737 0.051 Uiso 1 1 calc R . . H47C H -0.1386 0.5515 0.5276 0.051 Uiso 1 1 calc R . . C48 C -0.2788(3) 0.6339(2) 0.39522(15) 0.0304(6) Uani 1 1 d . . . H48A H -0.3038 0.5987 0.3625 0.046 Uiso 1 1 calc R . . H48B H -0.2228 0.6729 0.3714 0.046 Uiso 1 1 calc R . . H48C H -0.3532 0.6839 0.4215 0.046 Uiso 1 1 calc R . . C49 C -0.2968(3) 0.4860(2) 0.47655(17) 0.0358(7) Uani 1 1 d . . . H49A H -0.3147 0.4480 0.4425 0.054 Uiso 1 1 calc R . . H49B H -0.3750 0.5344 0.5007 0.054 Uiso 1 1 calc R . . H49C H -0.2553 0.4345 0.5084 0.054 Uiso 1 1 calc R . . C50 C 0.5953(3) 0.2170(2) 0.41838(14) 0.0275(6) Uani 1 1 d . . . C51 C -0.6550(3) 0.7575(3) 0.18013(18) 0.0441(8) Uani 1 1 d . . . H51A H -0.7304 0.7861 0.1599 0.053 Uiso 1 1 calc R A 1 H51B H -0.6750 0.7122 0.2194 0.053 Uiso 1 1 calc R A 1 S1 S 0.69246(6) 0.19716(5) 0.48152(3) 0.02014(13) Uani 1 1 d . . . F1 F 0.49347(16) 0.18835(16) 0.44214(9) 0.0422(4) Uani 1 1 d . . . F2 F 0.55681(19) 0.31917(15) 0.39952(10) 0.0466(5) Uani 1 1 d . . . F3 F 0.65496(17) 0.16077(15) 0.36289(9) 0.0410(4) Uani 1 1 d . . . O5 O 0.72328(18) 0.08445(14) 0.49666(10) 0.0281(4) Uani 1 1 d . . . O6 O 0.61082(19) 0.26559(16) 0.53449(10) 0.0322(4) Uani 1 1 d . . . O7 O 0.79759(17) 0.22944(15) 0.44612(11) 0.0309(4) Uani 1 1 d . . . Cl1 Cl -0.62192(8) 0.86503(8) 0.20882(5) 0.0511(2) Uani 1 1 d . B . Cl2 Cl -0.53273(10) 0.67582(9) 0.12006(6) 0.0437(2) Uiso 0.80 1 d P B 1 Cl2A Cl -0.5118(4) 0.6733(3) 0.1522(2) 0.0397(9) Uiso 0.20 1 d P B 2 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 0.02028(18) 0.01645(17) 0.01653(18) -0.00084(13) -0.00296(13) -0.00441(13) Fe2 0.01528(17) 0.01590(17) 0.01700(18) 0.00029(13) -0.00265(13) -0.00459(13) O1 0.0299(10) 0.0285(10) 0.0221(9) -0.0051(7) -0.0050(8) -0.0088(8) O2 0.0301(11) 0.0325(11) 0.0351(11) -0.0021(9) -0.0039(9) 0.0008(9) O3 0.0193(9) 0.0418(12) 0.0236(10) -0.0043(8) -0.0046(7) -0.0075(8) O4 0.0242(9) 0.0183(9) 0.0253(9) -0.0011(7) 0.0040(7) -0.0082(7) N1 0.0216(11) 0.0180(10) 0.0219(11) -0.0011(8) -0.0033(8) -0.0069(8) N2 0.0253(11) 0.0187(10) 0.0211(11) 0.0006(8) -0.0058(9) -0.0064(9) N3 0.0239(11) 0.0206(11) 0.0215(11) -0.0016(8) -0.0029(9) -0.0076(9) N4 0.0180(10) 0.0160(10) 0.0195(10) -0.0004(8) -0.0031(8) -0.0058(8) N5 0.0334(13) 0.0273(12) 0.0211(11) -0.0005(9) -0.0033(10) -0.0074(10) N6 0.0205(12) 0.0289(12) 0.0241(12) -0.0025(9) -0.0028(10) -0.0039(10) N7 0.0177(10) 0.0185(10) 0.0200(10) 0.0017(8) -0.0011(8) -0.0053(8) N8 0.0218(11) 0.0175(10) 0.0198(10) 0.0013(8) -0.0020(8) -0.0060(8) N9 0.0174(10) 0.0167(10) 0.0177(10) -0.0006(8) -0.0030(8) -0.0040(8) N10 0.0159(10) 0.0163(10) 0.0198(10) 0.0012(8) -0.0022(8) -0.0050(8) N11 0.0298(13) 0.0404(14) 0.0261(12) -0.0025(10) -0.0072(10) -0.0162(11) N12 0.0147(10) 0.0168(10) 0.0211(11) 0.0005(8) 0.0005(8) -0.0058(8) C1 0.0293(14) 0.0169(12) 0.0262(14) -0.0035(10) -0.0056(11) -0.0071(10) C2 0.0313(14) 0.0173(12) 0.0265(14) 0.0021(10) -0.0106(11) -0.0051(10) C3 0.056(2) 0.0227(14) 0.0330(16) 0.0011(12) -0.0119(14) -0.0186(14) C4 0.068(2) 0.0318(16) 0.0378(18) 0.0124(13) -0.0119(16) -0.0302(16) C5 0.0520(19) 0.0318(16) 0.0246(15) 0.0110(12) -0.0085(13) -0.0180(14) C6 0.0301(14) 0.0227(13) 0.0246(13) 0.0043(10) -0.0090(11) -0.0070(11) C7 0.0282(14) 0.0237(13) 0.0200(13) 0.0003(10) -0.0093(11) -0.0004(11) C8 0.0360(16) 0.0295(15) 0.0220(14) -0.0041(11) -0.0076(12) -0.0030(12) C9 0.0406(19) 0.054(2) 0.045(2) -0.0232(17) -0.0122(16) 0.0048(16) C10 0.0394(17) 0.0392(17) 0.0201(14) -0.0019(12) -0.0071(12) -0.0114(13) C11 0.067(2) 0.0259(15) 0.0290(16) -0.0052(12) -0.0169(15) -0.0077(15) C12 0.0261(13) 0.0242(13) 0.0177(12) -0.0019(10) -0.0017(10) -0.0076(10) C13 0.0264(13) 0.0158(12) 0.0211(12) -0.0024(9) -0.0018(10) -0.0073(10) C14 0.0289(14) 0.0178(12) 0.0232(13) -0.0032(10) 0.0013(10) -0.0081(10) C15 0.0257(13) 0.0197(13) 0.0283(14) -0.0006(10) 0.0032(11) -0.0077(10) C16 0.0232(13) 0.0236(13) 0.0345(15) 0.0001(11) -0.0058(11) -0.0077(11) C17 0.0235(13) 0.0211(12) 0.0251(13) -0.0012(10) -0.0040(10) -0.0068(10) C18 0.0249(14) 0.0254(14) 0.0305(14) -0.0002(11) -0.0070(11) -0.0091(11) C19 0.0284(14) 0.0294(15) 0.0288(15) 0.0020(11) -0.0076(12) -0.0065(12) C20 0.0421(18) 0.0375(17) 0.0342(16) 0.0040(13) -0.0053(14) -0.0178(14) C21 0.0397(18) 0.0459(19) 0.0398(18) 0.0064(15) -0.0164(15) -0.0009(15) C22 0.0344(16) 0.0397(17) 0.0274(15) -0.0040(12) -0.0036(12) -0.0133(13) C23 0.0242(13) 0.0211(12) 0.0226(13) -0.0020(10) -0.0059(10) -0.0093(10) C24 0.0223(12) 0.0199(12) 0.0180(12) 0.0005(9) -0.0035(10) -0.0085(10) C25 0.0199(12) 0.0247(13) 0.0215(12) 0.0013(10) -0.0071(10) -0.0083(10) C26 0.0164(11) 0.0211(12) 0.0193(12) 0.0024(9) -0.0023(9) -0.0070(9) C27 0.0173(12) 0.0215(12) 0.0263(13) 0.0014(10) -0.0059(10) -0.0051(10) C28 0.0175(12) 0.0242(13) 0.0247(13) 0.0008(10) 0.0020(10) -0.0069(10) C29 0.0248(13) 0.0176(12) 0.0232(13) 0.0028(10) -0.0001(10) -0.0044(10) C30 0.0272(14) 0.0328(15) 0.0270(14) -0.0025(11) 0.0042(11) -0.0078(12) C31 0.0466(19) 0.0434(18) 0.0207(14) -0.0081(12) 0.0057(13) -0.0117(15) C32 0.0403(17) 0.0348(16) 0.0239(14) -0.0054(12) -0.0053(12) -0.0130(13) C33 0.0307(14) 0.0199(12) 0.0229(13) 0.0012(10) -0.0058(11) -0.0080(11) C34 0.0248(14) 0.0463(17) 0.0252(14) 0.0009(12) -0.0081(11) -0.0130(13) C35 0.0292(18) 0.123(4) 0.0332(18) -0.005(2) -0.0074(14) -0.033(2) C36 0.042(2) 0.140(5) 0.080(4) -0.025(3) -0.019(2) 0.011(3) C37 0.054(3) 0.223(8) 0.070(3) -0.025(4) 0.007(2) -0.087(4) C38 0.032(2) 0.166(5) 0.060(3) -0.055(3) -0.0090(19) -0.022(3) C39 0.0167(12) 0.0188(12) 0.0266(13) 0.0002(10) -0.0003(10) -0.0024(9) C40 0.0183(12) 0.0171(12) 0.0208(12) -0.0021(9) -0.0032(9) -0.0040(9) C41 0.0195(12) 0.0178(12) 0.0271(13) -0.0013(10) -0.0056(10) -0.0016(10) C42 0.0267(13) 0.0166(12) 0.0237(13) 0.0033(10) -0.0087(10) -0.0061(10) C43 0.0236(13) 0.0200(12) 0.0197(12) 0.0024(9) -0.0064(10) -0.0082(10) C44 0.0171(11) 0.0176(11) 0.0172(11) -0.0025(9) -0.0038(9) -0.0047(9) C45 0.0199(12) 0.0182(12) 0.0160(11) 0.0002(9) -0.0040(9) -0.0066(9) C46 0.0187(12) 0.0173(12) 0.0229(13) -0.0021(9) 0.0011(10) -0.0050(9) C47 0.0312(15) 0.0406(17) 0.0267(15) -0.0139(12) -0.0002(12) -0.0077(13) C48 0.0288(15) 0.0234(14) 0.0320(15) -0.0002(11) -0.0030(12) -0.0004(11) C49 0.0269(15) 0.0211(14) 0.0491(19) -0.0030(12) 0.0134(13) -0.0060(11) C50 0.0239(13) 0.0285(14) 0.0270(14) 0.0003(11) -0.0052(11) -0.0041(11) C51 0.0314(17) 0.052(2) 0.045(2) -0.0001(16) 0.0011(14) -0.0135(15) S1 0.0189(3) 0.0171(3) 0.0259(3) 0.0001(2) -0.0057(2) -0.0069(2) F1 0.0256(9) 0.0640(13) 0.0435(11) -0.0063(9) -0.0109(8) -0.0192(9) F2 0.0494(11) 0.0332(10) 0.0511(12) 0.0115(8) -0.0235(9) 0.0010(8) F3 0.0389(10) 0.0519(11) 0.0267(9) -0.0083(8) -0.0082(8) -0.0036(8) O5 0.0333(11) 0.0206(9) 0.0328(11) 0.0051(8) -0.0115(8) -0.0099(8) O6 0.0297(10) 0.0340(11) 0.0339(11) -0.0125(9) -0.0031(9) -0.0103(9) O7 0.0209(9) 0.0242(10) 0.0484(13) 0.0012(9) -0.0033(9) -0.0107(8) Cl1 0.0431(5) 0.0671(6) 0.0504(5) 0.0016(4) -0.0054(4) -0.0299(4) _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 O1 1.9696(18) . ? Fe1 N4 2.066(2) . ? Fe1 N2 2.112(2) . ? Fe1 N3 2.143(2) . ? Fe1 N1 2.226(2) . ? Fe2 O3 1.9569(19) . ? Fe2 N10 2.137(2) . ? Fe2 N8 2.193(2) . ? Fe2 N9 2.216(2) . ? Fe2 N7 2.264(2) . ? Fe2 O4 2.2671(18) . ? O1 C7 1.300(3) . ? O2 C18 1.212(3) . ? O3 C34 1.283(3) . ? O4 C45 1.231(3) . ? N1 C12 1.474(3) . ? N1 C23 1.474(3) . ? N1 C1 1.475(3) . ? N2 C6 1.350(3) . ? N2 C2 1.361(3) . ? N3 C17 1.348(3) . ? N3 C13 1.356(3) . ? N4 C24 1.354(3) . ? N4 N10 1.381(3) . ? N5 C7 1.302(4) . ? N5 C6 1.388(4) . ? N6 C18 1.383(4) . ? N6 C17 1.405(3) . ? N6 H6 0.76(3) . ? N7 C39 1.464(3) . ? N7 C28 1.471(3) . ? N7 C27 1.471(3) . ? N8 C29 1.358(3) . ? N8 C33 1.361(3) . ? N9 C44 1.343(3) . ? N9 C40 1.355(3) . ? N10 C26 1.345(3) . ? N11 C34 1.307(4) . ? N11 C33 1.368(4) . ? N12 C45 1.358(3) . ? N12 C44 1.402(3) . ? N12 H12 0.81(3) . ? C1 C2 1.510(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.374(4) . ? C3 C4 1.392(4) . ? C3 H3A 0.9500 . ? C4 C5 1.369(4) . ? C4 H4A 0.9500 . ? C5 C6 1.402(4) . ? C5 H5A 0.9500 . ? C7 C8 1.541(4) . ? C8 C11 1.521(4) . ? C8 C10 1.531(4) . ? C8 C9 1.533(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.510(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.381(4) . ? C14 C15 1.378(4) . ? C14 H14A 0.9500 . ? C15 C16 1.384(4) . ? C15 H15A 0.9500 . ? C16 C17 1.387(4) . ? C16 H16A 0.9500 . ? C18 C19 1.534(4) . ? C19 C22 1.530(4) . ? C19 C21 1.535(4) . ? C19 C20 1.540(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.503(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.386(4) . ? C25 C26 1.389(3) . ? C25 H25A 0.9500 . ? C26 C27 1.504(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.499(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.375(4) . ? C30 C31 1.402(4) . ? C30 H30A 0.9500 . ? C31 C32 1.360(4) . ? C31 H31A 0.9500 . ? C32 C33 1.411(4) . ? C32 H32A 0.9500 . ? C34 C35 1.538(4) . ? C35 C37 1.459(7) . ? C35 C38 1.479(5) . ? C35 C36 1.610(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.510(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.382(3) . ? C41 C42 1.383(4) . ? C41 H41A 0.9500 . ? C42 C43 1.381(4) . ? C42 H42A 0.9500 . ? C43 C44 1.395(3) . ? C43 H43A 0.9500 . ? C45 C46 1.537(3) . ? C46 C48 1.525(4) . ? C46 C49 1.525(4) . ? C46 C47 1.539(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 F2 1.331(3) . ? C50 F1 1.331(3) . ? C50 F3 1.336(3) . ? C50 S1 1.824(3) . ? C51 Cl2A 1.679(5) . ? C51 Cl1 1.760(4) . ? C51 Cl2 1.779(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? S1 O6 1.434(2) . ? S1 O5 1.4409(19) . ? S1 O7 1.4436(19) . ? 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 O1 Fe1 N4 115.12(8) . . ? O1 Fe1 N2 84.55(8) . . ? N4 Fe1 N2 114.49(8) . . ? O1 Fe1 N3 107.67(8) . . ? N4 Fe1 N3 120.34(8) . . ? N2 Fe1 N3 108.94(8) . . ? O1 Fe1 N1 160.98(8) . . ? N4 Fe1 N1 76.47(8) . . ? N2 Fe1 N1 76.72(8) . . ? N3 Fe1 N1 75.93(8) . . ? O3 Fe2 N10 125.23(8) . . ? O3 Fe2 N8 82.90(8) . . ? N10 Fe2 N8 108.39(8) . . ? O3 Fe2 N9 103.51(8) . . ? N10 Fe2 N9 120.99(8) . . ? N8 Fe2 N9 108.68(7) . . ? O3 Fe2 N7 154.12(8) . . ? N10 Fe2 N7 74.33(8) . . ? N8 Fe2 N7 74.01(8) . . ? N9 Fe2 N7 73.86(7) . . ? O3 Fe2 O4 83.27(7) . . ? N10 Fe2 O4 79.07(7) . . ? N8 Fe2 O4 166.13(7) . . ? N9 Fe2 O4 75.60(7) . . ? N7 Fe2 O4 119.71(7) . . ? C7 O1 Fe1 123.66(17) . . ? C34 O3 Fe2 132.96(18) . . ? C45 O4 Fe2 123.03(16) . . ? C12 N1 C23 112.1(2) . . ? C12 N1 C1 113.0(2) . . ? C23 N1 C1 112.2(2) . . ? C12 N1 Fe1 104.51(15) . . ? C23 N1 Fe1 108.49(15) . . ? C1 N1 Fe1 106.00(15) . . ? C6 N2 C2 119.3(2) . . ? C6 N2 Fe1 124.09(18) . . ? C2 N2 Fe1 116.37(17) . . ? C17 N3 C13 118.0(2) . . ? C17 N3 Fe1 127.85(17) . . ? C13 N3 Fe1 113.40(17) . . ? C24 N4 N10 107.43(19) . . ? C24 N4 Fe1 116.08(16) . . ? N10 N4 Fe1 135.17(15) . . ? C7 N5 C6 123.9(2) . . ? C18 N6 C17 122.5(2) . . ? C18 N6 H6 119(3) . . ? C17 N6 H6 116(3) . . ? C39 N7 C28 110.9(2) . . ? C39 N7 C27 112.9(2) . . ? C28 N7 C27 112.1(2) . . ? C39 N7 Fe2 109.31(15) . . ? C28 N7 Fe2 105.84(15) . . ? C27 N7 Fe2 105.34(14) . . ? C29 N8 C33 118.4(2) . . ? C29 N8 Fe2 116.05(17) . . ? C33 N8 Fe2 125.52(17) . . ? C44 N9 C40 117.4(2) . . ? C44 N9 Fe2 126.28(16) . . ? C40 N9 Fe2 116.00(16) . . ? C26 N10 N4 106.93(19) . . ? C26 N10 Fe2 111.90(15) . . ? N4 N10 Fe2 133.86(15) . . ? C34 N11 C33 123.4(2) . . ? C45 N12 C44 126.6(2) . . ? C45 N12 H12 116(2) . . ? C44 N12 H12 116(2) . . ? N1 C1 C2 109.2(2) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C3 122.4(3) . . ? N2 C2 C1 115.0(2) . . ? C3 C2 C1 122.6(2) . . ? C2 C3 C4 118.4(3) . . ? C2 C3 H3A 120.8 . . ? C4 C3 H3A 120.8 . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? N2 C6 N5 123.2(2) . . ? N2 C6 C5 120.2(3) . . ? N5 C6 C5 116.6(3) . . ? O1 C7 N5 127.6(2) . . ? O1 C7 C8 116.3(2) . . ? N5 C7 C8 116.1(2) . . ? C11 C8 C10 109.8(2) . . ? C11 C8 C9 109.7(3) . . ? C10 C8 C9 109.4(3) . . ? C11 C8 C7 110.8(2) . . ? C10 C8 C7 108.4(2) . . ? C9 C8 C7 108.7(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 111.0(2) . . ? N1 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? N1 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N3 C13 C14 122.2(2) . . ? N3 C13 C12 116.3(2) . . ? C14 C13 C12 121.5(2) . . ? C15 C14 C13 119.0(2) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? C14 C15 C16 119.5(2) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C15 C16 C17 118.5(3) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? N3 C17 C16 122.4(2) . . ? N3 C17 N6 116.0(2) . . ? C16 C17 N6 121.6(2) . . ? O2 C18 N6 121.7(3) . . ? O2 C18 C19 122.9(3) . . ? N6 C18 C19 115.4(2) . . ? C22 C19 C18 111.2(2) . . ? C22 C19 C21 109.6(3) . . ? C18 C19 C21 108.2(2) . . ? C22 C19 C20 110.4(2) . . ? C18 C19 C20 108.2(2) . . ? C21 C19 C20 109.1(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 C24 108.7(2) . . ? N1 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? N1 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.3 . . ? N4 C24 C25 110.8(2) . . ? N4 C24 C23 118.4(2) . . ? C25 C24 C23 130.7(2) . . ? C24 C25 C26 103.4(2) . . ? C24 C25 H25A 128.3 . . ? C26 C25 H25A 128.3 . . ? N10 C26 C25 111.4(2) . . ? N10 C26 C27 118.9(2) . . ? C25 C26 C27 129.6(2) . . ? N7 C27 C26 109.1(2) . . ? N7 C27 H27A 109.9 . . ? C26 C27 H27A 109.9 . . ? N7 C27 H27B 109.9 . . ? C26 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? N7 C28 C29 109.7(2) . . ? N7 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? N7 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? N8 C29 C30 123.4(3) . . ? N8 C29 C28 115.0(2) . . ? C30 C29 C28 121.6(2) . . ? C29 C30 C31 118.1(3) . . ? C29 C30 H30A 120.9 . . ? C31 C30 H30A 120.9 . . ? C32 C31 C30 119.3(3) . . ? C32 C31 H31A 120.3 . . ? C30 C31 H31A 120.3 . . ? C31 C32 C33 120.5(3) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? N8 C33 N11 124.6(2) . . ? N8 C33 C32 120.2(3) . . ? N11 C33 C32 115.3(2) . . ? O3 C34 N11 129.0(3) . . ? O3 C34 C35 113.9(3) . . ? N11 C34 C35 117.0(3) . . ? C37 C35 C38 120.5(4) . . ? C37 C35 C34 109.2(3) . . ? C38 C35 C34 112.7(3) . . ? C37 C35 C36 104.0(4) . . ? C38 C35 C36 102.9(4) . . ? C34 C35 C36 105.9(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C39 C40 111.3(2) . . ? N7 C39 H39A 109.4 . . ? C40 C39 H39A 109.4 . . ? N7 C39 H39B 109.4 . . ? C40 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? N9 C40 C41 123.1(2) . . ? N9 C40 C39 116.6(2) . . ? C41 C40 C39 120.3(2) . . ? C40 C41 C42 118.7(2) . . ? C40 C41 H41A 120.6 . . ? C42 C41 H41A 120.6 . . ? C43 C42 C41 119.2(2) . . ? C43 C42 H42A 120.4 . . ? C41 C42 H42A 120.4 . . ? C42 C43 C44 118.9(2) . . ? C42 C43 H43A 120.6 . . ? C44 C43 H43A 120.6 . . ? N9 C44 C43 122.6(2) . . ? N9 C44 N12 119.6(2) . . ? C43 C44 N12 117.8(2) . . ? O4 C45 N12 122.4(2) . . ? O4 C45 C46 119.7(2) . . ? N12 C45 C46 117.8(2) . . ? C48 C46 C49 109.2(2) . . ? C48 C46 C45 107.8(2) . . ? C49 C46 C45 114.6(2) . . ? C48 C46 C47 109.8(2) . . ? C49 C46 C47 109.8(2) . . ? C45 C46 C47 105.5(2) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? 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 . . ? F2 C50 F1 107.0(2) . . ? F2 C50 F3 107.3(2) . . ? F1 C50 F3 106.9(2) . . ? F2 C50 S1 111.1(2) . . ? F1 C50 S1 111.40(19) . . ? F3 C50 S1 112.74(19) . . ? Cl2A C51 Cl1 102.4(2) . . ? Cl2A C51 Cl2 24.43(15) . . ? Cl1 C51 Cl2 115.05(19) . . ? Cl2A C51 H51A 132.8 . . ? Cl1 C51 H51A 108.5 . . ? Cl2 C51 H51A 108.5 . . ? Cl2A C51 H51B 94.9 . . ? Cl1 C51 H51B 108.5 . . ? Cl2 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? O6 S1 O5 115.60(12) . . ? O6 S1 O7 115.89(12) . . ? O5 S1 O7 113.69(12) . . ? O6 S1 C50 102.55(12) . . ? O5 S1 C50 103.60(12) . . ? O7 S1 C50 102.99(13) . . ? 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 N4 Fe1 O1 C7 -76.2(2) . . . . ? N2 Fe1 O1 C7 38.3(2) . . . . ? N3 Fe1 O1 C7 146.48(19) . . . . ? N1 Fe1 O1 C7 48.4(3) . . . . ? N10 Fe2 O3 C34 121.2(3) . . . . ? N8 Fe2 O3 C34 13.7(3) . . . . ? N9 Fe2 O3 C34 -93.9(3) . . . . ? N7 Fe2 O3 C34 -13.1(4) . . . . ? O4 Fe2 O3 C34 -167.3(3) . . . . ? O3 Fe2 O4 C45 55.1(2) . . . . ? N10 Fe2 O4 C45 -177.0(2) . . . . ? N8 Fe2 O4 C45 59.1(4) . . . . ? N9 Fe2 O4 C45 -50.79(19) . . . . ? N7 Fe2 O4 C45 -112.30(19) . . . . ? O1 Fe1 N1 C12 140.7(2) . . . . ? N4 Fe1 N1 C12 -89.40(15) . . . . ? N2 Fe1 N1 C12 150.94(16) . . . . ? N3 Fe1 N1 C12 37.18(15) . . . . ? O1 Fe1 N1 C23 -99.6(3) . . . . ? N4 Fe1 N1 C23 30.38(15) . . . . ? N2 Fe1 N1 C23 -89.28(16) . . . . ? N3 Fe1 N1 C23 156.96(17) . . . . ? O1 Fe1 N1 C1 21.1(3) . . . . ? N4 Fe1 N1 C1 151.02(17) . . . . ? N2 Fe1 N1 C1 31.36(15) . . . . ? N3 Fe1 N1 C1 -82.40(16) . . . . ? O1 Fe1 N2 C6 -22.8(2) . . . . ? N4 Fe1 N2 C6 92.4(2) . . . . ? N3 Fe1 N2 C6 -129.6(2) . . . . ? N1 Fe1 N2 C6 160.6(2) . . . . ? O1 Fe1 N2 C2 162.61(19) . . . . ? N4 Fe1 N2 C2 -82.2(2) . . . . ? N3 Fe1 N2 C2 55.8(2) . . . . ? N1 Fe1 N2 C2 -14.04(18) . . . . ? O1 Fe1 N3 C17 1.9(2) . . . . ? N4 Fe1 N3 C17 -132.7(2) . . . . ? N2 Fe1 N3 C17 92.2(2) . . . . ? N1 Fe1 N3 C17 162.5(2) . . . . ? O1 Fe1 N3 C13 171.45(16) . . . . ? N4 Fe1 N3 C13 36.8(2) . . . . ? N2 Fe1 N3 C13 -98.33(17) . . . . ? N1 Fe1 N3 C13 -27.98(16) . . . . ? O1 Fe1 N4 C24 142.34(17) . . . . ? N2 Fe1 N4 C24 46.70(19) . . . . ? N3 Fe1 N4 C24 -86.13(18) . . . . ? N1 Fe1 N4 C24 -21.63(17) . . . . ? O1 Fe1 N4 N10 -22.6(2) . . . . ? N2 Fe1 N4 N10 -118.2(2) . . . . ? N3 Fe1 N4 N10 109.0(2) . . . . ? N1 Fe1 N4 N10 173.5(2) . . . . ? O3 Fe2 N7 C39 -56.7(3) . . . . ? N10 Fe2 N7 C39 160.66(17) . . . . ? N8 Fe2 N7 C39 -84.43(16) . . . . ? N9 Fe2 N7 C39 31.02(15) . . . . ? O4 Fe2 N7 C39 93.42(16) . . . . ? O3 Fe2 N7 C28 62.8(2) . . . . ? N10 Fe2 N7 C28 -79.84(16) . . . . ? N8 Fe2 N7 C28 35.07(15) . . . . ? N9 Fe2 N7 C28 150.52(17) . . . . ? O4 Fe2 N7 C28 -147.08(14) . . . . ? O3 Fe2 N7 C27 -178.29(17) . . . . ? N10 Fe2 N7 C27 39.10(14) . . . . ? N8 Fe2 N7 C27 154.01(16) . . . . ? N9 Fe2 N7 C27 -90.53(15) . . . . ? O4 Fe2 N7 C27 -28.13(17) . . . . ? O3 Fe2 N8 C29 172.59(18) . . . . ? N10 Fe2 N8 C29 47.76(19) . . . . ? N9 Fe2 N8 C29 -85.49(18) . . . . ? N7 Fe2 N8 C29 -19.20(17) . . . . ? O4 Fe2 N8 C29 168.6(2) . . . . ? O3 Fe2 N8 C33 -8.4(2) . . . . ? N10 Fe2 N8 C33 -133.2(2) . . . . ? N9 Fe2 N8 C33 93.5(2) . . . . ? N7 Fe2 N8 C33 159.8(2) . . . . ? O4 Fe2 N8 C33 -12.4(4) . . . . ? O3 Fe2 N9 C44 -41.4(2) . . . . ? N10 Fe2 N9 C44 105.40(19) . . . . ? N8 Fe2 N9 C44 -128.33(19) . . . . ? N7 Fe2 N9 C44 165.3(2) . . . . ? O4 Fe2 N9 C44 37.90(19) . . . . ? O3 Fe2 N9 C40 132.15(17) . . . . ? N10 Fe2 N9 C40 -81.08(18) . . . . ? N8 Fe2 N9 C40 45.19(19) . . . . ? N7 Fe2 N9 C40 -21.20(17) . . . . ? O4 Fe2 N9 C40 -148.58(18) . . . . ? C24 N4 N10 C26 -0.3(2) . . . . ? Fe1 N4 N10 C26 165.53(18) . . . . ? C24 N4 N10 Fe2 146.17(18) . . . . ? Fe1 N4 N10 Fe2 -48.0(3) . . . . ? O3 Fe2 N10 C26 165.55(15) . . . . ? N8 Fe2 N10 C26 -100.14(17) . . . . ? N9 Fe2 N10 C26 26.27(19) . . . . ? N7 Fe2 N10 C26 -33.39(16) . . . . ? O4 Fe2 N10 C26 91.96(17) . . . . ? O3 Fe2 N10 N4 20.3(2) . . . . ? N8 Fe2 N10 N4 114.6(2) . . . . ? N9 Fe2 N10 N4 -119.0(2) . . . . ? N7 Fe2 N10 N4 -178.6(2) . . . . ? O4 Fe2 N10 N4 -53.3(2) . . . . ? C12 N1 C1 C2 -157.4(2) . . . . ? C23 N1 C1 C2 74.7(3) . . . . ? Fe1 N1 C1 C2 -43.5(2) . . . . ? C6 N2 C2 C3 -0.2(4) . . . . ? Fe1 N2 C2 C3 174.7(2) . . . . ? C6 N2 C2 C1 178.3(2) . . . . ? Fe1 N2 C2 C1 -6.8(3) . . . . ? N1 C1 C2 N2 35.1(3) . . . . ? N1 C1 C2 C3 -146.4(3) . . . . ? N2 C2 C3 C4 -0.1(5) . . . . ? C1 C2 C3 C4 -178.5(3) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C3 C4 C5 C6 0.2(5) . . . . ? C2 N2 C6 N5 177.2(2) . . . . ? Fe1 N2 C6 N5 2.7(4) . . . . ? C2 N2 C6 C5 0.5(4) . . . . ? Fe1 N2 C6 C5 -174.0(2) . . . . ? C7 N5 C6 N2 14.8(4) . . . . ? C7 N5 C6 C5 -168.4(3) . . . . ? C4 C5 C6 N2 -0.5(5) . . . . ? C4 C5 C6 N5 -177.4(3) . . . . ? Fe1 O1 C7 N5 -36.9(4) . . . . ? Fe1 O1 C7 C8 144.52(19) . . . . ? C6 N5 C7 O1 2.5(4) . . . . ? C6 N5 C7 C8 -179.0(2) . . . . ? O1 C7 C8 C11 -8.0(3) . . . . ? N5 C7 C8 C11 173.3(2) . . . . ? O1 C7 C8 C10 112.5(3) . . . . ? N5 C7 C8 C10 -66.2(3) . . . . ? O1 C7 C8 C9 -128.7(3) . . . . ? N5 C7 C8 C9 52.6(3) . . . . ? C23 N1 C12 C13 -159.4(2) . . . . ? C1 N1 C12 C13 72.7(3) . . . . ? Fe1 N1 C12 C13 -42.1(2) . . . . ? C17 N3 C13 C14 2.8(4) . . . . ? Fe1 N3 C13 C14 -167.84(19) . . . . ? C17 N3 C13 C12 -177.0(2) . . . . ? Fe1 N3 C13 C12 12.4(3) . . . . ? N1 C12 C13 N3 21.9(3) . . . . ? N1 C12 C13 C14 -157.9(2) . . . . ? N3 C13 C14 C15 2.3(4) . . . . ? C12 C13 C14 C15 -177.9(2) . . . . ? C13 C14 C15 C16 -3.7(4) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C13 N3 C17 C16 -6.6(4) . . . . ? Fe1 N3 C17 C16 162.5(2) . . . . ? C13 N3 C17 N6 172.4(2) . . . . ? Fe1 N3 C17 N6 -18.5(3) . . . . ? C15 C16 C17 N3 5.2(4) . . . . ? C15 C16 C17 N6 -173.8(2) . . . . ? C18 N6 C17 N3 -136.5(3) . . . . ? C18 N6 C17 C16 42.5(4) . . . . ? C17 N6 C18 O2 -6.6(4) . . . . ? C17 N6 C18 C19 172.2(2) . . . . ? O2 C18 C19 C22 -131.6(3) . . . . ? N6 C18 C19 C22 49.6(3) . . . . ? O2 C18 C19 C21 -11.2(4) . . . . ? N6 C18 C19 C21 170.1(3) . . . . ? O2 C18 C19 C20 106.9(3) . . . . ? N6 C18 C19 C20 -71.8(3) . . . . ? C12 N1 C23 C24 81.3(2) . . . . ? C1 N1 C23 C24 -150.3(2) . . . . ? Fe1 N1 C23 C24 -33.6(2) . . . . ? N10 N4 C24 C25 0.3(3) . . . . ? Fe1 N4 C24 C25 -168.56(16) . . . . ? N10 N4 C24 C23 177.8(2) . . . . ? Fe1 N4 C24 C23 8.9(3) . . . . ? N1 C23 C24 N4 18.2(3) . . . . ? N1 C23 C24 C25 -164.9(3) . . . . ? N4 C24 C25 C26 -0.3(3) . . . . ? C23 C24 C25 C26 -177.3(3) . . . . ? N4 N10 C26 C25 0.1(3) . . . . ? Fe2 N10 C26 C25 -154.44(17) . . . . ? N4 N10 C26 C27 176.6(2) . . . . ? Fe2 N10 C26 C27 22.1(3) . . . . ? C24 C25 C26 N10 0.1(3) . . . . ? C24 C25 C26 C27 -176.0(2) . . . . ? C39 N7 C27 C26 -158.1(2) . . . . ? C28 N7 C27 C26 75.8(2) . . . . ? Fe2 N7 C27 C26 -38.9(2) . . . . ? N10 C26 C27 N7 13.5(3) . . . . ? C25 C26 C27 N7 -170.7(2) . . . . ? C39 N7 C28 C29 71.6(3) . . . . ? C27 N7 C28 C29 -161.2(2) . . . . ? Fe2 N7 C28 C29 -46.9(2) . . . . ? C33 N8 C29 C30 0.0(4) . . . . ? Fe2 N8 C29 C30 179.1(2) . . . . ? C33 N8 C29 C28 179.6(2) . . . . ? Fe2 N8 C29 C28 -1.3(3) . . . . ? N7 C28 C29 N8 33.6(3) . . . . ? N7 C28 C29 C30 -146.7(2) . . . . ? N8 C29 C30 C31 -0.5(4) . . . . ? C28 C29 C30 C31 179.9(3) . . . . ? C29 C30 C31 C32 0.1(5) . . . . ? C30 C31 C32 C33 0.7(5) . . . . ? C29 N8 C33 N11 -179.8(2) . . . . ? Fe2 N8 C33 N11 1.2(4) . . . . ? C29 N8 C33 C32 0.9(4) . . . . ? Fe2 N8 C33 C32 -178.10(19) . . . . ? C34 N11 C33 N8 6.5(4) . . . . ? C34 N11 C33 C32 -174.1(3) . . . . ? C31 C32 C33 N8 -1.3(4) . . . . ? C31 C32 C33 N11 179.4(3) . . . . ? Fe2 O3 C34 N11 -11.7(5) . . . . ? Fe2 O3 C34 C35 170.0(2) . . . . ? C33 N11 C34 O3 -2.1(5) . . . . ? C33 N11 C34 C35 176.1(3) . . . . ? O3 C34 C35 C37 -55.1(5) . . . . ? N11 C34 C35 C37 126.4(4) . . . . ? O3 C34 C35 C38 168.2(4) . . . . ? N11 C34 C35 C38 -10.3(6) . . . . ? O3 C34 C35 C36 56.4(4) . . . . ? N11 C34 C35 C36 -122.1(4) . . . . ? C28 N7 C39 C40 -153.5(2) . . . . ? C27 N7 C39 C40 79.7(3) . . . . ? Fe2 N7 C39 C40 -37.2(2) . . . . ? C44 N9 C40 C41 3.1(4) . . . . ? Fe2 N9 C40 C41 -171.03(19) . . . . ? C44 N9 C40 C39 -178.6(2) . . . . ? Fe2 N9 C40 C39 7.3(3) . . . . ? N7 C39 C40 N9 20.9(3) . . . . ? N7 C39 C40 C41 -160.8(2) . . . . ? N9 C40 C41 C42 0.4(4) . . . . ? C39 C40 C41 C42 -177.8(2) . . . . ? C40 C41 C42 C43 -2.5(4) . . . . ? C41 C42 C43 C44 1.1(4) . . . . ? C40 N9 C44 C43 -4.6(3) . . . . ? Fe2 N9 C44 C43 168.81(18) . . . . ? C40 N9 C44 N12 174.2(2) . . . . ? Fe2 N9 C44 N12 -12.4(3) . . . . ? C42 C43 C44 N9 2.6(4) . . . . ? C42 C43 C44 N12 -176.2(2) . . . . ? C45 N12 C44 N9 -28.2(4) . . . . ? C45 N12 C44 C43 150.7(2) . . . . ? Fe2 O4 C45 N12 36.2(3) . . . . ? Fe2 O4 C45 C46 -146.34(17) . . . . ? C44 N12 C45 O4 15.0(4) . . . . ? C44 N12 C45 C46 -162.5(2) . . . . ? O4 C45 C46 C48 55.1(3) . . . . ? N12 C45 C46 C48 -127.4(2) . . . . ? O4 C45 C46 C49 176.9(2) . . . . ? N12 C45 C46 C49 -5.6(3) . . . . ? O4 C45 C46 C47 -62.2(3) . . . . ? N12 C45 C46 C47 115.3(2) . . . . ? F2 C50 S1 O6 58.4(2) . . . . ? F1 C50 S1 O6 -60.8(2) . . . . ? F3 C50 S1 O6 178.9(2) . . . . ? F2 C50 S1 O5 179.04(19) . . . . ? F1 C50 S1 O5 59.8(2) . . . . ? F3 C50 S1 O5 -60.4(2) . . . . ? F2 C50 S1 O7 -62.3(2) . . . . ? F1 C50 S1 O7 178.50(19) . . . . ? F3 C50 S1 O7 58.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.811 _refine_diff_density_min -1.660 _refine_diff_density_rms 0.075 #===END data_asb119 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H89 B Cl2 Co2 N12 O5' _chemical_formula_weight 1438.15 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5951(6) _cell_length_b 14.1855(7) _cell_length_c 21.3797(11) _cell_angle_alpha 98.6178(6) _cell_angle_beta 95.1664(6) _cell_angle_gamma 105.5654(6) _cell_volume 3604.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 148(2) _cell_measurement_reflns_used 9943 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 28.07 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8191 _exptl_absorpt_correction_T_max 0.9430 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 148(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41320 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0290 _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 -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16092 _reflns_number_gt 13339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+3.8460P] 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 16092 _refine_ls_number_parameters 886 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.12361(2) 0.56190(2) 0.313917(13) 0.01663(8) Uani 1 1 d . . . Co2 Co 0.25896(2) 0.30623(2) 0.245693(13) 0.01554(8) Uani 1 1 d . . . O1 O 0.05771(13) 0.51276(11) 0.22454(7) 0.0196(3) Uani 1 1 d . . . O2 O 0.15240(19) 0.86394(14) 0.17352(10) 0.0463(6) Uani 1 1 d . . . O3 O 0.32012(13) 0.40972(11) 0.19673(7) 0.0185(3) Uani 1 1 d . . . O4 O 0.22037(16) 0.14424(14) -0.00466(8) 0.0337(4) Uani 1 1 d . . . N1 N 0.16510(17) 0.62637(14) 0.41490(9) 0.0218(4) Uani 1 1 d . . . N2 N -0.02373(16) 0.57935(14) 0.33664(9) 0.0211(4) Uani 1 1 d . . . N3 N 0.22497(15) 0.70945(13) 0.31505(9) 0.0185(4) Uani 1 1 d . . . N4 N 0.18209(16) 0.45536(13) 0.34919(9) 0.0185(4) Uani 1 1 d . . . N5 N -0.12839(16) 0.46786(14) 0.24226(9) 0.0223(4) Uani 1 1 d . . . N6 N 0.14828(16) 0.72442(14) 0.21554(9) 0.0219(4) Uani 1 1 d . . . H6A H 0.1172 0.6597 0.2094 0.026 Uiso 1 1 calc R . . N7 N 0.22300(16) 0.18245(13) 0.29652(9) 0.0198(4) Uani 1 1 d . . . N8 N 0.40682(15) 0.27591(13) 0.25518(9) 0.0192(4) Uani 1 1 d . . . N9 N 0.15113(15) 0.18806(13) 0.17744(9) 0.0189(4) Uani 1 1 d . . . N10 N 0.20618(15) 0.36776(13) 0.32600(9) 0.0183(4) Uani 1 1 d . . . N11 N 0.50766(16) 0.43508(14) 0.23491(9) 0.0218(4) Uani 1 1 d . . . N12 N 0.22124(17) 0.24468(14) 0.08885(9) 0.0222(4) Uani 1 1 d . . . H12A H 0.2486 0.3054 0.1111 0.027 Uiso 1 1 calc R . . C1 C 0.0908(2) 0.68836(17) 0.43119(11) 0.0261(5) Uani 1 1 d . . . H1A H 0.1245 0.7568 0.4241 0.031 Uiso 1 1 calc R . . H1B H 0.0813 0.6918 0.4769 0.031 Uiso 1 1 calc R . . C2 C -0.0214(2) 0.64469(16) 0.39037(11) 0.0239(5) Uani 1 1 d . . . C3 C -0.1139(2) 0.67332(19) 0.40485(13) 0.0324(6) Uani 1 1 d . . . H3B H -0.1104 0.7201 0.4423 0.039 Uiso 1 1 calc R . . C4 C -0.2127(2) 0.6319(2) 0.36307(15) 0.0379(6) Uani 1 1 d . . . H4A H -0.2776 0.6506 0.3719 0.045 Uiso 1 1 calc R . . C5 C -0.2167(2) 0.5641(2) 0.30912(13) 0.0314(5) Uani 1 1 d . . . H5A H -0.2845 0.5348 0.2811 0.038 Uiso 1 1 calc R . . C6 C -0.11966(19) 0.53857(17) 0.29581(11) 0.0230(5) Uani 1 1 d . . . C7 C -0.04527(18) 0.45721(15) 0.21287(10) 0.0192(4) Uani 1 1 d . . . C8 C -0.0722(2) 0.36642(17) 0.15858(12) 0.0246(5) Uani 1 1 d . . . C9 C -0.1766(3) 0.3606(3) 0.11391(15) 0.0466(8) Uani 1 1 d . . . H9A H -0.1630 0.4191 0.0932 0.070 Uiso 1 1 calc R . . H9B H -0.2388 0.3588 0.1386 0.070 Uiso 1 1 calc R . . H9C H -0.1950 0.3002 0.0813 0.070 Uiso 1 1 calc R . . C10 C -0.0927(3) 0.27595(19) 0.19169(15) 0.0409(7) Uani 1 1 d . . . H10B H -0.0266 0.2818 0.2216 0.061 Uiso 1 1 calc R . . H10C H -0.1079 0.2152 0.1596 0.061 Uiso 1 1 calc R . . H10D H -0.1567 0.2729 0.2150 0.061 Uiso 1 1 calc R . . C11 C 0.0247(2) 0.36842(18) 0.12014(12) 0.0291(5) Uani 1 1 d . . . H11A H 0.0356 0.4243 0.0971 0.044 Uiso 1 1 calc R . . H11B H 0.0080 0.3059 0.0895 0.044 Uiso 1 1 calc R . . H11C H 0.0926 0.3763 0.1492 0.044 Uiso 1 1 calc R . . C12 C 0.2823(2) 0.68523(17) 0.42166(11) 0.0235(5) Uani 1 1 d . . . H12B H 0.3305 0.6405 0.4170 0.028 Uiso 1 1 calc R . . H12C H 0.3046 0.7281 0.4644 0.028 Uiso 1 1 calc R . . C13 C 0.29495(19) 0.74848(16) 0.37054(10) 0.0196(4) Uani 1 1 d . . . C14 C 0.37136(19) 0.84100(16) 0.38093(11) 0.0215(4) Uani 1 1 d . . . H14A H 0.4192 0.8665 0.4203 0.026 Uiso 1 1 calc R . . C15 C 0.37654(19) 0.89605(16) 0.33215(12) 0.0231(5) Uani 1 1 d . . . H15A H 0.4303 0.9591 0.3374 0.028 Uiso 1 1 calc R . . C16 C 0.3043(2) 0.85983(17) 0.27629(11) 0.0234(5) Uani 1 1 d . . . H16A H 0.3066 0.8977 0.2431 0.028 Uiso 1 1 calc R . . C17 C 0.22718(18) 0.76590(16) 0.26938(10) 0.0188(4) Uani 1 1 d . . . C18 C 0.1140(2) 0.77505(18) 0.17075(12) 0.0290(5) Uani 1 1 d . . . C19 C 0.0212(3) 0.7103(2) 0.11834(13) 0.0386(7) Uani 1 1 d . . . C20 C -0.0023(3) 0.7742(2) 0.06982(15) 0.0517(9) Uani 1 1 d . . . H20A H 0.0654 0.8005 0.0512 0.078 Uiso 1 1 calc R . . H20B H -0.0260 0.8296 0.0914 0.078 Uiso 1 1 calc R . . H20C H -0.0613 0.7334 0.0359 0.078 Uiso 1 1 calc R . . C21 C -0.0840(3) 0.6719(3) 0.14912(18) 0.0586(10) Uani 1 1 d . . . H21A H -0.0685 0.6322 0.1807 0.088 Uiso 1 1 calc R . . H21B H -0.1443 0.6305 0.1161 0.088 Uiso 1 1 calc R . . H21C H -0.1062 0.7285 0.1702 0.088 Uiso 1 1 calc R . . C22 C 0.0573(4) 0.6247(2) 0.08402(15) 0.0584(10) Uani 1 1 d . . . H22A H 0.1246 0.6511 0.0651 0.088 Uiso 1 1 calc R . . H22B H -0.0023 0.5842 0.0502 0.088 Uiso 1 1 calc R . . H22C H 0.0727 0.5834 0.1146 0.088 Uiso 1 1 calc R . . C23 C 0.1482(2) 0.54263(17) 0.44993(11) 0.0260(5) Uani 1 1 d . . . H23A H 0.0692 0.5201 0.4566 0.031 Uiso 1 1 calc R . . H23B H 0.1944 0.5645 0.4923 0.031 Uiso 1 1 calc R . . C24 C 0.1797(2) 0.45889(17) 0.41257(10) 0.0223(5) Uani 1 1 d . . . C25 C 0.2007(2) 0.37583(17) 0.43136(11) 0.0252(5) Uani 1 1 d . . . H25A H 0.2037 0.3600 0.4730 0.030 Uiso 1 1 calc R . . C26 C 0.21635(19) 0.32130(16) 0.37570(11) 0.0215(4) Uani 1 1 d . . . C27 C 0.2472(2) 0.22560(17) 0.36509(11) 0.0238(5) Uani 1 1 d . . . H27A H 0.3273 0.2383 0.3801 0.029 Uiso 1 1 calc R . . H27B H 0.2040 0.1784 0.3896 0.029 Uiso 1 1 calc R . . C28 C 0.29568(19) 0.11998(16) 0.27799(12) 0.0228(5) Uani 1 1 d . . . H28A H 0.2592 0.0709 0.2389 0.027 Uiso 1 1 calc R . . H28B H 0.3078 0.0830 0.3125 0.027 Uiso 1 1 calc R . . C29 C 0.40651(19) 0.18385(16) 0.26587(11) 0.0202(4) Uani 1 1 d . . . C30 C 0.4990(2) 0.15062(17) 0.26321(12) 0.0251(5) Uani 1 1 d . . . H30A H 0.4970 0.0859 0.2707 0.030 Uiso 1 1 calc R . . C31 C 0.5960(2) 0.21372(18) 0.24931(12) 0.0275(5) Uani 1 1 d . . . H31A H 0.6606 0.1918 0.2466 0.033 Uiso 1 1 calc R . . C32 C 0.59808(19) 0.30778(17) 0.23946(12) 0.0239(5) Uani 1 1 d . . . H32A H 0.6644 0.3516 0.2308 0.029 Uiso 1 1 calc R . . C33 C 0.50124(18) 0.33842(16) 0.24238(11) 0.0198(4) Uani 1 1 d . . . C34 C 0.42273(18) 0.46391(15) 0.21532(10) 0.0185(4) Uani 1 1 d . . . C35 C 0.44582(19) 0.57598(16) 0.21552(11) 0.0225(5) Uani 1 1 d . . . C36 C 0.4605(3) 0.62491(18) 0.28585(13) 0.0343(6) Uani 1 1 d . . . H36A H 0.4722 0.6967 0.2890 0.051 Uiso 1 1 calc R . . H36B H 0.5250 0.6129 0.3090 0.051 Uiso 1 1 calc R . . H36C H 0.3936 0.5964 0.3046 0.051 Uiso 1 1 calc R . . C37 C 0.3489(2) 0.59907(18) 0.17929(14) 0.0318(6) Uani 1 1 d . . . H37A H 0.3409 0.5700 0.1339 0.048 Uiso 1 1 calc R . . H37B H 0.3630 0.6713 0.1840 0.048 Uiso 1 1 calc R . . H37C H 0.2802 0.5707 0.1966 0.048 Uiso 1 1 calc R . . C38 C 0.5524(2) 0.6153(2) 0.18719(16) 0.0383(7) Uani 1 1 d . . . H38A H 0.5451 0.5795 0.1434 0.058 Uiso 1 1 calc R . . H38B H 0.6152 0.6051 0.2130 0.058 Uiso 1 1 calc R . . H38C H 0.5653 0.6865 0.1869 0.058 Uiso 1 1 calc R . . C39 C 0.10447(19) 0.13118(16) 0.27563(11) 0.0224(5) Uani 1 1 d . . . H39A H 0.0584 0.1707 0.2957 0.027 Uiso 1 1 calc R . . H39B H 0.0849 0.0653 0.2887 0.027 Uiso 1 1 calc R . . C40 C 0.08240(18) 0.11872(16) 0.20399(11) 0.0206(4) Uani 1 1 d . . . C41 C -0.00230(19) 0.04136(17) 0.16798(12) 0.0248(5) Uani 1 1 d . . . H41A H -0.0477 -0.0075 0.1877 0.030 Uiso 1 1 calc R . . C42 C -0.0196(2) 0.03657(17) 0.10245(12) 0.0268(5) Uani 1 1 d . . . H42A H -0.0809 -0.0128 0.0770 0.032 Uiso 1 1 calc R . . C43 C 0.0526(2) 0.10372(17) 0.07428(12) 0.0252(5) Uani 1 1 d . . . H43A H 0.0430 0.1002 0.0293 0.030 Uiso 1 1 calc R . . C44 C 0.14031(19) 0.17726(16) 0.11342(11) 0.0200(4) Uani 1 1 d . . . C45 C 0.2611(2) 0.22261(18) 0.03220(11) 0.0260(5) Uani 1 1 d . . . C46 C 0.3610(2) 0.3031(2) 0.01919(12) 0.0333(6) Uani 1 1 d . . . C47 C 0.3869(3) 0.2713(3) -0.04748(15) 0.0620(11) Uani 1 1 d . . . H47A H 0.3207 0.2599 -0.0786 0.093 Uiso 1 1 calc R . . H47B H 0.4089 0.2099 -0.0493 0.093 Uiso 1 1 calc R . . H47C H 0.4479 0.3239 -0.0575 0.093 Uiso 1 1 calc R . . C48 C 0.3339(3) 0.4026(2) 0.02406(16) 0.0476(8) Uani 1 1 d . . . H48A H 0.2698 0.3959 -0.0076 0.071 Uiso 1 1 calc R . . H48B H 0.3983 0.4537 0.0160 0.071 Uiso 1 1 calc R . . H48C H 0.3162 0.4219 0.0670 0.071 Uiso 1 1 calc R . . C49 C 0.4619(2) 0.3136(3) 0.06835(15) 0.0448(7) Uani 1 1 d . . . H49A H 0.4772 0.2491 0.0664 0.067 Uiso 1 1 calc R . . H49B H 0.4461 0.3359 0.1112 0.067 Uiso 1 1 calc R . . H49C H 0.5269 0.3624 0.0588 0.067 Uiso 1 1 calc R . . B1 B 0.2287(2) 0.98666(18) 0.63301(12) 0.0199(5) Uani 1 1 d . . . C50 C 0.29953(18) 1.05162(16) 0.58486(11) 0.0198(4) Uani 1 1 d . . . C51 C 0.32921(19) 1.01168(17) 0.52724(11) 0.0218(4) Uani 1 1 d . . . H51A H 0.3107 0.9414 0.5152 0.026 Uiso 1 1 calc R . . C52 C 0.3846(2) 1.07034(17) 0.48682(11) 0.0236(5) Uani 1 1 d . . . H52A H 0.4035 1.0396 0.4484 0.028 Uiso 1 1 calc R . . C53 C 0.41247(19) 1.17331(17) 0.50219(11) 0.0234(5) Uani 1 1 d . . . H53A H 0.4504 1.2136 0.4748 0.028 Uiso 1 1 calc R . . C54 C 0.3837(2) 1.21615(17) 0.55850(12) 0.0273(5) Uani 1 1 d . . . H54A H 0.4020 1.2865 0.5699 0.033 Uiso 1 1 calc R . . C55 C 0.3285(2) 1.15661(17) 0.59824(12) 0.0265(5) Uani 1 1 d . . . H55A H 0.3093 1.1880 0.6363 0.032 Uiso 1 1 calc R . . C56 C 0.29054(19) 1.01634(15) 0.70754(11) 0.0198(4) Uani 1 1 d . . . C57 C 0.23955(19) 0.96615(17) 0.75401(11) 0.0237(5) Uani 1 1 d . . . H57A H 0.1687 0.9186 0.7415 0.028 Uiso 1 1 calc R . . C58 C 0.2878(2) 0.98298(18) 0.81689(12) 0.0274(5) Uani 1 1 d . . . H58A H 0.2497 0.9477 0.8465 0.033 Uiso 1 1 calc R . . C59 C 0.3921(2) 1.05148(18) 0.83699(12) 0.0281(5) Uani 1 1 d . . . H59A H 0.4264 1.0626 0.8799 0.034 Uiso 1 1 calc R . . C60 C 0.4443(2) 1.10267(18) 0.79306(13) 0.0295(5) Uani 1 1 d . . . H60A H 0.5154 1.1498 0.8059 0.035 Uiso 1 1 calc R . . C61 C 0.3938(2) 1.08588(17) 0.72991(12) 0.0249(5) Uani 1 1 d . . . H61A H 0.4312 1.1233 0.7010 0.030 Uiso 1 1 calc R . . C62 C 0.2153(2) 0.86657(16) 0.61493(11) 0.0214(4) Uani 1 1 d . . . C63 C 0.3077(2) 0.83205(17) 0.60496(11) 0.0245(5) Uani 1 1 d . . . H63A H 0.3751 0.8785 0.6001 0.029 Uiso 1 1 calc R . . C64 C 0.3052(2) 0.73258(19) 0.60188(12) 0.0307(5) Uani 1 1 d . . . H64A H 0.3696 0.7124 0.5942 0.037 Uiso 1 1 calc R . . C65 C 0.2088(3) 0.66303(18) 0.61003(12) 0.0340(6) Uani 1 1 d . . . H65A H 0.2074 0.5957 0.6098 0.041 Uiso 1 1 calc R . . C66 C 0.1148(3) 0.69362(18) 0.61853(12) 0.0335(6) Uani 1 1 d . . . H66A H 0.0478 0.6468 0.6236 0.040 Uiso 1 1 calc R . . C67 C 0.1178(2) 0.79274(18) 0.61965(12) 0.0280(5) Uani 1 1 d . . . H67A H 0.0513 0.8112 0.6238 0.034 Uiso 1 1 calc R . . C68 C 0.10886(19) 1.01234(17) 0.62989(11) 0.0225(5) Uani 1 1 d . . . C69 C 0.0238(2) 0.96779(19) 0.57856(12) 0.0275(5) Uani 1 1 d . . . H69A H 0.0349 0.9190 0.5462 0.033 Uiso 1 1 calc R . . C70 C -0.0766(2) 0.9923(2) 0.57314(13) 0.0324(6) Uani 1 1 d . . . H70A H -0.1325 0.9601 0.5378 0.039 Uiso 1 1 calc R . . C71 C -0.0944(2) 1.0637(2) 0.61936(14) 0.0345(6) Uani 1 1 d . . . H71A H -0.1627 1.0802 0.6163 0.041 Uiso 1 1 calc R . . C72 C -0.0115(2) 1.11107(19) 0.67029(14) 0.0324(6) Uani 1 1 d . . . H72A H -0.0224 1.1611 0.7018 0.039 Uiso 1 1 calc R . . C73 C 0.0880(2) 1.08521(17) 0.67527(12) 0.0261(5) Uani 1 1 d . . . H73A H 0.1436 1.1181 0.7106 0.031 Uiso 1 1 calc R . . C74 C 0.2763(4) -0.0350(3) 0.0578(2) 0.0682(11) Uiso 1 1 d . . . H74A H 0.2647 -0.0058 0.0194 0.082 Uiso 0.75 1 calc PR A 1 H74B H 0.2043 -0.0540 0.0746 0.082 Uiso 0.75 1 calc PR A 1 H74C H 0.2349 -0.0028 0.0326 0.082 Uiso 0.25 1 d PR A 2 H74D H 0.2252 -0.0794 0.0784 0.082 Uiso 0.25 1 d PR A 2 Cl1 Cl 0.37160(9) 0.05264(7) 0.11444(5) 0.0656(3) Uani 1 1 d . B . Cl2A Cl 0.3194(2) -0.14320(16) 0.03572(14) 0.1236(9) Uani 0.75 1 d P B 1 Cl2B Cl 0.3605(7) -0.0977(5) -0.0013(4) 0.1236(9) Uani 0.25 1 d P B 2 O5 O 0.5112(2) 0.4698(2) 0.41209(15) 0.0714(8) Uani 1 1 d . . . H5 H 0.5714 0.4879 0.3972 0.107 Uiso 1 1 calc R . . C75 C 0.5310(3) 0.4471(2) 0.46908(17) 0.0525(9) Uani 1 1 d . . . H75A H 0.6108 0.4726 0.4846 0.079 Uiso 1 1 calc R . . H75B H 0.5072 0.3746 0.4658 0.079 Uiso 1 1 calc R . . H75C H 0.4896 0.4772 0.4990 0.079 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 0.01976(15) 0.01424(14) 0.01532(14) 0.00199(10) 0.00290(11) 0.00414(11) Co2 0.01750(15) 0.01259(14) 0.01670(14) 0.00384(10) 0.00241(11) 0.00392(11) O1 0.0209(8) 0.0185(7) 0.0174(7) 0.0020(6) 0.0017(6) 0.0032(6) O2 0.0619(14) 0.0230(9) 0.0470(12) 0.0136(9) -0.0176(10) 0.0047(9) O3 0.0203(8) 0.0151(7) 0.0193(7) 0.0048(6) 0.0020(6) 0.0028(6) O4 0.0370(10) 0.0307(9) 0.0251(9) -0.0071(7) 0.0039(8) 0.0024(8) N1 0.0298(10) 0.0165(9) 0.0187(9) 0.0026(7) 0.0057(8) 0.0054(8) N2 0.0243(10) 0.0171(9) 0.0226(9) 0.0034(7) 0.0080(8) 0.0059(7) N3 0.0204(9) 0.0153(8) 0.0187(9) 0.0014(7) 0.0017(7) 0.0047(7) N4 0.0232(9) 0.0144(8) 0.0173(9) 0.0023(7) 0.0039(7) 0.0043(7) N5 0.0219(10) 0.0194(9) 0.0252(10) 0.0021(8) 0.0027(8) 0.0064(7) N6 0.0279(10) 0.0150(8) 0.0217(9) 0.0034(7) -0.0007(8) 0.0054(7) N7 0.0226(9) 0.0159(8) 0.0217(9) 0.0051(7) 0.0033(7) 0.0057(7) N8 0.0198(9) 0.0155(8) 0.0224(9) 0.0044(7) 0.0014(7) 0.0051(7) N9 0.0199(9) 0.0132(8) 0.0234(9) 0.0027(7) 0.0033(7) 0.0044(7) N10 0.0221(9) 0.0141(8) 0.0188(9) 0.0042(7) 0.0023(7) 0.0047(7) N11 0.0206(9) 0.0167(9) 0.0277(10) 0.0049(7) 0.0039(8) 0.0040(7) N12 0.0280(10) 0.0163(9) 0.0191(9) 0.0010(7) 0.0033(8) 0.0024(8) C1 0.0372(13) 0.0186(11) 0.0227(11) 0.0004(9) 0.0113(10) 0.0078(10) C2 0.0325(13) 0.0173(10) 0.0232(11) 0.0049(9) 0.0105(9) 0.0066(9) C3 0.0418(15) 0.0265(12) 0.0326(13) 0.0010(10) 0.0162(11) 0.0146(11) C4 0.0364(15) 0.0384(15) 0.0465(16) 0.0057(13) 0.0156(13) 0.0213(12) C5 0.0255(12) 0.0308(13) 0.0397(15) 0.0042(11) 0.0058(11) 0.0122(10) C6 0.0235(11) 0.0202(11) 0.0272(12) 0.0067(9) 0.0068(9) 0.0070(9) C7 0.0226(11) 0.0150(10) 0.0198(10) 0.0039(8) -0.0013(8) 0.0059(8) C8 0.0236(11) 0.0198(11) 0.0265(12) -0.0029(9) 0.0009(9) 0.0044(9) C9 0.0355(16) 0.0555(19) 0.0384(16) -0.0188(14) -0.0117(13) 0.0157(14) C10 0.0530(18) 0.0172(12) 0.0524(18) 0.0043(11) 0.0215(14) 0.0063(12) C11 0.0358(14) 0.0227(11) 0.0271(12) -0.0025(9) 0.0063(10) 0.0088(10) C12 0.0287(12) 0.0194(10) 0.0188(11) 0.0011(8) -0.0018(9) 0.0037(9) C13 0.0230(11) 0.0174(10) 0.0191(10) 0.0016(8) 0.0021(8) 0.0081(8) C14 0.0208(11) 0.0178(10) 0.0239(11) -0.0011(8) 0.0007(9) 0.0056(8) C15 0.0216(11) 0.0150(10) 0.0314(12) 0.0017(9) 0.0046(9) 0.0039(8) C16 0.0275(12) 0.0187(10) 0.0265(12) 0.0069(9) 0.0072(9) 0.0082(9) C17 0.0213(11) 0.0167(10) 0.0199(10) 0.0025(8) 0.0044(8) 0.0081(8) C18 0.0388(14) 0.0220(11) 0.0261(12) 0.0073(9) -0.0019(10) 0.0092(10) C19 0.0538(18) 0.0271(13) 0.0303(14) 0.0090(11) -0.0137(12) 0.0079(12) C20 0.072(2) 0.0350(15) 0.0416(17) 0.0135(13) -0.0232(16) 0.0118(15) C21 0.0443(19) 0.060(2) 0.064(2) 0.0278(18) -0.0209(16) 0.0014(16) C22 0.101(3) 0.0343(16) 0.0335(16) -0.0020(13) -0.0215(17) 0.0226(18) C23 0.0411(14) 0.0187(11) 0.0173(11) 0.0038(8) 0.0075(10) 0.0056(10) C24 0.0285(12) 0.0192(10) 0.0162(10) 0.0021(8) 0.0036(9) 0.0024(9) C25 0.0336(13) 0.0231(11) 0.0179(11) 0.0071(9) 0.0034(9) 0.0045(10) C26 0.0253(11) 0.0194(10) 0.0191(10) 0.0068(8) 0.0028(9) 0.0036(9) C27 0.0330(13) 0.0202(11) 0.0205(11) 0.0086(9) 0.0041(9) 0.0084(9) C28 0.0258(12) 0.0157(10) 0.0289(12) 0.0069(9) 0.0030(9) 0.0077(9) C29 0.0247(11) 0.0155(10) 0.0207(10) 0.0037(8) 0.0013(9) 0.0067(8) C30 0.0296(12) 0.0197(11) 0.0286(12) 0.0061(9) 0.0021(10) 0.0113(9) C31 0.0239(12) 0.0278(12) 0.0338(13) 0.0054(10) 0.0026(10) 0.0132(10) C32 0.0199(11) 0.0224(11) 0.0293(12) 0.0038(9) 0.0029(9) 0.0063(9) C33 0.0211(11) 0.0165(10) 0.0205(10) 0.0020(8) 0.0001(8) 0.0047(8) C34 0.0228(11) 0.0146(10) 0.0173(10) 0.0022(8) 0.0059(8) 0.0037(8) C35 0.0241(11) 0.0144(10) 0.0291(12) 0.0054(9) 0.0066(9) 0.0038(8) C36 0.0465(16) 0.0190(11) 0.0329(14) -0.0033(10) 0.0013(12) 0.0073(11) C37 0.0348(14) 0.0177(11) 0.0438(15) 0.0085(10) -0.0005(11) 0.0091(10) C38 0.0357(15) 0.0251(13) 0.0633(19) 0.0243(13) 0.0237(14) 0.0096(11) C39 0.0232(11) 0.0175(10) 0.0267(12) 0.0076(9) 0.0068(9) 0.0028(9) C40 0.0196(10) 0.0156(10) 0.0276(12) 0.0048(8) 0.0053(9) 0.0058(8) C41 0.0222(11) 0.0173(10) 0.0333(13) 0.0030(9) 0.0049(9) 0.0033(9) C42 0.0217(11) 0.0182(11) 0.0353(13) -0.0038(9) 0.0005(10) 0.0025(9) C43 0.0271(12) 0.0213(11) 0.0250(12) -0.0010(9) 0.0003(9) 0.0072(9) C44 0.0220(11) 0.0163(10) 0.0213(11) 0.0020(8) 0.0025(8) 0.0058(8) C45 0.0310(13) 0.0253(12) 0.0201(11) 0.0030(9) 0.0016(9) 0.0066(10) C46 0.0405(15) 0.0329(13) 0.0208(12) 0.0033(10) 0.0088(11) 0.0006(11) C47 0.076(3) 0.062(2) 0.0304(16) -0.0017(15) 0.0273(16) -0.0111(19) C48 0.057(2) 0.0299(14) 0.0506(18) 0.0148(13) 0.0091(15) -0.0013(13) C49 0.0315(15) 0.0579(19) 0.0412(16) 0.0109(14) 0.0113(12) 0.0034(13) B1 0.0200(12) 0.0159(11) 0.0244(12) 0.0040(9) 0.0059(10) 0.0050(9) C50 0.0181(10) 0.0192(10) 0.0244(11) 0.0068(8) 0.0044(8) 0.0072(8) C51 0.0233(11) 0.0173(10) 0.0236(11) 0.0027(8) 0.0001(9) 0.0049(8) C52 0.0262(12) 0.0253(11) 0.0185(11) 0.0018(9) 0.0037(9) 0.0072(9) C53 0.0234(11) 0.0247(11) 0.0243(11) 0.0109(9) 0.0047(9) 0.0067(9) C54 0.0333(13) 0.0173(11) 0.0341(13) 0.0073(9) 0.0098(10) 0.0090(9) C55 0.0341(13) 0.0202(11) 0.0298(12) 0.0052(9) 0.0143(10) 0.0119(10) C56 0.0225(11) 0.0143(10) 0.0248(11) 0.0024(8) 0.0062(9) 0.0087(8) C57 0.0210(11) 0.0208(11) 0.0275(12) 0.0035(9) 0.0037(9) 0.0033(9) C58 0.0313(13) 0.0261(12) 0.0264(12) 0.0064(10) 0.0067(10) 0.0093(10) C59 0.0321(13) 0.0262(12) 0.0258(12) -0.0001(10) 0.0004(10) 0.0118(10) C60 0.0249(12) 0.0209(11) 0.0372(14) -0.0016(10) 0.0017(10) 0.0020(9) C61 0.0238(12) 0.0189(11) 0.0314(13) 0.0033(9) 0.0064(9) 0.0048(9) C62 0.0272(12) 0.0181(10) 0.0183(10) 0.0033(8) 0.0043(9) 0.0054(9) C63 0.0304(12) 0.0214(11) 0.0229(11) 0.0049(9) 0.0026(9) 0.0090(9) C64 0.0496(16) 0.0259(12) 0.0210(11) 0.0034(9) 0.0049(11) 0.0189(11) C65 0.0642(19) 0.0167(11) 0.0195(11) 0.0020(9) 0.0032(12) 0.0106(11) C66 0.0489(16) 0.0204(11) 0.0239(12) 0.0028(9) 0.0073(11) -0.0022(11) C67 0.0343(13) 0.0225(11) 0.0238(12) 0.0031(9) 0.0070(10) 0.0019(10) C68 0.0211(11) 0.0235(11) 0.0266(12) 0.0122(9) 0.0079(9) 0.0073(9) C69 0.0254(12) 0.0336(13) 0.0268(12) 0.0130(10) 0.0069(10) 0.0090(10) C70 0.0232(12) 0.0421(15) 0.0357(14) 0.0232(12) 0.0040(10) 0.0067(11) C71 0.0239(12) 0.0404(15) 0.0523(17) 0.0287(13) 0.0147(12) 0.0170(11) C72 0.0310(13) 0.0285(13) 0.0480(16) 0.0165(12) 0.0172(12) 0.0168(11) C73 0.0255(12) 0.0218(11) 0.0348(13) 0.0103(10) 0.0096(10) 0.0085(9) Cl1 0.0702(6) 0.0553(5) 0.0636(6) -0.0067(4) -0.0112(5) 0.0214(5) Cl2A 0.1137(17) 0.0744(13) 0.153(2) -0.0535(13) -0.0076(14) 0.0260(12) Cl2B 0.1137(17) 0.0744(13) 0.153(2) -0.0535(13) -0.0076(14) 0.0260(12) O5 0.0624(17) 0.0651(18) 0.083(2) 0.0197(15) 0.0208(15) 0.0055(14) C75 0.059(2) 0.0172(12) 0.062(2) -0.0035(13) -0.0351(17) -0.0015(12) _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 O1 1.9573(15) . ? Co1 N2 2.0283(19) . ? Co1 N4 2.0577(18) . ? Co1 N3 2.1346(18) . ? Co1 N1 2.1725(19) . ? Co2 O3 1.9605(15) . ? Co2 N8 2.0205(19) . ? Co2 N10 2.0541(18) . ? Co2 N9 2.1147(18) . ? Co2 N7 2.1686(18) . ? O1 C7 1.304(3) . ? O2 C18 1.213(3) . ? O3 C34 1.305(3) . ? O4 C45 1.216(3) . ? N1 C12 1.470(3) . ? N1 C23 1.475(3) . ? N1 C1 1.476(3) . ? N2 C2 1.356(3) . ? N2 C6 1.356(3) . ? N3 C17 1.350(3) . ? N3 C13 1.358(3) . ? N4 C24 1.352(3) . ? N4 N10 1.388(2) . ? N5 C7 1.299(3) . ? N5 C6 1.380(3) . ? N6 C18 1.385(3) . ? N6 C17 1.391(3) . ? N7 C39 1.469(3) . ? N7 C27 1.472(3) . ? N7 C28 1.475(3) . ? N8 C33 1.357(3) . ? N8 C29 1.358(3) . ? N9 C44 1.345(3) . ? N9 C40 1.356(3) . ? N10 C26 1.346(3) . ? N11 C34 1.301(3) . ? N11 C33 1.386(3) . ? N12 C45 1.377(3) . ? N12 C44 1.398(3) . ? C1 C2 1.512(4) . ? C2 C3 1.378(3) . ? C3 C4 1.394(4) . ? C4 C5 1.374(4) . ? C5 C6 1.406(3) . ? C7 C8 1.539(3) . ? C8 C11 1.528(3) . ? C8 C9 1.530(4) . ? C8 C10 1.530(4) . ? C12 C13 1.508(3) . ? C13 C14 1.376(3) . ? C14 C15 1.390(3) . ? C15 C16 1.374(3) . ? C16 C17 1.400(3) . ? C18 C19 1.531(4) . ? C19 C22 1.520(5) . ? C19 C20 1.535(4) . ? C19 C21 1.537(5) . ? C23 C24 1.494(3) . ? C24 C25 1.382(3) . ? C25 C26 1.379(3) . ? C26 C27 1.500(3) . ? C28 C29 1.514(3) . ? C29 C30 1.372(3) . ? C30 C31 1.392(3) . ? C31 C32 1.375(3) . ? C32 C33 1.404(3) . ? C34 C35 1.537(3) . ? C35 C37 1.523(3) . ? C35 C38 1.525(3) . ? C35 C36 1.531(3) . ? C39 C40 1.507(3) . ? C40 C41 1.380(3) . ? C41 C42 1.387(4) . ? C42 C43 1.379(3) . ? C43 C44 1.401(3) . ? C45 C46 1.534(3) . ? C46 C47 1.520(4) . ? C46 C48 1.530(4) . ? C46 C49 1.534(4) . ? B1 C68 1.643(3) . ? B1 C50 1.647(3) . ? B1 C62 1.648(3) . ? B1 C56 1.650(3) . ? C50 C51 1.402(3) . ? C50 C55 1.412(3) . ? C51 C52 1.392(3) . ? C52 C53 1.387(3) . ? C53 C54 1.388(3) . ? C54 C55 1.387(3) . ? C56 C61 1.397(3) . ? C56 C57 1.410(3) . ? C57 C58 1.383(3) . ? C58 C59 1.394(4) . ? C59 C60 1.379(4) . ? C60 C61 1.397(4) . ? C62 C63 1.399(3) . ? C62 C67 1.407(3) . ? C63 C64 1.394(3) . ? C64 C65 1.387(4) . ? C65 C66 1.384(4) . ? C66 C67 1.393(4) . ? C68 C69 1.403(4) . ? C68 C73 1.403(3) . ? C69 C70 1.399(4) . ? C70 C71 1.383(4) . ? C71 C72 1.388(4) . ? C72 C73 1.397(3) . ? C74 Cl1 1.715(4) . ? C74 Cl2A 1.774(5) . ? C74 Cl2B 1.979(9) . ? O5 C75 1.325(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N2 90.20(7) . . ? O1 Co1 N4 109.87(7) . . ? N2 Co1 N4 118.64(7) . . ? O1 Co1 N3 104.37(7) . . ? N2 Co1 N3 104.54(7) . . ? N4 Co1 N3 123.43(7) . . ? O1 Co1 N1 167.85(7) . . ? N2 Co1 N1 77.99(8) . . ? N4 Co1 N1 78.79(7) . . ? N3 Co1 N1 76.32(7) . . ? O3 Co2 N8 90.07(7) . . ? O3 Co2 N10 109.87(7) . . ? N8 Co2 N10 118.33(7) . . ? O3 Co2 N9 104.91(7) . . ? N8 Co2 N9 106.27(7) . . ? N10 Co2 N9 122.00(7) . . ? O3 Co2 N7 167.80(7) . . ? N8 Co2 N7 78.05(7) . . ? N10 Co2 N7 78.72(7) . . ? N9 Co2 N7 76.23(7) . . ? C7 O1 Co1 117.81(14) . . ? C34 O3 Co2 117.16(13) . . ? C12 N1 C23 112.92(19) . . ? C12 N1 C1 112.55(18) . . ? C23 N1 C1 111.54(18) . . ? C12 N1 Co1 104.21(13) . . ? C23 N1 Co1 106.79(13) . . ? C1 N1 Co1 108.29(14) . . ? C2 N2 C6 120.1(2) . . ? C2 N2 Co1 117.55(16) . . ? C6 N2 Co1 121.77(15) . . ? C17 N3 C13 118.37(19) . . ? C17 N3 Co1 128.99(15) . . ? C13 N3 Co1 112.64(14) . . ? C24 N4 N10 106.72(17) . . ? C24 N4 Co1 113.63(15) . . ? N10 N4 Co1 138.42(14) . . ? C7 N5 C6 124.5(2) . . ? C18 N6 C17 126.32(19) . . ? C39 N7 C27 112.84(18) . . ? C39 N7 C28 112.83(17) . . ? C27 N7 C28 111.67(18) . . ? C39 N7 Co2 104.64(13) . . ? C27 N7 Co2 106.64(13) . . ? C28 N7 Co2 107.63(13) . . ? C33 N8 C29 119.82(19) . . ? C33 N8 Co2 121.97(14) . . ? C29 N8 Co2 117.55(15) . . ? C44 N9 C40 118.44(19) . . ? C44 N9 Co2 128.22(15) . . ? C40 N9 Co2 113.25(15) . . ? C26 N10 N4 107.22(18) . . ? C26 N10 Co2 113.24(15) . . ? N4 N10 Co2 138.11(14) . . ? C34 N11 C33 124.05(19) . . ? C45 N12 C44 124.45(19) . . ? N1 C1 C2 110.16(18) . . ? N2 C2 C3 122.0(2) . . ? N2 C2 C1 115.6(2) . . ? C3 C2 C1 122.3(2) . . ? C2 C3 C4 118.3(2) . . ? C5 C4 C3 120.2(2) . . ? C4 C5 C6 119.4(2) . . ? N2 C6 N5 122.5(2) . . ? N2 C6 C5 120.0(2) . . ? N5 C6 C5 117.4(2) . . ? N5 C7 O1 128.0(2) . . ? N5 C7 C8 115.5(2) . . ? O1 C7 C8 116.52(19) . . ? C11 C8 C9 109.6(2) . . ? C11 C8 C10 109.2(2) . . ? C9 C8 C10 110.0(2) . . ? C11 C8 C7 111.89(19) . . ? C9 C8 C7 110.7(2) . . ? C10 C8 C7 105.3(2) . . ? N1 C12 C13 108.31(18) . . ? N3 C13 C14 122.8(2) . . ? N3 C13 C12 115.90(19) . . ? C14 C13 C12 121.3(2) . . ? C13 C14 C15 118.1(2) . . ? C16 C15 C14 120.4(2) . . ? C15 C16 C17 118.5(2) . . ? N3 C17 N6 115.57(19) . . ? N3 C17 C16 121.7(2) . . ? N6 C17 C16 122.7(2) . . ? O2 C18 N6 122.8(2) . . ? O2 C18 C19 122.6(2) . . ? N6 C18 C19 114.6(2) . . ? C22 C19 C18 110.1(3) . . ? C22 C19 C20 108.7(3) . . ? C18 C19 C20 108.8(2) . . ? C22 C19 C21 111.1(3) . . ? C18 C19 C21 108.5(2) . . ? C20 C19 C21 109.5(3) . . ? N1 C23 C24 109.50(18) . . ? N4 C24 C25 111.0(2) . . ? N4 C24 C23 118.8(2) . . ? C25 C24 C23 130.1(2) . . ? C26 C25 C24 104.0(2) . . ? N10 C26 C25 111.1(2) . . ? N10 C26 C27 119.0(2) . . ? C25 C26 C27 129.9(2) . . ? N7 C27 C26 109.15(18) . . ? N7 C28 C29 110.37(17) . . ? N8 C29 C30 122.0(2) . . ? N8 C29 C28 114.98(19) . . ? C30 C29 C28 123.0(2) . . ? C29 C30 C31 118.7(2) . . ? C32 C31 C30 120.0(2) . . ? C31 C32 C33 119.3(2) . . ? N8 C33 N11 122.0(2) . . ? N8 C33 C32 120.2(2) . . ? N11 C33 C32 117.8(2) . . ? N11 C34 O3 128.00(19) . . ? N11 C34 C35 115.88(19) . . ? O3 C34 C35 116.11(19) . . ? C37 C35 C38 110.2(2) . . ? C37 C35 C36 109.2(2) . . ? C38 C35 C36 109.7(2) . . ? C37 C35 C34 111.63(19) . . ? C38 C35 C34 110.41(19) . . ? C36 C35 C34 105.60(19) . . ? N7 C39 C40 108.61(18) . . ? N9 C40 C41 122.4(2) . . ? N9 C40 C39 115.68(19) . . ? C41 C40 C39 121.9(2) . . ? C40 C41 C42 118.5(2) . . ? C43 C42 C41 119.8(2) . . ? C42 C43 C44 118.5(2) . . ? N9 C44 N12 115.67(19) . . ? N9 C44 C43 121.8(2) . . ? N12 C44 C43 122.5(2) . . ? O4 C45 N12 122.2(2) . . ? O4 C45 C46 122.3(2) . . ? N12 C45 C46 115.4(2) . . ? C47 C46 C48 110.1(3) . . ? C47 C46 C45 108.5(2) . . ? C48 C46 C45 109.9(2) . . ? C47 C46 C49 109.4(3) . . ? C48 C46 C49 109.6(2) . . ? C45 C46 C49 109.3(2) . . ? C68 B1 C50 105.54(18) . . ? C68 B1 C62 113.12(19) . . ? C50 B1 C62 113.14(18) . . ? C68 B1 C56 109.29(18) . . ? C50 B1 C56 113.01(18) . . ? C62 B1 C56 102.90(17) . . ? C51 C50 C55 114.6(2) . . ? C51 C50 B1 125.43(19) . . ? C55 C50 B1 119.9(2) . . ? C52 C51 C50 123.0(2) . . ? C53 C52 C51 120.5(2) . . ? C52 C53 C54 118.5(2) . . ? C55 C54 C53 120.3(2) . . ? C54 C55 C50 123.1(2) . . ? C61 C56 C57 114.9(2) . . ? C61 C56 B1 125.9(2) . . ? C57 C56 B1 119.2(2) . . ? C58 C57 C56 123.1(2) . . ? C57 C58 C59 120.3(2) . . ? C60 C59 C58 118.4(2) . . ? C59 C60 C61 120.7(2) . . ? C56 C61 C60 122.7(2) . . ? C63 C62 C67 115.0(2) . . ? C63 C62 B1 120.9(2) . . ? C67 C62 B1 123.1(2) . . ? C64 C63 C62 122.9(2) . . ? C65 C64 C63 120.2(3) . . ? C66 C65 C64 118.7(2) . . ? C65 C66 C67 120.4(2) . . ? C66 C67 C62 122.7(3) . . ? C69 C68 C73 115.7(2) . . ? C69 C68 B1 121.6(2) . . ? C73 C68 B1 122.5(2) . . ? C70 C69 C68 122.6(2) . . ? C71 C70 C69 119.8(3) . . ? C70 C71 C72 119.4(2) . . ? C71 C72 C73 120.1(3) . . ? C72 C73 C68 122.3(2) . . ? Cl1 C74 Cl2A 112.4(3) . . ? Cl1 C74 Cl2B 107.4(3) . . ? Cl2A C74 Cl2B 35.6(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.880 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.075 #===END data_asb149 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.50 H74 F3 Fe2 N12 O9.50 S' _chemical_formula_weight 1250.02 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8889(5) _cell_length_b 21.3269(9) _cell_length_c 26.8112(12) _cell_angle_alpha 93.1871(6) _cell_angle_beta 95.8320(6) _cell_angle_gamma 104.1291(6) _cell_volume 5985.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 9677 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.30 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8228 _exptl_absorpt_correction_T_max 0.9007 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 72181 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.31 _reflns_number_total 28486 _reflns_number_gt 23176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+13.4589P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'geom & difmap' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28486 _refine_ls_number_parameters 1502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1625 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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 0.14701(4) 0.749094(18) 1.609633(14) 0.01375(9) Uani 1 1 d . . . Fe2 Fe 0.16398(3) 0.714222(18) 1.453315(14) 0.01262(9) Uani 1 1 d . . . O5 O 0.04497(19) 0.79063(10) 1.56541(8) 0.0176(4) Uani 1 1 d . . . O4 O 0.03387(18) 0.63800(9) 1.49053(7) 0.0176(4) Uani 1 1 d . . . O3 O 0.00514(19) 0.74583(10) 1.44258(8) 0.0187(4) Uani 1 1 d . . . O1 O 0.3048(3) 1.01608(11) 1.61746(9) 0.0321(5) Uani 1 1 d . . . O2 O -0.34943(19) 0.74718(11) 1.64476(8) 0.0230(4) Uani 1 1 d . . . N1 N 0.2469(2) 0.70136(11) 1.66788(8) 0.0148(4) Uani 1 1 d . . . N2 N 0.2413(2) 0.82872(12) 1.66666(9) 0.0198(5) Uani 1 1 d . . . N3 N -0.0093(2) 0.69020(11) 1.64579(8) 0.0150(4) Uani 1 1 d . . . N4 N 0.2731(2) 0.71628(11) 1.57041(8) 0.0145(4) Uani 1 1 d . . . N5 N 0.2149(3) 0.90700(12) 1.61315(10) 0.0226(5) Uani 1 1 d . . . N6 N -0.1573(2) 0.74585(12) 1.61850(9) 0.0178(5) Uani 1 1 d . . . N7 N 0.3537(2) 0.70459(11) 1.42916(8) 0.0150(4) Uani 1 1 d . . . N8 N 0.2433(2) 0.80221(11) 1.41582(9) 0.0164(4) Uani 1 1 d . . . N9 N 0.1167(2) 0.63080(11) 1.39676(8) 0.0142(4) Uani 1 1 d . . . N10 N 0.2827(2) 0.70914(11) 1.51999(8) 0.0142(4) Uani 1 1 d . . . N11 N 0.0452(2) 0.82690(12) 1.38714(9) 0.0202(5) Uani 1 1 d . . . N12 N -0.0839(2) 0.57629(11) 1.42201(9) 0.0148(4) Uani 1 1 d . . . H1 H 0.030(4) 0.774(2) 1.5365(16) 0.031(11) Uiso 1 1 d . . . H5 H 0.170(3) 0.8749(18) 1.5943(14) 0.020(9) Uiso 1 1 d . . . H6 H -0.101(4) 0.7620(18) 1.6013(14) 0.024(9) Uiso 1 1 d . . . H12 H -0.152(4) 0.5474(18) 1.4118(14) 0.021(9) Uiso 1 1 d . . . C1 C 0.2621(3) 0.73931(14) 1.71651(10) 0.0194(5) Uani 1 1 d . . . H1A H 0.3324 0.7300 1.7389 0.023 Uiso 1 1 calc R . . H1C H 0.1828 0.7262 1.7326 0.023 Uiso 1 1 calc R . . C2 C 0.2908(3) 0.81088(15) 1.71040(11) 0.0247(6) Uani 1 1 d . . . C3 C 0.3605(5) 0.85501(18) 1.74874(13) 0.0445(10) Uani 1 1 d . . . H3A H 0.3965 0.8408 1.7785 0.053 Uiso 1 1 calc R . . C4 C 0.3767(6) 0.9206(2) 1.74274(15) 0.0632(16) Uani 1 1 d . . . H4A H 0.4216 0.9520 1.7690 0.076 Uiso 1 1 calc R . . C5 C 0.3273(5) 0.94009(18) 1.69852(14) 0.0498(12) Uani 1 1 d . . . H5A H 0.3378 0.9849 1.6941 0.060 Uiso 1 1 calc R . . C6 C 0.2615(3) 0.89293(15) 1.66026(12) 0.0268(7) Uani 1 1 d . . . C7 C 0.2537(3) 0.96561(14) 1.59220(11) 0.0215(6) Uani 1 1 d . . . C8 C 0.2345(3) 0.96032(14) 1.53472(11) 0.0218(6) Uani 1 1 d . . . C9 C 0.2788(4) 1.02804(16) 1.51670(13) 0.0332(8) Uani 1 1 d . . . H9A H 0.2285 1.0562 1.5298 0.050 Uiso 1 1 calc R . . H9B H 0.2670 1.0252 1.4798 0.050 Uiso 1 1 calc R . . H9C H 0.3692 1.0462 1.5289 0.050 Uiso 1 1 calc R . . C10 C 0.0947(3) 0.93120(16) 1.51334(13) 0.0285(7) Uani 1 1 d . . . H10S H 0.0415 0.9577 1.5266 0.043 Uiso 1 1 calc R . . H10T H 0.0670 0.8868 1.5232 0.043 Uiso 1 1 calc R . . H10U H 0.0864 0.9305 1.4766 0.043 Uiso 1 1 calc R . . C11 C 0.3194(3) 0.91758(17) 1.51701(12) 0.0288(7) Uani 1 1 d . . . H11A H 0.4062 0.9340 1.5342 0.043 Uiso 1 1 calc R . . H11B H 0.3211 0.9187 1.4806 0.043 Uiso 1 1 calc R . . H11C H 0.2850 0.8728 1.5249 0.043 Uiso 1 1 calc R . . C12 C 0.1595(3) 0.63691(13) 1.66869(10) 0.0173(5) Uani 1 1 d . . . H12A H 0.1874 0.6154 1.6980 0.021 Uiso 1 1 calc R . . H12C H 0.1614 0.6097 1.6378 0.021 Uiso 1 1 calc R . . C13 C 0.0257(3) 0.64335(13) 1.67189(10) 0.0160(5) Uani 1 1 d . . . C14 C -0.0559(3) 0.60292(14) 1.69971(11) 0.0189(5) Uani 1 1 d . . . H14A H -0.0271 0.5725 1.7194 0.023 Uiso 1 1 calc R . . C15 C -0.1808(3) 0.60809(14) 1.69791(11) 0.0204(6) Uani 1 1 d . . . H15A H -0.2394 0.5803 1.7160 0.024 Uiso 1 1 calc R . . C16 C -0.2200(3) 0.65336(14) 1.67007(11) 0.0190(5) Uani 1 1 d . . . H16A H -0.3062 0.6560 1.6675 0.023 Uiso 1 1 calc R . . C17 C -0.1306(3) 0.69555(13) 1.64551(10) 0.0159(5) Uani 1 1 d . . . C18 C -0.2639(3) 0.76956(14) 1.61980(10) 0.0170(5) Uani 1 1 d . . . C19 C -0.2674(3) 0.82718(14) 1.58855(11) 0.0204(6) Uani 1 1 d . . . C20 C -0.1542(3) 0.88475(15) 1.60859(13) 0.0256(6) Uani 1 1 d . . . H20A H -0.0741 0.8731 1.6042 0.038 Uiso 1 1 calc R . . H20B H -0.1574 0.8954 1.6444 0.038 Uiso 1 1 calc R . . H20C H -0.1591 0.9225 1.5899 0.038 Uiso 1 1 calc R . . C21 C -0.3931(3) 0.84608(16) 1.59360(13) 0.0273(7) Uani 1 1 d . . . H21A H -0.4650 0.8090 1.5815 0.041 Uiso 1 1 calc R . . H21B H -0.3973 0.8827 1.5735 0.041 Uiso 1 1 calc R . . H21C H -0.3973 0.8586 1.6290 0.041 Uiso 1 1 calc R . . C22 C -0.2618(3) 0.80669(15) 1.53321(11) 0.0236(6) Uani 1 1 d . . . H22A H -0.3285 0.7669 1.5225 0.035 Uiso 1 1 calc R . . H22B H -0.1781 0.7989 1.5294 0.035 Uiso 1 1 calc R . . H22C H -0.2753 0.8413 1.5123 0.035 Uiso 1 1 calc R . . C23 C 0.3710(3) 0.69682(14) 1.65168(10) 0.0174(5) Uani 1 1 d . . . H23A H 0.3960 0.6590 1.6655 0.021 Uiso 1 1 calc R . . H23B H 0.4380 0.7365 1.6645 0.021 Uiso 1 1 calc R . . C24 C 0.3586(2) 0.68947(13) 1.59542(10) 0.0152(5) Uani 1 1 d . . . C25 C 0.4251(3) 0.66351(13) 1.56157(10) 0.0167(5) Uani 1 1 d . . . H25A H 0.4904 0.6416 1.5686 0.020 Uiso 1 1 calc R . . C26 C 0.3740(2) 0.67707(13) 1.51494(10) 0.0150(5) Uani 1 1 d . . . C27 C 0.3994(3) 0.66019(14) 1.46239(10) 0.0166(5) Uani 1 1 d . . . H27A H 0.4919 0.6651 1.4614 0.020 Uiso 1 1 calc R . . H27B H 0.3540 0.6147 1.4512 0.020 Uiso 1 1 calc R . . C28 C 0.4390(3) 0.77039(13) 1.43668(10) 0.0172(5) Uani 1 1 d . . . H28A H 0.5166 0.7714 1.4201 0.021 Uiso 1 1 calc R . . H28B H 0.4654 0.7825 1.4731 0.021 Uiso 1 1 calc R . . C29 C 0.3715(3) 0.81805(14) 1.41490(10) 0.0176(5) Uani 1 1 d . . . C30 C 0.4380(3) 0.87365(15) 1.39635(11) 0.0218(6) Uani 1 1 d . . . H30A H 0.5276 0.8822 1.3957 0.026 Uiso 1 1 calc R . . C31 C 0.3698(3) 0.91704(15) 1.37848(11) 0.0248(6) Uani 1 1 d . . . H31A H 0.4130 0.9567 1.3667 0.030 Uiso 1 1 calc R . . C32 C 0.2401(3) 0.90176(15) 1.37819(11) 0.0234(6) Uani 1 1 d . . . H32A H 0.1929 0.9310 1.3662 0.028 Uiso 1 1 calc R . . C33 C 0.1762(3) 0.84266(14) 1.39562(10) 0.0187(5) Uani 1 1 d . . . C34 C -0.0277(3) 0.77915(14) 1.40723(10) 0.0181(5) Uani 1 1 d . . . C35 C -0.1677(3) 0.76055(15) 1.38377(11) 0.0211(6) Uani 1 1 d . . . C36 C -0.2499(3) 0.70980(15) 1.41217(12) 0.0243(6) Uani 1 1 d . . . H36A H -0.2478 0.7273 1.4469 0.036 Uiso 1 1 calc R . . H36B H -0.2170 0.6709 1.4121 0.036 Uiso 1 1 calc R . . H36C H -0.3380 0.6985 1.3958 0.036 Uiso 1 1 calc R . . C37 C -0.2207(3) 0.82068(18) 1.38234(16) 0.0361(8) Uani 1 1 d . . . H37A H -0.2209 0.8386 1.4168 0.054 Uiso 1 1 calc R . . H37B H -0.3080 0.8086 1.3652 0.054 Uiso 1 1 calc R . . H37C H -0.1671 0.8533 1.3641 0.054 Uiso 1 1 calc R . . C38 C -0.1704(3) 0.7311(2) 1.32966(12) 0.0340(8) Uani 1 1 d . . . H38A H -0.2588 0.7172 1.3137 0.051 Uiso 1 1 calc R . . H38B H -0.1332 0.6937 1.3306 0.051 Uiso 1 1 calc R . . H38C H -0.1210 0.7638 1.3103 0.051 Uiso 1 1 calc R . . C39 C 0.3311(3) 0.68022(14) 1.37587(10) 0.0177(5) Uani 1 1 d . . . H39A H 0.3964 0.6569 1.3685 0.021 Uiso 1 1 calc R . . H39B H 0.3404 0.7174 1.3548 0.021 Uiso 1 1 calc R . . C40 C 0.2001(3) 0.63503(13) 1.36208(10) 0.0160(5) Uani 1 1 d . . . C41 C 0.1692(3) 0.60162(14) 1.31523(11) 0.0197(6) Uani 1 1 d . . . H41A H 0.2305 0.6050 1.2921 0.024 Uiso 1 1 calc R . . C42 C 0.0458(3) 0.56277(14) 1.30271(11) 0.0214(6) Uani 1 1 d . . . H42A H 0.0202 0.5413 1.2699 0.026 Uiso 1 1 calc R . . C43 C -0.0391(3) 0.55561(14) 1.33811(11) 0.0195(5) Uani 1 1 d . . . H43A H -0.1230 0.5285 1.3305 0.023 Uiso 1 1 calc R . . C44 C 0.0012(3) 0.58911(13) 1.38529(10) 0.0153(5) Uani 1 1 d . . . C45 C -0.0608(3) 0.59629(13) 1.47216(10) 0.0149(5) Uani 1 1 d . . . C46 C -0.1604(3) 0.56514(13) 1.50640(10) 0.0163(5) Uani 1 1 d . . . C47 C -0.0853(3) 0.55110(17) 1.55437(11) 0.0253(6) Uani 1 1 d . . . H47A H -0.1442 0.5362 1.5791 0.038 Uiso 1 1 calc R . . H47B H -0.0221 0.5908 1.5685 0.038 Uiso 1 1 calc R . . H47C H -0.0417 0.5174 1.5462 0.038 Uiso 1 1 calc R . . C48 C -0.2319(3) 0.61605(17) 1.52005(13) 0.0297(7) Uani 1 1 d . . . H48A H -0.2827 0.6019 1.5474 0.045 Uiso 1 1 calc R . . H48B H -0.2883 0.6213 1.4905 0.045 Uiso 1 1 calc R . . H48C H -0.1704 0.6576 1.5310 0.045 Uiso 1 1 calc R . . C49 C -0.2536(3) 0.50237(17) 1.48376(12) 0.0324(8) Uani 1 1 d . . . H49A H -0.3129 0.4859 1.5080 0.049 Uiso 1 1 calc R . . H49B H -0.2065 0.4701 1.4758 0.049 Uiso 1 1 calc R . . H49C H -0.3016 0.5106 1.4529 0.049 Uiso 1 1 calc R . . Fe3 Fe -0.42530(4) 0.736136(19) 0.888329(15) 0.01673(9) Uani 1 1 d . . . Fe4 Fe -0.32578(4) 0.72202(2) 1.043044(15) 0.01803(9) Uani 1 1 d . . . O5B O -0.5075(2) 0.78604(10) 0.92984(8) 0.0198(4) Uani 1 1 d . . . O4B O -0.4803(2) 0.63970(12) 1.00407(8) 0.0286(5) Uani 1 1 d . . . O3B O -0.4671(2) 0.76583(12) 1.04295(8) 0.0262(5) Uani 1 1 d . . . O1B O -0.9112(2) 0.74690(11) 0.81183(9) 0.0283(5) Uani 1 1 d . . . O2B O -0.2343(3) 0.99674(13) 0.88845(10) 0.0521(9) Uani 1 1 d . . . N1B N -0.3603(2) 0.67652(13) 0.82914(10) 0.0242(5) Uani 1 1 d . . . N2B N -0.6024(2) 0.67533(12) 0.84485(9) 0.0184(5) Uani 1 1 d . . . N3B N -0.3646(3) 0.80473(13) 0.83336(9) 0.0257(6) Uani 1 1 d . . . N4B N -0.2790(2) 0.70698(12) 0.92668(9) 0.0194(5) Uani 1 1 d . . . N5B N -0.7326(2) 0.74364(12) 0.86274(10) 0.0200(5) Uani 1 1 d . . . N6B N -0.3543(3) 0.89329(13) 0.88922(10) 0.0235(5) Uani 1 1 d . . . N7B N -0.1261(2) 0.71341(13) 1.06899(10) 0.0238(5) Uani 1 1 d . . . N8B N -0.2212(2) 0.81593(13) 1.08498(9) 0.0223(5) Uani 1 1 d . . . N9B N -0.3491(2) 0.64896(12) 1.09868(9) 0.0221(5) Uani 1 1 d . . . N10B N -0.2434(2) 0.70604(12) 0.97706(10) 0.0199(5) Uani 1 1 d . . . N11B N -0.4045(3) 0.85231(16) 1.10502(11) 0.0334(6) Uani 1 1 d . . . N12B N -0.5655(2) 0.59294(13) 1.07115(10) 0.0225(5) Uani 1 1 d . . . H1B H -0.510(4) 0.779(2) 0.9563(18) 0.042(13) Uiso 1 1 d . . . H5B H -0.676(4) 0.7627(19) 0.8842(15) 0.027(10) Uiso 1 1 d . . . H6B H -0.388(4) 0.864(2) 0.9066(16) 0.034(11) Uiso 1 1 d . . . H12B H -0.631(4) 0.5681(18) 1.0816(14) 0.024(9) Uiso 1 1 d . . . C1B C -0.4502(3) 0.61217(15) 0.82752(12) 0.0240(6) Uani 1 1 d . . . H1BA H -0.4305 0.5907 0.8581 0.029 Uiso 1 1 calc R . . H1BB H -0.4407 0.5848 0.7979 0.029 Uiso 1 1 calc R . . C2B C -0.5856(3) 0.61868(14) 0.82457(11) 0.0204(6) Uani 1 1 d . . . C3B C -0.6865(3) 0.56892(15) 0.80281(11) 0.0231(6) Uani 1 1 d . . . H3BA H -0.6720 0.5305 0.7875 0.028 Uiso 1 1 calc R . . C4B C -0.8091(3) 0.57608(15) 0.80367(11) 0.0229(6) Uani 1 1 d . . . H4BA H -0.8800 0.5413 0.7908 0.027 Uiso 1 1 calc R . . C5B C -0.8286(3) 0.63351(14) 0.82321(11) 0.0207(6) Uani 1 1 d . . . H5BA H -0.9123 0.6393 0.8234 0.025 Uiso 1 1 calc R . . C6B C -0.7217(3) 0.68300(14) 0.84271(10) 0.0179(5) Uani 1 1 d . . . C7B C -0.8303(3) 0.77133(15) 0.84682(11) 0.0229(6) Uani 1 1 d . . . C8B C -0.8349(3) 0.83403(15) 0.87718(13) 0.0286(7) Uani 1 1 d . . . C9B C -0.7029(3) 0.87981(16) 0.89220(14) 0.0312(7) Uani 1 1 d . . . H9BA H -0.7117 0.9200 0.9093 0.047 Uiso 1 1 calc R . . H9BB H -0.6605 0.8898 0.8620 0.047 Uiso 1 1 calc R . . H9BC H -0.6518 0.8589 0.9149 0.047 Uiso 1 1 calc R . . C10B C -0.9005(4) 0.8134(2) 0.92335(18) 0.0480(11) Uani 1 1 d . . . H10V H -0.9069 0.8520 0.9435 0.072 Uiso 1 1 calc R . . H10W H -0.8506 0.7893 0.9436 0.072 Uiso 1 1 calc R . . H10X H -0.9862 0.7856 0.9126 0.072 Uiso 1 1 calc R . . C11B C -0.9158(5) 0.8695(2) 0.8443(2) 0.0700(18) Uani 1 1 d . . . H11D H -0.9269 0.9074 0.8639 0.105 Uiso 1 1 calc R . . H11E H -0.9995 0.8400 0.8329 0.105 Uiso 1 1 calc R . . H11F H -0.8726 0.8836 0.8150 0.105 Uiso 1 1 calc R . . C12B C -0.3726(3) 0.70616(16) 0.78106(12) 0.0295(7) Uani 1 1 d . . . H12D H -0.4602 0.6887 0.7638 0.035 Uiso 1 1 calc R . . H12E H -0.3125 0.6943 0.7591 0.035 Uiso 1 1 calc R . . C13B C -0.3454(4) 0.77881(18) 0.78878(13) 0.0394(9) Uani 1 1 d . . . C14B C -0.3060(7) 0.8167(2) 0.75088(16) 0.084(2) Uani 1 1 d . . . H14B H -0.2897 0.7975 0.7202 0.100 Uiso 1 1 calc R . . C15B C -0.2903(8) 0.8829(2) 0.75769(17) 0.093(3) Uani 1 1 d . . . H15B H -0.2663 0.9094 0.7312 0.112 Uiso 1 1 calc R . . C16B C -0.3093(6) 0.9105(2) 0.80282(15) 0.0599(15) Uani 1 1 d . . . H16B H -0.3000 0.9560 0.8079 0.072 Uiso 1 1 calc R . . C17B C -0.3426(4) 0.87011(16) 0.84083(12) 0.0326(8) Uani 1 1 d . . . C18B C -0.2834(3) 0.95218(15) 0.91215(12) 0.0257(6) Uani 1 1 d . . . C19B C -0.2638(3) 0.95499(14) 0.96943(11) 0.0223(6) Uani 1 1 d . . . C20B C -0.1841(4) 1.02296(17) 0.98958(13) 0.0353(8) Uani 1 1 d . . . H20D H -0.2313 1.0551 0.9803 0.053 Uiso 1 1 calc R . . H20E H -0.1033 1.0324 0.9750 0.053 Uiso 1 1 calc R . . H20F H -0.1669 1.0249 1.0263 0.053 Uiso 1 1 calc R . . C21B C -0.1886(3) 0.90484(16) 0.98328(12) 0.0264(6) Uani 1 1 d . . . H21D H -0.2441 0.8610 0.9752 0.040 Uiso 1 1 calc R . . H21E H -0.1586 0.9112 1.0194 0.040 Uiso 1 1 calc R . . H21F H -0.1153 0.9103 0.9641 0.040 Uiso 1 1 calc R . . C22B C -0.3912(3) 0.93958(18) 0.99111(14) 0.0336(8) Uani 1 1 d . . . H22D H -0.4409 0.9698 0.9797 0.050 Uiso 1 1 calc R . . H22E H -0.3757 0.9440 1.0279 0.050 Uiso 1 1 calc R . . H22F H -0.4386 0.8950 0.9796 0.050 Uiso 1 1 calc R . . C23B C -0.2277(3) 0.67274(17) 0.84533(13) 0.0298(7) Uani 1 1 d . . . H23C H -0.1660 0.7096 0.8337 0.036 Uiso 1 1 calc R . . H23D H -0.2134 0.6319 0.8305 0.036 Uiso 1 1 calc R . . C24B C -0.2090(3) 0.67476(15) 0.90128(12) 0.0245(6) Uani 1 1 d . . . C25B C -0.1267(3) 0.65219(16) 0.93470(13) 0.0278(7) Uani 1 1 d . . . H25B H -0.0672 0.6281 0.9272 0.033 Uiso 1 1 calc R . . C26B C -0.1522(3) 0.67329(15) 0.98181(13) 0.0244(6) Uani 1 1 d . . . C27B C -0.1017(3) 0.66307(16) 1.03403(14) 0.0295(7) Uani 1 1 d . . . H27C H -0.1449 0.6194 1.0430 0.035 Uiso 1 1 calc R . . H27D H -0.0090 0.6664 1.0361 0.035 Uiso 1 1 calc R . . C28B C -0.0403(3) 0.77727(15) 1.06477(13) 0.0255(6) Uani 1 1 d . . . H28C H -0.0317 0.7838 1.0289 0.031 Uiso 1 1 calc R . . H28D H 0.0453 0.7794 1.0823 0.031 Uiso 1 1 calc R . . C29B C -0.0924(3) 0.82969(15) 1.08766(12) 0.0241(6) Uani 1 1 d . . . C30B C -0.0122(3) 0.88771(17) 1.10872(13) 0.0314(7) Uani 1 1 d . . . H30B H 0.0778 0.8952 1.1102 0.038 Uiso 1 1 calc R . . C31B C -0.0673(4) 0.93467(18) 1.12768(14) 0.0392(9) Uani 1 1 d . . . H31B H -0.0152 0.9756 1.1416 0.047 Uiso 1 1 calc R . . C32B C -0.1974(4) 0.92169(18) 1.12617(13) 0.0361(8) Uani 1 1 d . . . H32B H -0.2356 0.9533 1.1399 0.043 Uiso 1 1 calc R . . C33B C -0.2742(3) 0.86162(16) 1.10437(12) 0.0272(6) Uani 1 1 d . . . C34B C -0.4876(3) 0.80711(19) 1.07588(12) 0.0307(7) Uani 1 1 d . . . C35B C -0.6285(4) 0.8031(2) 1.08038(15) 0.0422(10) Uani 1 1 d . . . C36B C -0.6874(5) 0.8215(6) 1.0359(3) 0.163(6) Uani 1 1 d . . . H36D H -0.7093 0.7849 1.0101 0.244 Uiso 1 1 calc R . . H36E H -0.6286 0.8583 1.0238 0.244 Uiso 1 1 calc R . . H36F H -0.7652 0.8339 1.0432 0.244 Uiso 1 1 calc R . . C37B C -0.6752(5) 0.7582(6) 1.1131(4) 0.199(7) Uani 1 1 d . . . H37D H -0.7166 0.7165 1.0941 0.299 Uiso 1 1 calc R . . H37E H -0.7375 0.7732 1.1315 0.299 Uiso 1 1 calc R . . H37F H -0.6048 0.7529 1.1370 0.299 Uiso 1 1 calc R . . C38B C -0.6353(7) 0.8685(4) 1.1143(3) 0.096(2) Uani 1 1 d . . . H38D H -0.7245 0.8671 1.1180 0.144 Uiso 1 1 calc R . . H38E H -0.5978 0.9071 1.0976 0.144 Uiso 1 1 calc R . . H38F H -0.5876 0.8702 1.1476 0.144 Uiso 1 1 calc R . . C39B C -0.1214(3) 0.69791(17) 1.12169(13) 0.0293(7) Uani 1 1 d . . . H39C H -0.0989 0.7388 1.1438 0.035 Uiso 1 1 calc R . . H39D H -0.0536 0.6749 1.1290 0.035 Uiso 1 1 calc R . . C40B C -0.2462(3) 0.65634(15) 1.13344(12) 0.0250(6) Uani 1 1 d . . . C41B C -0.2529(3) 0.62987(17) 1.17949(13) 0.0304(7) Uani 1 1 d . . . H41B H -0.1788 0.6360 1.2030 0.037 Uiso 1 1 calc R . . C42B C -0.3697(4) 0.59448(17) 1.19036(12) 0.0313(7) Uani 1 1 d . . . H42B H -0.3782 0.5782 1.2224 0.038 Uiso 1 1 calc R . . C43B C -0.4734(3) 0.58297(16) 1.15443(12) 0.0270(6) Uani 1 1 d . . . H43B H -0.5538 0.5572 1.1608 0.032 Uiso 1 1 calc R . . C44B C -0.4593(3) 0.60964(15) 1.10824(11) 0.0220(6) Uani 1 1 d . . . C45B C -0.5691(3) 0.60373(16) 1.02138(11) 0.0243(6) Uani 1 1 d . . . C46B C -0.6884(3) 0.56736(19) 0.98594(12) 0.0342(8) Uani 1 1 d . . . C47B C -0.7952(3) 0.52677(19) 1.01107(13) 0.0341(8) Uani 1 1 d . . . H47D H -0.7642 0.4938 1.0290 0.051 Uiso 1 1 calc R . . H47E H -0.8662 0.5055 0.9855 0.051 Uiso 1 1 calc R . . H47F H -0.8245 0.5548 1.0350 0.051 Uiso 1 1 calc R . . C48B C -0.7391(5) 0.6191(3) 0.9585(2) 0.103(3) Uani 1 1 d . . . H48D H -0.8057 0.5979 0.9313 0.155 Uiso 1 1 calc R . . H48E H -0.6691 0.6483 0.9445 0.155 Uiso 1 1 calc R . . H48F H -0.7748 0.6442 0.9824 0.155 Uiso 1 1 calc R . . C49B C -0.6433(5) 0.5246(4) 0.9487(2) 0.103(3) Uani 1 1 d . . . H49D H -0.6162 0.4901 0.9661 0.154 Uiso 1 1 calc R . . H49E H -0.5713 0.5507 0.9338 0.154 Uiso 1 1 calc R . . H49F H -0.7132 0.5052 0.9222 0.154 Uiso 1 1 calc R . . S1 S 0.58804(7) 0.48504(3) 1.32688(3) 0.01818(14) Uani 1 1 d . . . F1 F 0.5475(2) 0.56991(10) 1.39379(9) 0.0416(5) Uani 1 1 d . . . F2 F 0.4333(2) 0.47261(11) 1.39682(9) 0.0430(5) Uani 1 1 d . . . F3 F 0.3876(2) 0.53031(12) 1.33758(11) 0.0545(7) Uani 1 1 d . . . O6 O 0.68471(19) 0.47392(10) 1.36405(8) 0.0215(4) Uani 1 1 d . . . O7 O 0.5048(2) 0.42734(11) 1.30028(8) 0.0266(5) Uani 1 1 d . . . O8 O 0.6339(3) 0.53732(13) 1.29671(10) 0.0398(6) Uani 1 1 d . . . C50 C 0.4834(3) 0.51593(16) 1.36571(14) 0.0291(7) Uani 1 1 d . . . S2 S 0.12818(13) 0.50335(5) 1.15064(5) 0.0214(4) Uani 0.808(5) 1 d P A 1 S2B S 0.1871(5) 0.5216(2) 1.1731(2) 0.0226(16) Uani 0.192(5) 1 d P A 2 F4 F 0.1375(3) 0.61774(13) 1.12100(9) 0.0583(8) Uani 1 1 d . . . F5 F 0.2486(3) 0.61827(15) 1.19413(11) 0.0693(9) Uani 1 1 d . . . F6 F 0.0369(3) 0.59665(16) 1.18525(11) 0.0738(10) Uani 1 1 d . . . O9 O 0.1206(2) 0.47756(12) 1.19942(9) 0.0310(5) Uani 1 1 d . . . O10 O 0.2453(2) 0.50346(11) 1.12964(8) 0.0262(5) Uani 1 1 d . . . O11 O 0.0119(3) 0.4841(2) 1.11551(12) 0.0636(10) Uani 1 1 d . . . C51 C 0.1392(5) 0.5886(2) 1.16339(17) 0.0519(12) Uani 1 1 d . A . O12 O -0.5301(5) 0.7647(3) 1.2802(2) 0.1022(16) Uani 1 1 d . . . C52 C -0.4552(5) 0.8001(3) 1.25783(17) 0.0518(11) Uani 1 1 d . . . C53 C -0.3851(6) 0.7707(3) 1.2196(2) 0.0725(16) Uani 1 1 d . . . H53A H -0.4168 0.7233 1.2166 0.109 Uiso 1 1 calc R . . H53B H -0.2935 0.7826 1.2310 0.109 Uiso 1 1 calc R . . H53C H -0.4004 0.7873 1.1868 0.109 Uiso 1 1 calc R . . C54 C -0.4307(8) 0.8706(3) 1.2648(3) 0.092(2) Uani 1 1 d . . . H54A H -0.5008 0.8822 1.2802 0.138 Uiso 1 1 calc R . . H54B H -0.4242 0.8887 1.2321 0.138 Uiso 1 1 calc R . . H54C H -0.3506 0.8881 1.2868 0.138 Uiso 1 1 calc R . . O13 O -0.8693(8) 0.9936(4) 1.2929(3) 0.1430(12) Uiso 1 1 d . . . C55 C -0.9928(12) 0.9785(6) 1.2771(5) 0.1430(12) Uiso 1 1 d . . . C56 C -1.0402(11) 1.0331(5) 1.2585(4) 0.1430(12) Uiso 1 1 d . . . H56A H -0.9678 1.0698 1.2555 0.214 Uiso 1 1 calc R . . H56B H -1.0940 1.0462 1.2822 0.214 Uiso 1 1 calc R . . H56C H -1.0904 1.0196 1.2255 0.214 Uiso 1 1 calc R . . C57 C -1.0586(11) 0.9150(5) 1.2786(4) 0.1430(12) Uiso 1 1 d . . . H57A H -1.0075 0.8863 1.2671 0.214 Uiso 1 1 calc R . . H57B H -1.1395 0.9064 1.2567 0.214 Uiso 1 1 calc R . . H57C H -1.0757 0.9071 1.3132 0.214 Uiso 1 1 calc R . . O14 O -0.8006(7) 0.8637(4) 1.2368(3) 0.1430(12) Uiso 1 1 d . . . C58 C -0.8777(12) 0.8023(6) 1.2361(5) 0.1430(12) Uiso 1 1 d . . . C59 C -1.0065(11) 0.7918(5) 1.2185(4) 0.1430(12) Uiso 1 1 d . . . H59A H -1.0555 0.7537 1.2330 0.214 Uiso 1 1 calc R . . H59B H -1.0183 0.7843 1.1818 0.214 Uiso 1 1 calc R . . H59C H -1.0363 0.8299 1.2285 0.214 Uiso 1 1 calc R . . C60 C -0.8462(11) 0.7598(5) 1.2679(4) 0.1430(12) Uiso 1 1 d . . . H60A H -0.7660 0.7807 1.2889 0.214 Uiso 1 1 calc R . . H60B H -0.8358 0.7216 1.2483 0.214 Uiso 1 1 calc R . . H60C H -0.9140 0.7464 1.2894 0.214 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01270(18) 0.01558(18) 0.01393(18) 0.00301(14) 0.00403(14) 0.00398(14) Fe2 0.01210(17) 0.01386(18) 0.01206(17) 0.00148(13) 0.00218(13) 0.00316(13) O5 0.0181(10) 0.0186(10) 0.0174(10) 0.0046(8) 0.0043(8) 0.0057(8) O4 0.0166(9) 0.0189(10) 0.0146(9) 0.0009(7) 0.0019(7) -0.0005(7) O3 0.0168(9) 0.0216(10) 0.0210(10) 0.0080(8) 0.0057(8) 0.0081(8) O1 0.0462(15) 0.0179(11) 0.0277(12) 0.0011(9) 0.0075(10) -0.0016(10) O2 0.0144(9) 0.0314(12) 0.0254(11) 0.0066(9) 0.0054(8) 0.0079(8) N1 0.0142(10) 0.0184(11) 0.0125(10) 0.0035(8) 0.0037(8) 0.0042(9) N2 0.0246(12) 0.0184(12) 0.0156(11) 0.0013(9) 0.0065(9) 0.0022(9) N3 0.0163(11) 0.0165(11) 0.0123(10) 0.0019(8) 0.0037(8) 0.0033(9) N4 0.0136(10) 0.0181(11) 0.0117(10) 0.0025(8) 0.0021(8) 0.0033(8) N5 0.0304(14) 0.0137(11) 0.0213(12) 0.0024(10) 0.0040(10) 0.0002(10) N6 0.0152(11) 0.0210(12) 0.0188(11) 0.0050(9) 0.0067(9) 0.0054(9) N7 0.0157(11) 0.0152(11) 0.0131(10) 0.0007(8) 0.0026(8) 0.0019(8) N8 0.0167(11) 0.0168(11) 0.0152(11) 0.0030(8) 0.0024(8) 0.0027(9) N9 0.0153(11) 0.0155(11) 0.0126(10) 0.0030(8) 0.0034(8) 0.0042(8) N10 0.0137(10) 0.0169(11) 0.0119(10) 0.0002(8) 0.0028(8) 0.0033(8) N11 0.0197(12) 0.0205(12) 0.0207(12) 0.0052(9) 0.0000(9) 0.0058(9) N12 0.0121(10) 0.0151(11) 0.0153(11) 0.0004(8) 0.0013(8) 0.0000(9) C1 0.0226(14) 0.0220(14) 0.0126(12) 0.0031(10) 0.0024(10) 0.0032(11) C2 0.0319(16) 0.0235(15) 0.0157(13) 0.0007(11) 0.0044(12) 0.0009(12) C3 0.073(3) 0.0314(19) 0.0165(15) 0.0011(13) -0.0101(16) -0.0047(18) C4 0.117(4) 0.027(2) 0.0253(19) -0.0038(15) -0.017(2) -0.009(2) C5 0.095(4) 0.0174(16) 0.0261(18) -0.0013(13) -0.004(2) -0.0015(19) C6 0.0392(18) 0.0192(14) 0.0201(14) 0.0018(11) 0.0065(13) 0.0027(13) C7 0.0242(14) 0.0166(13) 0.0239(15) 0.0039(11) 0.0065(11) 0.0036(11) C8 0.0247(15) 0.0172(13) 0.0240(15) 0.0051(11) 0.0043(11) 0.0045(11) C9 0.044(2) 0.0219(16) 0.0289(17) 0.0090(13) 0.0046(15) -0.0022(14) C10 0.0250(16) 0.0274(16) 0.0327(17) 0.0128(13) 0.0009(13) 0.0047(12) C11 0.0310(17) 0.0365(18) 0.0212(15) 0.0010(13) 0.0041(12) 0.0131(14) C12 0.0165(13) 0.0193(13) 0.0174(13) 0.0059(10) 0.0045(10) 0.0052(10) C13 0.0174(13) 0.0159(12) 0.0138(12) 0.0005(10) 0.0023(10) 0.0023(10) C14 0.0210(14) 0.0184(13) 0.0172(13) 0.0035(10) 0.0052(10) 0.0032(11) C15 0.0211(14) 0.0202(14) 0.0193(13) 0.0028(11) 0.0092(11) 0.0013(11) C16 0.0169(13) 0.0202(13) 0.0194(13) 0.0015(10) 0.0058(10) 0.0024(10) C17 0.0161(12) 0.0170(13) 0.0143(12) -0.0001(10) 0.0035(10) 0.0033(10) C18 0.0136(12) 0.0211(13) 0.0157(12) -0.0022(10) -0.0001(10) 0.0048(10) C19 0.0169(13) 0.0219(14) 0.0232(14) 0.0041(11) 0.0025(11) 0.0059(11) C20 0.0228(15) 0.0213(14) 0.0313(16) -0.0003(12) 0.0017(12) 0.0040(12) C21 0.0210(15) 0.0278(16) 0.0364(18) 0.0075(13) 0.0050(13) 0.0108(12) C22 0.0230(14) 0.0268(15) 0.0217(14) 0.0056(12) 0.0007(11) 0.0077(12) C23 0.0145(12) 0.0238(14) 0.0147(12) 0.0048(10) 0.0025(10) 0.0055(10) C24 0.0124(12) 0.0161(12) 0.0157(12) 0.0035(10) 0.0015(9) 0.0009(9) C25 0.0146(12) 0.0175(13) 0.0189(13) 0.0025(10) 0.0024(10) 0.0055(10) C26 0.0131(12) 0.0154(12) 0.0165(12) 0.0010(10) 0.0031(10) 0.0026(9) C27 0.0148(12) 0.0197(13) 0.0168(13) 0.0020(10) 0.0040(10) 0.0063(10) C28 0.0145(12) 0.0184(13) 0.0176(13) 0.0019(10) 0.0048(10) 0.0007(10) C29 0.0179(13) 0.0186(13) 0.0148(12) 0.0004(10) 0.0042(10) 0.0012(10) C30 0.0197(14) 0.0223(14) 0.0206(14) 0.0029(11) 0.0046(11) -0.0014(11) C31 0.0289(16) 0.0212(14) 0.0214(14) 0.0073(11) 0.0035(12) -0.0009(12) C32 0.0264(15) 0.0215(14) 0.0223(14) 0.0080(11) 0.0019(12) 0.0051(12) C33 0.0221(14) 0.0177(13) 0.0159(13) 0.0028(10) 0.0024(10) 0.0042(11) C34 0.0188(13) 0.0198(13) 0.0175(13) 0.0018(10) 0.0031(10) 0.0081(11) C35 0.0158(13) 0.0256(15) 0.0241(14) 0.0070(11) 0.0036(11) 0.0074(11) C36 0.0177(14) 0.0254(15) 0.0296(16) 0.0071(12) 0.0034(12) 0.0038(11) C37 0.0221(16) 0.0349(19) 0.058(2) 0.0198(17) 0.0106(15) 0.0139(14) C38 0.0245(16) 0.053(2) 0.0210(16) 0.0022(14) -0.0008(12) 0.0050(15) C39 0.0170(13) 0.0214(13) 0.0143(12) 0.0000(10) 0.0048(10) 0.0032(10) C40 0.0173(13) 0.0158(12) 0.0153(12) 0.0029(10) 0.0029(10) 0.0044(10) C41 0.0204(14) 0.0236(14) 0.0152(13) 0.0009(10) 0.0068(10) 0.0038(11) C42 0.0244(14) 0.0224(14) 0.0147(13) -0.0027(10) 0.0024(11) 0.0019(11) C43 0.0189(13) 0.0194(13) 0.0173(13) -0.0004(10) 0.0012(10) 0.0003(10) C44 0.0170(12) 0.0151(12) 0.0152(12) 0.0029(9) 0.0035(10) 0.0056(10) C45 0.0169(12) 0.0155(12) 0.0135(12) 0.0035(9) 0.0024(9) 0.0056(10) C46 0.0160(12) 0.0185(13) 0.0129(12) 0.0024(10) 0.0019(10) 0.0013(10) C47 0.0263(15) 0.0344(17) 0.0176(14) 0.0101(12) 0.0042(11) 0.0095(13) C48 0.0307(17) 0.0341(17) 0.0330(17) 0.0156(14) 0.0184(14) 0.0161(14) C49 0.0324(17) 0.0344(18) 0.0187(15) 0.0017(13) 0.0051(13) -0.0147(14) Fe3 0.01567(19) 0.01713(19) 0.01532(19) -0.00092(14) 0.00282(14) 0.00027(15) Fe4 0.01278(18) 0.0217(2) 0.0188(2) 0.00652(15) 0.00086(14) 0.00211(15) O5B 0.0217(10) 0.0207(10) 0.0159(10) -0.0007(8) 0.0012(8) 0.0037(8) O4B 0.0210(11) 0.0375(13) 0.0202(11) 0.0085(9) 0.0017(8) -0.0072(9) O3B 0.0157(10) 0.0379(13) 0.0262(11) 0.0058(9) 0.0017(8) 0.0087(9) O1B 0.0269(12) 0.0317(12) 0.0242(11) 0.0003(9) -0.0059(9) 0.0074(9) O2B 0.084(2) 0.0234(13) 0.0289(14) 0.0076(10) -0.0126(14) -0.0178(13) N1B 0.0205(12) 0.0262(13) 0.0219(13) -0.0056(10) 0.0060(10) -0.0019(10) N2B 0.0193(12) 0.0190(11) 0.0149(11) 0.0001(9) 0.0028(9) 0.0007(9) N3B 0.0312(14) 0.0234(13) 0.0154(12) -0.0017(10) 0.0021(10) -0.0055(11) N4B 0.0156(11) 0.0205(12) 0.0210(12) -0.0005(9) 0.0038(9) 0.0022(9) N5B 0.0193(12) 0.0190(12) 0.0186(12) -0.0008(9) -0.0026(10) 0.0016(9) N6B 0.0299(14) 0.0172(12) 0.0185(12) 0.0024(10) -0.0016(10) -0.0019(10) N7B 0.0168(12) 0.0235(13) 0.0300(14) 0.0090(10) -0.0016(10) 0.0030(10) N8B 0.0196(12) 0.0254(13) 0.0207(12) 0.0052(10) 0.0000(9) 0.0037(10) N9B 0.0219(12) 0.0216(12) 0.0203(12) 0.0068(10) 0.0003(10) 0.0007(10) N10B 0.0146(11) 0.0198(12) 0.0244(12) 0.0032(9) 0.0029(9) 0.0019(9) N11B 0.0348(16) 0.0456(18) 0.0253(14) 0.0021(12) 0.0059(12) 0.0196(14) N12B 0.0184(12) 0.0255(13) 0.0196(12) 0.0040(10) 0.0037(10) -0.0035(10) C1B 0.0211(14) 0.0233(15) 0.0242(15) -0.0070(11) 0.0045(11) 0.0006(11) C2B 0.0211(14) 0.0205(14) 0.0167(13) -0.0012(10) 0.0027(11) 0.0002(11) C3B 0.0271(15) 0.0191(14) 0.0191(14) -0.0036(11) 0.0031(11) -0.0006(11) C4B 0.0236(14) 0.0219(14) 0.0167(13) 0.0003(11) 0.0005(11) -0.0055(11) C5B 0.0181(13) 0.0240(14) 0.0169(13) 0.0031(11) 0.0002(10) -0.0006(11) C6B 0.0196(13) 0.0189(13) 0.0122(12) 0.0020(10) 0.0007(10) -0.0001(10) C7B 0.0226(14) 0.0237(15) 0.0211(14) 0.0029(11) 0.0010(11) 0.0034(11) C8B 0.0253(16) 0.0202(15) 0.0381(18) -0.0011(13) -0.0035(13) 0.0055(12) C9B 0.0306(17) 0.0217(15) 0.0388(19) -0.0006(13) 0.0033(14) 0.0032(13) C10B 0.045(2) 0.034(2) 0.061(3) -0.0153(18) 0.024(2) -0.0024(17) C11B 0.068(3) 0.040(2) 0.096(4) -0.016(3) -0.046(3) 0.029(2) C12B 0.0333(17) 0.0319(17) 0.0173(14) -0.0061(12) 0.0098(12) -0.0043(13) C13B 0.055(2) 0.0331(19) 0.0191(16) -0.0029(13) 0.0109(15) -0.0114(16) C14B 0.157(6) 0.045(3) 0.023(2) -0.0078(18) 0.036(3) -0.032(3) C15B 0.185(7) 0.044(3) 0.023(2) 0.0059(18) 0.029(3) -0.032(3) C16B 0.106(4) 0.029(2) 0.0259(19) 0.0061(15) 0.003(2) -0.019(2) C17B 0.046(2) 0.0237(16) 0.0181(15) 0.0014(12) -0.0018(13) -0.0081(14) C18B 0.0297(16) 0.0170(14) 0.0261(15) 0.0026(11) -0.0063(12) 0.0012(12) C19B 0.0244(15) 0.0179(13) 0.0227(14) -0.0019(11) -0.0018(11) 0.0043(11) C20B 0.047(2) 0.0234(16) 0.0281(17) -0.0073(13) -0.0062(15) 0.0010(15) C21B 0.0275(16) 0.0288(16) 0.0245(15) 0.0041(12) 0.0007(12) 0.0106(13) C22B 0.0292(17) 0.0365(19) 0.0352(18) -0.0086(15) 0.0039(14) 0.0108(14) C23B 0.0204(15) 0.0338(17) 0.0320(17) -0.0112(14) 0.0092(13) 0.0016(13) C24B 0.0167(13) 0.0225(15) 0.0319(16) -0.0058(12) 0.0071(12) 0.0001(11) C25B 0.0185(14) 0.0238(15) 0.0407(19) -0.0049(13) 0.0052(13) 0.0054(12) C26B 0.0164(13) 0.0193(14) 0.0379(18) 0.0041(12) 0.0043(12) 0.0042(11) C27B 0.0199(15) 0.0277(16) 0.0428(19) 0.0081(14) 0.0007(13) 0.0098(12) C28B 0.0143(13) 0.0275(16) 0.0321(16) 0.0075(13) -0.0001(12) 0.0003(11) C29B 0.0212(14) 0.0253(15) 0.0231(15) 0.0092(12) -0.0020(11) 0.0012(12) C30B 0.0286(17) 0.0293(17) 0.0292(17) 0.0084(13) -0.0083(13) -0.0028(13) C31B 0.051(2) 0.0279(18) 0.0300(18) -0.0004(14) -0.0101(16) 0.0009(16) C32B 0.048(2) 0.0325(18) 0.0262(17) -0.0020(14) -0.0024(15) 0.0112(16) C33B 0.0310(17) 0.0308(17) 0.0203(14) 0.0036(12) 0.0009(12) 0.0092(13) C34B 0.0252(16) 0.050(2) 0.0245(16) 0.0131(14) 0.0089(13) 0.0185(15) C35B 0.0274(18) 0.075(3) 0.035(2) 0.0171(19) 0.0135(15) 0.0279(19) C36B 0.032(3) 0.315(13) 0.183(8) 0.209(10) 0.049(4) 0.068(5) C37B 0.031(3) 0.339(15) 0.274(12) 0.274(13) 0.063(5) 0.063(5) C38B 0.066(4) 0.129(6) 0.107(6) -0.001(5) 0.018(4) 0.051(4) C39B 0.0219(15) 0.0314(17) 0.0316(17) 0.0123(13) -0.0072(12) 0.0030(13) C40B 0.0239(15) 0.0241(15) 0.0254(15) 0.0084(12) -0.0024(12) 0.0036(12) C41B 0.0317(17) 0.0342(18) 0.0244(16) 0.0110(13) -0.0044(13) 0.0076(14) C42B 0.0397(19) 0.0334(18) 0.0212(15) 0.0108(13) 0.0009(13) 0.0092(15) C43B 0.0293(16) 0.0269(16) 0.0234(15) 0.0089(12) 0.0050(12) 0.0023(13) C44B 0.0234(14) 0.0215(14) 0.0194(14) 0.0033(11) 0.0011(11) 0.0027(11) C45B 0.0216(14) 0.0280(16) 0.0192(14) 0.0046(11) 0.0018(11) -0.0017(12) C46B 0.0253(16) 0.048(2) 0.0166(14) 0.0041(13) 0.0022(12) -0.0157(14) C47B 0.0244(16) 0.044(2) 0.0231(16) 0.0039(14) 0.0031(13) -0.0118(14) C48B 0.063(3) 0.105(5) 0.095(4) 0.079(4) -0.057(3) -0.055(3) C49B 0.047(3) 0.159(7) 0.062(3) -0.075(4) 0.024(3) -0.040(3) S1 0.0178(3) 0.0216(3) 0.0142(3) 0.0025(2) 0.0020(2) 0.0029(3) F1 0.0311(11) 0.0317(11) 0.0585(14) -0.0214(10) -0.0017(10) 0.0094(9) F2 0.0337(11) 0.0481(13) 0.0444(13) -0.0055(10) 0.0244(10) -0.0008(10) F3 0.0305(12) 0.0445(13) 0.088(2) -0.0176(13) -0.0180(12) 0.0239(10) O6 0.0183(10) 0.0258(11) 0.0200(10) -0.0002(8) -0.0005(8) 0.0064(8) O7 0.0222(11) 0.0303(12) 0.0244(11) -0.0067(9) -0.0010(8) 0.0045(9) O8 0.0446(15) 0.0419(15) 0.0281(13) 0.0196(11) 0.0017(11) -0.0009(12) C50 0.0210(15) 0.0258(16) 0.0391(18) -0.0098(13) -0.0004(13) 0.0077(12) S2 0.0206(7) 0.0257(5) 0.0185(7) 0.0064(4) 0.0067(6) 0.0042(5) S2B 0.019(3) 0.032(2) 0.018(3) 0.0036(19) 0.002(2) 0.008(2) F4 0.102(2) 0.0534(15) 0.0423(14) 0.0304(12) 0.0359(14) 0.0467(15) F5 0.086(2) 0.0575(17) 0.0546(17) -0.0153(14) 0.0145(16) 0.0002(16) F6 0.114(3) 0.100(2) 0.0540(16) 0.0440(16) 0.0543(17) 0.089(2) O9 0.0296(12) 0.0416(14) 0.0270(12) 0.0167(10) 0.0113(9) 0.0126(10) O10 0.0260(11) 0.0272(11) 0.0259(11) 0.0032(9) 0.0105(9) 0.0045(9) O11 0.0358(16) 0.100(3) 0.0387(17) -0.0045(17) 0.0064(13) -0.0132(17) C51 0.078(3) 0.057(3) 0.039(2) 0.022(2) 0.029(2) 0.040(3) O12 0.116(4) 0.103(4) 0.092(3) 0.018(3) 0.044(3) 0.020(3) C52 0.054(3) 0.063(3) 0.036(2) 0.012(2) 0.0012(19) 0.010(2) C53 0.087(4) 0.068(3) 0.062(3) 0.013(3) -0.018(3) 0.027(3) C54 0.129(6) 0.078(4) 0.068(4) 0.003(3) -0.004(4) 0.030(4) _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 O5 1.938(2) . ? Fe1 N4 2.040(2) . ? Fe1 N2 2.195(3) . ? Fe1 N3 2.200(2) . ? Fe1 N1 2.243(2) . ? Fe2 O3 2.005(2) . ? Fe2 N10 2.121(2) . ? Fe2 N9 2.196(2) . ? Fe2 N8 2.208(2) . ? Fe2 O4 2.233(2) . ? Fe2 N7 2.279(2) . ? O4 C45 1.224(3) . ? O3 C34 1.289(3) . ? O1 C7 1.215(4) . ? O2 C18 1.220(4) . ? N1 C1 1.468(4) . ? N1 C12 1.471(4) . ? N1 C23 1.485(3) . ? N2 C2 1.354(4) . ? N2 C6 1.357(4) . ? N3 C17 1.353(4) . ? N3 C13 1.357(4) . ? N4 C24 1.349(3) . ? N4 N10 1.369(3) . ? N5 C7 1.387(4) . ? N5 C6 1.389(4) . ? N6 C18 1.378(4) . ? N6 C17 1.398(4) . ? N7 C39 1.468(3) . ? N7 C28 1.472(3) . ? N7 C27 1.474(3) . ? N8 C29 1.357(4) . ? N8 C33 1.361(4) . ? N9 C44 1.346(4) . ? N9 C40 1.356(3) . ? N10 C26 1.350(3) . ? N11 C34 1.308(4) . ? N11 C33 1.375(4) . ? N12 C45 1.367(3) . ? N12 C44 1.412(3) . ? C1 C2 1.503(4) . ? C2 C3 1.380(5) . ? C3 C4 1.386(6) . ? C4 C5 1.379(6) . ? C5 C6 1.401(5) . ? C7 C8 1.528(4) . ? C8 C9 1.529(4) . ? C8 C10 1.533(4) . ? C8 C11 1.538(4) . ? C12 C13 1.507(4) . ? C13 C14 1.386(4) . ? C14 C15 1.388(4) . ? C15 C16 1.374(4) . ? C16 C17 1.400(4) . ? C18 C19 1.531(4) . ? C19 C21 1.535(4) . ? C19 C22 1.535(4) . ? C19 C20 1.539(4) . ? C23 C24 1.497(4) . ? C24 C25 1.389(4) . ? C25 C26 1.391(4) . ? C26 C27 1.504(4) . ? C28 C29 1.503(4) . ? C29 C30 1.377(4) . ? C30 C31 1.396(4) . ? C31 C32 1.369(5) . ? C32 C33 1.412(4) . ? C34 C35 1.536(4) . ? C35 C36 1.520(4) . ? C35 C37 1.530(4) . ? C35 C38 1.543(5) . ? C39 C40 1.511(4) . ? C40 C41 1.377(4) . ? C41 C42 1.392(4) . ? C42 C43 1.380(4) . ? C43 C44 1.392(4) . ? C45 C46 1.542(4) . ? C46 C49 1.520(4) . ? C46 C48 1.531(4) . ? C46 C47 1.537(4) . ? Fe3 O5B 1.926(2) . ? Fe3 N4B 2.050(3) . ? Fe3 N3B 2.171(3) . ? Fe3 N2B 2.217(2) . ? Fe3 N1B 2.254(3) . ? Fe4 O3B 1.985(2) . ? Fe4 N10B 2.111(3) . ? Fe4 N9B 2.204(2) . ? Fe4 N8B 2.224(3) . ? Fe4 O4B 2.237(2) . ? Fe4 N7B 2.268(3) . ? O4B C45B 1.228(4) . ? O3B C34B 1.286(4) . ? O1B C7B 1.217(4) . ? O2B C18B 1.217(4) . ? N1B C1B 1.474(4) . ? N1B C12B 1.475(4) . ? N1B C23B 1.487(4) . ? N2B C6B 1.344(4) . ? N2B C2B 1.358(4) . ? N3B C13B 1.346(4) . ? N3B C17B 1.356(4) . ? N4B C24B 1.352(4) . ? N4B N10B 1.370(3) . ? N5B C7B 1.380(4) . ? N5B C6B 1.409(4) . ? N6B C18B 1.377(4) . ? N6B C17B 1.392(4) . ? N7B C39B 1.468(4) . ? N7B C28B 1.469(4) . ? N7B C27B 1.476(4) . ? N8B C33B 1.353(4) . ? N8B C29B 1.355(4) . ? N9B C44B 1.343(4) . ? N9B C40B 1.355(4) . ? N10B C26B 1.346(4) . ? N11B C34B 1.306(5) . ? N11B C33B 1.386(5) . ? N12B C45B 1.365(4) . ? N12B C44B 1.407(4) . ? C1B C2B 1.508(4) . ? C2B C3B 1.380(4) . ? C3B C4B 1.383(5) . ? C4B C5B 1.378(4) . ? C5B C6B 1.399(4) . ? C7B C8B 1.541(4) . ? C8B C10B 1.524(6) . ? C8B C9B 1.528(5) . ? C8B C11B 1.539(5) . ? C12B C13B 1.503(5) . ? C13B C14B 1.371(5) . ? C14B C15B 1.380(8) . ? C15B C16B 1.373(7) . ? C16B C17B 1.391(5) . ? C18B C19B 1.525(4) . ? C19B C22B 1.528(5) . ? C19B C20B 1.533(4) . ? C19B C21B 1.537(4) . ? C23B C24B 1.490(5) . ? C24B C25B 1.390(5) . ? C25B C26B 1.394(5) . ? C26B C27B 1.499(5) . ? C28B C29B 1.500(5) . ? C29B C30B 1.381(4) . ? C30B C31B 1.385(6) . ? C31B C32B 1.372(6) . ? C32B C33B 1.406(5) . ? C34B C35B 1.533(5) . ? C35B C37B 1.375(7) . ? C35B C36B 1.416(7) . ? C35B C38B 1.644(9) . ? C39B C40B 1.504(4) . ? C40B C41B 1.387(4) . ? C41B C42B 1.379(5) . ? C42B C43B 1.372(5) . ? C43B C44B 1.398(4) . ? C45B C46B 1.539(4) . ? C46B C49B 1.511(7) . ? C46B C47B 1.513(4) . ? C46B C48B 1.540(7) . ? S1 O8 1.434(2) . ? S1 O7 1.439(2) . ? S1 O6 1.447(2) . ? S1 C50 1.829(3) . ? F1 C50 1.336(4) . ? F2 C50 1.334(4) . ? F3 C50 1.332(4) . ? S2 O10 1.445(2) . ? S2 O9 1.449(2) . ? S2 O11 1.456(3) . ? S2 C51 1.804(5) . ? S2B O9 1.322(5) . ? S2B O10 1.459(5) . ? S2B C51 1.662(6) . ? S2B F5 2.034(6) . ? F4 C51 1.326(5) . ? F5 C51 1.368(6) . ? F6 C51 1.352(5) . ? O12 C52 1.202(6) . ? C52 C54 1.458(8) . ? C52 C53 1.532(8) . ? O13 C55 1.323(13) . ? C55 C57 1.373(14) . ? C55 C56 1.475(14) . ? O14 C58 1.370(13) . ? C58 C60 1.358(14) . ? C58 C59 1.392(14) . ? 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 O5 Fe1 N4 109.71(9) . . ? O5 Fe1 N2 101.92(10) . . ? N4 Fe1 N2 112.66(10) . . ? O5 Fe1 N3 97.68(9) . . ? N4 Fe1 N3 126.98(9) . . ? N2 Fe1 N3 104.38(9) . . ? O5 Fe1 N1 172.62(9) . . ? N4 Fe1 N1 77.50(9) . . ? N2 Fe1 N1 76.04(9) . . ? N3 Fe1 N1 76.18(8) . . ? O3 Fe2 N10 131.17(9) . . ? O3 Fe2 N9 100.36(9) . . ? N10 Fe2 N9 117.83(9) . . ? O3 Fe2 N8 81.86(8) . . ? N10 Fe2 N8 110.89(9) . . ? N9 Fe2 N8 108.13(8) . . ? O3 Fe2 O4 81.20(8) . . ? N10 Fe2 O4 79.08(8) . . ? N9 Fe2 O4 77.22(8) . . ? N8 Fe2 O4 162.92(8) . . ? O3 Fe2 N7 150.71(8) . . ? N10 Fe2 N7 73.39(8) . . ? N9 Fe2 N7 74.26(8) . . ? N8 Fe2 N7 72.99(9) . . ? O4 Fe2 N7 123.91(8) . . ? C45 O4 Fe2 129.48(17) . . ? C34 O3 Fe2 128.21(18) . . ? C1 N1 C12 111.0(2) . . ? C1 N1 C23 112.4(2) . . ? C12 N1 C23 111.8(2) . . ? C1 N1 Fe1 108.62(17) . . ? C12 N1 Fe1 103.96(16) . . ? C23 N1 Fe1 108.74(16) . . ? C2 N2 C6 118.4(3) . . ? C2 N2 Fe1 115.7(2) . . ? C6 N2 Fe1 125.7(2) . . ? C17 N3 C13 118.2(2) . . ? C17 N3 Fe1 128.73(18) . . ? C13 N3 Fe1 113.11(18) . . ? C24 N4 N10 108.6(2) . . ? C24 N4 Fe1 118.73(18) . . ? N10 N4 Fe1 132.28(17) . . ? C7 N5 C6 125.4(3) . . ? C18 N6 C17 125.8(2) . . ? C39 N7 C28 111.3(2) . . ? C39 N7 C27 113.2(2) . . ? C28 N7 C27 111.5(2) . . ? C39 N7 Fe2 107.80(16) . . ? C28 N7 Fe2 105.77(16) . . ? C27 N7 Fe2 106.79(16) . . ? C29 N8 C33 117.9(2) . . ? C29 N8 Fe2 116.15(18) . . ? C33 N8 Fe2 125.92(19) . . ? C44 N9 C40 117.6(2) . . ? C44 N9 Fe2 125.65(18) . . ? C40 N9 Fe2 113.65(18) . . ? C26 N10 N4 106.7(2) . . ? C26 N10 Fe2 116.18(17) . . ? N4 N10 Fe2 134.83(17) . . ? C34 N11 C33 123.3(2) . . ? C45 N12 C44 127.9(2) . . ? N1 C1 C2 111.5(2) . . ? N2 C2 C3 123.0(3) . . ? N2 C2 C1 116.5(3) . . ? C3 C2 C1 120.5(3) . . ? C2 C3 C4 118.3(3) . . ? C5 C4 C3 119.9(4) . . ? C4 C5 C6 119.1(3) . . ? N2 C6 N5 114.7(3) . . ? N2 C6 C5 121.3(3) . . ? N5 C6 C5 124.0(3) . . ? O1 C7 N5 122.6(3) . . ? O1 C7 C8 123.1(3) . . ? N5 C7 C8 114.2(3) . . ? C7 C8 C9 108.8(3) . . ? C7 C8 C10 112.4(3) . . ? C9 C8 C10 109.0(3) . . ? C7 C8 C11 106.6(2) . . ? C9 C8 C11 109.3(3) . . ? C10 C8 C11 110.7(3) . . ? N1 C12 C13 110.1(2) . . ? N3 C13 C14 122.7(3) . . ? N3 C13 C12 116.1(2) . . ? C14 C13 C12 121.1(2) . . ? C13 C14 C15 118.1(3) . . ? C16 C15 C14 120.1(3) . . ? C15 C16 C17 118.8(3) . . ? N3 C17 N6 114.1(2) . . ? N3 C17 C16 121.8(3) . . ? N6 C17 C16 124.0(3) . . ? O2 C18 N6 122.7(3) . . ? O2 C18 C19 121.7(3) . . ? N6 C18 C19 115.6(2) . . ? C18 C19 C21 108.4(2) . . ? C18 C19 C22 108.9(2) . . ? C21 C19 C22 109.4(3) . . ? C18 C19 C20 109.4(2) . . ? C21 C19 C20 109.6(3) . . ? C22 C19 C20 111.1(3) . . ? N1 C23 C24 109.1(2) . . ? N4 C24 C25 109.9(2) . . ? N4 C24 C23 117.2(2) . . ? C25 C24 C23 132.8(2) . . ? C24 C25 C26 103.8(2) . . ? N10 C26 C25 111.0(2) . . ? N10 C26 C27 117.5(2) . . ? C25 C26 C27 131.5(2) . . ? N7 C27 C26 107.8(2) . . ? N7 C28 C29 109.9(2) . . ? N8 C29 C30 123.9(3) . . ? N8 C29 C28 115.0(2) . . ? C30 C29 C28 121.1(3) . . ? C29 C30 C31 118.1(3) . . ? C32 C31 C30 119.2(3) . . ? C31 C32 C33 120.3(3) . . ? N8 C33 N11 123.1(3) . . ? N8 C33 C32 120.5(3) . . ? N11 C33 C32 116.2(3) . . ? O3 C34 N11 127.8(3) . . ? O3 C34 C35 117.8(2) . . ? N11 C34 C35 114.3(2) . . ? C36 C35 C37 109.8(3) . . ? C36 C35 C34 111.8(2) . . ? C37 C35 C34 110.4(3) . . ? C36 C35 C38 108.3(3) . . ? C37 C35 C38 109.7(3) . . ? C34 C35 C38 106.9(2) . . ? N7 C39 C40 112.2(2) . . ? N9 C40 C41 123.0(3) . . ? N9 C40 C39 117.4(2) . . ? C41 C40 C39 119.6(2) . . ? C40 C41 C42 118.3(3) . . ? C43 C42 C41 119.7(3) . . ? C42 C43 C44 118.4(3) . . ? N9 C44 C43 122.7(2) . . ? N9 C44 N12 120.4(2) . . ? C43 C44 N12 116.9(2) . . ? O4 C45 N12 122.8(2) . . ? O4 C45 C46 119.3(2) . . ? N12 C45 C46 117.9(2) . . ? C49 C46 C48 110.5(3) . . ? C49 C46 C47 108.7(3) . . ? C48 C46 C47 109.0(2) . . ? C49 C46 C45 114.9(2) . . ? C48 C46 C45 107.0(2) . . ? C47 C46 C45 106.5(2) . . ? O5B Fe3 N4B 113.94(10) . . ? O5B Fe3 N3B 100.17(10) . . ? N4B Fe3 N3B 113.94(11) . . ? O5B Fe3 N2B 96.36(9) . . ? N4B Fe3 N2B 128.50(10) . . ? N3B Fe3 N2B 99.29(9) . . ? O5B Fe3 N1B 169.44(10) . . ? N4B Fe3 N1B 76.36(10) . . ? N3B Fe3 N1B 76.57(10) . . ? N2B Fe3 N1B 74.50(9) . . ? O3B Fe4 N10B 121.86(10) . . ? O3B Fe4 N9B 109.21(10) . . ? N10B Fe4 N9B 119.94(10) . . ? O3B Fe4 N8B 80.52(10) . . ? N10B Fe4 N8B 110.87(10) . . ? N9B Fe4 N8B 106.44(9) . . ? O3B Fe4 O4B 82.68(10) . . ? N10B Fe4 O4B 80.47(9) . . ? N9B Fe4 O4B 76.64(9) . . ? N8B Fe4 O4B 162.99(10) . . ? O3B Fe4 N7B 152.92(10) . . ? N10B Fe4 N7B 73.92(10) . . ? N9B Fe4 N7B 74.33(9) . . ? N8B Fe4 N7B 72.91(10) . . ? O4B Fe4 N7B 123.49(10) . . ? C45B O4B Fe4 129.2(2) . . ? C34B O3B Fe4 129.9(2) . . ? C1B N1B C12B 111.6(2) . . ? C1B N1B C23B 110.7(3) . . ? C12B N1B C23B 112.9(3) . . ? C1B N1B Fe3 103.48(17) . . ? C12B N1B Fe3 108.1(2) . . ? C23B N1B Fe3 109.57(18) . . ? C6B N2B C2B 118.3(2) . . ? C6B N2B Fe3 128.79(19) . . ? C2B N2B Fe3 112.12(19) . . ? C13B N3B C17B 118.7(3) . . ? C13B N3B Fe3 115.7(2) . . ? C17B N3B Fe3 125.6(2) . . ? C24B N4B N10B 107.9(2) . . ? C24B N4B Fe3 119.7(2) . . ? N10B N4B Fe3 131.88(19) . . ? C7B N5B C6B 123.7(3) . . ? C18B N6B C17B 123.8(3) . . ? C39B N7B C28B 110.2(3) . . ? C39B N7B C27B 114.2(3) . . ? C28B N7B C27B 111.5(3) . . ? C39B N7B Fe4 108.31(19) . . ? C28B N7B Fe4 106.14(18) . . ? C27B N7B Fe4 106.03(18) . . ? C33B N8B C29B 118.0(3) . . ? C33B N8B Fe4 126.2(2) . . ? C29B N8B Fe4 115.6(2) . . ? C44B N9B C40B 117.4(3) . . ? C44B N9B Fe4 126.6(2) . . ? C40B N9B Fe4 114.07(19) . . ? C26B N10B N4B 107.5(2) . . ? C26B N10B Fe4 115.9(2) . . ? N4B N10B Fe4 134.54(19) . . ? C34B N11B C33B 122.2(3) . . ? C45B N12B C44B 127.8(3) . . ? N1B C1B C2B 110.4(3) . . ? N2B C2B C3B 122.2(3) . . ? N2B C2B C1B 116.6(2) . . ? C3B C2B C1B 121.2(3) . . ? C2B C3B C4B 118.7(3) . . ? C5B C4B C3B 120.1(3) . . ? C4B C5B C6B 118.1(3) . . ? N2B C6B C5B 122.4(3) . . ? N2B C6B N5B 115.6(2) . . ? C5B C6B N5B 122.0(3) . . ? O1B C7B N5B 122.4(3) . . ? O1B C7B C8B 121.3(3) . . ? N5B C7B C8B 116.3(3) . . ? C10B C8B C9B 111.2(3) . . ? C10B C8B C11B 109.5(4) . . ? C9B C8B C11B 108.4(3) . . ? C10B C8B C7B 106.7(3) . . ? C9B C8B C7B 112.8(3) . . ? C11B C8B C7B 108.0(3) . . ? N1B C12B C13B 111.8(3) . . ? N3B C13B C14B 121.7(4) . . ? N3B C13B C12B 117.7(3) . . ? C14B C13B C12B 120.6(3) . . ? C13B C14B C15B 119.4(4) . . ? C16B C15B C14B 119.9(4) . . ? C15B C16B C17B 118.1(4) . . ? N3B C17B C16B 122.0(3) . . ? N3B C17B N6B 115.0(3) . . ? C16B C17B N6B 123.0(3) . . ? O2B C18B N6B 122.5(3) . . ? O2B C18B C19B 123.0(3) . . ? N6B C18B C19B 114.3(3) . . ? C18B C19B C22B 111.2(3) . . ? C18B C19B C20B 108.5(3) . . ? C22B C19B C20B 110.4(3) . . ? C18B C19B C21B 106.9(3) . . ? C22B C19B C21B 110.4(3) . . ? C20B C19B C21B 109.3(3) . . ? N1B C23B C24B 108.6(2) . . ? N4B C24B C25B 110.3(3) . . ? N4B C24B C23B 116.9(3) . . ? C25B C24B C23B 132.7(3) . . ? C24B C25B C26B 103.7(3) . . ? N10B C26B C25B 110.7(3) . . ? N10B C26B C27B 117.5(3) . . ? C25B C26B C27B 131.8(3) . . ? N7B C27B C26B 108.1(3) . . ? N7B C28B C29B 110.0(3) . . ? N8B C29B C30B 123.8(3) . . ? N8B C29B C28B 115.1(3) . . ? C30B C29B C28B 121.1(3) . . ? C29B C30B C31B 117.9(3) . . ? C32B C31B C30B 119.6(3) . . ? C31B C32B C33B 120.0(4) . . ? N8B C33B N11B 123.1(3) . . ? N8B C33B C32B 120.7(3) . . ? N11B C33B C32B 116.1(3) . . ? O3B C34B N11B 128.5(3) . . ? O3B C34B C35B 115.1(3) . . ? N11B C34B C35B 116.4(3) . . ? C37B C35B C36B 131.2(6) . . ? C37B C35B C34B 110.9(4) . . ? C36B C35B C34B 110.3(4) . . ? C37B C35B C38B 97.9(7) . . ? C36B C35B C38B 93.5(6) . . ? C34B C35B C38B 107.6(4) . . ? N7B C39B C40B 112.3(3) . . ? N9B C40B C41B 122.9(3) . . ? N9B C40B C39B 117.4(3) . . ? C41B C40B C39B 119.6(3) . . ? C42B C41B C40B 118.5(3) . . ? C43B C42B C41B 119.4(3) . . ? C42B C43B C44B 119.1(3) . . ? N9B C44B C43B 122.3(3) . . ? N9B C44B N12B 120.4(3) . . ? C43B C44B N12B 117.3(3) . . ? O4B C45B N12B 122.6(3) . . ? O4B C45B C46B 119.5(3) . . ? N12B C45B C46B 117.8(3) . . ? C49B C46B C47B 109.8(4) . . ? C49B C46B C45B 106.1(3) . . ? C47B C46B C45B 115.6(3) . . ? C49B C46B C48B 110.0(5) . . ? C47B C46B C48B 108.4(4) . . ? C45B C46B C48B 106.7(3) . . ? O8 S1 O7 115.86(15) . . ? O8 S1 O6 113.86(15) . . ? O7 S1 O6 115.08(14) . . ? O8 S1 C50 103.85(17) . . ? O7 S1 C50 103.32(14) . . ? O6 S1 C50 102.48(14) . . ? F3 C50 F2 107.8(3) . . ? F3 C50 F1 107.4(3) . . ? F2 C50 F1 107.6(3) . . ? F3 C50 S1 111.5(3) . . ? F2 C50 S1 111.4(2) . . ? F1 C50 S1 111.0(2) . . ? O10 S2 O9 114.33(16) . . ? O10 S2 O11 115.94(18) . . ? O9 S2 O11 115.83(18) . . ? O10 S2 C51 102.89(19) . . ? O9 S2 C51 104.30(18) . . ? O11 S2 C51 100.7(3) . . ? O9 S2B O10 121.8(4) . . ? O9 S2B C51 119.0(3) . . ? O10 S2B C51 109.5(3) . . ? O9 S2B F5 125.5(3) . . ? O10 S2B F5 111.7(3) . . ? C51 S2B F5 42.0(3) . . ? C51 F5 S2B 54.3(3) . . ? S2B O9 S2 34.8(3) . . ? S2 O10 S2B 33.5(2) . . ? F4 C51 F6 106.4(4) . . ? F4 C51 F5 109.1(4) . . ? F6 C51 F5 109.6(4) . . ? F4 C51 S2B 126.7(3) . . ? F6 C51 S2B 117.6(3) . . ? F5 C51 S2B 83.7(4) . . ? F4 C51 S2 110.7(3) . . ? F6 C51 S2 110.0(4) . . ? F5 C51 S2 110.9(3) . . ? S2B C51 S2 27.5(2) . . ? O12 C52 C54 122.2(6) . . ? O12 C52 C53 119.3(5) . . ? C54 C52 C53 118.5(5) . . ? O13 C55 C57 117.0(12) . . ? O13 C55 C56 114.2(11) . . ? C57 C55 C56 128.8(12) . . ? C60 C58 O14 120.3(12) . . ? C60 C58 C59 116.6(12) . . ? O14 C58 C59 118.4(11) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.269 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.101 #===END data_asb175 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H69 Cl4 Co2 F3 N12 O8 S' _chemical_formula_weight 1338.91 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1790(4) _cell_length_b 30.5726(9) _cell_length_c 14.9417(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.8767(4) _cell_angle_gamma 90.00 _cell_volume 5963.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9895 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 24.91 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8254 _exptl_absorpt_correction_T_max 0.8948 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 68267 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.10 _reflns_number_total 13150 _reflns_number_gt 9829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+10.7478P] 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 13150 _refine_ls_number_parameters 813 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 1.200 _refine_ls_shift/su_mean 0.002 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 0.37693(3) 0.142727(12) 0.24431(3) 0.01789(10) Uani 1 1 d . . . Co2 Co 0.05570(3) 0.151657(13) 0.27100(3) 0.02366(11) Uani 1 1 d . . . O5 O 0.29603(15) 0.09334(7) 0.19594(14) 0.0228(4) Uani 1 1 d . . . H1 H 0.2435 0.0913 0.2218 0.034 Uiso 1 1 calc R . . O1 O 0.5642(2) -0.01320(9) 0.3123(2) 0.0564(8) Uani 1 1 d . . . O3 O 0.09945(17) 0.09078(7) 0.30188(19) 0.0369(6) Uani 1 1 d . C . O2 O 0.29444(18) 0.14379(8) -0.11972(15) 0.0337(5) Uani 1 1 d . . . O4 O 0.1189(2) 0.15290(12) 0.6347(2) 0.0622(9) Uani 1 1 d . . . N1 N 0.47972(18) 0.19572(8) 0.29647(16) 0.0223(5) Uani 1 1 d . . . N2 N 0.47732(18) 0.11218(8) 0.34905(16) 0.0212(5) Uani 1 1 d . . . N3 N 0.45457(18) 0.15671(8) 0.13198(16) 0.0201(5) Uani 1 1 d . . . N4 N 0.27683(18) 0.19083(8) 0.26879(17) 0.0215(5) Uani 1 1 d . . . N5 N 0.4503(2) 0.04257(8) 0.28868(18) 0.0280(6) Uani 1 1 d . . . H5B H 0.3935 0.0516 0.2560 0.034 Uiso 1 1 calc R . . N6 N 0.33262(18) 0.12263(8) 0.02708(17) 0.0221(5) Uani 1 1 d . . . H6A H 0.3117 0.1075 0.0712 0.027 Uiso 1 1 calc R . . N7 N -0.0280(2) 0.21089(9) 0.2230(2) 0.0313(6) Uani 1 1 d . . . N8 N -0.0359(2) 0.12951(10) 0.15965(19) 0.0340(7) Uani 1 1 d . . . N9 N -0.02424(18) 0.16871(9) 0.38057(18) 0.0256(6) Uani 1 1 d . . . N10 N 0.17155(18) 0.19367(8) 0.26045(18) 0.0236(5) Uani 1 1 d . . . N11 N -0.0187(2) 0.05302(11) 0.1970(3) 0.0460(9) Uani 1 1 d . C . N12 N 0.0846(2) 0.13046(10) 0.48850(19) 0.0312(6) Uani 1 1 d . . . H12A H 0.1037 0.1126 0.4478 0.037 Uiso 1 1 calc R . . C1 C 0.5017(2) 0.18778(10) 0.3944(2) 0.0264(7) Uani 1 1 d . . . H1A H 0.4428 0.1976 0.4240 0.032 Uiso 1 1 calc R . . H1B H 0.5626 0.2049 0.4200 0.032 Uiso 1 1 calc R . . C2 C 0.5211(2) 0.13982(10) 0.4130(2) 0.0236(6) Uani 1 1 d . . . C3 C 0.5777(2) 0.12557(12) 0.4925(2) 0.0318(7) Uani 1 1 d . . . H3A H 0.6084 0.1458 0.5363 0.038 Uiso 1 1 calc R . . C4 C 0.5883(3) 0.08099(13) 0.5064(2) 0.0363(8) Uani 1 1 d . . . H4A H 0.6244 0.0703 0.5614 0.044 Uiso 1 1 calc R . . C5 C 0.5469(2) 0.05211(12) 0.4409(2) 0.0310(7) Uani 1 1 d . . . H5C H 0.5550 0.0215 0.4497 0.037 Uiso 1 1 calc R . . C6 C 0.4924(2) 0.06866(10) 0.3610(2) 0.0251(6) Uani 1 1 d . . . C7 C 0.4919(3) 0.00371(11) 0.2654(3) 0.0361(8) Uani 1 1 d . A . C8 C 0.4467(3) -0.01694(11) 0.1763(3) 0.0553(12) Uani 1 1 d D . . C9 C 0.3251(4) -0.0187(3) 0.1695(6) 0.050(2) Uiso 0.525(7) 1 d PD A 1 H9A H 0.2985 0.0109 0.1765 0.075 Uiso 0.525(7) 1 calc PR A 1 H9B H 0.3058 -0.0376 0.2174 0.075 Uiso 0.525(7) 1 calc PR A 1 H9C H 0.2962 -0.0305 0.1105 0.075 Uiso 0.525(7) 1 calc PR A 1 C10 C 0.4534(7) 0.0183(2) 0.1020(4) 0.0412(18) Uiso 0.525(7) 1 d PD A 1 H10A H 0.4150 0.0444 0.1156 0.062 Uiso 0.525(7) 1 calc PR A 1 H10B H 0.4241 0.0066 0.0431 0.062 Uiso 0.525(7) 1 calc PR A 1 H10C H 0.5253 0.0261 0.1006 0.062 Uiso 0.525(7) 1 calc PR A 1 C11 C 0.4810(7) -0.0614(2) 0.1521(6) 0.054(2) Uiso 0.525(7) 1 d PD A 1 H11A H 0.4723 -0.0819 0.2009 0.081 Uiso 0.525(7) 1 calc PR A 1 H11B H 0.5534 -0.0603 0.1436 0.081 Uiso 0.525(7) 1 calc PR A 1 H11C H 0.4399 -0.0711 0.0960 0.081 Uiso 0.525(7) 1 calc PR A 1 C9B C 0.3946(7) -0.0583(2) 0.2058(6) 0.049(2) Uiso 0.475(7) 1 d PD A 2 H9BA H 0.3333 -0.0502 0.2325 0.073 Uiso 0.475(7) 1 calc PR A 2 H9BB H 0.4422 -0.0741 0.2507 0.073 Uiso 0.475(7) 1 calc PR A 2 H9BC H 0.3749 -0.0771 0.1532 0.073 Uiso 0.475(7) 1 calc PR A 2 C10B C 0.3998(7) 0.0108(3) 0.1003(5) 0.042(2) Uiso 0.475(7) 1 d PD A 2 H10D H 0.3383 0.0250 0.1168 0.063 Uiso 0.475(7) 1 calc PR A 2 H10E H 0.3810 -0.0074 0.0466 0.063 Uiso 0.475(7) 1 calc PR A 2 H10F H 0.4490 0.0332 0.0872 0.063 Uiso 0.475(7) 1 calc PR A 2 C11B C 0.5453(6) -0.0396(3) 0.1465(7) 0.054(3) Uiso 0.475(7) 1 d PD A 2 H11D H 0.5950 -0.0171 0.1353 0.081 Uiso 0.475(7) 1 calc PR A 2 H11E H 0.5254 -0.0565 0.0911 0.081 Uiso 0.475(7) 1 calc PR A 2 H11F H 0.5762 -0.0592 0.1946 0.081 Uiso 0.475(7) 1 calc PR A 2 C12 C 0.5715(2) 0.19135(11) 0.2511(2) 0.0247(6) Uani 1 1 d . . . H12B H 0.6163 0.1681 0.2808 0.030 Uiso 1 1 calc R . . H12C H 0.6105 0.2191 0.2564 0.030 Uiso 1 1 calc R . . C13 C 0.5418(2) 0.18023(10) 0.1528(2) 0.0230(6) Uani 1 1 d . . . C14 C 0.6018(2) 0.19274(10) 0.0885(2) 0.0277(7) Uani 1 1 d . . . H14A H 0.6606 0.2105 0.1044 0.033 Uiso 1 1 calc R . . C15 C 0.5744(2) 0.17894(10) 0.0004(2) 0.0273(7) Uani 1 1 d . . . H15A H 0.6166 0.1860 -0.0444 0.033 Uiso 1 1 calc R . . C16 C 0.4861(2) 0.15500(10) -0.0225(2) 0.0256(6) Uani 1 1 d . . . H16A H 0.4666 0.1454 -0.0829 0.031 Uiso 1 1 calc R . . C17 C 0.4258(2) 0.14517(9) 0.0447(2) 0.0213(6) Uani 1 1 d . . . C18 C 0.2719(2) 0.12287(10) -0.0558(2) 0.0246(6) Uani 1 1 d . B . C19 C 0.1742(2) 0.09541(12) -0.0653(2) 0.0387(9) Uani 1 1 d D . . C20 C 0.0897(5) 0.1165(2) -0.1306(5) 0.0509(18) Uiso 0.630(7) 1 d PD B 1 H20A H 0.0660 0.1431 -0.1034 0.076 Uiso 0.630(7) 1 calc PR B 1 H20B H 0.0325 0.0960 -0.1437 0.076 Uiso 0.630(7) 1 calc PR B 1 H20C H 0.1162 0.1240 -0.1869 0.076 Uiso 0.630(7) 1 calc PR B 1 C21 C 0.1402(5) 0.0760(2) 0.0205(4) 0.0487(18) Uiso 0.630(7) 1 d PD B 1 H21A H 0.1203 0.0997 0.0587 0.073 Uiso 0.630(7) 1 calc PR B 1 H21B H 0.1969 0.0594 0.0537 0.073 Uiso 0.630(7) 1 calc PR B 1 H21C H 0.0816 0.0565 0.0038 0.073 Uiso 0.630(7) 1 calc PR B 1 C22 C 0.2069(5) 0.05257(18) -0.1125(4) 0.0466(17) Uiso 0.630(7) 1 d PD B 1 H22A H 0.2256 0.0599 -0.1720 0.070 Uiso 0.630(7) 1 calc PR B 1 H22B H 0.1496 0.0319 -0.1198 0.070 Uiso 0.630(7) 1 calc PR B 1 H22C H 0.2658 0.0393 -0.0752 0.070 Uiso 0.630(7) 1 calc PR B 1 C20B C 0.1173(11) 0.1048(5) -0.1604(6) 0.063(4) Uiso 0.370(7) 1 d PD B 2 H20D H 0.1133 0.1365 -0.1702 0.095 Uiso 0.370(7) 1 calc PR B 2 H20E H 0.0479 0.0927 -0.1656 0.095 Uiso 0.370(7) 1 calc PR B 2 H20F H 0.1544 0.0913 -0.2058 0.095 Uiso 0.370(7) 1 calc PR B 2 C21B C 0.1100(9) 0.1249(4) -0.0092(8) 0.061(4) Uiso 0.370(7) 1 d PD B 2 H21D H 0.1063 0.1546 -0.0342 0.091 Uiso 0.370(7) 1 calc PR B 2 H21E H 0.1426 0.1258 0.0538 0.091 Uiso 0.370(7) 1 calc PR B 2 H21F H 0.0407 0.1130 -0.0119 0.091 Uiso 0.370(7) 1 calc PR B 2 C22B C 0.1811(13) 0.0510(3) -0.0194(11) 0.084(5) Uiso 0.370(7) 1 d PD B 2 H22D H 0.1132 0.0373 -0.0268 0.125 Uiso 0.370(7) 1 calc PR B 2 H22E H 0.2057 0.0546 0.0451 0.125 Uiso 0.370(7) 1 calc PR B 2 H22F H 0.2289 0.0323 -0.0468 0.125 Uiso 0.370(7) 1 calc PR B 2 C23 C 0.4271(2) 0.23826(10) 0.2772(2) 0.0273(7) Uani 1 1 d . . . H23A H 0.4429 0.2500 0.2189 0.033 Uiso 1 1 calc R . . H23B H 0.4517 0.2596 0.3252 0.033 Uiso 1 1 calc R . . C24 C 0.3140(2) 0.23195(10) 0.2731(2) 0.0254(6) Uani 1 1 d . . . C25 C 0.2352(3) 0.26213(11) 0.2672(2) 0.0336(8) Uani 1 1 d . . . H25A H 0.2400 0.2931 0.2685 0.040 Uiso 1 1 calc R . . C26 C 0.1478(2) 0.23674(10) 0.2590(2) 0.0301(7) Uani 1 1 d . . . C27 C 0.0364(3) 0.24933(11) 0.2523(3) 0.0373(8) Uani 1 1 d . . . H27A H 0.0211 0.2596 0.3119 0.045 Uiso 1 1 calc R . . H27B H 0.0213 0.2734 0.2083 0.045 Uiso 1 1 calc R . . C39 C -0.1247(2) 0.21013(12) 0.2615(2) 0.0347(8) Uani 1 1 d . . . H39A H -0.1737 0.1902 0.2257 0.042 Uiso 1 1 calc R . . H39B H -0.1550 0.2398 0.2586 0.042 Uiso 1 1 calc R . . C40 C -0.1066(2) 0.19502(10) 0.3577(2) 0.0269(7) Uani 1 1 d . . . C41 C -0.1722(2) 0.20653(11) 0.4186(2) 0.0314(7) Uani 1 1 d . . . H41A H -0.2274 0.2262 0.4017 0.038 Uiso 1 1 calc R . . C42 C -0.1559(2) 0.18887(12) 0.5046(2) 0.0345(8) Uani 1 1 d . . . H42A H -0.2024 0.1948 0.5464 0.041 Uiso 1 1 calc R . . C43 C -0.0716(2) 0.16266(13) 0.5293(2) 0.0356(8) Uani 1 1 d . . . H43A H -0.0585 0.1507 0.5885 0.043 Uiso 1 1 calc R . . C44 C -0.0060(2) 0.15401(11) 0.4659(2) 0.0294(7) Uani 1 1 d . . . C45 C 0.1466(3) 0.13355(13) 0.5713(2) 0.0383(8) Uani 1 1 d . . . C46 C 0.2480(3) 0.10916(12) 0.5784(2) 0.0346(8) Uani 1 1 d . . . C47 C 0.2978(2) 0.11298(12) 0.4916(2) 0.0347(8) Uani 1 1 d . . . H47A H 0.2514 0.1010 0.4406 0.052 Uiso 1 1 calc R . . H47B H 0.3623 0.0965 0.4988 0.052 Uiso 1 1 calc R . . H47C H 0.3116 0.1438 0.4800 0.052 Uiso 1 1 calc R . . C48 C 0.3218(3) 0.12825(14) 0.6573(3) 0.0430(9) Uani 1 1 d . . . H48A H 0.2913 0.1256 0.7133 0.065 Uiso 1 1 calc R . . H48B H 0.3345 0.1592 0.6455 0.065 Uiso 1 1 calc R . . H48C H 0.3866 0.1121 0.6635 0.065 Uiso 1 1 calc R . . C49 C 0.2247(3) 0.06124(14) 0.5983(3) 0.0466(10) Uani 1 1 d . . . H49A H 0.1966 0.0594 0.6556 0.070 Uiso 1 1 calc R . . H49B H 0.2880 0.0441 0.6026 0.070 Uiso 1 1 calc R . . H49C H 0.1748 0.0496 0.5495 0.070 Uiso 1 1 calc R . . C28 C -0.0462(3) 0.20590(13) 0.1240(2) 0.0393(9) Uani 1 1 d . . . H28A H 0.0176 0.2124 0.0983 0.047 Uiso 1 1 calc R . . H28B H -0.0996 0.2268 0.0979 0.047 Uiso 1 1 calc R . . C29 C -0.0799(3) 0.16018(14) 0.1009(2) 0.0388(9) Uani 1 1 d . . . C30 C -0.1493(3) 0.14960(19) 0.0263(3) 0.0623(14) Uani 1 1 d . . . H30A H -0.1795 0.1716 -0.0136 0.075 Uiso 1 1 calc R . . C31 C -0.1734(5) 0.1063(2) 0.0114(3) 0.088(2) Uani 1 1 d . . . H31A H -0.2209 0.0982 -0.0395 0.105 Uiso 1 1 calc R . . C32 C -0.1302(4) 0.07509(19) 0.0684(3) 0.0703(16) Uani 1 1 d . . . H32A H -0.1480 0.0453 0.0575 0.084 Uiso 1 1 calc R . . C33 C -0.0583(3) 0.08657(14) 0.1445(3) 0.0443(10) Uani 1 1 d . . . C34 C 0.0532(3) 0.05595(12) 0.2650(4) 0.0511(12) Uani 1 1 d . . . C35A C 0.0922(5) 0.0108(2) 0.2789(5) 0.0248(16) Uani 0.474(7) 1 d P C 1 C36A C 0.1141(6) -0.0145(2) 0.1955(5) 0.037(2) Uani 0.474(7) 1 d P C 1 H36A H 0.0526 -0.0147 0.1504 0.056 Uiso 0.474(7) 1 calc PR C 1 H36B H 0.1332 -0.0446 0.2127 0.056 Uiso 0.474(7) 1 calc PR C 1 H36C H 0.1704 -0.0004 0.1699 0.056 Uiso 0.474(7) 1 calc PR C 1 C37A C 0.0088(7) -0.0142(3) 0.3227(7) 0.043(2) Uani 0.474(7) 1 d P C 1 H37A H -0.0526 -0.0177 0.2782 0.064 Uiso 0.474(7) 1 calc PR C 1 H37B H -0.0085 0.0023 0.3747 0.064 Uiso 0.474(7) 1 calc PR C 1 H37C H 0.0350 -0.0431 0.3427 0.064 Uiso 0.474(7) 1 calc PR C 1 C38A C 0.1919(3) 0.01232(13) 0.3602(4) 0.0555(12) Uani 0.474(7) 1 d P C 1 H38A H 0.2528 0.0220 0.3348 0.083 Uiso 0.474(7) 1 calc PR C 1 H38B H 0.2038 -0.0170 0.3862 0.083 Uiso 0.474(7) 1 calc PR C 1 H38C H 0.1777 0.0328 0.4074 0.083 Uiso 0.474(7) 1 calc PR C 1 C35B C 0.0781(5) 0.0140(2) 0.3383(6) 0.0371(18) Uani 0.526(7) 1 d P C 2 C36B C 0.0162(6) 0.0173(2) 0.4183(5) 0.0424(19) Uani 0.526(7) 1 d P C 2 H36D H 0.0291 -0.0086 0.4568 0.064 Uiso 0.526(7) 1 calc PR C 2 H36E H -0.0570 0.0192 0.3954 0.064 Uiso 0.526(7) 1 calc PR C 2 H36F H 0.0372 0.0436 0.4537 0.064 Uiso 0.526(7) 1 calc PR C 2 C37B C 0.0472(7) -0.0270(3) 0.2856(7) 0.053(2) Uani 0.526(7) 1 d P C 2 H37D H 0.0587 -0.0525 0.3256 0.080 Uiso 0.526(7) 1 calc PR C 2 H37E H 0.0883 -0.0299 0.2360 0.080 Uiso 0.526(7) 1 calc PR C 2 H37F H -0.0255 -0.0253 0.2609 0.080 Uiso 0.526(7) 1 calc PR C 2 C38B C 0.1919(3) 0.01232(13) 0.3602(4) 0.0555(12) Uani 0.526(7) 1 d P C 2 H38D H 0.2106 0.0014 0.4219 0.083 Uiso 0.526(7) 1 calc PR C 2 H38E H 0.2201 0.0417 0.3553 0.083 Uiso 0.526(7) 1 calc PR C 2 H38F H 0.2197 -0.0073 0.3177 0.083 Uiso 0.526(7) 1 calc PR C 2 C50 C 0.7837(3) 0.14785(12) 0.7407(2) 0.0334(7) Uani 1 1 d . . . O6 O 0.7015(2) 0.20875(9) 0.82347(17) 0.0445(7) Uani 1 1 d . . . O7 O 0.6849(2) 0.21096(9) 0.66012(17) 0.0451(7) Uani 1 1 d . . . O8 O 0.5887(2) 0.15725(10) 0.7339(2) 0.0590(8) Uani 1 1 d . . . S1 S 0.67673(7) 0.18528(3) 0.73939(6) 0.0345(2) Uani 1 1 d . . . F1 F 0.77323(17) 0.12202(7) 0.66731(14) 0.0416(5) Uani 1 1 d . . . F2 F 0.87238(16) 0.16897(8) 0.74212(15) 0.0466(5) Uani 1 1 d . . . F3 F 0.79376(19) 0.12150(8) 0.81235(15) 0.0542(6) Uani 1 1 d . . . C51 C 0.2420(4) 0.27119(17) 0.5245(4) 0.0796(17) Uani 1 1 d . . . H51A H 0.2433 0.2936 0.4768 0.095 Uiso 1 1 calc R D 1 H51B H 0.2339 0.2866 0.5814 0.095 Uiso 1 1 calc R D 1 Cl1 Cl 0.35498(9) 0.24401(4) 0.53836(7) 0.0566(3) Uani 1 1 d . E . Cl2A Cl 0.13858(13) 0.23780(6) 0.49585(15) 0.0465(7) Uani 0.708(7) 1 d P E 1 Cl2B Cl 0.1208(5) 0.2675(5) 0.4690(3) 0.113(4) Uani 0.292(7) 1 d P E 2 C52 C -0.2505(3) 0.05150(14) 0.2731(4) 0.0612(13) Uani 1 1 d . . . H52A H -0.2869 0.0288 0.3036 0.073 Uiso 1 1 calc R F 1 H52B H -0.1896 0.0381 0.2520 0.073 Uiso 1 1 calc R F 1 Cl3A Cl -0.3403(3) 0.07665(12) 0.1722(4) 0.0618(11) Uani 0.553(9) 1 d P G 1 Cl4A Cl -0.2155(3) 0.09360(16) 0.3440(4) 0.0816(18) Uani 0.553(9) 1 d P G 1 Cl3B Cl -0.3166(3) 0.08780(15) 0.2213(4) 0.0578(12) Uani 0.447(9) 1 d P G 2 Cl4B Cl -0.1785(4) 0.07314(16) 0.3877(3) 0.0577(14) Uani 0.447(9) 1 d P G 2 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 0.01504(19) 0.01818(19) 0.0201(2) 0.00118(15) 0.00118(14) -0.00078(14) Co2 0.0154(2) 0.0252(2) 0.0305(2) -0.00179(17) 0.00401(16) 0.00259(15) O5 0.0190(10) 0.0225(11) 0.0272(11) -0.0009(9) 0.0040(8) -0.0028(8) O1 0.0626(19) 0.0335(15) 0.072(2) 0.0019(14) 0.0041(16) 0.0204(14) O3 0.0206(11) 0.0265(12) 0.0636(17) 0.0021(11) 0.0062(11) -0.0016(9) O2 0.0376(13) 0.0357(13) 0.0258(12) 0.0056(10) -0.0032(10) -0.0041(10) O4 0.0338(15) 0.109(3) 0.0421(17) -0.0221(17) -0.0001(12) 0.0219(16) N1 0.0197(12) 0.0253(13) 0.0213(13) 0.0006(10) 0.0013(10) -0.0029(10) N2 0.0178(12) 0.0262(13) 0.0195(12) 0.0041(10) 0.0023(9) 0.0000(10) N3 0.0187(12) 0.0192(12) 0.0217(12) 0.0015(10) 0.0006(9) -0.0015(9) N4 0.0172(12) 0.0199(12) 0.0268(13) -0.0001(10) 0.0010(10) 0.0002(9) N5 0.0267(14) 0.0249(14) 0.0321(15) 0.0055(11) 0.0024(11) 0.0011(11) N6 0.0215(13) 0.0243(13) 0.0203(12) -0.0004(10) 0.0015(10) -0.0012(10) N7 0.0208(13) 0.0347(15) 0.0386(16) 0.0024(12) 0.0049(11) 0.0095(11) N8 0.0240(14) 0.0488(18) 0.0312(15) -0.0072(13) 0.0113(12) -0.0049(12) N9 0.0157(12) 0.0307(14) 0.0299(14) -0.0044(11) 0.0013(10) 0.0019(10) N10 0.0180(12) 0.0214(13) 0.0311(14) -0.0002(10) 0.0028(10) 0.0036(10) N11 0.0350(18) 0.0399(18) 0.068(2) -0.0205(17) 0.0243(17) -0.0149(14) N12 0.0235(14) 0.0405(16) 0.0301(15) 0.0008(12) 0.0053(11) 0.0070(12) C1 0.0233(15) 0.0329(17) 0.0224(15) -0.0047(13) 0.0011(12) -0.0056(13) C2 0.0169(14) 0.0351(17) 0.0194(14) 0.0018(13) 0.0043(11) -0.0016(12) C3 0.0220(16) 0.050(2) 0.0231(16) 0.0006(15) 0.0011(12) -0.0032(14) C4 0.0263(17) 0.055(2) 0.0266(17) 0.0131(16) -0.0014(14) 0.0044(15) C5 0.0247(16) 0.0376(18) 0.0310(18) 0.0129(15) 0.0054(13) 0.0053(14) C6 0.0198(15) 0.0303(16) 0.0264(16) 0.0077(13) 0.0077(12) 0.0017(12) C7 0.045(2) 0.0210(16) 0.044(2) 0.0081(15) 0.0138(17) -0.0016(15) C8 0.081(3) 0.039(2) 0.050(3) -0.0098(19) 0.026(2) -0.026(2) C12 0.0170(14) 0.0320(17) 0.0246(16) 0.0021(13) 0.0013(12) -0.0058(12) C13 0.0202(14) 0.0223(15) 0.0262(16) 0.0029(12) 0.0021(12) 0.0003(11) C14 0.0209(15) 0.0300(17) 0.0321(17) 0.0052(13) 0.0034(13) -0.0047(12) C15 0.0260(16) 0.0296(16) 0.0282(16) 0.0055(13) 0.0106(13) 0.0000(13) C16 0.0283(16) 0.0270(16) 0.0214(15) 0.0008(12) 0.0034(12) 0.0011(12) C17 0.0221(14) 0.0189(14) 0.0227(15) 0.0013(11) 0.0022(11) 0.0022(11) C18 0.0267(16) 0.0242(15) 0.0233(15) -0.0078(12) 0.0046(12) 0.0036(12) C19 0.0267(17) 0.066(3) 0.0236(17) -0.0046(17) 0.0031(13) -0.0124(17) C23 0.0296(17) 0.0198(15) 0.0321(17) -0.0019(13) 0.0033(13) -0.0058(12) C24 0.0261(16) 0.0207(15) 0.0292(16) -0.0001(12) 0.0033(13) -0.0008(12) C25 0.0376(19) 0.0185(15) 0.045(2) -0.0010(14) 0.0088(16) 0.0028(13) C26 0.0267(16) 0.0219(15) 0.042(2) 0.0015(14) 0.0057(14) 0.0068(12) C27 0.0281(18) 0.0263(17) 0.058(2) 0.0032(16) 0.0098(16) 0.0096(14) C39 0.0213(16) 0.042(2) 0.041(2) -0.0004(16) 0.0052(14) 0.0117(14) C40 0.0182(15) 0.0281(16) 0.0345(18) -0.0047(13) 0.0036(13) 0.0024(12) C41 0.0197(15) 0.0340(18) 0.040(2) -0.0086(15) 0.0037(14) 0.0046(13) C42 0.0207(16) 0.044(2) 0.040(2) -0.0099(16) 0.0081(14) -0.0020(14) C43 0.0223(16) 0.050(2) 0.0342(19) -0.0050(16) 0.0041(14) -0.0003(15) C44 0.0200(15) 0.0350(18) 0.0330(18) -0.0053(14) 0.0023(13) 0.0011(13) C45 0.0247(17) 0.057(2) 0.0337(19) 0.0028(17) 0.0047(14) 0.0058(16) C46 0.0241(16) 0.046(2) 0.0349(19) 0.0117(16) 0.0082(14) 0.0042(14) C47 0.0216(16) 0.046(2) 0.0387(19) 0.0140(16) 0.0108(14) 0.0054(14) C48 0.0270(18) 0.066(3) 0.036(2) 0.0093(18) 0.0018(15) 0.0035(17) C49 0.041(2) 0.055(3) 0.046(2) 0.0251(19) 0.0166(18) 0.0043(18) C28 0.0256(17) 0.057(2) 0.036(2) 0.0131(17) 0.0051(14) 0.0134(16) C29 0.0244(17) 0.066(3) 0.0273(18) 0.0027(17) 0.0076(14) -0.0029(16) C30 0.046(2) 0.114(4) 0.027(2) 0.009(2) 0.0047(17) -0.023(3) C31 0.105(4) 0.130(5) 0.026(2) -0.001(3) 0.003(2) -0.077(4) C32 0.096(4) 0.088(4) 0.030(2) -0.019(2) 0.020(2) -0.057(3) C33 0.048(2) 0.053(2) 0.038(2) -0.0188(19) 0.0256(18) -0.0233(19) C34 0.0215(18) 0.0265(18) 0.108(4) -0.007(2) 0.019(2) -0.0051(14) C35A 0.021(3) 0.028(4) 0.027(4) -0.003(3) 0.008(3) -0.005(3) C36A 0.036(4) 0.035(4) 0.042(4) -0.014(3) 0.008(3) 0.002(3) C37A 0.032(4) 0.040(5) 0.060(6) 0.012(4) 0.022(4) -0.002(4) C38A 0.034(2) 0.0264(19) 0.104(4) 0.002(2) 0.003(2) -0.0005(16) C35B 0.033(4) 0.029(4) 0.050(5) 0.001(3) 0.009(3) -0.001(3) C36B 0.042(4) 0.036(4) 0.051(5) 0.010(3) 0.010(3) -0.008(3) C37B 0.048(5) 0.037(5) 0.072(7) -0.004(4) 0.005(5) -0.009(4) C38B 0.034(2) 0.0264(19) 0.104(4) 0.002(2) 0.003(2) -0.0005(16) C50 0.0403(19) 0.0365(19) 0.0225(16) 0.0039(14) 0.0014(13) -0.0079(15) O6 0.0571(17) 0.0495(16) 0.0309(14) -0.0100(12) 0.0198(12) -0.0145(13) O7 0.0632(18) 0.0410(15) 0.0334(14) 0.0034(11) 0.0152(13) 0.0140(13) O8 0.0390(16) 0.064(2) 0.074(2) -0.0093(16) 0.0077(15) -0.0178(14) S1 0.0393(5) 0.0363(5) 0.0297(4) -0.0045(4) 0.0110(4) -0.0073(4) F1 0.0534(13) 0.0332(11) 0.0359(11) -0.0043(9) -0.0018(10) 0.0047(9) F2 0.0369(12) 0.0501(13) 0.0528(14) -0.0007(11) 0.0065(10) -0.0138(10) F3 0.0652(16) 0.0599(15) 0.0345(12) 0.0224(11) -0.0038(11) -0.0097(12) C51 0.085(4) 0.051(3) 0.094(4) -0.023(3) -0.018(3) -0.004(3) Cl1 0.0707(7) 0.0536(6) 0.0502(6) -0.0213(5) 0.0255(5) -0.0191(5) Cl2A 0.0504(9) 0.0429(11) 0.0462(12) -0.0104(8) 0.0066(7) -0.0149(7) Cl2B 0.085(4) 0.208(12) 0.047(3) 0.041(4) 0.008(2) 0.004(5) C52 0.036(2) 0.039(2) 0.115(4) -0.012(2) 0.032(2) -0.0046(18) Cl3A 0.0470(14) 0.0502(16) 0.093(3) 0.0280(17) 0.0272(17) 0.0111(11) Cl4A 0.0428(15) 0.071(2) 0.134(4) -0.044(3) 0.022(2) -0.0129(15) Cl3B 0.0479(18) 0.0516(19) 0.078(3) 0.0201(19) 0.0243(19) 0.0178(14) Cl4B 0.049(2) 0.058(2) 0.069(2) -0.0168(17) 0.0163(15) -0.0127(17) _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 O5 1.931(2) . ? Co1 N4 2.042(2) . ? Co1 N2 2.122(2) . ? Co1 N3 2.125(2) . ? Co1 N1 2.186(2) . ? Co2 O3 1.984(2) . ? Co2 N10 2.018(3) . ? Co2 N8 2.033(3) . ? Co2 N9 2.130(3) . ? Co2 N7 2.190(3) . ? O1 C7 1.217(5) . ? O3 C34 1.310(4) . ? O2 C18 1.220(4) . ? O4 C45 1.214(4) . ? N1 C1 1.472(4) . ? N1 C12 1.472(4) . ? N1 C23 1.483(4) . ? N2 C2 1.345(4) . ? N2 C6 1.354(4) . ? N3 C17 1.354(4) . ? N3 C13 1.356(4) . ? N4 C24 1.348(4) . ? N4 N10 1.379(3) . ? N5 C7 1.373(4) . ? N5 C6 1.395(4) . ? N6 C18 1.379(4) . ? N6 C17 1.402(4) . ? N7 C39 1.468(4) . ? N7 C28 1.472(5) . ? N7 C27 1.481(4) . ? N8 C33 1.357(5) . ? N8 C29 1.359(5) . ? N9 C44 1.342(4) . ? N9 C40 1.357(4) . ? N10 C26 1.353(4) . ? N11 C34 1.294(6) . ? N11 C33 1.351(6) . ? N12 C45 1.389(4) . ? N12 C44 1.396(4) . ? C1 C2 1.508(4) . ? C2 C3 1.383(4) . ? C3 C4 1.383(5) . ? C4 C5 1.374(5) . ? C5 C6 1.400(4) . ? C7 C8 1.519(5) . ? C8 C10B 1.483(5) . ? C8 C11 1.491(5) . ? C8 C9B 1.534(5) . ? C8 C10 1.558(4) . ? C8 C11B 1.589(5) . ? C8 C9 1.593(5) . ? C12 C13 1.506(4) . ? C13 C14 1.379(4) . ? C14 C15 1.382(5) . ? C15 C16 1.378(4) . ? C16 C17 1.397(4) . ? C18 C19 1.527(4) . ? C19 C22B 1.519(5) . ? C19 C20 1.520(4) . ? C19 C21 1.534(4) . ? C19 C20B 1.540(5) . ? C19 C21B 1.559(5) . ? C19 C22 1.575(4) . ? C23 C24 1.496(4) . ? C24 C25 1.384(4) . ? C25 C26 1.380(5) . ? C26 C27 1.507(4) . ? C39 C40 1.498(5) . ? C40 C41 1.385(4) . ? C41 C42 1.383(5) . ? C42 C43 1.378(5) . ? C43 C44 1.393(5) . ? C45 C46 1.521(5) . ? C46 C49 1.534(5) . ? C46 C47 1.536(5) . ? C46 C48 1.537(5) . ? C28 C29 1.493(6) . ? C29 C30 1.380(5) . ? C30 C31 1.372(8) . ? C31 C32 1.352(8) . ? C32 C33 1.421(6) . ? C34 C35A 1.476(8) . ? C34 C35B 1.690(9) . ? C35A C36A 1.528(10) . ? C35A C37A 1.555(10) . ? C35A C38A 1.663(8) . ? C35B C37B 1.506(11) . ? C35B C36B 1.540(11) . ? C50 F3 1.331(4) . ? C50 F2 1.333(4) . ? C50 F1 1.344(4) . ? C50 S1 1.813(4) . ? O6 S1 1.445(3) . ? O7 S1 1.437(3) . ? O8 S1 1.436(3) . ? C51 Cl1 1.693(6) . ? C51 Cl2B 1.700(8) . ? C51 Cl2A 1.709(5) . ? C52 Cl3B 1.551(6) . ? C52 Cl4A 1.691(5) . ? C52 Cl3A 1.943(7) . ? C52 Cl4B 1.956(6) . ? 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 O5 Co1 N4 107.04(9) . . ? O5 Co1 N2 100.86(9) . . ? N4 Co1 N2 122.52(10) . . ? O5 Co1 N3 99.36(9) . . ? N4 Co1 N3 112.91(10) . . ? N2 Co1 N3 110.61(9) . . ? O5 Co1 N1 175.25(9) . . ? N4 Co1 N1 77.66(9) . . ? N2 Co1 N1 76.70(9) . . ? N3 Co1 N1 77.91(9) . . ? O3 Co2 N10 114.61(9) . . ? O3 Co2 N8 89.94(12) . . ? N10 Co2 N8 121.26(11) . . ? O3 Co2 N9 102.09(11) . . ? N10 Co2 N9 111.32(10) . . ? N8 Co2 N9 114.18(10) . . ? O3 Co2 N7 165.79(10) . . ? N10 Co2 N7 78.48(10) . . ? N8 Co2 N7 77.95(12) . . ? N9 Co2 N7 76.67(10) . . ? C34 O3 Co2 124.1(2) . . ? C1 N1 C12 112.4(2) . . ? C1 N1 C23 111.1(2) . . ? C12 N1 C23 112.4(2) . . ? C1 N1 Co1 105.06(18) . . ? C12 N1 Co1 106.07(18) . . ? C23 N1 Co1 109.29(17) . . ? C2 N2 C6 118.9(3) . . ? C2 N2 Co1 114.3(2) . . ? C6 N2 Co1 126.5(2) . . ? C17 N3 C13 118.4(3) . . ? C17 N3 Co1 127.35(19) . . ? C13 N3 Co1 114.23(19) . . ? C24 N4 N10 107.5(2) . . ? C24 N4 Co1 116.1(2) . . ? N10 N4 Co1 134.12(19) . . ? C7 N5 C6 124.1(3) . . ? C18 N6 C17 123.5(3) . . ? C39 N7 C28 111.2(3) . . ? C39 N7 C27 112.9(3) . . ? C28 N7 C27 112.8(3) . . ? C39 N7 Co2 106.5(2) . . ? C28 N7 Co2 104.4(2) . . ? C27 N7 Co2 108.46(19) . . ? C33 N8 C29 119.8(3) . . ? C33 N8 Co2 123.3(3) . . ? C29 N8 Co2 116.9(3) . . ? C44 N9 C40 118.1(3) . . ? C44 N9 Co2 127.2(2) . . ? C40 N9 Co2 114.5(2) . . ? C26 N10 N4 106.9(2) . . ? C26 N10 Co2 116.4(2) . . ? N4 N10 Co2 135.69(19) . . ? C34 N11 C33 125.8(3) . . ? C45 N12 C44 124.1(3) . . ? N1 C1 C2 110.4(2) . . ? N2 C2 C3 122.7(3) . . ? N2 C2 C1 115.7(3) . . ? C3 C2 C1 121.5(3) . . ? C4 C3 C2 118.1(3) . . ? C5 C4 C3 120.3(3) . . ? C4 C5 C6 118.8(3) . . ? N2 C6 N5 115.1(3) . . ? N2 C6 C5 121.1(3) . . ? N5 C6 C5 123.8(3) . . ? O1 C7 N5 122.0(4) . . ? O1 C7 C8 120.7(3) . . ? N5 C7 C8 117.4(3) . . ? C10B C8 C11 116.3(6) . . ? C10B C8 C7 120.4(4) . . ? C11 C8 C7 119.7(5) . . ? C10B C8 C9B 122.4(6) . . ? C11 C8 C9B 58.7(5) . . ? C7 C8 C9B 103.2(4) . . ? C10B C8 C10 28.0(4) . . ? C11 C8 C10 114.1(5) . . ? C7 C8 C10 106.5(4) . . ? C9B C8 C10 147.9(6) . . ? C10B C8 C11B 107.8(5) . . ? C11 C8 C11B 41.3(5) . . ? C7 C8 C11B 100.9(5) . . ? C9B C8 C11B 97.9(5) . . ? C10 C8 C11B 88.5(5) . . ? C10B C8 C9 70.1(5) . . ? C11 C8 C9 106.8(5) . . ? C7 C8 C9 109.9(4) . . ? C9B C8 C9 60.2(5) . . ? C10 C8 C9 97.6(5) . . ? C11B C8 C9 145.2(5) . . ? N1 C12 C13 110.5(2) . . ? N3 C13 C14 122.4(3) . . ? N3 C13 C12 116.3(3) . . ? C14 C13 C12 121.3(3) . . ? C13 C14 C15 118.7(3) . . ? C16 C15 C14 120.0(3) . . ? C15 C16 C17 118.7(3) . . ? N3 C17 C16 121.7(3) . . ? N3 C17 N6 115.6(3) . . ? C16 C17 N6 122.7(3) . . ? O2 C18 N6 122.1(3) . . ? O2 C18 C19 120.5(3) . . ? N6 C18 C19 117.3(3) . . ? C22B C19 C20 131.5(7) . . ? C22B C19 C18 116.9(7) . . ? C20 C19 C18 111.1(4) . . ? C22B C19 C21 44.2(7) . . ? C20 C19 C21 115.3(4) . . ? C18 C19 C21 118.3(3) . . ? C22B C19 C20B 125.1(9) . . ? C20 C19 C20B 26.7(6) . . ? C18 C19 C20B 106.3(6) . . ? C21 C19 C20B 132.9(7) . . ? C22B C19 C21B 106.1(8) . . ? C20 C19 C21B 72.3(6) . . ? C18 C19 C21B 98.3(5) . . ? C21 C19 C21B 62.1(6) . . ? C20B C19 C21B 99.0(8) . . ? C22B C19 C22 57.0(7) . . ? C20 C19 C22 106.6(4) . . ? C18 C19 C22 102.7(3) . . ? C21 C19 C22 100.5(4) . . ? C20B C19 C22 82.6(7) . . ? C21B C19 C22 157.6(6) . . ? N1 C23 C24 109.3(2) . . ? N4 C24 C25 110.7(3) . . ? N4 C24 C23 118.4(3) . . ? C25 C24 C23 130.7(3) . . ? C26 C25 C24 104.0(3) . . ? N10 C26 C25 110.9(3) . . ? N10 C26 C27 118.1(3) . . ? C25 C26 C27 130.9(3) . . ? N7 C27 C26 109.3(3) . . ? N7 C39 C40 110.4(3) . . ? N9 C40 C41 122.4(3) . . ? N9 C40 C39 116.2(3) . . ? C41 C40 C39 121.4(3) . . ? C42 C41 C40 118.7(3) . . ? C43 C42 C41 119.6(3) . . ? C42 C43 C44 118.7(3) . . ? N9 C44 C43 122.4(3) . . ? N9 C44 N12 116.1(3) . . ? C43 C44 N12 121.5(3) . . ? O4 C45 N12 121.7(3) . . ? O4 C45 C46 122.7(3) . . ? N12 C45 C46 115.6(3) . . ? C45 C46 C49 106.5(3) . . ? C45 C46 C47 112.2(3) . . ? C49 C46 C47 110.9(3) . . ? C45 C46 C48 108.9(3) . . ? C49 C46 C48 109.6(3) . . ? C47 C46 C48 108.7(3) . . ? N7 C28 C29 109.4(3) . . ? N8 C29 C30 122.5(4) . . ? N8 C29 C28 114.2(3) . . ? C30 C29 C28 123.4(4) . . ? C31 C30 C29 118.0(5) . . ? C32 C31 C30 120.7(4) . . ? C31 C32 C33 120.4(5) . . ? N11 C33 N8 125.4(4) . . ? N11 C33 C32 116.0(4) . . ? N8 C33 C32 118.5(4) . . ? N11 C34 O3 129.4(4) . . ? N11 C34 C35A 104.4(4) . . ? O3 C34 C35A 124.6(4) . . ? N11 C34 C35B 120.8(4) . . ? O3 C34 C35B 107.9(4) . . ? C35A C34 C35B 33.5(3) . . ? C34 C35A C36A 117.3(6) . . ? C34 C35A C37A 105.5(6) . . ? C36A C35A C37A 108.5(7) . . ? C34 C35A C38A 107.6(5) . . ? C36A C35A C38A 113.0(5) . . ? C37A C35A C38A 103.9(6) . . ? C37B C35B C36B 109.2(7) . . ? C37B C35B C34 106.2(6) . . ? C36B C35B C34 112.1(5) . . ? F3 C50 F2 106.8(3) . . ? F3 C50 F1 106.8(3) . . ? F2 C50 F1 106.8(3) . . ? F3 C50 S1 112.5(3) . . ? F2 C50 S1 111.9(2) . . ? F1 C50 S1 111.7(2) . . ? O8 S1 O7 115.46(19) . . ? O8 S1 O6 115.52(18) . . ? O7 S1 O6 114.32(16) . . ? O8 S1 C50 104.17(18) . . ? O7 S1 C50 102.01(16) . . ? O6 S1 C50 102.77(17) . . ? Cl1 C51 Cl2B 141.1(5) . . ? Cl1 C51 Cl2A 113.3(3) . . ? Cl2B C51 Cl2A 34.3(4) . . ? Cl3B C52 Cl4A 81.6(3) . . ? Cl3B C52 Cl3A 24.31(19) . . ? Cl4A C52 Cl3A 105.6(3) . . ? Cl3B C52 Cl4B 111.5(3) . . ? Cl4A C52 Cl4B 30.20(17) . . ? Cl3A C52 Cl4B 135.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.022 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.077