# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1512 data_global _audit_creation_method 'manual editing of form.cif' # SUBMISSION DETAILS _publ_contact_author_name 'Dr Berthold Kersting' _publ_contact_author_address ; Institut fuer Anorganische und Analytische Chemie Universit\"at Freiburg, Albertstr. 21 79104 Freiburg Germany ; _publ_contact_author_email 'kerstber@sun2.ruf.uni-freiburg.de' _publ_contact_author_phone '+49/(0)761/203 6129' _publ_contact_author_fax '+49/(0)761/203 6001' _publ_contact_letter ; Please consider this CIF submission for publication in Chem. Commun. ; _publ_requested_journal 'Chem. Commun.' # TITLE AND AUTHORLIST _publ_section_title ; Characterisation of a triply thiolate-bridged Ni-Fe amine-thiolate complex: insights into the electronic structure of the active site of [NiFe] hydrogenase ; _publ_author_list 'B. Kersting, G. Steinfeld' ###################################################################### data_nife #CHEMICAL DATA _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_formula_sum 'C178 H224 B3 Cl Fe2 N24 Ni2 O S6' _chemical_formula_weight 3205.17 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from CH3CN ; #CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R3(bar)c, No. 167' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 19.849(3) _cell_length_b 19.849(3) _cell_length_c 79.082(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 26982.7(79) _cell_formula_units_Z 6 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagon _exptl_crystal_colour black _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_F_000 10224 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 1.00 #EXPERIMENTAL DATA _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'BRUKER AXS' _diffrn_radiation_source ? _diffrn_radiation_monochromator graphite _diffrn_measurement_method 'multirun' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54984 _diffrn_reflns_av_R_equivalents 0.1943 _diffrn_reflns_av_sigmaI/netI 0.1523 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -95 _diffrn_reflns_limit_l_max 104 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.34 #REFINEMENT DATA _reflns_number_total 7430 _reflns_number_observed 3045 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0987P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7429 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1744 _refine_ls_R_factor_obs 0.0686 _refine_ls_wR_factor_all 0.2165 _refine_ls_wR_factor_obs 0.1675 _refine_ls_goodness_of_fit_all 0.917 _refine_ls_goodness_of_fit_obs 1.130 _refine_ls_restrained_S_all 0.918 _refine_ls_restrained_S_obs 1.130 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.316 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.101 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.6667 0.3333 0.033320(12) 0.0282(3) Uani 1 d S . Ni Ni 0.6667 0.3333 -0.004995(12) 0.0286(2) Uani 1 d S . Cl Cl 0.6667 0.3333 0.0833 0.0498(8) Uani 1 d S . S1 S 0.65287(7) 0.23612(7) 0.015534(14) 0.0326(3) Uani 1 d . . N1 N 0.7447(2) 0.3183(2) -0.01987(4) 0.0305(8) Uani 1 d . . H1 H 0.7938(2) 0.3576(2) -0.01659(4) 0.037 Uiso 1 calc R . N2 N 0.7423(2) 0.3196(2) 0.04858(4) 0.0350(9) Uani 1 d . . H2A H 0.7914(2) 0.3607(2) 0.04661(4) 0.042 Uiso 1 calc R . H2B H 0.7300(2) 0.3235(2) 0.05962(4) 0.042 Uiso 1 calc R . C101 C 0.7453(3) 0.2427(3) 0.01527(6) 0.0310(9) Uani 1 d . . C102 C 0.7814(3) 0.2440(3) 0.03043(6) 0.0345(11) Uani 1 d . . C103 C 0.8523(3) 0.2462(3) 0.03013(6) 0.0373(11) Uani 1 d . . H103 H 0.8765(3) 0.2472(3) 0.04056(6) 0.045 Uiso 1 calc R . C104 C 0.8892(3) 0.2471(3) 0.01515(6) 0.0385(11) Uani 1 d . . C105 C 0.8522(3) 0.2474(3) 0.00026(6) 0.0362(11) Uani 1 d . . H105 H 0.8768(3) 0.2498(3) -0.01020(6) 0.043 Uiso 1 calc R . C106 C 0.7810(3) 0.2443(2) 0.00000(6) 0.0333(11) Uani 1 d . . C107 C 0.7448(3) 0.2433(3) -0.01674(5) 0.0327(10) Uani 1 d . . H10A H 0.6906(3) 0.1994(3) -0.01698(5) 0.039 Uiso 1 calc R . H10B H 0.7740(3) 0.2351(3) -0.02590(5) 0.039 Uiso 1 calc R . C108 C 0.7457(3) 0.2463(3) 0.04699(5) 0.0387(11) Uani 1 d . . H10C H 0.6925(3) 0.2009(3) 0.04779(5) 0.046 Uiso 1 calc R . H10D H 0.7769(3) 0.2431(3) 0.05640(5) 0.046 Uiso 1 calc R . C109 C 0.9668(3) 0.2486(3) 0.01467(7) 0.0484(13) Uani 1 d . . C110 C 1.0298(3) 0.3265(4) 0.00707(9) 0.083(2) Uani 1 d . . H11A H 1.0309(3) 0.3697(4) 0.01333(9) 0.124 Uiso 1 calc R . H11B H 1.0177(3) 0.3294(4) -0.00483(9) 0.124 Uiso 1 calc R . H11C H 1.0807(3) 0.3300(4) 0.00790(9) 0.124 Uiso 1 calc R . C111 C 0.9591(4) 0.1825(5) 0.00353(11) 0.105(3) Uani 1 d . . H11D H 1.0094(4) 0.1977(5) -0.00175(11) 0.158 Uiso 1 calc R . H11E H 0.9202(4) 0.1715(5) -0.00528(11) 0.158 Uiso 1 calc R . H11F H 0.9428(4) 0.1359(5) 0.01044(11) 0.158 Uiso 1 calc R . C112 C 0.9951(4) 0.2412(6) 0.03202(9) 0.109(3) Uani 1 d . . H11G H 0.9541(4) 0.1950(6) 0.03773(9) 0.164 Uiso 1 calc R . H11H H 1.0078(4) 0.2876(6) 0.03873(9) 0.164 Uiso 1 calc R . H11I H 1.0416(4) 0.2363(6) 0.03081(9) 0.164 Uiso 1 calc R . C113 C 0.7393(3) 0.3311(3) -0.03838(5) 0.0417(12) Uani 1 d . . H11J H 0.7413(3) 0.2891(3) -0.04472(5) 0.050 Uiso 1 calc R . H11K H 0.7857(3) 0.3809(3) -0.04165(5) 0.050 Uiso 1 calc R . C114 C 0.6667 0.3333 -0.04393(8) 0.030(2) Uani 1 d S . C115 C 0.6667 0.3333 -0.06350(10) 0.045(2) Uani 1 d S . H11L H 0.6233 0.3392 -0.06763(10) 0.068 Uiso 0.33 calc PR . H11M H 0.6608 0.2841 -0.06763(10) 0.068 Uiso 0.33 calc PR . H11N H 0.7159 0.3767 -0.06763(10) 0.068 Uiso 0.33 calc PR . B1 B 0.1847(4) 0.3333 0.0833 0.043(2) Uani 1 d S . C201 C 0.1679(3) 0.4049(3) 0.07887(6) 0.0464(13) Uani 1 d . . C202 C 0.1677(3) 0.4557(3) 0.09076(8) 0.060(2) Uani 1 d . . H202 H 0.1842(3) 0.4535(3) 0.10191(8) 0.072 Uiso 1 calc R . C203 C 0.1445(4) 0.5099(4) 0.08730(9) 0.074(2) Uani 1 d . . H203 H 0.1459(4) 0.5440(4) 0.09592(9) 0.088 Uiso 1 calc R . C204 C 0.1197(4) 0.5137(4) 0.07133(10) 0.071(2) Uani 1 d . . H204 H 0.1031(4) 0.5500(4) 0.06887(10) 0.086 Uiso 1 calc R . C205 C 0.1189(3) 0.4655(4) 0.05902(8) 0.063(2) Uani 1 d . . H205 H 0.1019(3) 0.4683(4) 0.04794(8) 0.076 Uiso 1 calc R . C206 C 0.1429(3) 0.4119(3) 0.06259(7) 0.0511(14) Uani 1 d . . H206 H 0.1424(3) 0.3791(3) 0.05378(7) 0.061 Uiso 1 calc R . C301 C 0.2252(3) 0.3140(3) 0.06769(6) 0.0473(13) Uani 1 d . . C302 C 0.2806(3) 0.3730(4) 0.05720(7) 0.0566(15) Uani 1 d . . H302 H 0.2907(3) 0.4247(4) 0.05877(7) 0.068 Uiso 1 calc R . C303 C 0.3211(4) 0.3592(4) 0.04470(8) 0.071(2) Uani 1 d . . H303 H 0.3570(4) 0.4006(4) 0.03772(8) 0.085 Uiso 1 calc R . C304 C 0.3090(5) 0.2856(5) 0.04247(8) 0.089(3) Uani 1 d . . H304 H 0.3374(5) 0.2760(5) 0.03406(8) 0.106 Uiso 1 calc R . C305 C 0.2556(5) 0.2249(5) 0.05243(9) 0.086(2) Uani 1 d . . H305 H 0.2469(5) 0.1737(5) 0.05087(9) 0.104 Uiso 1 calc R . C306 C 0.2151(4) 0.2399(4) 0.06463(7) 0.063(2) Uani 1 d . . H306 H 0.1783(4) 0.1977(4) 0.07132(7) 0.075 Uiso 1 calc R . N3 N 1.0887(3) 0.5505(3) 0.01639(6) 0.0624(13) Uiso 1 d . . C1 C 1.0284(3) 0.5110(3) 0.02117(6) 0.0470(12) Uiso 1 d . . C2 C 0.9505(4) 0.4594(4) 0.02727(8) 0.083(2) Uiso 1 d . . H2C H 0.9150(4) 0.4755(4) 0.02259(8) 0.124 Uiso 1 calc R . H2D H 0.9499(4) 0.4618(4) 0.03964(8) 0.124 Uiso 1 calc R . H2E H 0.9338(4) 0.4061(4) 0.02370(8) 0.124 Uiso 1 calc R . N4 N 0.5413(7) 0.4347(6) 0.06797(13) 0.067(3) Uiso 0.50 d P 1 C3 C 0.4863(7) 0.3937(7) 0.07512(14) 0.053(3) Uiso 0.50 d P 1 C4 C 0.4133(6) 0.3333 0.0833 0.089(3) Uiso 1 d S 1 N5 N 0.5944(7) 0.4910(7) 0.06849(14) 0.074(3) Uiso 0.50 d P 1 C5 C 0.6234(7) 0.5471(7) 0.07634(15) 0.059(3) Uiso 0.50 d P 1 C6 C 0.6667 0.6209(6) 0.0833 0.095(3) Uiso 1 d S 1 O1 O 0.6667 0.3333 -0.1141(4) 0.239(16) Uiso 0.50 d SP 1 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 Fe 0.0286(4) 0.0286(4) 0.0274(5) 0.000 0.000 0.0143(2) Ni 0.0279(3) 0.0279(3) 0.0301(5) 0.000 0.000 0.0139(2) Cl 0.0607(12) 0.0607(12) 0.0281(14) 0.000 0.000 0.0304(6) S1 0.0318(6) 0.0305(6) 0.0361(6) -0.0007(5) -0.0004(5) 0.0161(5) N1 0.029(2) 0.028(2) 0.034(2) 0.001(2) -0.001(2) 0.014(2) N2 0.036(2) 0.040(2) 0.030(2) -0.002(2) 0.001(2) 0.020(2) C101 0.027(2) 0.025(2) 0.041(2) -0.002(2) -0.003(2) 0.013(2) C102 0.035(3) 0.030(3) 0.040(3) 0.002(2) 0.001(2) 0.018(2) C103 0.034(3) 0.038(3) 0.040(3) 0.002(2) -0.005(2) 0.019(2) C104 0.033(3) 0.035(3) 0.049(3) 0.000(2) -0.001(2) 0.018(2) C105 0.037(3) 0.036(3) 0.039(3) 0.001(2) 0.005(2) 0.021(2) C106 0.036(3) 0.027(2) 0.040(3) -0.004(2) -0.005(2) 0.018(2) C107 0.033(3) 0.032(3) 0.036(2) -0.003(2) 0.001(2) 0.019(2) C108 0.038(3) 0.041(3) 0.038(3) 0.008(2) -0.001(2) 0.021(2) C109 0.034(3) 0.058(4) 0.056(3) -0.004(3) -0.003(2) 0.025(3) C110 0.038(4) 0.088(5) 0.112(6) 0.011(4) 0.012(4) 0.023(4) C111 0.066(5) 0.106(6) 0.174(8) -0.065(6) -0.033(5) 0.066(5) C112 0.073(5) 0.207(10) 0.086(5) 0.018(6) 0.001(4) 0.099(6) C113 0.049(3) 0.050(3) 0.034(3) 0.008(2) 0.007(2) 0.030(3) C114 0.035(3) 0.035(3) 0.021(3) 0.000 0.000 0.0175(13) C115 0.047(3) 0.047(3) 0.042(5) 0.000 0.000 0.023(2) B1 0.046(4) 0.040(5) 0.041(5) 0.009(4) 0.005(2) 0.020(2) C201 0.041(3) 0.046(3) 0.048(3) 0.016(3) 0.014(2) 0.018(3) C202 0.065(4) 0.057(4) 0.060(4) 0.018(3) 0.019(3) 0.034(3) C203 0.084(5) 0.064(4) 0.086(5) 0.020(4) 0.030(4) 0.047(4) C204 0.058(4) 0.052(4) 0.117(6) 0.035(4) 0.030(4) 0.037(3) C205 0.045(3) 0.065(4) 0.082(5) 0.041(4) 0.014(3) 0.029(3) C206 0.039(3) 0.054(3) 0.058(3) 0.017(3) 0.008(3) 0.021(3) C301 0.052(3) 0.055(4) 0.042(3) 0.011(2) 0.003(2) 0.031(3) C302 0.061(4) 0.068(4) 0.050(3) 0.020(3) 0.009(3) 0.039(3) C303 0.071(4) 0.099(6) 0.061(4) 0.036(4) 0.030(3) 0.056(4) C304 0.115(7) 0.141(8) 0.056(4) 0.015(5) 0.020(4) 0.098(6) C305 0.119(7) 0.090(6) 0.080(5) 0.009(4) 0.025(5) 0.075(5) C306 0.082(5) 0.064(4) 0.059(4) 0.012(3) 0.017(3) 0.049(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 Fe N2 2.047(4) . ? Fe N2 2.047(4) 3_665 ? Fe N2 2.047(4) 2_655 ? Fe S1 2.2909(13) . ? Fe S1 2.2909(13) 2_655 ? Fe S1 2.2909(13) 3_665 ? Ni N1 2.083(4) . ? Ni N1 2.083(4) 3_665 ? Ni N1 2.083(4) 2_655 ? Ni S1 2.4302(13) . ? Ni S1 2.4302(13) 2_655 ? Ni S1 2.4302(13) 3_665 ? S1 C101 1.772(4) . ? N1 C113 1.499(5) . ? N1 C107 1.509(5) . ? N2 C108 1.496(6) . ? C101 C102 1.391(6) . ? C101 C106 1.394(6) . ? C102 C103 1.385(6) . ? C102 C108 1.501(6) . ? C103 C104 1.389(6) . ? C104 C105 1.390(6) . ? C104 C109 1.526(7) . ? C105 C106 1.383(6) . ? C106 C107 1.502(6) . ? C109 C112 1.516(8) . ? C109 C111 1.522(8) . ? C109 C110 1.544(8) . ? C113 C114 1.529(5) . ? C114 C113 1.529(5) 3_665 ? C114 C113 1.529(5) 2_655 ? C114 C115 1.548(10) . ? B1 C301 1.622(7) . ? B1 C301 1.622(7) 17_554 ? B1 C201 1.652(7) 17_554 ? B1 C201 1.652(7) . ? C201 C202 1.380(7) . ? C201 C206 1.412(7) . ? C202 C203 1.393(8) . ? C203 C204 1.371(9) . ? C204 C205 1.360(9) . ? C205 C206 1.393(7) . ? C301 C306 1.403(7) . ? C301 C302 1.407(7) . ? C302 C303 1.385(8) . ? C303 C304 1.369(10) . ? C304 C305 1.385(10) . ? C305 C306 1.380(8) . ? N3 C1 1.119(6) . ? C1 C2 1.445(8) . ? N4 N5 1.088(13) . ? N4 C3 1.134(13) . ? C3 C4 1.490(13) . ? C4 C3 1.490(13) 17_554 ? N5 C5 1.146(14) . ? C5 C6 1.390(14) . ? C5 C5 1.85(2) 18_654 ? C6 C5 1.390(14) 18_654 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe N2 88.77(14) . 3_665 ? N2 Fe N2 88.77(14) . 2_655 ? N2 Fe N2 88.77(14) 3_665 2_655 ? N2 Fe S1 92.11(11) . . ? N2 Fe S1 92.85(11) 3_665 . ? N2 Fe S1 178.17(11) 2_655 . ? N2 Fe S1 92.85(11) . 2_655 ? N2 Fe S1 178.17(11) 3_665 2_655 ? N2 Fe S1 92.11(11) 2_655 2_655 ? S1 Fe S1 86.25(5) . 2_655 ? N2 Fe S1 178.17(11) . 3_665 ? N2 Fe S1 92.11(11) 3_665 3_665 ? N2 Fe S1 92.85(11) 2_655 3_665 ? S1 Fe S1 86.25(5) . 3_665 ? S1 Fe S1 86.25(5) 2_655 3_665 ? N1 Ni N1 91.23(13) . 3_665 ? N1 Ni N1 91.23(13) . 2_655 ? N1 Ni N1 91.23(13) 3_665 2_655 ? N1 Ni S1 93.44(10) . . ? N1 Ni S1 94.63(10) 3_665 . ? N1 Ni S1 172.42(10) 2_655 . ? N1 Ni S1 94.63(10) . 2_655 ? N1 Ni S1 172.42(10) 3_665 2_655 ? N1 Ni S1 93.44(10) 2_655 2_655 ? S1 Ni S1 80.24(5) . 2_655 ? N1 Ni S1 172.42(10) . 3_665 ? N1 Ni S1 93.44(10) 3_665 3_665 ? N1 Ni S1 94.63(10) 2_655 3_665 ? S1 Ni S1 80.24(5) . 3_665 ? S1 Ni S1 80.24(5) 2_655 3_665 ? C101 S1 Fe 105.15(15) . . ? C101 S1 Ni 103.4(2) . . ? Fe S1 Ni 79.79(5) . . ? C113 N1 C107 111.3(3) . . ? C113 N1 Ni 113.9(3) . . ? C107 N1 Ni 114.6(3) . . ? C108 N2 Fe 118.2(3) . . ? C102 C101 C106 119.6(4) . . ? C102 C101 S1 119.8(3) . . ? C106 C101 S1 120.6(3) . . ? C103 C102 C101 119.5(4) . . ? C103 C102 C108 120.1(4) . . ? C101 C102 C108 120.4(4) . . ? C102 C103 C104 122.5(4) . . ? C103 C104 C105 116.4(4) . . ? C103 C104 C109 122.9(4) . . ? C105 C104 C109 120.7(4) . . ? C106 C105 C104 122.9(4) . . ? C105 C106 C101 119.1(4) . . ? C105 C106 C107 119.1(4) . . ? C101 C106 C107 121.8(4) . . ? C106 C107 N1 111.6(3) . . ? N2 C108 C102 110.7(4) . . ? C112 C109 C111 108.9(6) . . ? C112 C109 C104 113.2(5) . . ? C111 C109 C104 109.4(4) . . ? C112 C109 C110 107.2(5) . . ? C111 C109 C110 108.7(6) . . ? C104 C109 C110 109.4(5) . . ? N1 C113 C114 115.7(4) . . ? C113 C114 C113 112.1(3) . 3_665 ? C113 C114 C113 112.1(3) . 2_655 ? C113 C114 C113 112.1(3) 3_665 2_655 ? C113 C114 C115 106.7(3) . . ? C113 C114 C115 106.7(3) 3_665 . ? C113 C114 C115 106.7(3) 2_655 . ? C301 B1 C301 104.3(6) . 17_554 ? C301 B1 C201 113.5(3) . 17_554 ? C301 B1 C201 112.2(2) 17_554 17_554 ? C301 B1 C201 112.2(2) . . ? C301 B1 C201 113.5(3) 17_554 . ? C201 B1 C201 101.6(6) 17_554 . ? C202 C201 C206 114.8(5) . . ? C202 C201 B1 124.0(4) . . ? C206 C201 B1 120.8(4) . . ? C201 C202 C203 123.6(6) . . ? C204 C203 C202 119.3(6) . . ? C205 C204 C203 119.9(6) . . ? C204 C205 C206 120.2(6) . . ? C205 C206 C201 122.1(6) . . ? C306 C301 C302 114.4(5) . . ? C306 C301 B1 123.4(4) . . ? C302 C301 B1 121.8(5) . . ? C303 C302 C301 123.1(6) . . ? C304 C303 C302 119.6(6) . . ? C303 C304 C305 120.3(6) . . ? C306 C305 C304 119.1(7) . . ? C305 C306 C301 123.6(6) . . ? N3 C1 C2 179.5(7) . . ? N5 N4 C3 144.0(14) . . ? N4 C3 C4 174.1(12) . . ? C3 C4 C3 110.4(11) . 17_554 ? N4 N5 C5 140.9(14) . . ? N5 C5 C6 169.9(13) . . ? N5 C5 C5 132.2(9) . 18_654 ? C6 C5 C5 48.1(6) . 18_654 ? C5 C6 C5 83.7(12) . 18_654 ? #===END