# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Hiroki Oshio' _publ_contact_author_address ;Graduate School of Pure and Applied Sciences, University of Tsukuba Tennodai 1-1-1, Tsukuba, Ibaraki 305-8571, Japan ; _publ_contact_author_email oshio@chem.tsukuba.ac.jp _publ_contact_author_phone +81-29-853-4238 _publ_contact_author_fax +81-29-853-4238 loop_ _publ_author_name _publ_author_address H.Oshio ;Graduate School of Pure and Applied Sciences, University of Tsukuba Tennodai 1-1-1, Tsukuba, Ibaraki 305-8571, Japan ; M.Nihei ;Graduate School of Pure and Applied Sciences, University of Tsukuba Tennodai 1-1-1, Tsukuba, Ibaraki 305-8571, Japan ; N.Takahashi ;Graduate School of Pure and Applied Sciences, University of Tsukuba Tennodai 1-1-1, Tsukuba, Ibaraki 305-8571, Japan ; H.Nishikawa ;College of Science, Ibaraki University Bunkyo 2-1-1, Mito, Ibaraki 310-8512, Japan ; data_a_dcc1tf _database_code_depnum_ccdc_archive 'CCDC 796347' #TrackingRef '- FedppTTF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H74 B2 Fe N11 O2.50 S8' _chemical_formula_weight 1671.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 monoclinic _symmetry_space_group_name_H-M P21/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 21.3301(18) _cell_length_b 22.1460(18) _cell_length_c 17.3065(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.123(2) _cell_angle_gamma 90.00 _cell_volume 8142.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1072 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 15.08 _exptl_crystal_description needle _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3476 _exptl_absorpt_coefficient_mu 0.448 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8772 _exptl_absorpt_correction_T_max 0.9565 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 55 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 510 _diffrn_standards_decay_% ? _diffrn_reflns_number 45908 _diffrn_reflns_av_R_equivalents 0.1533 _diffrn_reflns_av_sigmaI/netI 0.2493 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15968 _reflns_number_gt 5120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHLXTL' _computing_publication_material 'Bruker SHLXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The restrains to the anisotropic thermal displacement parameters were applied to the phenyl carbon atoms of counter anions by using the SHELXL SIMU command, because the anisotropic thermal displacement parameters for the atoms were relatively large due to disorders. ; _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^)+(0.1065P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15968 _refine_ls_number_parameters 964 _refine_ls_number_restraints 276 _refine_ls_R_factor_all 0.2552 _refine_ls_R_factor_gt 0.1026 _refine_ls_wR_factor_ref 0.2710 _refine_ls_wR_factor_gt 0.2129 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.879 _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 0.24289(5) 0.43027(4) 0.24669(7) 0.0439(4) Uani 1 1 d . . . S1 S 0.31481(11) 0.03335(9) 0.40041(13) 0.0537(6) Uani 1 1 d . . . S2 S 0.44703(11) -0.00552(9) 0.39583(13) 0.0538(6) Uani 1 1 d . . . S3 S 0.29321(12) -0.08257(9) 0.51518(15) 0.0644(7) Uani 1 1 d . . . S4 S 0.42704(12) -0.11674(9) 0.50895(14) 0.0578(7) Uani 1 1 d . . . S5 S 0.21689(13) 0.84804(10) 0.24125(18) 0.0810(9) Uani 1 1 d . . . S6 S 0.33508(13) 0.91511(10) 0.23435(17) 0.0774(8) Uani 1 1 d . . . S7 S 0.14023(19) 0.97634(14) 0.2231(3) 0.172(2) Uani 1 1 d . . . S8 S 0.25681(17) 1.03796(13) 0.1912(2) 0.1219(14) Uani 1 1 d . . . N1 N 0.2483(3) 0.3445(3) 0.2593(4) 0.0423(17) Uani 1 1 d . . . N2 N 0.3033(3) 0.4100(3) 0.1681(4) 0.0448(18) Uani 1 1 d . . . N3 N 0.3200(3) 0.3488(2) 0.1709(4) 0.0365(16) Uani 1 1 d . . . N4 N 0.1838(3) 0.4181(3) 0.3250(4) 0.0485(18) Uani 1 1 d . . . N5 N 0.1778(3) 0.3577(3) 0.3470(4) 0.0463(18) Uani 1 1 d . . . N6 N 0.2421(3) 0.5170(3) 0.2443(4) 0.0426(17) Uani 1 1 d . . . N7 N 0.3110(3) 0.4489(3) 0.3288(4) 0.0457(18) Uani 1 1 d . . . N8 N 0.3179(3) 0.5096(3) 0.3416(4) 0.0426(17) Uani 1 1 d . . . N9 N 0.1733(3) 0.4432(3) 0.1662(4) 0.060(2) Uani 1 1 d . . . N10 N 0.1630(3) 0.5039(3) 0.1488(4) 0.058(2) Uani 1 1 d . . . C1 C 0.2160(4) 0.3170(3) 0.3110(5) 0.039(2) Uani 1 1 d . . . C2 C 0.2239(4) 0.2575(3) 0.3284(5) 0.043(2) Uani 1 1 d . . . H2 H 0.1978 0.2382 0.3626 0.052 Uiso 1 1 calc R . . C3 C 0.2711(4) 0.2250(3) 0.2954(5) 0.043(2) Uani 1 1 d . . . C4 C 0.3047(4) 0.2546(3) 0.2411(5) 0.044(2) Uani 1 1 d . . . H4 H 0.3366 0.2341 0.2164 0.052 Uiso 1 1 calc R . . C5 C 0.2910(4) 0.3137(3) 0.2240(5) 0.037(2) Uani 1 1 d . . . C6 C 0.3574(4) 0.3361(4) 0.1156(5) 0.048(2) Uani 1 1 d . . . H6 H 0.3740 0.2975 0.1047 0.058 Uiso 1 1 calc R . . C7 C 0.3675(4) 0.3885(4) 0.0773(5) 0.051(2) Uani 1 1 d . . . H7 H 0.3930 0.3937 0.0355 0.062 Uiso 1 1 calc R . . C8 C 0.3331(4) 0.4326(4) 0.1116(5) 0.049(2) Uani 1 1 d . . . H8 H 0.3314 0.4737 0.0962 0.059 Uiso 1 1 calc R . . C9 C 0.1415(4) 0.3516(4) 0.4044(6) 0.064(3) Uani 1 1 d . . . H9 H 0.1316 0.3149 0.4289 0.077 Uiso 1 1 calc R . . C10 C 0.1210(5) 0.4078(5) 0.4220(7) 0.098(4) Uani 1 1 d . . . H10 H 0.0937 0.4180 0.4604 0.118 Uiso 1 1 calc R . . C11 C 0.1484(5) 0.4471(4) 0.3722(6) 0.073(3) Uani 1 1 d . . . H11 H 0.1425 0.4896 0.3720 0.087 Uiso 1 1 calc R . . C12 C 0.2872(4) 0.1633(3) 0.3248(5) 0.047(2) Uani 1 1 d . . . H12 H 0.2560 0.1414 0.3489 0.057 Uiso 1 1 calc R . . C13 C 0.3429(4) 0.1370(3) 0.3192(4) 0.042(2) Uani 1 1 d . . . H13 H 0.3713 0.1581 0.2896 0.051 Uiso 1 1 calc R . . C14 C 0.3653(4) 0.0807(3) 0.3522(4) 0.041(2) Uani 1 1 d . . . C15 C 0.4240(4) 0.0609(3) 0.3490(5) 0.050(2) Uani 1 1 d . . . H15 H 0.4529 0.0830 0.3213 0.060 Uiso 1 1 calc R . . C16 C 0.3752(4) -0.0190(3) 0.4330(5) 0.046(2) Uani 1 1 d . . . C17 C 0.3656(4) -0.0654(3) 0.4800(5) 0.051(2) Uani 1 1 d . . . C18 C 0.3224(5) -0.1458(3) 0.5667(5) 0.059(3) Uani 1 1 d . . . H18 H 0.2959 -0.1685 0.5971 0.071 Uiso 1 1 calc R . . C19 C 0.3813(5) -0.1617(3) 0.5633(5) 0.057(3) Uani 1 1 d . . . H19 H 0.3981 -0.1965 0.5895 0.068 Uiso 1 1 calc R . . C20 C 0.1995(4) 0.5450(4) 0.1940(5) 0.046(2) Uani 1 1 d . . . C21 C 0.1940(4) 0.6072(3) 0.1916(5) 0.049(2) Uani 1 1 d . . . H21 H 0.1640 0.6267 0.1562 0.058 Uiso 1 1 calc R . . C22 C 0.2347(4) 0.6405(3) 0.2440(5) 0.046(2) Uani 1 1 d . . . C23 C 0.2788(4) 0.6102(4) 0.2970(5) 0.054(2) Uani 1 1 d . . . H23 H 0.3063 0.6318 0.3333 0.065 Uiso 1 1 calc R . . C24 C 0.2797(4) 0.5486(3) 0.2932(4) 0.040(2) Uani 1 1 d . . . C25 C 0.3618(4) 0.5204(4) 0.4011(5) 0.061(3) Uani 1 1 d . . . H25 H 0.3750 0.5590 0.4203 0.073 Uiso 1 1 calc R . . C26 C 0.3841(4) 0.4660(4) 0.4290(5) 0.064(3) Uani 1 1 d . . . H26 H 0.4153 0.4590 0.4707 0.077 Uiso 1 1 calc R . . C27 C 0.3511(4) 0.4230(4) 0.3828(5) 0.048(2) Uani 1 1 d . . . H27 H 0.3564 0.3807 0.3889 0.058 Uiso 1 1 calc R . . C28 C 0.1146(5) 0.5124(4) 0.0934(6) 0.099(4) Uani 1 1 d . . . H28 H 0.0994 0.5496 0.0719 0.119 Uiso 1 1 calc R . . C29 C 0.0925(5) 0.4555(5) 0.0754(7) 0.108(4) Uani 1 1 d . . . H29 H 0.0573 0.4457 0.0401 0.130 Uiso 1 1 calc R . . C30 C 0.1309(5) 0.4152(4) 0.1181(6) 0.085(3) Uani 1 1 d . . . H30 H 0.1275 0.3725 0.1136 0.102 Uiso 1 1 calc R . . C31 C 0.2329(4) 0.7059(4) 0.2407(5) 0.058(3) Uani 1 1 d . . . H31 H 0.1928 0.7247 0.2315 0.070 Uiso 1 1 calc R . . C32 C 0.2832(4) 0.7414(4) 0.2496(4) 0.051(2) Uani 1 1 d . . . H32 H 0.3224 0.7213 0.2594 0.061 Uiso 1 1 calc R . . C33 C 0.2863(4) 0.8056(4) 0.2463(5) 0.056(2) Uani 1 1 d . . . C34 C 0.3378(5) 0.8386(4) 0.2436(6) 0.074(3) Uani 1 1 d . . . H34 H 0.3775 0.8190 0.2468 0.089 Uiso 1 1 calc R . . C35 C 0.2548(4) 0.9173(4) 0.2257(5) 0.064(3) Uani 1 1 d . . . C36 C 0.2237(5) 0.9689(5) 0.2123(7) 0.099(4) Uani 1 1 d . . . C37 C 0.1336(8) 1.0557(5) 0.2134(12) 0.198(10) Uani 1 1 d . . . H37 H 0.0964 1.0777 0.2210 0.238 Uiso 1 1 calc R . . C38 C 0.1847(7) 1.0805(5) 0.1950(8) 0.132(5) Uani 1 1 d . . . H38 H 0.1846 1.1224 0.1829 0.158 Uiso 1 1 calc R . . C39 C 0.0693(5) 0.2063(5) 0.4683(6) 0.075(3) Uani 1 1 d U . . C40 C 0.1283(6) 0.1796(6) 0.4585(7) 0.108(4) Uani 1 1 d U . . H40 H 0.1317 0.1516 0.4174 0.130 Uiso 1 1 calc R . . C41 C 0.1828(7) 0.1939(7) 0.5091(10) 0.139(6) Uani 1 1 d U . . H41 H 0.2226 0.1759 0.5034 0.166 Uiso 1 1 calc R . . C42 C 0.1744(9) 0.2351(7) 0.5663(9) 0.128(7) Uani 1 1 d U . . H42 H 0.2106 0.2454 0.5999 0.153 Uiso 1 1 calc R . . C43 C 0.1203(8) 0.2624(7) 0.5797(9) 0.133(6) Uani 1 1 d U . . H43 H 0.1174 0.2905 0.6208 0.160 Uiso 1 1 calc R . . C44 C 0.0667(6) 0.2460(5) 0.5271(7) 0.104(4) Uani 1 1 d U . . H44 H 0.0273 0.2642 0.5342 0.124 Uiso 1 1 calc R . . C45 C 0.0090(6) 0.1313(4) 0.3557(7) 0.089(3) Uani 1 1 d U . . C46 C -0.0353(5) 0.1277(5) 0.2830(8) 0.105(4) Uani 1 1 d U . . H46 H -0.0574 0.1633 0.2666 0.126 Uiso 1 1 calc R . . C47 C -0.0462(5) 0.0762(5) 0.2382(8) 0.115(4) Uani 1 1 d U . . H47 H -0.0722 0.0765 0.1907 0.138 Uiso 1 1 calc R . . C48 C -0.0159(7) 0.0229(5) 0.2679(10) 0.138(5) Uani 1 1 d U . . H48 H -0.0245 -0.0143 0.2418 0.165 Uiso 1 1 calc R . . C49 C 0.0290(7) 0.0239(5) 0.3392(8) 0.122(5) Uani 1 1 d U . . H49 H 0.0536 -0.0101 0.3562 0.146 Uiso 1 1 calc R . . C50 C 0.0317(5) 0.0763(4) 0.3769(7) 0.097(4) Uani 1 1 d U . . H50 H 0.0534 0.0747 0.4272 0.116 Uiso 1 1 calc R . . C51 C -0.0552(5) 0.1921(4) 0.4532(6) 0.062(3) Uani 1 1 d U . . C52 C -0.1131(5) 0.2196(5) 0.4270(6) 0.077(3) Uani 1 1 d U . . H52 H -0.1155 0.2411 0.3794 0.093 Uiso 1 1 calc R . . C53 C -0.1655(5) 0.2168(5) 0.4662(7) 0.088(3) Uani 1 1 d U . . H53 H -0.2029 0.2369 0.4464 0.106 Uiso 1 1 calc R . . C54 C -0.1644(6) 0.1846(6) 0.5355(8) 0.104(4) Uani 1 1 d U . . H54 H -0.2001 0.1833 0.5646 0.125 Uiso 1 1 calc R . . C55 C -0.1081(7) 0.1540(5) 0.5607(8) 0.106(4) Uani 1 1 d U . . H55 H -0.1063 0.1296 0.6060 0.127 Uiso 1 1 calc R . . C56 C -0.0567(6) 0.1593(5) 0.5204(7) 0.088(3) Uani 1 1 d U . . H56 H -0.0193 0.1390 0.5399 0.105 Uiso 1 1 calc R . . C57 C 0.0074(4) 0.2518(4) 0.3468(5) 0.052(2) Uani 1 1 d U . . C58 C -0.0135(5) 0.3079(4) 0.3609(6) 0.080(3) Uani 1 1 d U . . H58 H -0.0315 0.3141 0.4085 0.097 Uiso 1 1 calc R . . C59 C -0.0112(5) 0.3576(4) 0.3118(7) 0.085(3) Uani 1 1 d U . . H59 H -0.0281 0.3954 0.3256 0.102 Uiso 1 1 calc R . . C60 C 0.0143(6) 0.3514(5) 0.2467(7) 0.106(4) Uani 1 1 d U . . H60 H 0.0112 0.3831 0.2096 0.127 Uiso 1 1 calc R . . C61 C 0.0456(7) 0.2996(6) 0.2315(7) 0.121(4) Uani 1 1 d U . . H61 H 0.0706 0.2972 0.1888 0.146 Uiso 1 1 calc R . . C62 C 0.0397(6) 0.2497(5) 0.2812(7) 0.102(4) Uani 1 1 d U . . H62 H 0.0590 0.2127 0.2687 0.122 Uiso 1 1 calc R . . C63 C 0.4444(4) 0.6766(3) 0.4333(5) 0.037(2) Uani 1 1 d U . . C64 C 0.4477(4) 0.6410(4) 0.4991(5) 0.052(2) Uani 1 1 d U . . H64 H 0.4847 0.6179 0.5119 0.062 Uiso 1 1 calc R . . C65 C 0.4002(5) 0.6375(4) 0.5460(5) 0.055(2) Uani 1 1 d U . . H65 H 0.4049 0.6116 0.5899 0.066 Uiso 1 1 calc R . . C66 C 0.3455(5) 0.6703(4) 0.5325(5) 0.059(3) Uani 1 1 d U . . H66 H 0.3130 0.6684 0.5665 0.071 Uiso 1 1 calc R . . C67 C 0.3401(4) 0.7064(4) 0.4664(6) 0.056(2) Uani 1 1 d U . . H67 H 0.3029 0.7291 0.4536 0.067 Uiso 1 1 calc R . . C68 C 0.3897(4) 0.7091(3) 0.4189(5) 0.048(2) Uani 1 1 d U . . H68 H 0.3854 0.7345 0.3745 0.058 Uiso 1 1 calc R . . C69 C 0.5688(4) 0.6776(3) 0.4215(4) 0.0340(19) Uani 1 1 d U . . C70 C 0.6230(4) 0.6518(3) 0.3940(4) 0.044(2) Uani 1 1 d U . . H70 H 0.6188 0.6280 0.3482 0.053 Uiso 1 1 calc R . . C71 C 0.6827(4) 0.6605(3) 0.4326(5) 0.052(2) Uani 1 1 d U . . H71 H 0.7184 0.6417 0.4137 0.063 Uiso 1 1 calc R . . C72 C 0.6900(4) 0.6958(4) 0.4972(5) 0.055(2) Uani 1 1 d U . . H72 H 0.7307 0.7019 0.5229 0.067 Uiso 1 1 calc R . . C73 C 0.6385(4) 0.7226(3) 0.5254(5) 0.051(2) Uani 1 1 d U . . H73 H 0.6435 0.7475 0.5703 0.061 Uiso 1 1 calc R . . C74 C 0.5799(4) 0.7131(3) 0.4880(4) 0.045(2) Uani 1 1 d U . . H74 H 0.5448 0.7316 0.5085 0.054 Uiso 1 1 calc R . . C75 C 0.4854(3) 0.6101(3) 0.3249(4) 0.0358(19) Uani 1 1 d U . . C76 C 0.4392(3) 0.6073(3) 0.2640(4) 0.0358(19) Uani 1 1 d U . . H76 H 0.4180 0.6435 0.2479 0.043 Uiso 1 1 calc R . . C77 C 0.4217(4) 0.5535(3) 0.2248(5) 0.046(2) Uani 1 1 d U . . H77 H 0.3891 0.5536 0.1836 0.056 Uiso 1 1 calc R . . C78 C 0.4523(4) 0.5009(3) 0.2464(5) 0.043(2) Uani 1 1 d U . . H78 H 0.4411 0.4640 0.2207 0.052 Uiso 1 1 calc R . . C79 C 0.4997(4) 0.5023(3) 0.3062(5) 0.047(2) Uani 1 1 d U . . H79 H 0.5215 0.4661 0.3209 0.057 Uiso 1 1 calc R . . C80 C 0.5162(4) 0.5549(3) 0.3447(5) 0.048(2) Uani 1 1 d U . . H80 H 0.5489 0.5542 0.3857 0.058 Uiso 1 1 calc R . . C81 C 0.4999(3) 0.7319(3) 0.3151(5) 0.0349(19) Uani 1 1 d U . . C82 C 0.5142(4) 0.7274(3) 0.2382(5) 0.045(2) Uani 1 1 d U . . H82 H 0.5181 0.6883 0.2164 0.054 Uiso 1 1 calc R . . C83 C 0.5230(4) 0.7776(4) 0.1921(5) 0.058(2) Uani 1 1 d U . . H83 H 0.5345 0.7719 0.1409 0.069 Uiso 1 1 calc R . . C84 C 0.5156(4) 0.8342(4) 0.2184(6) 0.056(2) Uani 1 1 d U . . H84 H 0.5212 0.8684 0.1864 0.067 Uiso 1 1 calc R . . C85 C 0.4998(4) 0.8406(3) 0.2928(6) 0.055(2) Uani 1 1 d U . . H85 H 0.4939 0.8801 0.3123 0.066 Uiso 1 1 calc R . . C86 C 0.4920(4) 0.7917(3) 0.3405(5) 0.047(2) Uani 1 1 d . . . H86 H 0.4811 0.7986 0.3918 0.057 Uiso 1 1 calc R . . B1 B 0.0077(5) 0.1952(5) 0.4052(6) 0.061(3) Uani 1 1 d . . . B2 B 0.4981(4) 0.6740(3) 0.3739(5) 0.039(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0459(8) 0.0264(6) 0.0570(8) -0.0040(6) -0.0088(6) 0.0049(5) S1 0.0595(16) 0.0350(12) 0.0662(16) 0.0008(11) 0.0025(13) 0.0035(10) S2 0.0570(16) 0.0399(12) 0.0640(16) 0.0132(11) 0.0026(13) 0.0030(10) S3 0.0675(18) 0.0403(13) 0.0878(19) 0.0017(13) 0.0192(15) -0.0031(11) S4 0.0723(18) 0.0363(12) 0.0645(16) 0.0037(12) 0.0046(13) 0.0016(11) S5 0.0708(19) 0.0346(13) 0.141(3) 0.0090(15) 0.0253(18) -0.0038(12) S6 0.074(2) 0.0493(15) 0.109(2) -0.0153(15) 0.0097(17) -0.0197(13) S7 0.110(3) 0.066(2) 0.340(7) 0.046(3) 0.025(4) 0.003(2) S8 0.118(3) 0.0620(18) 0.173(3) 0.044(2) -0.057(2) -0.0354(18) N1 0.045(4) 0.028(4) 0.051(5) -0.003(3) -0.016(4) 0.007(3) N2 0.054(5) 0.024(3) 0.054(5) -0.008(3) -0.007(4) 0.005(3) N3 0.038(4) 0.025(4) 0.046(4) -0.003(3) -0.003(4) 0.012(3) N4 0.050(5) 0.028(4) 0.066(5) 0.010(4) -0.008(4) 0.008(3) N5 0.033(4) 0.051(5) 0.056(5) 0.002(4) 0.010(4) 0.003(3) N6 0.048(4) 0.035(4) 0.043(4) -0.009(3) -0.006(4) 0.002(3) N7 0.052(5) 0.028(4) 0.058(5) -0.002(3) 0.010(4) 0.002(3) N8 0.040(4) 0.044(4) 0.042(4) 0.004(3) -0.006(4) -0.008(3) N9 0.071(6) 0.031(4) 0.074(5) -0.008(4) -0.012(4) 0.004(4) N10 0.070(6) 0.053(5) 0.044(4) -0.012(4) -0.036(4) 0.004(4) C1 0.038(5) 0.029(4) 0.049(6) -0.003(4) -0.005(4) -0.008(4) C2 0.029(5) 0.043(5) 0.056(6) 0.003(4) -0.007(4) -0.007(4) C3 0.051(6) 0.030(5) 0.045(5) 0.001(4) -0.016(5) -0.004(4) C4 0.032(5) 0.032(4) 0.063(6) -0.007(4) -0.014(4) 0.003(4) C5 0.031(5) 0.034(5) 0.043(5) -0.013(4) -0.019(4) 0.008(4) C6 0.045(6) 0.040(5) 0.058(6) -0.006(5) -0.004(5) 0.012(4) C7 0.052(6) 0.055(6) 0.046(6) 0.011(5) 0.001(5) -0.003(5) C8 0.053(6) 0.030(5) 0.062(6) -0.001(5) -0.008(5) 0.007(4) C9 0.058(7) 0.051(6) 0.086(8) 0.010(5) 0.023(6) 0.023(5) C10 0.113(10) 0.066(7) 0.127(10) 0.024(7) 0.076(9) 0.029(7) C11 0.072(8) 0.058(6) 0.093(8) -0.005(6) 0.033(6) 0.027(5) C12 0.060(6) 0.031(5) 0.050(6) -0.001(4) -0.001(5) -0.004(4) C13 0.052(6) 0.039(5) 0.036(5) -0.005(4) 0.002(4) -0.008(4) C14 0.047(6) 0.026(4) 0.050(5) 0.004(4) 0.002(4) 0.000(4) C15 0.058(6) 0.031(4) 0.059(6) 0.010(4) -0.007(5) 0.001(4) C16 0.069(6) 0.015(4) 0.052(5) 0.000(4) 0.000(5) 0.005(4) C17 0.055(6) 0.029(4) 0.068(6) -0.019(4) -0.002(5) 0.010(4) C18 0.085(8) 0.034(5) 0.060(6) 0.001(4) 0.014(6) -0.002(5) C19 0.081(8) 0.030(5) 0.059(6) -0.004(4) 0.003(6) -0.011(5) C20 0.041(6) 0.048(5) 0.049(6) -0.002(4) -0.006(5) 0.004(4) C21 0.044(5) 0.038(5) 0.060(6) 0.015(4) -0.013(5) 0.001(4) C22 0.044(6) 0.032(4) 0.061(6) 0.002(4) -0.001(5) -0.005(4) C23 0.052(6) 0.045(5) 0.061(6) 0.004(5) -0.012(5) -0.003(4) C24 0.041(5) 0.041(5) 0.033(5) 0.005(4) -0.015(4) -0.003(4) C25 0.062(7) 0.058(6) 0.058(6) -0.005(5) -0.016(5) -0.014(5) C26 0.060(7) 0.062(6) 0.065(7) 0.015(5) -0.028(5) -0.003(5) C27 0.046(6) 0.052(5) 0.044(5) 0.019(5) -0.007(4) 0.000(4) C28 0.115(10) 0.049(6) 0.118(9) -0.017(6) -0.075(8) 0.011(6) C29 0.105(10) 0.067(7) 0.137(10) -0.029(7) -0.086(8) 0.010(6) C30 0.087(8) 0.039(5) 0.118(9) -0.008(6) -0.047(7) 0.010(5) C31 0.054(6) 0.042(5) 0.075(7) 0.007(5) -0.006(5) 0.001(4) C32 0.059(6) 0.042(5) 0.050(6) 0.004(4) -0.005(5) 0.002(4) C33 0.060(6) 0.038(5) 0.068(6) -0.012(4) -0.003(5) -0.007(5) C34 0.076(8) 0.045(6) 0.097(8) 0.001(5) -0.015(6) -0.003(5) C35 0.067(7) 0.034(5) 0.090(7) 0.002(5) 0.001(6) -0.018(4) C36 0.053(7) 0.069(7) 0.172(12) 0.042(8) -0.012(7) -0.021(6) C37 0.117(13) 0.066(9) 0.42(3) 0.078(13) 0.063(16) -0.018(8) C38 0.124(13) 0.072(9) 0.187(14) 0.031(9) -0.045(11) 0.015(8) C39 0.054(7) 0.085(7) 0.079(8) 0.038(6) -0.028(6) -0.025(6) C40 0.087(9) 0.138(10) 0.093(9) 0.070(8) -0.032(8) -0.046(8) C41 0.101(11) 0.167(14) 0.142(13) 0.108(11) -0.024(11) -0.050(11) C42 0.145(14) 0.125(13) 0.100(12) 0.053(10) -0.058(12) -0.065(11) C43 0.136(14) 0.152(13) 0.105(11) 0.041(9) -0.030(11) -0.037(11) C44 0.126(11) 0.100(9) 0.075(8) -0.006(7) -0.042(8) -0.049(7) C45 0.118(10) 0.051(6) 0.101(9) 0.009(6) 0.023(8) 0.011(6) C46 0.083(9) 0.073(8) 0.155(12) -0.034(8) -0.007(8) 0.001(6) C47 0.085(8) 0.046(6) 0.212(13) -0.053(8) -0.005(8) -0.015(6) C48 0.127(12) 0.068(8) 0.218(15) -0.068(9) 0.014(11) -0.028(8) C49 0.163(13) 0.043(7) 0.151(12) -0.013(7) -0.025(10) -0.021(7) C50 0.118(9) 0.041(6) 0.123(9) 0.000(6) -0.032(7) -0.008(6) C51 0.064(7) 0.049(5) 0.070(7) -0.011(5) -0.001(6) -0.023(5) C52 0.061(8) 0.108(8) 0.060(7) 0.001(6) -0.010(6) -0.025(6) C53 0.063(8) 0.112(9) 0.089(9) -0.012(7) 0.003(7) -0.035(7) C54 0.087(10) 0.110(10) 0.117(11) -0.016(9) 0.025(9) -0.027(8) C55 0.111(11) 0.101(9) 0.108(10) 0.016(8) 0.026(9) -0.009(8) C56 0.090(9) 0.073(7) 0.101(9) 0.005(7) 0.014(8) -0.018(6) C57 0.063(7) 0.046(5) 0.045(6) -0.016(5) -0.004(5) -0.006(4) C58 0.110(9) 0.044(6) 0.083(8) -0.011(6) -0.012(6) 0.010(6) C59 0.117(10) 0.048(6) 0.084(8) -0.022(6) -0.018(7) 0.016(6) C60 0.167(12) 0.077(8) 0.074(8) 0.008(7) 0.014(9) 0.037(8) C61 0.177(13) 0.085(9) 0.100(10) 0.004(8) 0.003(9) 0.022(9) C62 0.158(12) 0.050(7) 0.088(9) -0.013(7) -0.032(8) 0.008(7) C63 0.032(5) 0.034(4) 0.045(5) -0.018(4) -0.006(4) 0.001(4) C64 0.058(7) 0.050(5) 0.045(6) 0.001(5) -0.009(5) -0.009(4) C65 0.075(7) 0.041(5) 0.048(6) 0.008(4) -0.001(6) -0.001(5) C66 0.066(7) 0.059(6) 0.054(6) -0.021(5) 0.013(5) -0.008(5) C67 0.042(6) 0.052(5) 0.068(7) -0.021(5) -0.019(5) 0.008(4) C68 0.045(6) 0.040(5) 0.059(6) -0.018(4) -0.003(5) -0.006(4) C69 0.046(5) 0.019(4) 0.034(5) 0.008(3) -0.009(4) -0.001(3) C70 0.070(7) 0.027(4) 0.033(5) 0.000(4) -0.008(5) -0.012(4) C71 0.051(6) 0.045(5) 0.058(6) -0.003(5) -0.015(5) 0.006(4) C72 0.038(6) 0.059(6) 0.065(7) 0.015(5) -0.017(5) -0.016(4) C73 0.062(7) 0.043(5) 0.042(5) -0.006(4) -0.018(5) -0.011(4) C74 0.062(6) 0.028(4) 0.042(5) 0.000(4) -0.017(5) -0.007(4) C75 0.041(5) 0.027(4) 0.038(5) -0.003(4) -0.004(4) -0.008(3) C76 0.036(5) 0.024(4) 0.046(5) 0.004(4) -0.001(4) 0.004(3) C77 0.043(5) 0.036(5) 0.058(6) 0.005(4) -0.003(4) 0.003(4) C78 0.038(5) 0.028(4) 0.062(6) -0.011(4) -0.002(5) -0.001(4) C79 0.049(6) 0.023(4) 0.068(6) -0.007(4) -0.011(5) 0.005(4) C80 0.052(6) 0.031(4) 0.056(6) -0.002(4) -0.025(4) 0.005(4) C81 0.026(5) 0.033(4) 0.043(5) -0.004(4) -0.007(4) -0.002(3) C82 0.049(6) 0.033(4) 0.052(6) 0.005(4) 0.001(5) 0.011(4) C83 0.075(7) 0.052(6) 0.047(6) 0.012(5) 0.011(5) 0.016(5) C84 0.065(7) 0.035(5) 0.067(7) 0.018(5) 0.001(5) 0.007(4) C85 0.049(6) 0.031(5) 0.082(7) 0.001(5) -0.009(5) 0.002(4) C86 0.050(6) 0.027(4) 0.064(6) -0.001(4) -0.004(5) 0.002(4) B1 0.062(8) 0.054(7) 0.061(7) 0.002(6) -0.026(6) -0.009(5) B2 0.058(7) 0.013(4) 0.042(6) -0.001(4) -0.020(5) 0.003(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 N1 1.914(6) . ? Fe1 N6 1.920(6) . ? Fe1 N4 1.950(7) . ? Fe1 N9 1.963(7) . ? Fe1 N7 1.983(7) . ? Fe1 N2 2.006(7) . ? S1 C14 1.765(8) . ? S1 C16 1.787(8) . ? S2 C15 1.729(7) . ? S2 C16 1.739(9) . ? S3 C18 1.745(9) . ? S3 C17 1.750(9) . ? S4 C19 1.729(9) . ? S4 C17 1.774(8) . ? S5 C33 1.748(9) . ? S5 C35 1.766(8) . ? S6 C34 1.701(8) . ? S6 C35 1.706(9) . ? S7 C37 1.771(12) . ? S7 C36 1.815(11) . ? S8 C36 1.737(10) . ? S8 C38 1.810(13) . ? N1 C1 1.326(9) . ? N1 C5 1.329(9) . ? N2 C8 1.312(9) . ? N2 N3 1.401(7) . ? N3 C6 1.330(9) . ? N3 C5 1.389(9) . ? N4 C11 1.326(10) . ? N4 N5 1.400(8) . ? N5 C9 1.319(10) . ? N5 C1 1.399(9) . ? N6 C24 1.315(9) . ? N6 C20 1.352(9) . ? N7 C27 1.338(9) . ? N7 N8 1.369(7) . ? N8 C25 1.350(9) . ? N8 C24 1.410(9) . ? N9 C30 1.327(10) . ? N9 N10 1.389(8) . ? N10 C28 1.356(10) . ? N10 C20 1.394(9) . ? C1 C2 1.358(9) . ? C2 C3 1.399(10) . ? C2 H2 0.9500 . ? C3 C4 1.396(10) . ? C3 C12 1.488(10) . ? C4 C5 1.368(9) . ? C4 H4 0.9500 . ? C6 C7 1.363(10) . ? C6 H6 0.9500 . ? C7 C8 1.385(10) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.362(11) . ? C9 H9 0.9500 . ? C10 C11 1.390(12) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.335(10) . ? C12 H12 0.9500 . ? C13 C14 1.435(9) . ? C13 H13 0.9500 . ? C14 C15 1.332(10) . ? C15 H15 0.9500 . ? C16 C17 1.339(10) . ? C18 C19 1.310(11) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.383(10) . ? C21 C22 1.406(10) . ? C21 H21 0.9500 . ? C22 C23 1.420(10) . ? C22 C31 1.451(10) . ? C23 C24 1.368(10) . ? C23 H23 0.9500 . ? C25 C26 1.367(10) . ? C25 H25 0.9500 . ? C26 C27 1.392(10) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.371(12) . ? C28 H28 0.9500 . ? C29 C30 1.382(12) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.329(10) . ? C31 H31 0.9500 . ? C32 C33 1.425(10) . ? C32 H32 0.9500 . ? C33 C34 1.324(11) . ? C34 H34 0.9500 . ? C35 C36 1.331(12) . ? C37 C38 1.285(16) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.349(14) . ? C39 C40 1.414(15) . ? C39 B1 1.651(13) . ? C40 C41 1.428(16) . ? C40 H40 0.9500 . ? C41 C42 1.371(19) . ? C41 H41 0.9500 . ? C42 C43 1.34(2) . ? C42 H42 0.9500 . ? C43 C44 1.443(17) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.351(12) . ? C45 C46 1.506(15) . ? C45 B1 1.655(14) . ? C46 C47 1.387(13) . ? C46 H46 0.9500 . ? C47 C48 1.419(16) . ? C47 H47 0.9500 . ? C48 C49 1.493(17) . ? C48 H48 0.9500 . ? C49 C50 1.330(13) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C56 1.376(13) . ? C51 C52 1.414(13) . ? C51 B1 1.641(14) . ? C52 C53 1.360(13) . ? C52 H52 0.9500 . ? C53 C54 1.393(15) . ? C53 H53 0.9500 . ? C54 C55 1.414(16) . ? C54 H54 0.9500 . ? C55 C56 1.356(14) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.351(11) . ? C57 C62 1.380(13) . ? C57 B1 1.609(13) . ? C58 C59 1.393(13) . ? C58 H58 0.9500 . ? C59 C60 1.301(13) . ? C59 H59 0.9500 . ? C60 C61 1.364(14) . ? C60 H60 0.9500 . ? C61 C62 1.414(14) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C68 1.375(10) . ? C63 C64 1.381(10) . ? C63 B2 1.607(12) . ? C64 C65 1.356(11) . ? C64 H64 0.9500 . ? C65 C66 1.378(11) . ? C65 H65 0.9500 . ? C66 C67 1.391(11) . ? C66 H66 0.9500 . ? C67 C68 1.397(11) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C74 1.396(9) . ? C69 C70 1.409(10) . ? C69 B2 1.656(11) . ? C70 C71 1.398(10) . ? C70 H70 0.9500 . ? C71 C72 1.362(11) . ? C71 H71 0.9500 . ? C72 C73 1.376(11) . ? C72 H72 0.9500 . ? C73 C74 1.373(10) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 C76 1.378(9) . ? C75 C80 1.415(9) . ? C75 B2 1.659(10) . ? C76 C77 1.405(9) . ? C76 H76 0.9500 . ? C77 C78 1.372(9) . ? C77 H77 0.9500 . ? C78 C79 1.380(10) . ? C78 H78 0.9500 . ? C79 C80 1.373(9) . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? C81 C82 1.395(10) . ? C81 C86 1.411(9) . ? C81 B2 1.639(10) . ? C82 C83 1.392(10) . ? C82 H82 0.9500 . ? C83 C84 1.347(10) . ? C83 H83 0.9500 . ? C84 C85 1.367(11) . ? C84 H84 0.9500 . ? C85 C86 1.381(10) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N6 174.2(3) . . ? N1 Fe1 N4 79.6(3) . . ? N6 Fe1 N4 98.5(3) . . ? N1 Fe1 N9 105.0(3) . . ? N6 Fe1 N9 80.4(3) . . ? N4 Fe1 N9 91.1(3) . . ? N1 Fe1 N7 95.3(2) . . ? N6 Fe1 N7 79.2(3) . . ? N4 Fe1 N7 90.4(3) . . ? N9 Fe1 N7 159.5(3) . . ? N1 Fe1 N2 79.6(3) . . ? N6 Fe1 N2 102.4(3) . . ? N4 Fe1 N2 159.2(3) . . ? N9 Fe1 N2 92.4(3) . . ? N7 Fe1 N2 93.4(3) . . ? C14 S1 C16 94.6(4) . . ? C15 S2 C16 95.5(4) . . ? C18 S3 C17 93.8(4) . . ? C19 S4 C17 94.8(5) . . ? C33 S5 C35 94.4(4) . . ? C34 S6 C35 93.6(5) . . ? C37 S7 C36 98.7(6) . . ? C36 S8 C38 95.1(6) . . ? C1 N1 C5 119.5(7) . . ? C1 N1 Fe1 120.3(5) . . ? C5 N1 Fe1 119.5(6) . . ? C8 N2 N3 104.8(6) . . ? C8 N2 Fe1 143.5(5) . . ? N3 N2 Fe1 111.6(5) . . ? C6 N3 C5 133.5(6) . . ? C6 N3 N2 110.3(6) . . ? C5 N3 N2 116.0(6) . . ? C11 N4 N5 102.9(7) . . ? C11 N4 Fe1 143.1(6) . . ? N5 N4 Fe1 113.7(5) . . ? C9 N5 C1 132.3(7) . . ? C9 N5 N4 112.2(7) . . ? C1 N5 N4 115.1(7) . . ? C24 N6 C20 120.4(6) . . ? C24 N6 Fe1 120.9(5) . . ? C20 N6 Fe1 118.6(5) . . ? C27 N7 N8 104.7(6) . . ? C27 N7 Fe1 142.5(6) . . ? N8 N7 Fe1 112.5(5) . . ? C25 N8 N7 110.8(6) . . ? C25 N8 C24 132.1(7) . . ? N7 N8 C24 117.1(6) . . ? C30 N9 N10 103.3(7) . . ? C30 N9 Fe1 143.7(6) . . ? N10 N9 Fe1 113.0(5) . . ? C28 N10 N9 112.6(7) . . ? C28 N10 C20 131.1(7) . . ? N9 N10 C20 116.1(6) . . ? N1 C1 C2 122.2(8) . . ? N1 C1 N5 111.3(7) . . ? C2 C1 N5 126.4(8) . . ? C1 C2 C3 119.2(8) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 117.7(7) . . ? C4 C3 C12 122.9(8) . . ? C2 C3 C12 119.1(8) . . ? C5 C4 C3 118.8(8) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.3(8) . . ? N1 C5 N3 112.4(7) . . ? C4 C5 N3 125.3(8) . . ? N3 C6 C7 107.5(7) . . ? N3 C6 H6 126.3 . . ? C7 C6 H6 126.3 . . ? C6 C7 C8 106.2(8) . . ? C6 C7 H7 126.9 . . ? C8 C7 H7 126.9 . . ? N2 C8 C7 111.2(7) . . ? N2 C8 H8 124.4 . . ? C7 C8 H8 124.4 . . ? N5 C9 C10 107.2(9) . . ? N5 C9 H9 126.4 . . ? C10 C9 H9 126.4 . . ? C9 C10 C11 105.8(9) . . ? C9 C10 H10 127.1 . . ? C11 C10 H10 127.1 . . ? N4 C11 C10 111.9(9) . . ? N4 C11 H11 124.1 . . ? C10 C11 H11 124.1 . . ? C13 C12 C3 123.8(8) . . ? C13 C12 H12 118.1 . . ? C3 C12 H12 118.1 . . ? C12 C13 C14 128.1(8) . . ? C12 C13 H13 116.0 . . ? C14 C13 H13 116.0 . . ? C15 C14 C13 123.3(7) . . ? C15 C14 S1 116.1(6) . . ? C13 C14 S1 120.6(6) . . ? C14 C15 S2 119.3(7) . . ? C14 C15 H15 120.4 . . ? S2 C15 H15 120.4 . . ? C17 C16 S2 123.0(6) . . ? C17 C16 S1 123.0(7) . . ? S2 C16 S1 114.0(4) . . ? C16 C17 S3 124.5(6) . . ? C16 C17 S4 120.9(7) . . ? S3 C17 S4 114.6(5) . . ? C19 C18 S3 119.5(7) . . ? C19 C18 H18 120.3 . . ? S3 C18 H18 120.3 . . ? C18 C19 S4 117.4(7) . . ? C18 C19 H19 121.3 . . ? S4 C19 H19 121.3 . . ? N6 C20 C21 121.8(7) . . ? N6 C20 N10 111.7(7) . . ? C21 C20 N10 126.4(8) . . ? C20 C21 C22 117.2(7) . . ? C20 C21 H21 121.4 . . ? C22 C21 H21 121.4 . . ? C21 C22 C23 120.3(7) . . ? C21 C22 C31 119.0(7) . . ? C23 C22 C31 120.7(8) . . ? C24 C23 C22 116.8(8) . . ? C24 C23 H23 121.6 . . ? C22 C23 H23 121.6 . . ? N6 C24 C23 123.5(7) . . ? N6 C24 N8 110.1(6) . . ? C23 C24 N8 126.3(7) . . ? N8 C25 C26 107.9(7) . . ? N8 C25 H25 126.0 . . ? C26 C25 H25 126.0 . . ? C25 C26 C27 105.0(8) . . ? C25 C26 H26 127.5 . . ? C27 C26 H26 127.5 . . ? N7 C27 C26 111.6(7) . . ? N7 C27 H27 124.2 . . ? C26 C27 H27 124.2 . . ? N10 C28 C29 104.9(8) . . ? N10 C28 H28 127.5 . . ? C29 C28 H28 127.5 . . ? C28 C29 C30 107.2(9) . . ? C28 C29 H29 126.4 . . ? C30 C29 H29 126.4 . . ? N9 C30 C29 111.8(8) . . ? N9 C30 H30 124.1 . . ? C29 C30 H30 124.1 . . ? C32 C31 C22 124.6(8) . . ? C32 C31 H31 117.7 . . ? C22 C31 H31 117.7 . . ? C31 C32 C33 128.7(8) . . ? C31 C32 H32 115.6 . . ? C33 C32 H32 115.6 . . ? C34 C33 C32 126.4(9) . . ? C34 C33 S5 113.8(7) . . ? C32 C33 S5 119.8(7) . . ? C33 C34 S6 122.1(8) . . ? C33 C34 H34 119.0 . . ? S6 C34 H34 118.9 . . ? C36 C35 S6 121.4(7) . . ? C36 C35 S5 122.9(8) . . ? S6 C35 S5 115.6(5) . . ? C35 C36 S8 125.9(8) . . ? C35 C36 S7 122.6(7) . . ? S8 C36 S7 111.2(6) . . ? C38 C37 S7 112.7(12) . . ? C38 C37 H37 123.7 . . ? S7 C37 H37 123.7 . . ? C37 C38 S8 121.9(11) . . ? C37 C38 H38 119.0 . . ? S8 C38 H38 119.0 . . ? C44 C39 C40 117.4(10) . . ? C44 C39 B1 120.8(11) . . ? C40 C39 B1 121.5(11) . . ? C39 C40 C41 121.2(14) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 116.0(17) . . ? C42 C41 H41 122.0 . . ? C40 C41 H41 122.0 . . ? C43 C42 C41 126.5(18) . . ? C43 C42 H42 116.8 . . ? C41 C42 H42 116.8 . . ? C42 C43 C44 115.0(17) . . ? C42 C43 H43 122.5 . . ? C44 C43 H43 122.5 . . ? C39 C44 C43 123.8(14) . . ? C39 C44 H44 118.1 . . ? C43 C44 H44 118.1 . . ? C50 C45 C46 111.2(10) . . ? C50 C45 B1 130.8(11) . . ? C46 C45 B1 116.1(9) . . ? C47 C46 C45 124.9(11) . . ? C47 C46 H46 117.6 . . ? C45 C46 H46 117.6 . . ? C46 C47 C48 115.7(13) . . ? C46 C47 H47 122.2 . . ? C48 C47 H47 122.2 . . ? C47 C48 C49 121.6(10) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C50 C49 C48 114.5(11) . . ? C50 C49 H49 122.7 . . ? C48 C49 H49 122.7 . . ? C49 C50 C45 131.0(12) . . ? C49 C50 H50 114.5 . . ? C45 C50 H50 114.5 . . ? C56 C51 C52 114.4(10) . . ? C56 C51 B1 122.1(10) . . ? C52 C51 B1 123.4(10) . . ? C53 C52 C51 123.7(11) . . ? C53 C52 H52 118.2 . . ? C51 C52 H52 118.2 . . ? C52 C53 C54 120.1(12) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C53 C54 C55 117.3(13) . . ? C53 C54 H54 121.3 . . ? C55 C54 H54 121.3 . . ? C56 C55 C54 120.3(13) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C51 124.1(12) . . ? C55 C56 H56 117.9 . . ? C51 C56 H56 117.9 . . ? C58 C57 C62 112.1(9) . . ? C58 C57 B1 125.9(9) . . ? C62 C57 B1 121.1(9) . . ? C57 C58 C59 125.9(10) . . ? C57 C58 H58 117.0 . . ? C59 C58 H58 117.0 . . ? C60 C59 C58 118.9(10) . . ? C60 C59 H59 120.5 . . ? C58 C59 H59 120.5 . . ? C59 C60 C61 120.4(12) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? C60 C61 C62 117.9(13) . . ? C60 C61 H61 121.1 . . ? C62 C61 H61 121.1 . . ? C57 C62 C61 123.5(11) . . ? C57 C62 H62 118.2 . . ? C61 C62 H62 118.2 . . ? C68 C63 C64 115.4(8) . . ? C68 C63 B2 122.9(8) . . ? C64 C63 B2 121.4(7) . . ? C65 C64 C63 122.7(9) . . ? C65 C64 H64 118.6 . . ? C63 C64 H64 118.6 . . ? C64 C65 C66 122.4(9) . . ? C64 C65 H65 118.8 . . ? C66 C65 H65 118.8 . . ? C65 C66 C67 116.7(9) . . ? C65 C66 H66 121.7 . . ? C67 C66 H66 121.7 . . ? C66 C67 C68 119.8(8) . . ? C66 C67 H67 120.1 . . ? C68 C67 H67 120.1 . . ? C63 C68 C67 123.0(8) . . ? C63 C68 H68 118.5 . . ? C67 C68 H68 118.5 . . ? C74 C69 C70 115.1(7) . . ? C74 C69 B2 121.1(7) . . ? C70 C69 B2 123.4(7) . . ? C71 C70 C69 121.6(7) . . ? C71 C70 H70 119.2 . . ? C69 C70 H70 119.2 . . ? C72 C71 C70 120.2(8) . . ? C72 C71 H71 119.9 . . ? C70 C71 H71 119.9 . . ? C71 C72 C73 120.2(8) . . ? C71 C72 H72 119.9 . . ? C73 C72 H72 119.9 . . ? C74 C73 C72 119.2(8) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? C73 C74 C69 123.7(8) . . ? C73 C74 H74 118.1 . . ? C69 C74 H74 118.1 . . ? C76 C75 C80 115.6(6) . . ? C76 C75 B2 120.1(6) . . ? C80 C75 B2 124.1(6) . . ? C75 C76 C77 123.2(7) . . ? C75 C76 H76 118.4 . . ? C77 C76 H76 118.4 . . ? C78 C77 C76 119.3(7) . . ? C78 C77 H77 120.3 . . ? C76 C77 H77 120.3 . . ? C77 C78 C79 118.9(7) . . ? C77 C78 H78 120.5 . . ? C79 C78 H78 120.5 . . ? C80 C79 C78 121.5(7) . . ? C80 C79 H79 119.3 . . ? C78 C79 H79 119.3 . . ? C79 C80 C75 121.5(7) . . ? C79 C80 H80 119.3 . . ? C75 C80 H80 119.3 . . ? C82 C81 C86 114.0(7) . . ? C82 C81 B2 123.7(6) . . ? C86 C81 B2 122.2(7) . . ? C83 C82 C81 122.8(7) . . ? C83 C82 H82 118.6 . . ? C81 C82 H82 118.6 . . ? C84 C83 C82 121.7(8) . . ? C84 C83 H83 119.2 . . ? C82 C83 H83 119.2 . . ? C83 C84 C85 117.4(8) . . ? C83 C84 H84 121.3 . . ? C85 C84 H84 121.3 . . ? C84 C85 C86 122.3(8) . . ? C84 C85 H85 118.8 . . ? C86 C85 H85 118.8 . . ? C85 C86 C81 121.8(8) . . ? C85 C86 H86 119.1 . . ? C81 C86 H86 119.1 . . ? C57 B1 C51 113.1(8) . . ? C57 B1 C39 105.0(7) . . ? C51 B1 C39 108.0(8) . . ? C57 B1 C45 109.9(8) . . ? C51 B1 C45 106.2(7) . . ? C39 B1 C45 114.9(9) . . ? C63 B2 C81 115.3(6) . . ? C63 B2 C69 110.4(6) . . ? C81 B2 C69 101.5(6) . . ? C63 B2 C75 105.3(6) . . ? C81 B2 C75 111.2(6) . . ? C69 B2 C75 113.3(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.113 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.090 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 435 110 'corresponds to 2 MeNO2 and 1 Et2O molecules ' 2 0.822 0.505 0.079 33 2 'due to possible disorderes of solvent molecules ' 3 0.000 0.500 0.500 435 110 'corresponds to 2 MeNO2 and 1 Et2O molecules ' 4 0.178 0.005 0.420 33 2 'due to possible disorderes of solvent molecules ' 5 0.822 0.995 0.579 33 2 'due to possible disorderes of solvent molecules ' 6 0.178 0.495 0.920 33 2 'due to possible disorderes of solvent molecules ' _platon_squeeze_details ; ; data_dcmn2e _database_code_depnum_ccdc_archive 'CCDC 796348' #TrackingRef '- FedppTTF_F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H31 B F4 Fe N19 Ni2 S16' _chemical_formula_weight 1803.09 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' 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6883(15) _cell_length_b 14.9004(18) _cell_length_c 18.364(2) _cell_angle_alpha 89.572(3) _cell_angle_beta 83.176(3) _cell_angle_gamma 74.454(3) _cell_volume 3581.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 723 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 18.79 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1818 _exptl_absorpt_coefficient_mu 1.253 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7876 _exptl_absorpt_correction_T_max 0.9400 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366[pixels/mm] _diffrn_standards_number 46 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 510 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16246 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.2070 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 23.29 _reflns_number_total 10251 _reflns_number_gt 4252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1212P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10251 _refine_ls_number_parameters 956 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1848 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2499 _refine_ls_wR_factor_gt 0.2079 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.888 _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 Ni1 Ni 0.97560(16) 0.62302(16) 0.00905(12) 0.0718(7) Uani 1 1 d . . . Ni2 Ni 0.38944(14) 0.91467(13) 0.89505(9) 0.0472(5) Uani 1 1 d . . . Fe1 Fe 0.71981(12) 0.69553(12) 0.50006(8) 0.0234(4) Uani 1 1 d . . . S1 S 0.9345(2) 0.8673(3) 0.03041(17) 0.0417(9) Uani 1 1 d . . . S2 S 1.1492(3) 0.8640(3) -0.00765(19) 0.0467(10) Uani 1 1 d . . . S3 S 0.8876(3) 0.9471(3) -0.1304(2) 0.0585(11) Uani 1 1 d . . . S4 S 1.1011(3) 0.9459(3) -0.16619(19) 0.0556(11) Uani 1 1 d . . . S5 S 0.6291(3) 0.5579(3) 0.99101(18) 0.0476(10) Uani 1 1 d . . . S6 S 0.6333(3) 0.3695(2) 1.03932(18) 0.0459(10) Uani 1 1 d . . . S7 S 0.5578(3) 0.6354(3) 1.1582(2) 0.0607(11) Uani 1 1 d . . . S8 S 0.5934(3) 0.4434(3) 1.20827(18) 0.0513(10) Uani 1 1 d . . . S9 S 0.8425(3) 0.6121(3) 0.0836(2) 0.0540(11) Uani 1 1 d . . . S10 S 1.0789(3) 0.5711(3) 0.0939(3) 0.0726(13) Uani 1 1 d . . . S11 S 0.8718(3) 0.6682(3) -0.0722(2) 0.0522(10) Uani 1 1 d . . . S12 S 1.1081(3) 0.6289(3) -0.0583(3) 0.0732(14) Uani 1 1 d . . . S13 S 0.3732(3) 0.9939(3) 0.7971(2) 0.0632(12) Uani 1 1 d . . . S14 S 0.4124(3) 0.7869(3) 0.83417(18) 0.0498(10) Uani 1 1 d . . . S15 S 0.3500(3) 1.0448(3) 0.9552(2) 0.0558(11) Uani 1 1 d . . . S16 S 0.4241(3) 0.8355(3) 0.99203(19) 0.0544(11) Uani 1 1 d . . . F1 F 0.7408(7) 0.2517(6) 0.7946(4) 0.077(3) Uani 1 1 d . A . F2 F 0.8642(15) 0.240(3) 0.7009(8) 0.096(15) Uani 0.76(8) 1 d P A 1 F3 F 0.7545(18) 0.1534(17) 0.6997(9) 0.066(7) Uani 0.76(8) 1 d P A 1 F2' F 0.827(7) 0.310(7) 0.706(4) 0.10(3) Uani 0.24(8) 1 d P A 2 F3' F 0.812(11) 0.171(5) 0.705(4) 0.10(4) Uani 0.24(8) 1 d P A 2 F4 F 0.6992(7) 0.3045(7) 0.6853(5) 0.096(3) Uani 1 1 d . A . N1 N 0.7716(7) 0.7281(7) 0.4009(5) 0.029(2) Uani 1 1 d . . . N2 N 0.8773(8) 0.6542(7) 0.5008(6) 0.038(3) Uani 1 1 d . . . N3 N 0.9292(7) 0.6707(7) 0.4365(5) 0.032(3) Uani 1 1 d . . . N4 N 0.5868(8) 0.7510(7) 0.4519(5) 0.036(3) Uani 1 1 d . . . N5 N 0.6034(7) 0.7808(7) 0.3827(5) 0.031(2) Uani 1 1 d . . . N6 N 0.6871(7) 0.6592(7) 0.6029(5) 0.030(2) Uani 1 1 d . . . N7 N 0.7069(7) 0.5596(7) 0.4879(5) 0.037(3) Uani 1 1 d . . . N8 N 0.6916(7) 0.5185(7) 0.5541(5) 0.032(3) Uani 1 1 d . . . N9 N 0.7021(8) 0.8185(7) 0.5591(5) 0.039(3) Uani 1 1 d . . . N10 N 0.6883(8) 0.8057(7) 0.6331(5) 0.039(3) Uani 1 1 d . . . N11 N 0.7768(11) 0.5568(10) 0.2757(8) 0.074(4) Uani 1 1 d . . . N12 N 1.0739(10) 0.4997(10) 0.2871(10) 0.087(5) Uani 1 1 d . . . N13 N 0.8794(9) 0.7528(9) -0.2639(7) 0.061(4) Uani 1 1 d . . . N14 N 1.1790(13) 0.7081(12) -0.2430(10) 0.105(6) Uani 1 1 d . . . N15 N 0.3796(13) 0.9720(12) 0.5968(7) 0.110(6) Uani 1 1 d . . . N16 N 0.4352(9) 0.6914(10) 0.6448(6) 0.060(4) Uani 1 1 d . . . N17 N 0.3441(11) 1.1361(11) 1.1427(7) 0.076(5) Uani 1 1 d . . . N18 N 0.4501(13) 0.8659(12) 1.1888(7) 0.104(6) Uani 1 1 d . . . C1 C 0.7077(9) 0.7668(8) 0.3530(6) 0.027(3) Uani 1 1 d . . . C2 C 0.7398(10) 0.7914(8) 0.2839(6) 0.031(3) Uani 1 1 d . . . H2 H 0.6921 0.8183 0.2510 0.037 Uiso 1 1 calc R . . C3 C 0.8443(10) 0.7755(8) 0.2636(6) 0.031(3) Uani 1 1 d . . . C4 C 0.9116(9) 0.7334(8) 0.3122(6) 0.028(3) Uani 1 1 d . . . H4 H 0.9833 0.7208 0.2992 0.034 Uiso 1 1 calc R . . C5 C 0.8714(10) 0.7102(8) 0.3803(6) 0.031(3) Uani 1 1 d . . . C6 C 1.0294(10) 0.6470(9) 0.4405(8) 0.044(4) Uani 1 1 d . . . H6 H 1.0812 0.6519 0.4026 0.053 Uiso 1 1 calc R . . C7 C 1.0433(11) 0.6149(10) 0.5075(9) 0.058(4) Uani 1 1 d . . . H7 H 1.1068 0.5936 0.5267 0.069 Uiso 1 1 calc R . . C8 C 0.9486(11) 0.6187(9) 0.5435(7) 0.045(4) Uani 1 1 d . . . H8 H 0.9360 0.5986 0.5921 0.054 Uiso 1 1 calc R . . C9 C 0.5153(9) 0.8148(9) 0.3538(7) 0.039(3) Uani 1 1 d . . . H9 H 0.5077 0.8416 0.3070 0.046 Uiso 1 1 calc R . . C10 C 0.4402(10) 0.8035(10) 0.4043(7) 0.046(4) Uani 1 1 d . . . H10 H 0.3691 0.8189 0.4002 0.055 Uiso 1 1 calc R . . C11 C 0.4896(11) 0.7639(9) 0.4643(7) 0.046(4) Uani 1 1 d . . . H11 H 0.4553 0.7485 0.5088 0.056 Uiso 1 1 calc R . . C12 C 0.8819(10) 0.8003(9) 0.1907(6) 0.041(3) Uani 1 1 d . . . H12 H 0.8328 0.8188 0.1572 0.050 Uiso 1 1 calc R . . C13 C 0.9781(9) 0.7999(8) 0.1658(7) 0.036(3) Uani 1 1 d . . . H13 H 1.0276 0.7774 0.1984 0.043 Uiso 1 1 calc R . . C14 C 1.0146(9) 0.8287(9) 0.0974(7) 0.040(3) Uani 1 1 d . . . C15 C 1.1120(10) 0.8261(9) 0.0792(7) 0.042(3) Uani 1 1 d . . . H15 H 1.1606 0.8041 0.1126 0.051 Uiso 1 1 calc R . . C16 C 1.0278(9) 0.8884(9) -0.0357(7) 0.039(3) Uani 1 1 d . . . C17 C 1.0071(9) 0.9234(9) -0.1005(7) 0.041(3) Uani 1 1 d . . . C18 C 0.9257(16) 0.9915(11) -0.2139(8) 0.073(5) Uani 1 1 d . . . H18 H 0.8784 1.0142 -0.2480 0.087 Uiso 1 1 calc R . . C19 C 1.0217(15) 0.9925(12) -0.2283(8) 0.075(5) Uani 1 1 d . . . H19 H 1.0454 1.0186 -0.2720 0.090 Uiso 1 1 calc R . . C20 C 0.6809(9) 0.7199(8) 0.6579(7) 0.032(3) Uani 1 1 d . . . C21 C 0.6696(9) 0.6962(8) 0.7292(7) 0.036(3) Uani 1 1 d . . . H21 H 0.6642 0.7405 0.7675 0.043 Uiso 1 1 calc R . . C22 C 0.6661(10) 0.6061(9) 0.7451(7) 0.038(3) Uani 1 1 d . . . C23 C 0.6757(9) 0.5405(9) 0.6886(6) 0.037(3) Uani 1 1 d . . . H23 H 0.6758 0.4779 0.6986 0.044 Uiso 1 1 calc R . . C24 C 0.6850(8) 0.5712(9) 0.6177(6) 0.030(3) Uani 1 1 d . . . C25 C 0.6767(9) 0.4339(9) 0.5452(7) 0.041(3) Uani 1 1 d . . . H25 H 0.6657 0.3925 0.5829 0.049 Uiso 1 1 calc R . . C26 C 0.6802(11) 0.4187(10) 0.4714(8) 0.056(4) Uani 1 1 d . . . H26 H 0.6714 0.3659 0.4472 0.067 Uiso 1 1 calc R . . C27 C 0.6999(9) 0.4987(10) 0.4400(7) 0.045(4) Uani 1 1 d . . . H27 H 0.7075 0.5077 0.3886 0.054 Uiso 1 1 calc R . . C28 C 0.7033(11) 0.9055(10) 0.5532(9) 0.058(4) Uani 1 1 d . . . H28 H 0.7133 0.9340 0.5075 0.070 Uiso 1 1 calc R . . C29 C 0.6885(12) 0.9527(10) 0.6213(9) 0.062(4) Uani 1 1 d . . . H29 H 0.6858 1.0160 0.6307 0.075 Uiso 1 1 calc R . . C30 C 0.6789(10) 0.8871(10) 0.6699(8) 0.051(4) Uani 1 1 d . . . H30 H 0.6674 0.8960 0.7217 0.061 Uiso 1 1 calc R . . C31 C 0.6581(9) 0.5795(9) 0.8226(7) 0.038(3) Uani 1 1 d . . . H31 H 0.6487 0.6273 0.8587 0.046 Uiso 1 1 calc R . . C32 C 0.6629(9) 0.4943(9) 0.8461(6) 0.039(3) Uani 1 1 d . . . H32 H 0.6763 0.4455 0.8102 0.047 Uiso 1 1 calc R . . C33 C 0.6491(10) 0.4700(9) 0.9227(7) 0.043(3) Uani 1 1 d . . . C34 C 0.6516(10) 0.3848(10) 0.9476(7) 0.046(4) Uani 1 1 d . . . H34 H 0.6634 0.3336 0.9142 0.055 Uiso 1 1 calc R . . C35 C 0.6175(10) 0.4847(10) 1.0628(7) 0.044(4) Uani 1 1 d . . . C36 C 0.5932(10) 0.5181(10) 1.1352(7) 0.045(4) Uani 1 1 d . . . C37 C 0.5252(12) 0.6168(13) 1.2503(8) 0.070(5) Uani 1 1 d . . . H37 H 0.4966 0.6678 1.2839 0.084 Uiso 1 1 calc R . . C38 C 0.5406(11) 0.5322(12) 1.2721(8) 0.060(5) Uani 1 1 d . . . H38 H 0.5233 0.5193 1.3219 0.072 Uiso 1 1 calc R . . C39 C 0.8985(14) 0.5748(11) 0.1607(9) 0.076(5) Uani 1 1 d . . . C40 C 0.9996(12) 0.5596(12) 0.1633(10) 0.074(5) Uani 1 1 d . . . C41 C 0.8238(14) 0.5575(11) 0.2247(9) 0.061(5) Uani 1 1 d . . . C42 C 1.0439(15) 0.5235(14) 0.2329(12) 0.095(7) Uani 1 1 d . . . C43 C 0.9536(13) 0.6898(11) -0.1452(10) 0.075(5) Uani 1 1 d . . . C44 C 1.0595(14) 0.6737(11) -0.1405(9) 0.071(5) Uani 1 1 d . . . C45 C 0.9083(13) 0.7215(11) -0.2141(9) 0.067(5) Uani 1 1 d . . . C46 C 1.1282(13) 0.6914(14) -0.1986(11) 0.075(6) Uani 1 1 d . . . C47 C 0.3866(11) 0.9137(11) 0.7288(8) 0.055(4) Uani 1 1 d . . . C48 C 0.4078(10) 0.8223(10) 0.7445(7) 0.043(4) Uani 1 1 d . . . C49 C 0.3838(12) 0.9440(11) 0.6550(9) 0.065(5) Uani 1 1 d . . . C50 C 0.4229(11) 0.7502(12) 0.6886(8) 0.049(4) Uani 1 1 d . . . C51 C 0.3710(10) 1.0130(11) 1.0433(7) 0.050(4) Uani 1 1 d . . . C52 C 0.4027(10) 0.9206(11) 1.0589(7) 0.051(4) Uani 1 1 d . . . C53 C 0.3586(10) 1.0846(11) 1.1030(8) 0.044(4) Uani 1 1 d . . . C54 C 0.4255(12) 0.8902(11) 1.1329(9) 0.064(5) Uani 1 1 d . . . B1 B 0.7684(14) 0.2425(17) 0.7206(10) 0.052(5) Uani 1 1 d . . . N1S N 1.0952(12) 0.0814(10) 0.6035(8) 0.082(5) Uani 1 1 d . . . C1S C 0.8726(14) 0.1213(11) 0.5198(9) 0.069(5) Uani 1 1 d . . . H1S H 0.8497 0.1014 0.5665 0.082 Uiso 1 1 calc R . . C2S C 0.8062(14) 0.1454(12) 0.4674(11) 0.083(5) Uani 1 1 d . . . H2S H 0.7366 0.1454 0.4778 0.099 Uiso 1 1 calc R . . C3S C 0.8441(14) 0.1691(11) 0.4008(9) 0.068(5) Uani 1 1 d . . . H3S H 0.8004 0.1842 0.3634 0.082 Uiso 1 1 calc R . . C4S C 0.9412(14) 0.1719(12) 0.3859(9) 0.076(5) Uani 1 1 d . . . H4S H 0.9650 0.1897 0.3388 0.091 Uiso 1 1 calc R . . C5S C 1.0053(13) 0.1499(11) 0.4371(8) 0.064(5) Uani 1 1 d . . . H5S H 1.0745 0.1509 0.4260 0.077 Uiso 1 1 calc R . . C6S C 0.9708(12) 0.1261(10) 0.5047(8) 0.049(4) Uani 1 1 d . . . C7S C 1.0378(15) 0.1005(12) 0.5605(9) 0.073(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0682(15) 0.0724(17) 0.0761(16) -0.0078(12) -0.0136(12) -0.0185(12) Ni2 0.0577(13) 0.0495(13) 0.0347(11) 0.0001(9) -0.0085(9) -0.0138(10) Fe1 0.0263(10) 0.0297(11) 0.0153(9) 0.0097(7) -0.0048(8) -0.0084(8) S1 0.035(2) 0.060(3) 0.032(2) 0.0070(17) 0.0021(16) -0.0195(18) S2 0.036(2) 0.062(3) 0.041(2) 0.0093(18) 0.0044(17) -0.0154(18) S3 0.068(3) 0.073(3) 0.044(2) 0.011(2) -0.020(2) -0.031(2) S4 0.064(3) 0.058(3) 0.041(2) 0.0047(19) 0.013(2) -0.019(2) S5 0.070(3) 0.047(2) 0.028(2) 0.0055(16) -0.0015(18) -0.022(2) S6 0.063(3) 0.043(2) 0.030(2) 0.0068(16) -0.0008(18) -0.0133(19) S7 0.074(3) 0.058(3) 0.051(3) -0.011(2) 0.003(2) -0.025(2) S8 0.059(3) 0.069(3) 0.029(2) 0.0083(18) -0.0045(18) -0.025(2) S9 0.049(2) 0.068(3) 0.044(2) -0.0071(19) -0.0086(19) -0.012(2) S10 0.049(3) 0.077(3) 0.092(3) -0.027(3) 0.004(2) -0.022(2) S11 0.048(2) 0.063(3) 0.042(2) -0.0030(19) -0.0076(19) -0.009(2) S12 0.045(3) 0.073(3) 0.103(4) -0.029(3) -0.004(2) -0.020(2) S13 0.099(3) 0.045(3) 0.050(3) 0.0122(19) -0.027(2) -0.019(2) S14 0.073(3) 0.048(2) 0.028(2) 0.0065(17) -0.0095(19) -0.014(2) S15 0.054(3) 0.058(3) 0.050(2) -0.009(2) -0.012(2) -0.002(2) S16 0.075(3) 0.063(3) 0.032(2) 0.0075(18) -0.014(2) -0.027(2) F1 0.091(7) 0.093(8) 0.044(6) -0.004(5) -0.002(5) -0.019(5) F2 0.035(11) 0.17(4) 0.086(11) 0.030(13) -0.006(8) -0.042(15) F3 0.092(14) 0.049(11) 0.066(9) -0.009(7) -0.011(8) -0.033(8) F2' 0.08(4) 0.07(5) 0.14(5) 0.08(4) 0.02(4) -0.01(4) F3' 0.17(12) 0.04(4) 0.10(4) 0.02(3) 0.01(5) -0.05(5) F4 0.097(8) 0.098(8) 0.089(7) 0.031(6) -0.034(6) -0.012(6) N1 0.026(6) 0.037(7) 0.024(6) 0.000(5) -0.002(5) -0.008(5) N2 0.041(7) 0.040(7) 0.034(7) 0.008(5) -0.016(6) -0.010(5) N3 0.029(7) 0.041(7) 0.025(6) 0.005(5) -0.008(5) -0.002(5) N4 0.028(7) 0.044(7) 0.037(7) 0.015(5) -0.002(5) -0.010(5) N5 0.033(7) 0.034(7) 0.022(6) 0.008(5) 0.000(5) -0.005(5) N6 0.036(6) 0.031(7) 0.026(6) 0.003(5) -0.005(5) -0.014(5) N7 0.040(7) 0.046(7) 0.021(6) 0.000(5) -0.009(5) -0.004(5) N8 0.041(7) 0.041(7) 0.021(6) 0.005(5) -0.010(5) -0.020(5) N9 0.048(7) 0.036(8) 0.031(7) 0.016(5) -0.005(5) -0.010(5) N10 0.059(8) 0.027(7) 0.034(7) 0.000(5) -0.008(6) -0.017(6) N11 0.081(11) 0.082(11) 0.064(10) 0.017(8) 0.007(9) -0.037(9) N12 0.060(10) 0.065(11) 0.136(15) 0.036(10) -0.030(10) -0.008(8) N13 0.058(9) 0.062(9) 0.064(9) 0.022(7) -0.011(7) -0.015(7) N14 0.078(13) 0.115(15) 0.117(15) 0.050(12) -0.027(11) -0.014(11) N15 0.170(17) 0.133(15) 0.043(9) 0.048(10) -0.034(10) -0.064(13) N16 0.065(9) 0.093(12) 0.027(7) -0.002(7) -0.003(7) -0.029(8) N17 0.078(11) 0.103(14) 0.054(10) -0.029(8) 0.002(8) -0.039(10) N18 0.176(17) 0.135(15) 0.040(9) 0.037(9) -0.043(10) -0.098(13) C1 0.025(7) 0.029(8) 0.023(7) 0.004(6) 0.002(6) -0.003(6) C2 0.049(9) 0.016(7) 0.028(7) -0.004(5) -0.009(7) -0.005(6) C3 0.039(8) 0.032(8) 0.025(7) -0.003(6) 0.001(7) -0.014(6) C4 0.024(7) 0.022(7) 0.034(8) -0.001(6) 0.004(6) -0.002(5) C5 0.041(9) 0.024(8) 0.027(7) 0.006(6) -0.011(7) -0.005(6) C6 0.026(8) 0.047(9) 0.055(10) 0.010(7) -0.009(7) -0.001(7) C7 0.034(9) 0.068(12) 0.077(12) 0.029(9) -0.034(9) -0.012(8) C8 0.054(10) 0.047(10) 0.035(8) 0.007(7) -0.024(8) -0.008(7) C9 0.034(8) 0.044(9) 0.036(8) 0.015(6) -0.014(7) -0.004(7) C10 0.029(8) 0.061(10) 0.049(9) -0.003(8) -0.003(8) -0.014(7) C11 0.044(10) 0.054(10) 0.041(9) 0.015(7) 0.006(8) -0.018(8) C12 0.054(10) 0.047(9) 0.024(8) -0.001(6) -0.005(7) -0.015(7) C13 0.029(8) 0.036(8) 0.040(8) 0.000(6) 0.000(7) -0.006(6) C14 0.025(8) 0.055(10) 0.033(8) -0.003(7) 0.018(6) -0.009(7) C15 0.049(9) 0.042(9) 0.035(8) 0.001(6) -0.008(7) -0.010(7) C16 0.041(8) 0.046(9) 0.030(8) 0.000(6) 0.006(7) -0.017(7) C17 0.040(8) 0.040(9) 0.046(9) 0.006(7) 0.006(7) -0.018(7) C18 0.129(17) 0.050(11) 0.048(10) 0.008(8) -0.044(11) -0.026(11) C19 0.107(15) 0.090(15) 0.040(10) 0.007(9) -0.014(11) -0.045(12) C20 0.048(9) 0.025(8) 0.033(8) 0.006(6) -0.009(6) -0.023(6) C21 0.044(8) 0.028(8) 0.034(8) -0.007(6) -0.003(6) -0.009(6) C22 0.054(9) 0.032(9) 0.029(8) -0.004(6) 0.001(7) -0.015(7) C23 0.055(9) 0.027(8) 0.031(8) 0.019(6) -0.008(7) -0.013(6) C24 0.018(7) 0.032(8) 0.035(8) -0.005(6) -0.004(6) 0.003(6) C25 0.049(9) 0.043(10) 0.039(9) 0.008(7) -0.019(7) -0.022(7) C26 0.078(11) 0.046(10) 0.057(11) 0.006(8) -0.018(9) -0.039(9) C27 0.050(9) 0.070(11) 0.015(7) 0.003(7) -0.012(7) -0.010(8) C28 0.076(12) 0.037(10) 0.065(11) 0.024(9) -0.032(9) -0.011(8) C29 0.093(13) 0.031(10) 0.070(12) 0.004(9) -0.021(10) -0.025(9) C30 0.067(11) 0.033(10) 0.050(9) 0.000(8) -0.005(8) -0.010(8) C31 0.050(9) 0.039(9) 0.027(7) 0.005(6) -0.005(6) -0.016(7) C32 0.052(9) 0.051(10) 0.014(7) 0.002(6) 0.003(6) -0.014(7) C33 0.049(9) 0.044(10) 0.031(8) -0.005(7) -0.001(7) -0.006(7) C34 0.070(10) 0.044(10) 0.028(8) 0.012(7) -0.018(7) -0.019(8) C35 0.044(9) 0.064(10) 0.021(7) 0.011(7) 0.004(6) -0.015(7) C36 0.051(9) 0.060(10) 0.029(8) 0.008(7) -0.002(7) -0.026(8) C37 0.084(13) 0.096(15) 0.040(10) -0.030(9) -0.001(9) -0.046(11) C38 0.073(12) 0.080(14) 0.037(9) 0.005(9) -0.001(8) -0.042(10) C39 0.083(14) 0.058(12) 0.082(13) -0.020(10) -0.004(11) -0.013(10) C40 0.049(11) 0.072(13) 0.105(15) 0.001(10) -0.038(11) -0.012(9) C41 0.078(13) 0.058(11) 0.049(11) 0.013(9) -0.010(10) -0.022(10) C42 0.077(14) 0.083(16) 0.125(19) 0.044(14) -0.024(14) -0.017(11) C43 0.065(12) 0.052(12) 0.104(15) -0.013(10) -0.034(11) -0.001(9) C44 0.089(14) 0.064(12) 0.065(12) -0.005(9) -0.008(11) -0.031(10) C45 0.077(13) 0.058(12) 0.050(11) 0.009(9) -0.011(10) 0.010(9) C46 0.050(12) 0.099(16) 0.076(14) -0.014(11) 0.014(10) -0.030(11) C47 0.064(10) 0.057(11) 0.046(10) 0.019(8) -0.011(8) -0.019(8) C48 0.050(9) 0.056(11) 0.027(8) 0.000(7) -0.006(7) -0.019(8) C49 0.089(13) 0.074(13) 0.048(11) 0.014(9) -0.015(10) -0.046(10) C50 0.053(10) 0.070(12) 0.028(9) 0.017(8) -0.013(8) -0.020(8) C51 0.042(9) 0.074(12) 0.038(9) -0.017(8) 0.006(7) -0.026(8) C52 0.047(9) 0.066(12) 0.043(9) 0.003(8) -0.008(7) -0.019(8) C53 0.021(8) 0.054(11) 0.045(10) -0.001(8) 0.019(7) 0.001(7) C54 0.090(13) 0.064(12) 0.047(10) 0.006(9) -0.019(10) -0.034(10) B1 0.044(13) 0.061(16) 0.042(12) 0.024(11) -0.009(10) 0.004(11) N1S 0.123(13) 0.062(10) 0.067(11) 0.012(8) -0.030(10) -0.025(9) C1S 0.077(13) 0.075(13) 0.043(10) -0.012(9) 0.026(10) -0.017(10) C2S 0.072(13) 0.078(14) 0.084(15) -0.018(11) 0.007(12) -0.003(10) C3S 0.079(14) 0.068(12) 0.062(12) 0.009(9) -0.020(11) -0.021(10) C4S 0.080(14) 0.100(15) 0.050(11) 0.019(10) 0.011(11) -0.038(12) C5S 0.087(13) 0.071(12) 0.043(10) 0.010(8) -0.005(10) -0.037(10) C6S 0.061(11) 0.041(9) 0.042(10) -0.006(7) 0.002(9) -0.014(8) C7S 0.115(16) 0.072(14) 0.042(11) -0.004(9) 0.008(11) -0.053(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 Ni1 S12 2.093(5) . ? Ni1 S11 2.162(4) . ? Ni1 S9 2.187(4) . ? Ni1 S10 2.224(5) . ? Ni2 S15 2.144(4) . ? Ni2 S14 2.145(4) . ? Ni2 S13 2.145(4) . ? Ni2 S16 2.158(4) . ? Fe1 N1 1.979(9) . ? Fe1 N6 1.994(9) . ? Fe1 N2 2.079(10) . ? Fe1 N9 2.079(11) . ? Fe1 N4 2.085(10) . ? Fe1 N7 2.096(11) . ? S1 C14 1.737(13) . ? S1 C16 1.746(12) . ? S2 C16 1.742(13) . ? S2 C15 1.752(13) . ? S3 C17 1.732(13) . ? S3 C18 1.744(16) . ? S4 C19 1.686(16) . ? S4 C17 1.755(12) . ? S5 C35 1.725(12) . ? S5 C33 1.764(13) . ? S6 C34 1.696(12) . ? S6 C35 1.723(14) . ? S7 C36 1.726(14) . ? S7 C37 1.737(15) . ? S8 C38 1.719(16) . ? S8 C36 1.737(13) . ? S9 C39 1.708(18) . ? S10 C40 1.612(18) . ? S11 C43 1.728(19) . ? S12 C44 1.776(17) . ? S13 C47 1.699(15) . ? S14 C48 1.728(13) . ? S15 C51 1.719(14) . ? S16 C52 1.714(15) . ? F1 B1 1.365(19) . ? F2 B1 1.31(2) . ? F3 B1 1.45(4) . ? F2' B1 1.45(6) . ? F3' B1 1.09(7) . ? F4 B1 1.355(19) . ? N1 C5 1.328(13) . ? N1 C1 1.333(13) . ? N2 C8 1.322(14) . ? N2 N3 1.360(12) . ? N3 C6 1.332(14) . ? N3 C5 1.405(13) . ? N4 C11 1.285(14) . ? N4 N5 1.356(12) . ? N5 C9 1.346(14) . ? N5 C1 1.427(13) . ? N6 C20 1.341(14) . ? N6 C24 1.344(14) . ? N7 C27 1.297(15) . ? N7 N8 1.377(12) . ? N8 C25 1.343(14) . ? N8 C24 1.394(14) . ? N9 C28 1.304(15) . ? N9 N10 1.368(12) . ? N10 C30 1.361(15) . ? N10 C20 1.379(14) . ? N11 C41 1.072(17) . ? N12 C42 1.14(2) . ? N13 C45 1.092(16) . ? N14 C46 1.080(19) . ? N15 C49 1.146(17) . ? N16 C50 1.158(17) . ? N17 C53 1.026(16) . ? N18 C54 1.145(17) . ? C1 C2 1.372(15) . ? C2 C3 1.392(15) . ? C2 H2 0.9500 . ? C3 C4 1.383(15) . ? C3 C12 1.457(16) . ? C4 C5 1.386(15) . ? C4 H4 0.9500 . ? C6 C7 1.334(17) . ? C6 H6 0.9500 . ? C7 C8 1.371(17) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.345(16) . ? C9 H9 0.9500 . ? C10 C11 1.405(17) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.340(15) . ? C12 H12 0.9500 . ? C13 C14 1.403(16) . ? C13 H13 0.9500 . ? C14 C15 1.325(15) . ? C15 H15 0.9500 . ? C16 C17 1.327(16) . ? C18 C19 1.31(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.355(15) . ? C21 C22 1.384(16) . ? C21 H21 0.9500 . ? C22 C23 1.401(16) . ? C22 C31 1.474(15) . ? C23 C24 1.379(15) . ? C23 H23 0.9500 . ? C25 C26 1.368(17) . ? C25 H25 0.9500 . ? C26 C27 1.398(18) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.407(19) . ? C28 H28 0.9500 . ? C29 C30 1.340(18) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.324(16) . ? C31 H31 0.9500 . ? C32 C33 1.453(16) . ? C32 H32 0.9500 . ? C33 C34 1.339(17) . ? C34 H34 0.9500 . ? C35 C36 1.393(17) . ? C37 C38 1.29(2) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.35(2) . ? C39 C41 1.53(2) . ? C40 C42 1.51(2) . ? C43 C44 1.42(2) . ? C43 C45 1.49(2) . ? C44 C46 1.41(2) . ? C47 C48 1.351(18) . ? C47 C49 1.427(19) . ? C48 C50 1.45(2) . ? C51 C52 1.367(19) . ? C51 C53 1.50(2) . ? C52 C54 1.471(19) . ? N1S C7S 1.159(19) . ? C1S C6S 1.360(19) . ? C1S C2S 1.38(2) . ? C1S H1S 0.9500 . ? C2S C3S 1.35(2) . ? C2S H2S 0.9500 . ? C3S C4S 1.34(2) . ? C3S H3S 0.9500 . ? C4S C5S 1.34(2) . ? C4S H4S 0.9500 . ? C5S C6S 1.354(18) . ? C5S H5S 0.9500 . ? C6S C7S 1.44(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S12 Ni1 S11 96.34(19) . . ? S12 Ni1 S9 176.8(2) . . ? S11 Ni1 S9 86.75(16) . . ? S12 Ni1 S10 85.52(19) . . ? S11 Ni1 S10 177.26(19) . . ? S9 Ni1 S10 91.35(17) . . ? S15 Ni2 S14 174.09(17) . . ? S15 Ni2 S13 87.43(16) . . ? S14 Ni2 S13 91.44(15) . . ? S15 Ni2 S16 92.42(16) . . ? S14 Ni2 S16 89.38(15) . . ? S13 Ni2 S16 173.33(18) . . ? N1 Fe1 N6 172.3(4) . . ? N1 Fe1 N2 77.2(4) . . ? N6 Fe1 N2 95.1(4) . . ? N1 Fe1 N9 101.5(4) . . ? N6 Fe1 N9 77.6(4) . . ? N2 Fe1 N9 93.5(4) . . ? N1 Fe1 N4 76.7(4) . . ? N6 Fe1 N4 110.9(4) . . ? N2 Fe1 N4 153.9(4) . . ? N9 Fe1 N4 92.2(4) . . ? N1 Fe1 N7 104.8(4) . . ? N6 Fe1 N7 76.6(4) . . ? N2 Fe1 N7 94.4(4) . . ? N9 Fe1 N7 153.6(4) . . ? N4 Fe1 N7 91.7(4) . . ? C14 S1 C16 96.4(6) . . ? C16 S2 C15 94.8(6) . . ? C17 S3 C18 94.6(8) . . ? C19 S4 C17 96.3(8) . . ? C35 S5 C33 94.4(6) . . ? C34 S6 C35 95.0(6) . . ? C36 S7 C37 93.3(8) . . ? C38 S8 C36 93.9(7) . . ? C39 S9 Ni1 100.5(6) . . ? C40 S10 Ni1 102.1(6) . . ? C43 S11 Ni1 101.2(6) . . ? C44 S12 Ni1 102.3(6) . . ? C47 S13 Ni2 104.8(5) . . ? C48 S14 Ni2 103.4(5) . . ? C51 S15 Ni2 103.9(6) . . ? C52 S16 Ni2 102.8(5) . . ? C5 N1 C1 118.5(10) . . ? C5 N1 Fe1 120.4(8) . . ? C1 N1 Fe1 121.1(8) . . ? C8 N2 N3 104.9(10) . . ? C8 N2 Fe1 142.3(10) . . ? N3 N2 Fe1 112.8(7) . . ? C6 N3 N2 110.8(10) . . ? C6 N3 C5 131.9(11) . . ? N2 N3 C5 117.3(10) . . ? C11 N4 N5 104.9(10) . . ? C11 N4 Fe1 141.0(9) . . ? N5 N4 Fe1 114.0(7) . . ? C9 N5 N4 111.6(10) . . ? C9 N5 C1 132.1(10) . . ? N4 N5 C1 116.2(9) . . ? C20 N6 C24 119.9(10) . . ? C20 N6 Fe1 119.0(8) . . ? C24 N6 Fe1 120.4(8) . . ? C27 N7 N8 103.7(10) . . ? C27 N7 Fe1 143.4(9) . . ? N8 N7 Fe1 112.7(7) . . ? C25 N8 N7 111.7(10) . . ? C25 N8 C24 130.4(11) . . ? N7 N8 C24 117.6(10) . . ? C28 N9 N10 104.5(11) . . ? C28 N9 Fe1 143.9(10) . . ? N10 N9 Fe1 111.5(7) . . ? C30 N10 N9 109.8(10) . . ? C30 N10 C20 131.2(11) . . ? N9 N10 C20 118.9(10) . . ? N1 C1 C2 123.3(11) . . ? N1 C1 N5 112.0(9) . . ? C2 C1 N5 124.7(11) . . ? C1 C2 C3 117.9(11) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 119.4(11) . . ? C4 C3 C12 120.8(12) . . ? C2 C3 C12 119.8(11) . . ? C3 C4 C5 118.1(11) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 122.7(10) . . ? N1 C5 N3 112.3(10) . . ? C4 C5 N3 125.0(11) . . ? N3 C6 C7 107.2(12) . . ? N3 C6 H6 126.4 . . ? C7 C6 H6 126.4 . . ? C6 C7 C8 106.9(12) . . ? C6 C7 H7 126.5 . . ? C8 C7 H7 126.5 . . ? N2 C8 C7 110.2(12) . . ? N2 C8 H8 124.9 . . ? C7 C8 H8 124.9 . . ? C10 C9 N5 106.5(11) . . ? C10 C9 H9 126.8 . . ? N5 C9 H9 126.8 . . ? C9 C10 C11 105.1(11) . . ? C9 C10 H10 127.4 . . ? C11 C10 H10 127.4 . . ? N4 C11 C10 111.8(11) . . ? N4 C11 H11 124.1 . . ? C10 C11 H11 124.1 . . ? C13 C12 C3 127.1(12) . . ? C13 C12 H12 116.5 . . ? C3 C12 H12 116.5 . . ? C12 C13 C14 127.9(12) . . ? C12 C13 H13 116.0 . . ? C14 C13 H13 116.0 . . ? C15 C14 C13 122.4(12) . . ? C15 C14 S1 116.0(10) . . ? C13 C14 S1 121.5(9) . . ? C14 C15 S2 118.6(10) . . ? C14 C15 H15 120.7 . . ? S2 C15 H15 120.7 . . ? C17 C16 S2 123.0(10) . . ? C17 C16 S1 122.8(10) . . ? S2 C16 S1 114.1(7) . . ? C16 C17 S3 124.1(10) . . ? C16 C17 S4 122.5(10) . . ? S3 C17 S4 113.3(7) . . ? C19 C18 S3 118.1(13) . . ? C19 C18 H18 121.0 . . ? S3 C18 H18 121.0 . . ? C18 C19 S4 117.5(13) . . ? C18 C19 H19 121.3 . . ? S4 C19 H19 121.3 . . ? N6 C20 C21 122.0(11) . . ? N6 C20 N10 112.4(10) . . ? C21 C20 N10 125.6(11) . . ? C20 C21 C22 118.5(11) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C21 C22 C23 120.6(11) . . ? C21 C22 C31 118.4(11) . . ? C23 C22 C31 121.0(11) . . ? C24 C23 C22 116.9(11) . . ? C24 C23 H23 121.5 . . ? C22 C23 H23 121.5 . . ? N6 C24 C23 122.0(11) . . ? N6 C24 N8 112.0(10) . . ? C23 C24 N8 126.0(12) . . ? N8 C25 C26 107.0(11) . . ? N8 C25 H25 126.5 . . ? C26 C25 H25 126.5 . . ? C25 C26 C27 104.1(12) . . ? C25 C26 H26 127.9 . . ? C27 C26 H26 127.9 . . ? N7 C27 C26 113.4(12) . . ? N7 C27 H27 123.3 . . ? C26 C27 H27 123.3 . . ? N9 C28 C29 113.1(13) . . ? N9 C28 H28 123.4 . . ? C29 C28 H28 123.4 . . ? C30 C29 C28 103.4(14) . . ? C30 C29 H29 128.3 . . ? C28 C29 H29 128.3 . . ? C29 C30 N10 109.1(13) . . ? C29 C30 H30 125.4 . . ? N10 C30 H30 125.4 . . ? C32 C31 C22 125.4(12) . . ? C32 C31 H31 117.3 . . ? C22 C31 H31 117.3 . . ? C31 C32 C33 124.8(12) . . ? C31 C32 H32 117.6 . . ? C33 C32 H32 117.6 . . ? C34 C33 C32 125.8(12) . . ? C34 C33 S5 115.3(10) . . ? C32 C33 S5 118.9(10) . . ? C33 C34 S6 119.3(11) . . ? C33 C34 H34 120.4 . . ? S6 C34 H34 120.4 . . ? C36 C35 S6 122.4(10) . . ? C36 C35 S5 121.5(11) . . ? S6 C35 S5 116.1(7) . . ? C35 C36 S7 122.7(10) . . ? C35 C36 S8 121.6(11) . . ? S7 C36 S8 115.6(7) . . ? C38 C37 S7 118.6(13) . . ? C38 C37 H37 120.7 . . ? S7 C37 H37 120.7 . . ? C37 C38 S8 118.2(12) . . ? C37 C38 H38 120.9 . . ? S8 C38 H38 120.9 . . ? C40 C39 C41 123.8(16) . . ? C40 C39 S9 122.5(15) . . ? C41 C39 S9 113.7(12) . . ? C39 C40 C42 119.2(17) . . ? C39 C40 S10 123.5(15) . . ? C42 C40 S10 117.2(12) . . ? N11 C41 C39 167.2(18) . . ? N12 C42 C40 177(2) . . ? C44 C43 C45 122.0(16) . . ? C44 C43 S11 121.1(13) . . ? C45 C43 S11 116.9(12) . . ? C46 C44 C43 122.7(16) . . ? C46 C44 S12 118.4(14) . . ? C43 C44 S12 118.9(13) . . ? N13 C45 C43 172.3(19) . . ? N14 C46 C44 178(2) . . ? C48 C47 C49 121.3(14) . . ? C48 C47 S13 119.5(11) . . ? C49 C47 S13 118.9(12) . . ? C47 C48 C50 122.3(12) . . ? C47 C48 S14 120.7(11) . . ? C50 C48 S14 116.9(11) . . ? N15 C49 C47 177(2) . . ? N16 C50 C48 178.8(16) . . ? C52 C51 C53 119.3(13) . . ? C52 C51 S15 119.4(11) . . ? C53 C51 S15 121.3(12) . . ? C51 C52 C54 121.3(13) . . ? C51 C52 S16 121.5(11) . . ? C54 C52 S16 117.2(12) . . ? N17 C53 C51 175.2(18) . . ? N18 C54 C52 175.4(18) . . ? F3' B1 F2 70(6) . . ? F3' B1 F4 130(7) . . ? F2 B1 F4 116(2) . . ? F3' B1 F1 111(4) . . ? F2 B1 F1 113.4(16) . . ? F4 B1 F1 110.3(16) . . ? F3' B1 F2' 113(5) . . ? F2 B1 F2' 43(3) . . ? F4 B1 F2' 83(3) . . ? F1 B1 F2' 103(4) . . ? F3' B1 F3 39(8) . . ? F2 B1 F3 108(2) . . ? F4 B1 F3 103.1(15) . . ? F1 B1 F3 105.5(16) . . ? F2' B1 F3 146(4) . . ? C6S C1S C2S 120.1(15) . . ? C6S C1S H1S 120.0 . . ? C2S C1S H1S 120.0 . . ? C3S C2S C1S 117.5(17) . . ? C3S C2S H2S 121.2 . . ? C1S C2S H2S 121.2 . . ? C4S C3S C2S 121.9(17) . . ? C4S C3S H3S 119.0 . . ? C2S C3S H3S 119.0 . . ? C3S C4S C5S 120.5(15) . . ? C3S C4S H4S 119.7 . . ? C5S C4S H4S 119.7 . . ? C4S C5S C6S 119.7(16) . . ? C4S C5S H5S 120.2 . . ? C6S C5S H5S 120.2 . . ? C5S C6S C1S 120.2(15) . . ? C5S C6S C7S 121.2(15) . . ? C1S C6S C7S 118.6(15) . . ? N1S C7S C6S 176.8(18) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 5.168 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.141 data_dc2ebf _database_code_depnum_ccdc_archive 'CCDC 796349' #TrackingRef '- FedppTTF_F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H62 B2 F8 Fe2 N38 Ni4 S32' _chemical_formula_weight 3606.18 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' 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.828(2) _cell_length_b 15.156(2) _cell_length_c 18.255(3) _cell_angle_alpha 89.772(2) _cell_angle_beta 83.344(2) _cell_angle_gamma 74.195(2) _cell_volume 3654.8(9) _cell_formula_units_Z 1 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 1023 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 23.01 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1818 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7912 _exptl_absorpt_correction_T_max 0.9411 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366[pixels/mm] _diffrn_standards_number 148 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 510 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14934 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 23.30 _reflns_number_total 10226 _reflns_number_gt 6340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1671P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10226 _refine_ls_number_parameters 965 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2463 _refine_ls_wR_factor_gt 0.2196 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 Ni1 Ni 0.97548(11) 0.62227(9) 0.00989(8) 0.0912(5) Uani 1 1 d . . . Ni2 Ni 0.38803(8) 0.91641(7) 0.89017(6) 0.0614(3) Uani 1 1 d . . . Fe1 Fe 0.71820(8) 0.69551(7) 0.49954(5) 0.0474(3) Uani 1 1 d . . . S1 S 0.93519(17) 0.86896(16) 0.02772(12) 0.0644(6) Uani 1 1 d . . . S2 S 1.14780(17) 0.86376(17) -0.01153(13) 0.0726(7) Uani 1 1 d . . . S3 S 0.8868(2) 0.9508(2) -0.13224(15) 0.0872(8) Uani 1 1 d . . . S4 S 1.0988(2) 0.94706(19) -0.16939(14) 0.0852(8) Uani 1 1 d . . . S5 S 0.6280(2) 0.55653(16) 0.99575(12) 0.0728(7) Uani 1 1 d . . . S6 S 0.6338(2) 0.37065(15) 1.04219(12) 0.0688(6) Uani 1 1 d . . . S7 S 0.5561(2) 0.63011(19) 1.16489(17) 0.0946(9) Uani 1 1 d . . . S8 S 0.5912(2) 0.44134(19) 1.21201(13) 0.0793(7) Uani 1 1 d . . . S9 S 0.8434(2) 0.6120(2) 0.08465(15) 0.0861(8) Uani 1 1 d . . . S10 S 1.0777(2) 0.5705(2) 0.09408(18) 0.0965(9) Uani 1 1 d . . . S11 S 0.8736(2) 0.66827(19) -0.07179(15) 0.0868(8) Uani 1 1 d . . . S12 S 1.1064(2) 0.6297(2) -0.05916(19) 0.1003(10) Uani 1 1 d . . . S13 S 0.3748(3) 0.99192(17) 0.79113(14) 0.0903(9) Uani 1 1 d . . . S14 S 0.4106(2) 0.78956(15) 0.83085(12) 0.0711(7) Uani 1 1 d . . . S15 S 0.35185(19) 1.04563(16) 0.94873(14) 0.0759(7) Uani 1 1 d . . . S16 S 0.4175(2) 0.84108(17) 0.98889(13) 0.0778(7) Uani 1 1 d . . . F1 F 0.7409(6) 0.2558(5) 0.7960(3) 0.128(2) Uani 1 1 d . A . F2 F 0.8676(18) 0.231(4) 0.7018(10) 0.132(14) Uani 0.55(6) 1 d P A 1 F3 F 0.7538(18) 0.162(2) 0.6979(15) 0.110(7) Uani 0.55(6) 1 d P A 1 F4 F 0.684(2) 0.3113(18) 0.6939(19) 0.112(9) Uani 0.55(6) 1 d P A 1 F2' F 0.831(3) 0.306(5) 0.715(3) 0.180(18) Uani 0.45(6) 1 d P A 2 F3' F 0.807(7) 0.171(3) 0.707(2) 0.19(3) Uani 0.45(6) 1 d P A 2 F4' F 0.721(3) 0.291(3) 0.679(2) 0.156(15) Uani 0.45(6) 1 d P A 2 N1 N 0.7731(5) 0.7297(4) 0.3969(3) 0.0475(15) Uani 1 1 d . . . N2 N 0.8778(5) 0.6559(4) 0.4986(3) 0.0554(16) Uani 1 1 d . . . N3 N 0.9287(5) 0.6717(4) 0.4350(3) 0.0555(16) Uani 1 1 d . . . N4 N 0.5880(5) 0.7493(5) 0.4443(3) 0.0597(17) Uani 1 1 d . . . N5 N 0.6088(5) 0.7801(4) 0.3776(3) 0.0511(16) Uani 1 1 d . . . N6 N 0.6874(5) 0.6599(4) 0.6055(3) 0.0537(16) Uani 1 1 d . . . N7 N 0.7036(5) 0.5589(4) 0.4899(3) 0.0580(17) Uani 1 1 d . . . N8 N 0.6913(5) 0.5189(4) 0.5566(3) 0.0523(16) Uani 1 1 d . . . N9 N 0.6956(6) 0.8194(5) 0.5636(4) 0.0665(19) Uani 1 1 d . . . N10 N 0.6833(6) 0.8052(4) 0.6371(4) 0.0630(18) Uani 1 1 d . . . N11 N 0.7763(9) 0.5543(8) 0.2778(6) 0.112(3) Uani 1 1 d . . . N12 N 1.0726(9) 0.4977(8) 0.2872(7) 0.131(4) Uani 1 1 d . . . N13 N 0.8802(8) 0.7521(7) -0.2658(6) 0.108(3) Uani 1 1 d . . . N14 N 1.1772(10) 0.7092(10) -0.2441(9) 0.166(6) Uani 1 1 d . . . N15 N 0.3816(11) 0.9643(9) 0.5899(6) 0.162(5) Uani 1 1 d . . . N16 N 0.4361(7) 0.6953(6) 0.6414(4) 0.090(3) Uani 1 1 d . . . N17 N 0.3400(8) 1.1443(8) 1.1353(5) 0.120(4) Uani 1 1 d . . . N18 N 0.4342(12) 0.8769(9) 1.1842(6) 0.167(6) Uani 1 1 d . . . C1 C 0.7107(6) 0.7676(5) 0.3490(4) 0.0503(19) Uani 1 1 d . . . C2 C 0.7435(6) 0.7904(5) 0.2801(4) 0.0525(19) Uani 1 1 d . . . H2 H 0.6976 0.8148 0.2470 0.063 Uiso 1 1 calc R . . C3 C 0.8469(6) 0.7766(5) 0.2601(4) 0.0519(19) Uani 1 1 d . . . C4 C 0.9129(6) 0.7343(5) 0.3102(4) 0.0530(19) Uani 1 1 d . . . H4 H 0.9827 0.7204 0.2980 0.064 Uiso 1 1 calc R . . C5 C 0.8718(6) 0.7140(5) 0.3776(4) 0.0491(18) Uani 1 1 d . . . C6 C 1.0294(6) 0.6479(6) 0.4395(5) 0.070(2) Uani 1 1 d . . . H6 H 1.0794 0.6540 0.4027 0.084 Uiso 1 1 calc R . . C7 C 1.0445(7) 0.6143(7) 0.5058(5) 0.076(3) Uani 1 1 d . . . H7 H 1.1064 0.5914 0.5238 0.092 Uiso 1 1 calc R . . C8 C 0.9490(8) 0.6205(6) 0.5429(5) 0.072(3) Uani 1 1 d . . . H8 H 0.9364 0.6027 0.5911 0.086 Uiso 1 1 calc R . . C9 C 0.5223(7) 0.8158(6) 0.3467(5) 0.064(2) Uani 1 1 d . . . H9 H 0.5175 0.8413 0.3004 0.077 Uiso 1 1 calc R . . C10 C 0.4462(7) 0.8074(6) 0.3945(5) 0.072(2) Uani 1 1 d . . . H10 H 0.3779 0.8255 0.3884 0.086 Uiso 1 1 calc R . . C11 C 0.4884(7) 0.7664(7) 0.4559(5) 0.076(3) Uani 1 1 d . . . H11 H 0.4521 0.7531 0.4987 0.091 Uiso 1 1 calc R . . C12 C 0.8859(7) 0.8028(5) 0.1876(4) 0.058(2) Uani 1 1 d . . . H12 H 0.8385 0.8239 0.1548 0.069 Uiso 1 1 calc R . . C13 C 0.9774(7) 0.8000(6) 0.1642(4) 0.060(2) Uani 1 1 d . . . H13 H 1.0243 0.7773 0.1970 0.073 Uiso 1 1 calc R . . C14 C 1.0183(6) 0.8272(5) 0.0939(4) 0.057(2) Uani 1 1 d . . . C15 C 1.1124(7) 0.8253(6) 0.0729(5) 0.069(2) Uani 1 1 d . . . H15 H 1.1611 0.8026 0.1044 0.083 Uiso 1 1 calc R . . C16 C 1.0286(6) 0.8906(6) -0.0371(5) 0.063(2) Uani 1 1 d . . . C17 C 1.0066(7) 0.9247(5) -0.1055(4) 0.063(2) Uani 1 1 d . . . C18 C 0.9239(13) 0.9960(8) -0.2153(6) 0.114(5) Uani 1 1 d . . . H18 H 0.8769 1.0199 -0.2478 0.137 Uiso 1 1 calc R . . C19 C 1.0208(12) 0.9958(8) -0.2319(6) 0.106(4) Uani 1 1 d . . . H19 H 1.0437 1.0208 -0.2749 0.127 Uiso 1 1 calc R . . C20 C 0.6792(6) 0.7165(5) 0.6620(4) 0.0533(19) Uani 1 1 d . . . C21 C 0.6711(6) 0.6933(5) 0.7332(4) 0.0528(19) Uani 1 1 d . . . H21 H 0.6670 0.7361 0.7706 0.063 Uiso 1 1 calc R . . C22 C 0.6691(6) 0.6050(5) 0.7496(4) 0.056(2) Uani 1 1 d . . . C23 C 0.6777(6) 0.5413(5) 0.6913(4) 0.056(2) Uani 1 1 d . . . H23 H 0.6783 0.4807 0.7004 0.067 Uiso 1 1 calc R . . C24 C 0.6850(6) 0.5727(5) 0.6203(4) 0.0524(19) Uani 1 1 d . . . C25 C 0.6788(7) 0.4361(6) 0.5483(5) 0.070(2) Uani 1 1 d . . . H25 H 0.6692 0.3970 0.5862 0.084 Uiso 1 1 calc R . . C26 C 0.6824(8) 0.4179(7) 0.4762(6) 0.085(3) Uani 1 1 d . . . H26 H 0.6774 0.3645 0.4539 0.102 Uiso 1 1 calc R . . C27 C 0.6951(8) 0.4961(7) 0.4422(5) 0.080(3) Uani 1 1 d . . . H27 H 0.6976 0.5040 0.3916 0.096 Uiso 1 1 calc R . . C28 C 0.6935(9) 0.9060(7) 0.5587(6) 0.089(3) Uani 1 1 d . . . H28 H 0.7006 0.9357 0.5145 0.107 Uiso 1 1 calc R . . C29 C 0.6792(10) 0.9479(6) 0.6288(6) 0.103(4) Uani 1 1 d . . . H29 H 0.6750 1.0089 0.6396 0.124 Uiso 1 1 calc R . . C30 C 0.6729(8) 0.8846(6) 0.6756(6) 0.081(3) Uani 1 1 d . . . H30 H 0.6629 0.8921 0.7267 0.097 Uiso 1 1 calc R . . C31 C 0.6586(7) 0.5785(6) 0.8263(4) 0.063(2) Uani 1 1 d . . . H31 H 0.6475 0.6250 0.8620 0.076 Uiso 1 1 calc R . . C32 C 0.6632(6) 0.4959(6) 0.8502(4) 0.063(2) Uani 1 1 d . . . H32 H 0.6772 0.4487 0.8149 0.076 Uiso 1 1 calc R . . C33 C 0.6484(7) 0.4720(6) 0.9264(4) 0.062(2) Uani 1 1 d . . . C34 C 0.6520(7) 0.3869(6) 0.9504(5) 0.067(2) Uani 1 1 d . . . H34 H 0.6644 0.3378 0.9170 0.081 Uiso 1 1 calc R . . C35 C 0.6156(6) 0.4859(5) 1.0671(4) 0.060(2) Uani 1 1 d . . . C36 C 0.5909(6) 0.5155(6) 1.1398(5) 0.064(2) Uani 1 1 d . . . C37 C 0.5243(9) 0.6116(9) 1.2561(6) 0.100(4) Uani 1 1 d . . . H37 H 0.4963 0.6602 1.2899 0.120 Uiso 1 1 calc R . . C38 C 0.5411(8) 0.5258(9) 1.2767(6) 0.091(3) Uani 1 1 d . . . H38 H 0.5256 0.5121 1.3256 0.110 Uiso 1 1 calc R . . C39 C 0.9011(10) 0.5740(7) 0.1614(7) 0.098(3) Uani 1 1 d . . . C40 C 0.9994(9) 0.5560(7) 0.1647(6) 0.089(3) Uani 1 1 d . . . C41 C 0.8238(10) 0.5591(8) 0.2266(7) 0.094(3) Uani 1 1 d . . . C42 C 1.0418(9) 0.5198(8) 0.2334(8) 0.102(4) Uani 1 1 d . . . C43 C 0.9544(8) 0.6901(7) -0.1448(6) 0.089(3) Uani 1 1 d . . . C44 C 1.0563(9) 0.6748(7) -0.1389(7) 0.096(3) Uani 1 1 d . . . C45 C 0.9115(9) 0.7226(9) -0.2130(8) 0.100(4) Uani 1 1 d . . . C46 C 1.1253(10) 0.6939(10) -0.1996(9) 0.115(4) Uani 1 1 d . . . C47 C 0.3887(7) 0.9108(7) 0.7242(5) 0.072(3) Uani 1 1 d . . . C48 C 0.4048(7) 0.8224(7) 0.7409(4) 0.065(2) Uani 1 1 d . . . C49 C 0.3851(10) 0.9391(8) 0.6472(6) 0.101(4) Uani 1 1 d . . . C50 C 0.4216(7) 0.7516(6) 0.6856(5) 0.068(2) Uani 1 1 d . . . C51 C 0.3702(7) 1.0137(8) 1.0370(5) 0.072(3) Uani 1 1 d . . . C52 C 0.3985(7) 0.9251(8) 1.0554(5) 0.076(3) Uani 1 1 d . . . C53 C 0.3538(7) 1.0867(8) 1.0920(6) 0.088(3) Uani 1 1 d . . . C54 C 0.4157(11) 0.9005(9) 1.1278(6) 0.112(4) Uani 1 1 d . . . B1 B 0.7688(11) 0.2498(11) 0.7238(7) 0.079(3) Uani 1 1 d . . . N1S N 1.1016(12) 0.0812(8) 0.5985(7) 0.144(5) Uani 1 1 d . . . C1S C 0.8784(14) 0.1253(10) 0.5222(8) 0.125(5) Uani 1 1 d . . . H1S H 0.8556 0.1107 0.5695 0.150 Uiso 1 1 calc R . . C2S C 0.8160(12) 0.1465(11) 0.4722(10) 0.134(5) Uani 1 1 d . . . H2S H 0.7491 0.1452 0.4839 0.160 Uiso 1 1 calc R . . C3S C 0.8469(15) 0.1699(11) 0.4041(10) 0.146(6) Uani 1 1 d . . . H3S H 0.8009 0.1845 0.3695 0.175 Uiso 1 1 calc R . . C4S C 0.9470(14) 0.1728(10) 0.3841(9) 0.132(5) Uani 1 1 d . . . H4S H 0.9678 0.1930 0.3383 0.159 Uiso 1 1 calc R . . C5S C 1.0128(11) 0.1441(9) 0.4360(8) 0.111(4) Uani 1 1 d . . . H5S H 1.0815 0.1380 0.4239 0.133 Uiso 1 1 calc R . . C6S C 0.9772(12) 0.1248(7) 0.5047(7) 0.093(3) Uani 1 1 d . . . C7S C 1.0460(15) 0.0991(9) 0.5547(8) 0.122(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0864(10) 0.0872(10) 0.1011(11) -0.0135(8) -0.0195(8) -0.0221(8) Ni2 0.0698(7) 0.0647(7) 0.0504(7) 0.0021(5) -0.0113(5) -0.0177(6) Fe1 0.0550(7) 0.0542(6) 0.0334(6) 0.0146(5) -0.0090(5) -0.0145(5) S1 0.0595(13) 0.0827(15) 0.0548(13) 0.0168(11) -0.0025(10) -0.0281(12) S2 0.0573(13) 0.0874(16) 0.0698(15) 0.0165(13) 0.0053(11) -0.0198(12) S3 0.099(2) 0.0975(19) 0.0767(17) 0.0172(14) -0.0281(15) -0.0398(16) S4 0.104(2) 0.0848(17) 0.0635(15) 0.0084(13) 0.0177(14) -0.0311(15) S5 0.1080(19) 0.0658(14) 0.0492(13) 0.0054(11) -0.0067(12) -0.0325(14) S6 0.0951(17) 0.0608(13) 0.0490(13) 0.0090(10) -0.0035(12) -0.0210(12) S7 0.112(2) 0.0794(17) 0.094(2) -0.0163(15) -0.0035(17) -0.0325(16) S8 0.0936(18) 0.0994(18) 0.0483(13) 0.0097(12) -0.0090(12) -0.0324(15) S9 0.0802(17) 0.103(2) 0.0772(17) -0.0138(15) -0.0207(14) -0.0226(15) S10 0.0762(18) 0.097(2) 0.116(2) -0.0285(18) -0.0105(16) -0.0224(16) S11 0.0769(17) 0.0955(19) 0.0859(19) -0.0081(15) -0.0182(14) -0.0164(15) S12 0.0705(17) 0.095(2) 0.136(3) -0.0249(19) -0.0125(17) -0.0233(15) S13 0.141(3) 0.0624(14) 0.0687(16) 0.0152(12) -0.0285(16) -0.0228(16) S14 0.1070(19) 0.0644(13) 0.0445(12) 0.0081(10) -0.0107(12) -0.0271(13) S15 0.0780(16) 0.0703(15) 0.0754(16) -0.0097(12) -0.0152(13) -0.0110(13) S16 0.108(2) 0.0814(16) 0.0536(14) 0.0096(12) -0.0221(13) -0.0370(15) F1 0.151(6) 0.163(7) 0.063(4) -0.006(4) -0.008(4) -0.036(5) F2 0.068(12) 0.22(4) 0.111(13) -0.004(15) -0.004(8) -0.045(18) F3 0.108(13) 0.133(14) 0.101(11) -0.024(10) -0.030(9) -0.048(11) F4 0.068(15) 0.095(12) 0.17(2) 0.036(11) -0.034(12) -0.009(11) F2' 0.081(18) 0.23(5) 0.23(3) 0.06(3) 0.003(19) -0.07(3) F3' 0.30(9) 0.13(3) 0.113(19) 0.029(18) -0.02(3) 0.01(4) F4' 0.09(2) 0.22(3) 0.109(17) 0.054(17) -0.020(16) 0.047(19) N1 0.048(4) 0.052(4) 0.042(3) 0.010(3) -0.010(3) -0.010(3) N2 0.055(4) 0.064(4) 0.048(4) 0.017(3) -0.014(3) -0.016(3) N3 0.062(4) 0.056(4) 0.048(4) 0.012(3) -0.011(3) -0.014(3) N4 0.053(4) 0.075(5) 0.050(4) 0.017(3) -0.010(3) -0.015(4) N5 0.051(4) 0.052(4) 0.047(4) 0.011(3) -0.009(3) -0.007(3) N6 0.062(4) 0.055(4) 0.047(4) 0.007(3) -0.011(3) -0.021(3) N7 0.077(5) 0.056(4) 0.041(4) 0.004(3) -0.016(3) -0.015(4) N8 0.069(4) 0.051(4) 0.040(4) 0.002(3) -0.015(3) -0.019(3) N9 0.090(5) 0.057(4) 0.054(4) 0.020(3) -0.014(4) -0.020(4) N10 0.085(5) 0.050(4) 0.053(4) 0.005(3) -0.011(4) -0.017(4) N11 0.117(8) 0.138(9) 0.093(8) 0.023(7) -0.008(6) -0.058(7) N12 0.116(9) 0.122(9) 0.159(11) 0.048(8) -0.060(8) -0.023(7) N13 0.093(7) 0.122(8) 0.120(8) 0.041(7) -0.021(6) -0.046(6) N14 0.102(10) 0.181(13) 0.199(15) 0.070(11) 0.002(9) -0.018(9) N15 0.236(15) 0.178(12) 0.077(7) 0.069(8) -0.052(8) -0.052(11) N16 0.114(7) 0.107(7) 0.056(5) -0.002(5) -0.015(5) -0.040(6) N17 0.121(8) 0.143(9) 0.092(7) -0.067(7) 0.001(6) -0.035(7) N18 0.283(18) 0.191(12) 0.079(8) 0.021(8) -0.046(10) -0.142(13) C1 0.052(5) 0.049(4) 0.051(5) 0.009(4) -0.009(4) -0.014(4) C2 0.060(5) 0.054(5) 0.041(4) 0.021(4) -0.010(4) -0.010(4) C3 0.061(5) 0.050(4) 0.045(4) 0.004(4) -0.003(4) -0.017(4) C4 0.050(5) 0.059(5) 0.051(5) 0.005(4) 0.000(4) -0.018(4) C5 0.053(5) 0.047(4) 0.051(5) 0.013(4) -0.014(4) -0.017(4) C6 0.047(5) 0.077(6) 0.084(7) 0.020(5) -0.014(5) -0.009(5) C7 0.060(6) 0.090(7) 0.083(7) 0.023(6) -0.028(5) -0.018(5) C8 0.085(7) 0.071(6) 0.065(6) 0.020(5) -0.035(5) -0.019(5) C9 0.067(6) 0.060(5) 0.064(6) 0.016(4) -0.023(5) -0.010(5) C10 0.046(5) 0.083(6) 0.082(7) 0.003(5) -0.012(5) -0.009(5) C11 0.059(6) 0.089(7) 0.071(6) 0.014(5) 0.002(5) -0.009(5) C12 0.068(6) 0.062(5) 0.049(5) 0.008(4) -0.008(4) -0.027(4) C13 0.070(6) 0.067(5) 0.046(5) 0.011(4) -0.007(4) -0.021(5) C14 0.052(5) 0.063(5) 0.056(5) 0.007(4) -0.003(4) -0.017(4) C15 0.070(6) 0.067(6) 0.067(6) 0.011(5) -0.008(5) -0.014(5) C16 0.064(5) 0.066(5) 0.056(5) 0.004(4) -0.002(4) -0.017(4) C17 0.078(6) 0.056(5) 0.051(5) 0.008(4) 0.007(4) -0.021(4) C18 0.197(15) 0.099(8) 0.069(7) 0.018(6) -0.065(9) -0.059(10) C19 0.173(13) 0.105(9) 0.054(6) 0.021(6) -0.012(8) -0.063(10) C20 0.058(5) 0.053(5) 0.051(5) 0.004(4) -0.008(4) -0.018(4) C21 0.064(5) 0.052(5) 0.042(5) 0.001(4) -0.006(4) -0.017(4) C22 0.070(5) 0.062(5) 0.042(5) 0.006(4) -0.008(4) -0.027(4) C23 0.067(5) 0.057(5) 0.045(5) 0.014(4) -0.008(4) -0.018(4) C24 0.051(5) 0.059(5) 0.046(5) 0.003(4) -0.006(4) -0.014(4) C25 0.101(7) 0.064(6) 0.056(6) 0.003(4) -0.020(5) -0.038(5) C26 0.115(8) 0.074(6) 0.080(7) -0.002(6) -0.030(6) -0.041(6) C27 0.095(7) 0.092(7) 0.054(6) -0.006(5) -0.029(5) -0.016(6) C28 0.122(9) 0.060(6) 0.088(8) 0.026(6) -0.033(7) -0.020(6) C29 0.162(11) 0.041(5) 0.100(9) 0.007(6) -0.028(8) -0.013(6) C30 0.114(8) 0.046(5) 0.077(6) 0.003(5) -0.012(6) -0.013(5) C31 0.085(6) 0.055(5) 0.047(5) -0.003(4) 0.003(4) -0.020(5) C32 0.073(6) 0.077(6) 0.041(5) 0.007(4) -0.008(4) -0.020(5) C33 0.084(6) 0.059(5) 0.043(5) -0.002(4) -0.008(4) -0.016(5) C34 0.076(6) 0.067(6) 0.052(5) -0.002(4) -0.006(4) -0.010(5) C35 0.072(6) 0.057(5) 0.053(5) 0.001(4) -0.004(4) -0.021(4) C36 0.065(5) 0.064(5) 0.060(5) 0.001(4) -0.005(4) -0.017(4) C37 0.108(9) 0.128(10) 0.076(7) -0.048(7) 0.017(6) -0.062(8) C38 0.096(8) 0.133(10) 0.058(6) -0.017(6) -0.005(5) -0.054(8) C39 0.108(9) 0.078(7) 0.112(9) -0.017(6) -0.030(8) -0.025(7) C40 0.082(8) 0.093(7) 0.098(8) -0.016(6) -0.037(6) -0.023(6) C41 0.109(10) 0.085(8) 0.089(9) -0.004(7) -0.024(8) -0.020(7) C42 0.086(8) 0.089(8) 0.125(11) -0.004(8) -0.018(8) -0.013(7) C43 0.078(7) 0.079(7) 0.106(9) 0.001(6) -0.028(6) -0.010(6) C44 0.092(8) 0.080(7) 0.118(10) -0.005(7) -0.012(7) -0.026(6) C45 0.084(8) 0.097(8) 0.114(10) 0.007(7) -0.012(7) -0.016(7) C46 0.079(9) 0.111(10) 0.150(14) 0.009(9) -0.004(9) -0.023(8) C47 0.093(7) 0.081(6) 0.047(5) 0.014(5) -0.020(5) -0.026(6) C48 0.071(6) 0.084(6) 0.043(5) 0.009(4) -0.017(4) -0.021(5) C49 0.138(10) 0.091(8) 0.084(8) 0.027(6) -0.039(7) -0.038(7) C50 0.089(7) 0.074(6) 0.046(5) -0.001(5) -0.014(5) -0.028(5) C51 0.055(5) 0.107(8) 0.056(5) -0.022(5) -0.005(4) -0.026(5) C52 0.078(7) 0.105(8) 0.053(6) 0.001(5) -0.006(5) -0.041(6) C53 0.065(6) 0.118(8) 0.078(7) -0.023(7) 0.004(5) -0.023(6) C54 0.169(12) 0.160(12) 0.041(6) 0.019(7) -0.028(7) -0.094(10) B1 0.073(9) 0.078(9) 0.078(9) 0.012(7) -0.016(7) -0.005(8) N1S 0.209(15) 0.101(8) 0.125(11) -0.011(8) -0.030(10) -0.040(9) C1S 0.158(15) 0.126(11) 0.083(10) -0.013(8) 0.033(10) -0.046(11) C2S 0.114(12) 0.156(14) 0.112(12) -0.006(11) 0.026(10) -0.021(10) C3S 0.149(16) 0.135(13) 0.123(14) -0.012(10) -0.012(11) 0.013(11) C4S 0.146(14) 0.119(11) 0.120(12) -0.014(9) 0.018(11) -0.030(11) C5S 0.118(10) 0.125(10) 0.099(10) 0.018(8) -0.006(8) -0.052(9) C6S 0.134(11) 0.072(7) 0.074(8) -0.007(6) 0.004(8) -0.035(7) C7S 0.198(17) 0.077(8) 0.095(10) 0.001(7) -0.033(11) -0.039(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S12 2.112(3) . ? Ni1 S11 2.153(3) . ? Ni1 S9 2.191(3) . ? Ni1 S10 2.206(3) . ? Ni2 S13 2.135(3) . ? Ni2 S14 2.139(2) . ? Ni2 S15 2.142(3) . ? Ni2 S16 2.149(3) . ? Fe1 N6 2.035(6) . ? Fe1 N1 2.057(6) . ? Fe1 N2 2.121(6) . ? Fe1 N4 2.131(6) . ? Fe1 N7 2.144(6) . ? Fe1 N9 2.145(7) . ? S1 C16 1.746(9) . ? S1 C14 1.761(8) . ? S2 C16 1.707(9) . ? S2 C15 1.712(9) . ? S3 C17 1.723(9) . ? S3 C18 1.741(13) . ? S4 C19 1.690(13) . ? S4 C17 1.729(8) . ? S5 C35 1.706(8) . ? S5 C33 1.749(8) . ? S6 C34 1.692(8) . ? S6 C35 1.749(8) . ? S7 C37 1.715(11) . ? S7 C36 1.720(9) . ? S8 C38 1.688(11) . ? S8 C36 1.728(9) . ? S9 C39 1.713(12) . ? S10 C40 1.639(12) . ? S11 C43 1.728(12) . ? S12 C44 1.742(12) . ? S13 C47 1.694(9) . ? S14 C48 1.719(8) . ? S15 C51 1.707(10) . ? S16 C52 1.709(10) . ? F1 B1 1.326(14) . ? F2 B1 1.33(2) . ? F3 B1 1.49(3) . ? F4 B1 1.44(3) . ? F2' B1 1.37(4) . ? F3' B1 1.19(4) . ? F4' B1 1.17(4) . ? N1 C1 1.319(9) . ? N1 C5 1.325(9) . ? N2 N3 1.342(9) . ? N2 C8 1.344(10) . ? N3 C6 1.352(10) . ? N3 C5 1.428(9) . ? N4 C11 1.322(11) . ? N4 N5 1.330(8) . ? N5 C9 1.357(10) . ? N5 C1 1.407(10) . ? N6 C20 1.319(9) . ? N6 C24 1.356(9) . ? N7 C27 1.330(11) . ? N7 N8 1.371(8) . ? N8 C25 1.324(10) . ? N8 C24 1.404(9) . ? N9 C28 1.308(11) . ? N9 N10 1.358(9) . ? N10 C30 1.360(11) . ? N10 C20 1.432(10) . ? N11 C41 1.093(14) . ? N12 C42 1.128(14) . ? N13 C45 1.141(14) . ? N14 C46 1.086(16) . ? N15 C49 1.113(12) . ? N16 C50 1.136(11) . ? N17 C53 1.142(12) . ? N18 C54 1.122(13) . ? C1 C2 1.363(10) . ? C2 C3 1.391(11) . ? C2 H2 0.9300 . ? C3 C4 1.397(10) . ? C3 C12 1.466(11) . ? C4 C5 1.365(10) . ? C4 H4 0.9300 . ? C6 C7 1.327(12) . ? C6 H6 0.9300 . ? C7 C8 1.391(13) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.320(12) . ? C9 H9 0.9300 . ? C10 C11 1.389(12) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.277(11) . ? C12 H12 0.9300 . ? C13 C14 1.447(11) . ? C13 H13 0.9300 . ? C14 C15 1.306(11) . ? C15 H15 0.9300 . ? C16 C17 1.383(11) . ? C18 C19 1.339(17) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.344(10) . ? C21 C22 1.377(10) . ? C21 H21 0.9300 . ? C22 C23 1.412(11) . ? C22 C31 1.457(11) . ? C23 C24 1.382(10) . ? C23 H23 0.9300 . ? C25 C26 1.339(12) . ? C25 H25 0.9300 . ? C26 C27 1.379(13) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.400(14) . ? C28 H28 0.9300 . ? C29 C30 1.297(13) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.312(11) . ? C31 H31 0.9300 . ? C32 C33 1.441(11) . ? C32 H32 0.9300 . ? C33 C34 1.351(11) . ? C34 H34 0.9300 . ? C35 C36 1.377(11) . ? C37 C38 1.318(15) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.319(14) . ? C39 C41 1.563(18) . ? C40 C42 1.486(16) . ? C43 C44 1.382(14) . ? C43 C45 1.467(16) . ? C44 C46 1.458(18) . ? C47 C48 1.337(12) . ? C47 C49 1.471(13) . ? C48 C50 1.429(12) . ? C51 C52 1.346(13) . ? C51 C53 1.450(14) . ? C52 C54 1.401(13) . ? N1S C7S 1.154(17) . ? C1S C2S 1.309(18) . ? C1S C6S 1.365(18) . ? C1S H1S 0.9300 . ? C2S C3S 1.35(2) . ? C2S H2S 0.9300 . ? C3S C4S 1.40(2) . ? C3S H3S 0.9300 . ? C4S C5S 1.378(18) . ? C4S H4S 0.9300 . ? C5S C6S 1.354(15) . ? C5S H5S 0.9300 . ? C6S C7S 1.373(18) . ? 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 S12 Ni1 S11 95.08(13) . . ? S12 Ni1 S9 177.81(14) . . ? S11 Ni1 S9 87.09(12) . . ? S12 Ni1 S10 86.17(13) . . ? S11 Ni1 S10 177.85(13) . . ? S9 Ni1 S10 91.65(12) . . ? S13 Ni2 S14 91.76(10) . . ? S13 Ni2 S15 87.25(10) . . ? S14 Ni2 S15 175.08(11) . . ? S13 Ni2 S16 174.00(13) . . ? S14 Ni2 S16 89.19(9) . . ? S15 Ni2 S16 92.30(10) . . ? N6 Fe1 N1 170.5(2) . . ? N6 Fe1 N2 95.5(2) . . ? N1 Fe1 N2 75.3(2) . . ? N6 Fe1 N4 114.5(3) . . ? N1 Fe1 N4 74.7(2) . . ? N2 Fe1 N4 150.0(2) . . ? N6 Fe1 N7 75.6(2) . . ? N1 Fe1 N7 107.3(2) . . ? N2 Fe1 N7 95.8(3) . . ? N4 Fe1 N7 91.4(3) . . ? N6 Fe1 N9 75.5(3) . . ? N1 Fe1 N9 102.4(2) . . ? N2 Fe1 N9 94.5(3) . . ? N4 Fe1 N9 93.6(3) . . ? N7 Fe1 N9 150.1(3) . . ? C16 S1 C14 94.6(4) . . ? C16 S2 C15 94.1(4) . . ? C17 S3 C18 93.2(6) . . ? C19 S4 C17 96.7(6) . . ? C35 S5 C33 95.4(4) . . ? C34 S6 C35 94.7(4) . . ? C37 S7 C36 94.1(5) . . ? C38 S8 C36 94.4(5) . . ? C39 S9 Ni1 99.5(5) . . ? C40 S10 Ni1 102.5(4) . . ? C43 S11 Ni1 101.6(4) . . ? C44 S12 Ni1 102.0(4) . . ? C47 S13 Ni2 104.0(3) . . ? C48 S14 Ni2 103.2(3) . . ? C51 S15 Ni2 102.6(4) . . ? C52 S16 Ni2 103.5(4) . . ? C1 N1 C5 118.7(6) . . ? C1 N1 Fe1 120.6(5) . . ? C5 N1 Fe1 120.7(5) . . ? N3 N2 C8 105.3(7) . . ? N3 N2 Fe1 114.1(4) . . ? C8 N2 Fe1 140.5(6) . . ? N2 N3 C6 110.7(6) . . ? N2 N3 C5 118.1(6) . . ? C6 N3 C5 131.1(7) . . ? C11 N4 N5 106.1(6) . . ? C11 N4 Fe1 140.1(6) . . ? N5 N4 Fe1 113.7(5) . . ? N4 N5 C9 110.5(7) . . ? N4 N5 C1 118.7(6) . . ? C9 N5 C1 130.7(7) . . ? C20 N6 C24 117.6(6) . . ? C20 N6 Fe1 122.1(5) . . ? C24 N6 Fe1 119.9(5) . . ? C27 N7 N8 102.7(7) . . ? C27 N7 Fe1 143.6(6) . . ? N8 N7 Fe1 113.5(4) . . ? C25 N8 N7 111.5(6) . . ? C25 N8 C24 131.1(7) . . ? N7 N8 C24 117.1(6) . . ? C28 N9 N10 104.7(7) . . ? C28 N9 Fe1 143.2(7) . . ? N10 N9 Fe1 112.0(5) . . ? N9 N10 C30 110.0(7) . . ? N9 N10 C20 119.2(6) . . ? C30 N10 C20 130.8(7) . . ? N1 C1 C2 122.7(7) . . ? N1 C1 N5 112.0(7) . . ? C2 C1 N5 125.3(7) . . ? C1 C2 C3 119.0(7) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 118.1(7) . . ? C2 C3 C12 121.1(7) . . ? C4 C3 C12 120.7(7) . . ? C5 C4 C3 117.9(7) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 123.4(7) . . ? N1 C5 N3 111.8(7) . . ? C4 C5 N3 124.8(7) . . ? C7 C6 N3 108.0(8) . . ? C7 C6 H6 126.0 . . ? N3 C6 H6 126.0 . . ? C6 C7 C8 106.2(8) . . ? C6 C7 H7 126.9 . . ? C8 C7 H7 126.9 . . ? N2 C8 C7 109.7(8) . . ? N2 C8 H8 125.1 . . ? C7 C8 H8 125.1 . . ? C10 C9 N5 107.3(7) . . ? C10 C9 H9 126.3 . . ? N5 C9 H9 126.3 . . ? C9 C10 C11 106.5(8) . . ? C9 C10 H10 126.7 . . ? C11 C10 H10 126.7 . . ? N4 C11 C10 109.6(8) . . ? N4 C11 H11 125.2 . . ? C10 C11 H11 125.2 . . ? C13 C12 C3 127.5(8) . . ? C13 C12 H12 116.2 . . ? C3 C12 H12 116.2 . . ? C12 C13 C14 129.2(8) . . ? C12 C13 H13 115.4 . . ? C14 C13 H13 115.4 . . ? C15 C14 C13 127.1(8) . . ? C15 C14 S1 114.4(7) . . ? C13 C14 S1 118.5(6) . . ? C14 C15 S2 121.2(7) . . ? C14 C15 H15 119.4 . . ? S2 C15 H15 119.4 . . ? C17 C16 S2 122.8(7) . . ? C17 C16 S1 121.4(7) . . ? S2 C16 S1 115.7(5) . . ? C16 C17 S3 123.2(6) . . ? C16 C17 S4 121.4(7) . . ? S3 C17 S4 115.3(5) . . ? C19 C18 S3 119.3(10) . . ? C19 C18 H18 120.3 . . ? S3 C18 H18 120.3 . . ? C18 C19 S4 115.4(9) . . ? C18 C19 H19 122.3 . . ? S4 C19 H19 122.3 . . ? N6 C20 C21 124.7(7) . . ? N6 C20 N10 110.7(7) . . ? C21 C20 N10 124.6(7) . . ? C20 C21 C22 118.7(7) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C21 C22 C23 119.1(7) . . ? C21 C22 C31 119.8(7) . . ? C23 C22 C31 121.0(7) . . ? C24 C23 C22 117.2(7) . . ? C24 C23 H23 121.4 . . ? C22 C23 H23 121.4 . . ? N6 C24 C23 122.5(7) . . ? N6 C24 N8 113.2(6) . . ? C23 C24 N8 124.3(7) . . ? N8 C25 C26 108.5(8) . . ? N8 C25 H25 125.7 . . ? C26 C25 H25 125.7 . . ? C25 C26 C27 104.7(8) . . ? C25 C26 H26 127.7 . . ? C27 C26 H26 127.7 . . ? N7 C27 C26 112.5(8) . . ? N7 C27 H27 123.7 . . ? C26 C27 H27 123.7 . . ? N9 C28 C29 110.9(9) . . ? N9 C28 H28 124.5 . . ? C29 C28 H28 124.5 . . ? C30 C29 C28 106.0(9) . . ? C30 C29 H29 127.0 . . ? C28 C29 H29 127.0 . . ? C29 C30 N10 108.3(9) . . ? C29 C30 H30 125.8 . . ? N10 C30 H30 125.8 . . ? C32 C31 C22 126.7(8) . . ? C32 C31 H31 116.7 . . ? C22 C31 H31 116.7 . . ? C31 C32 C33 125.7(8) . . ? C31 C32 H32 117.1 . . ? C33 C32 H32 117.1 . . ? C34 C33 C32 125.3(8) . . ? C34 C33 S5 115.2(6) . . ? C32 C33 S5 119.5(6) . . ? C33 C34 S6 119.1(7) . . ? C33 C34 H34 120.4 . . ? S6 C34 H34 120.4 . . ? C36 C35 S5 123.7(6) . . ? C36 C35 S6 120.8(6) . . ? S5 C35 S6 115.4(5) . . ? C35 C36 S7 121.9(7) . . ? C35 C36 S8 122.9(7) . . ? S7 C36 S8 115.2(5) . . ? C38 C37 S7 117.4(9) . . ? C38 C37 H37 121.3 . . ? S7 C37 H37 121.3 . . ? C37 C38 S8 118.4(9) . . ? C37 C38 H38 120.8 . . ? S8 C38 H38 120.8 . . ? C40 C39 C41 123.7(11) . . ? C40 C39 S9 124.4(11) . . ? C41 C39 S9 111.8(9) . . ? C39 C40 C42 119.8(12) . . ? C39 C40 S10 121.9(10) . . ? C42 C40 S10 118.3(9) . . ? N11 C41 C39 170.5(13) . . ? N12 C42 C40 175.8(14) . . ? C44 C43 C45 121.7(11) . . ? C44 C43 S11 120.4(9) . . ? C45 C43 S11 117.8(8) . . ? C43 C44 C46 121.2(12) . . ? C43 C44 S12 120.7(10) . . ? C46 C44 S12 118.1(10) . . ? N13 C45 C43 176.1(14) . . ? N14 C46 C44 179(2) . . ? C48 C47 C49 120.5(8) . . ? C48 C47 S13 120.6(7) . . ? C49 C47 S13 118.8(7) . . ? C47 C48 C50 122.2(8) . . ? C47 C48 S14 120.3(7) . . ? C50 C48 S14 117.4(7) . . ? N15 C49 C47 177.0(13) . . ? N16 C50 C48 179.1(11) . . ? C52 C51 C53 120.9(9) . . ? C52 C51 S15 122.1(7) . . ? C53 C51 S15 116.9(9) . . ? C51 C52 C54 121.1(10) . . ? C51 C52 S16 119.5(7) . . ? C54 C52 S16 119.4(9) . . ? N17 C53 C51 179.5(11) . . ? N18 C54 C52 176.0(18) . . ? F4' B1 F3' 114(3) . . ? F4' B1 F1 125(3) . . ? F3' B1 F1 108(2) . . ? F4' B1 F2 111(3) . . ? F3' B1 F2 67(3) . . ? F1 B1 F2 116.8(13) . . ? F4' B1 F2' 89(3) . . ? F3' B1 F2' 116(3) . . ? F1 B1 F2' 103(3) . . ? F2 B1 F2' 49.2(17) . . ? F4' B1 F4 22(2) . . ? F3' B1 F4 127(4) . . ? F1 B1 F4 103.9(19) . . ? F2 B1 F4 130(3) . . ? F2' B1 F4 96(3) . . ? F4' B1 F3 92(2) . . ? F3' B1 F3 33(5) . . ? F1 B1 F3 106.0(16) . . ? F2 B1 F3 97(2) . . ? F2' B1 F3 144(3) . . ? F4 B1 F3 97.8(15) . . ? C2S C1S C6S 119.6(15) . . ? C2S C1S H1S 120.2 . . ? C6S C1S H1S 120.2 . . ? C1S C2S C3S 121.2(17) . . ? C1S C2S H2S 119.4 . . ? C3S C2S H2S 119.4 . . ? C2S C3S C4S 121.3(17) . . ? C2S C3S H3S 119.3 . . ? C4S C3S H3S 119.3 . . ? C5S C4S C3S 116.3(15) . . ? C5S C4S H4S 121.9 . . ? C3S C4S H4S 121.9 . . ? C6S C5S C4S 119.9(14) . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C5S C6S C1S 121.4(14) . . ? C5S C6S C7S 117.2(15) . . ? C1S C6S C7S 121.3(15) . . ? N1S C7S C6S 176.9(16) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 4.338 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.117