# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/226 # Authors: Ha-Jin Lee and Dong-Youn Noh # Affiliation: Department of Chemistry, Seoul Women's University, # Seoul 139-774, Korea # Complex 1 data_ni _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'TBA[Ni(fcvdt)2](COMe2)0.5' _chemical_formula_moiety '(C16H36N)[Ni(C14H10S4Fe)2](C3H6O)0.5' _chemical_formula_sum 'C45.50 H59 Fe2 N Ni O0.50 S8' _chemical_formula_weight 1054.83 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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'S' 'S' 0.1246 0.1234 '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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 19.503(4) _cell_length_b 10.841(3) _cell_length_c 24.137(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.13(3) _cell_angle_gamma 90.00 _cell_volume 5064(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 23.47 _exptl_crystal_description 'parallelipiped' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2204 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4841 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.47 _reflns_number_total 4697 _reflns_number_gt 4519 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1589P)^2^+2.2799P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4697 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2003 _refine_ls_wR_factor_gt 0.1971 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.750 _refine_ls_shift/su_mean 0.046 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.35505(6) 0.52942(10) 0.27612(5) 0.0491(4) Uani 1 d . . . Fe1 Fe 0.10423(7) 0.20061(12) 0.50078(5) 0.0474(4) Uani 1 d . . . Fe3 Fe 0.62168(7) 0.93793(14) 0.08897(6) 0.0578(4) Uani 1 d . . . S1 S 0.40318(12) 0.3915(2) 0.33178(11) 0.0565(7) Uani 1 d . . . S2 S 0.25689(12) 0.5008(2) 0.30643(11) 0.0529(6) Uani 1 d . . . S3 S 0.36665(13) 0.2556(2) 0.42984(11) 0.0590(7) Uani 1 d . . . S4 S 0.21073(13) 0.3817(2) 0.40574(11) 0.0556(7) Uani 1 d . . . S5 S 0.45502(13) 0.5702(2) 0.25218(13) 0.0640(7) Uani 1 d . . . S6 S 0.30657(12) 0.6634(2) 0.21788(11) 0.0551(6) Uani 1 d . . . S7 S 0.50879(14) 0.7156(2) 0.16291(14) 0.0718(8) Uani 1 d . . . S8 S 0.35182(13) 0.8220(3) 0.12843(12) 0.0621(7) Uani 1 d . . . C1 C 0.3409(5) 0.3549(8) 0.3737(4) 0.045(2) Uani 1 d . . . C2 C 0.2763(5) 0.4051(8) 0.3635(4) 0.046(2) Uani 1 d . . . C3 C 0.2901(5) 0.1792(8) 0.4398(4) 0.051(2) Uani 1 d . . . H3 H 0.2938 0.0989 0.4533 0.061 Uiso 1 calc R . . C4 C 0.2259(5) 0.2278(8) 0.4294(4) 0.051(2) Uani 1 d . . . C5 C 0.4387(5) 0.6720(9) 0.1975(4) 0.056(3) Uani 1 d . . . C6 C 0.3729(5) 0.7143(8) 0.1827(4) 0.052(2) Uani 1 d . . . C7 C 0.4912(5) 0.8728(9) 0.1464(4) 0.055(2) Uani 1 d . . . C8 C 0.4263(5) 0.9124(9) 0.1335(4) 0.061(3) Uani 1 d . . . H8 H 0.4203 0.9963 0.1265 0.073 Uiso 1 calc R . . C11 C 0.1637(5) 0.1588(8) 0.4401(4) 0.049(2) Uani 1 d . . . C12 C 0.0943(5) 0.1830(9) 0.4155(4) 0.055(2) Uani 1 d . . . H12 H 0.0797 0.2439 0.3896 0.067 Uiso 1 calc R . . C13 C 0.0524(6) 0.0946(10) 0.4389(4) 0.063(3) Uani 1 d . . . H13 H 0.0046 0.0885 0.4306 0.076 Uiso 1 calc R . . C14 C 0.0927(5) 0.0191(9) 0.4756(5) 0.065(3) Uani 1 d . . . H14 H 0.0768 -0.0463 0.4955 0.078 Uiso 1 calc R . . C15 C 0.1617(6) 0.0578(8) 0.4780(4) 0.059(3) Uani 1 d . . . H15 H 0.1994 0.0238 0.5002 0.071 Uiso 1 calc R . . C16 C 0.1541(6) 0.3372(10) 0.5498(5) 0.067(3) Uani 1 d . . . H16 H 0.1981 0.3681 0.5473 0.080 Uiso 1 calc R . . C17 C 0.0913(7) 0.3807(10) 0.5205(5) 0.081(4) Uani 1 d . . . H17 H 0.0862 0.4454 0.4950 0.098 Uiso 1 calc R . . C18 C 0.0363(6) 0.3046(14) 0.5380(6) 0.091(4) Uani 1 d . . . H18 H -0.0107 0.3106 0.5258 0.110 Uiso 1 calc R . . C19 C 0.0683(7) 0.2210(11) 0.5765(5) 0.077(3) Uani 1 d . . . H19 H 0.0460 0.1612 0.5952 0.092 Uiso 1 calc R . . C20 C 0.1378(6) 0.2411(10) 0.5824(4) 0.068(3) Uani 1 d . . . H20 H 0.1699 0.1954 0.6057 0.081 Uiso 1 calc R . . C21 C 0.5521(5) 0.9525(8) 0.1452(4) 0.049(2) Uani 1 d . . . C22 C 0.6189(5) 0.9323(9) 0.1729(4) 0.054(2) Uani 1 d . . . H22 H 0.6324 0.8660 0.1962 0.064 Uiso 1 calc R . . C23 C 0.6622(5) 1.0291(10) 0.1594(4) 0.060(3) Uani 1 d . . . H23 H 0.7089 1.0382 0.1722 0.072 Uiso 1 calc R . . C24 C 0.6222(6) 1.1088(11) 0.1235(5) 0.075(3) Uani 1 d . . . H24 H 0.6377 1.1811 0.1085 0.090 Uiso 1 calc R . . C25 C 0.5537(5) 1.0612(9) 0.1135(4) 0.057(2) Uani 1 d . . . H25 H 0.5169 1.0955 0.0904 0.069 Uiso 1 calc R . . C26 C 0.6538(16) 0.7758(15) 0.0622(9) 0.139(8) Uani 1 d . . . H26 H 0.6625 0.7056 0.0842 0.167 Uiso 1 calc R . . C27 C 0.7011(8) 0.8645(17) 0.0542(6) 0.100(5) Uani 1 d . . . H27 H 0.7470 0.8668 0.0700 0.120 Uiso 1 calc R . . C28 C 0.6685(8) 0.9485(16) 0.0188(6) 0.101(5) Uani 1 d . . . H28 H 0.6897 1.0176 0.0057 0.121 Uiso 1 calc R . . C29 C 0.6008(9) 0.9189(19) 0.0049(6) 0.109(5) Uani 1 d . . . H29 H 0.5678 0.9633 -0.0180 0.130 Uiso 1 calc R . . C30 C 0.5910(11) 0.806(2) 0.0326(9) 0.139(9) Uani 1 d . . . H30 H 0.5501 0.7617 0.0312 0.167 Uiso 1 calc R . . N N 0.2258(4) 0.0550(7) 0.2593(3) 0.055(2) Uani 1 d . . . C31 C 0.1939(5) -0.0705(9) 0.2700(5) 0.065(3) Uani 1 d . . . H31A H 0.1503 -0.0777 0.2460 0.078 Uiso 1 calc R . . H31B H 0.2242 -0.1345 0.2590 0.078 Uiso 1 calc R . . C32 C 0.1808(6) -0.0950(9) 0.3300(5) 0.074(3) Uani 1 d . . . H32A H 0.2244 -0.0942 0.3542 0.089 Uiso 1 calc R . . H32B H 0.1519 -0.0300 0.3421 0.089 Uiso 1 calc R . . C33 C 0.1455(6) -0.2185(10) 0.3348(6) 0.080(3) Uani 1 d . . . H33A H 0.0996 -0.2145 0.3142 0.095 Uiso 1 calc R . . H33B H 0.1712 -0.2810 0.3173 0.095 Uiso 1 calc R . . C34 C 0.1394(8) -0.2572(13) 0.3929(6) 0.105(5) Uani 1 d . . . H34A H 0.1168 -0.3360 0.3926 0.158 Uiso 1 calc R . . H34B H 0.1128 -0.1973 0.4103 0.158 Uiso 1 calc R . . H34C H 0.1846 -0.2635 0.4135 0.158 Uiso 1 calc R . . C35 C 0.1782(5) 0.1604(9) 0.2738(4) 0.059(3) Uani 1 d . . . H35A H 0.1718 0.1539 0.3129 0.071 Uiso 1 calc R . . H35B H 0.2008 0.2384 0.2687 0.071 Uiso 1 calc R . . C36 C 0.1073(6) 0.1611(10) 0.2390(5) 0.073(3) Uani 1 d . . . H36A H 0.0833 0.0848 0.2449 0.088 Uiso 1 calc R . . H36B H 0.1129 0.1667 0.1997 0.088 Uiso 1 calc R . . C37 C 0.0645(7) 0.2706(12) 0.2554(5) 0.084(4) Uani 1 d . . . H37A H 0.0580 0.2639 0.2945 0.100 Uiso 1 calc R . . H37B H 0.0891 0.3468 0.2504 0.100 Uiso 1 calc R . . C38 C -0.0052(6) 0.2739(11) 0.2200(5) 0.080(4) Uani 1 d . . . H38A H -0.0313 0.3430 0.2309 0.120 Uiso 1 calc R . . H38B H -0.0298 0.1989 0.2253 0.120 Uiso 1 calc R . . H38C H 0.0012 0.2818 0.1814 0.120 Uiso 1 calc R . . C39 C 0.2367(6) 0.0585(11) 0.1990(4) 0.072(3) Uani 1 d . . . H39A H 0.1920 0.0511 0.1766 0.086 Uiso 1 calc R . . H39B H 0.2638 -0.0131 0.1913 0.086 Uiso 1 calc R . . C40 C 0.2727(7) 0.1735(12) 0.1799(5) 0.083(4) Uani 1 d . . . H40A H 0.2473 0.2461 0.1891 0.099 Uiso 1 calc R . . H40B H 0.3188 0.1787 0.2001 0.099 Uiso 1 calc R . . C41 C 0.2776(7) 0.1728(14) 0.1191(5) 0.096(4) Uani 1 d . . . H41A H 0.2314 0.1716 0.0988 0.115 Uiso 1 calc R . . H41B H 0.3011 0.0983 0.1096 0.115 Uiso 1 calc R . . C42 C 0.3164(10) 0.2847(17) 0.1007(7) 0.142(7) Uani 1 d . . . H42A H 0.3183 0.2806 0.0612 0.213 Uiso 1 calc R . . H42B H 0.3625 0.2853 0.1200 0.213 Uiso 1 calc R . . H42C H 0.2929 0.3587 0.1094 0.213 Uiso 1 calc R . . C43 C 0.2934(5) 0.0708(9) 0.2964(4) 0.062(3) Uani 1 d . . . H43A H 0.3099 0.1541 0.2916 0.074 Uiso 1 calc R . . H43B H 0.2847 0.0626 0.3349 0.074 Uiso 1 calc R . . C44 C 0.3503(5) -0.0179(9) 0.2865(4) 0.061(3) Uani 1 d . . . H44A H 0.3599 -0.0107 0.2482 0.073 Uiso 1 calc R . . H44B H 0.3353 -0.1017 0.2923 0.073 Uiso 1 calc R . . C45 C 0.4166(6) 0.0093(10) 0.3264(5) 0.070(3) Uani 1 d . . . H45A H 0.4288 0.0956 0.3234 0.083 Uiso 1 calc R . . H45B H 0.4081 -0.0060 0.3646 0.083 Uiso 1 calc R . . C46 C 0.4769(6) -0.0710(12) 0.3129(6) 0.091(4) Uani 1 d . . . H46A H 0.5176 -0.0510 0.3379 0.136 Uiso 1 calc R . . H46B H 0.4854 -0.0560 0.2751 0.136 Uiso 1 calc R . . H46C H 0.4656 -0.1564 0.3171 0.136 Uiso 1 calc R . . O O 0.0814(18) 0.084(2) 0.060(2) 0.26(2) Uani 0.50 d P . . C50 C 0.0000 0.0000 0.0000 0.21(2) Uani 1 d S . . C51 C 0.077(3) 0.026(5) -0.036(3) 0.59(6) Uani 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 Ni 0.0417(7) 0.0345(6) 0.0747(8) 0.0004(5) 0.0221(6) -0.0034(5) Fe1 0.0441(8) 0.0373(7) 0.0637(8) 0.0028(6) 0.0188(6) 0.0004(6) Fe3 0.0461(8) 0.0644(9) 0.0666(9) -0.0006(7) 0.0221(7) -0.0045(7) S1 0.0409(13) 0.0484(14) 0.0833(18) 0.0072(12) 0.0204(12) 0.0009(11) S2 0.0436(13) 0.0406(13) 0.0775(16) 0.0106(11) 0.0196(11) 0.0012(10) S3 0.0431(14) 0.0556(15) 0.0789(17) 0.0096(13) 0.0097(12) 0.0001(12) S4 0.0516(14) 0.0374(12) 0.0839(17) 0.0068(11) 0.0327(13) 0.0060(11) S5 0.0422(14) 0.0455(14) 0.108(2) 0.0196(13) 0.0251(13) 0.0030(11) S6 0.0393(13) 0.0441(13) 0.0859(17) 0.0081(12) 0.0232(12) -0.0007(11) S7 0.0541(16) 0.0459(15) 0.124(2) 0.0128(14) 0.0474(16) 0.0081(12) S8 0.0435(14) 0.0614(16) 0.0831(18) 0.0123(13) 0.0146(12) -0.0009(12) C1 0.045(5) 0.037(5) 0.057(5) -0.003(4) 0.014(4) -0.007(4) C2 0.039(5) 0.041(5) 0.061(6) -0.007(4) 0.017(4) -0.003(4) C3 0.048(6) 0.029(5) 0.079(6) 0.009(4) 0.020(5) 0.001(4) C4 0.050(6) 0.040(5) 0.067(6) 0.004(4) 0.022(5) -0.002(4) C5 0.035(5) 0.044(5) 0.095(7) 0.012(5) 0.033(5) 0.005(4) C6 0.054(6) 0.037(5) 0.069(6) 0.002(4) 0.022(5) -0.004(4) C7 0.045(6) 0.051(6) 0.074(6) 0.007(5) 0.026(5) 0.005(5) C8 0.051(6) 0.048(6) 0.088(7) 0.018(5) 0.031(5) 0.008(5) C11 0.055(6) 0.033(5) 0.062(6) -0.006(4) 0.023(4) -0.007(4) C12 0.052(6) 0.054(6) 0.063(6) 0.003(5) 0.015(5) -0.007(5) C13 0.057(6) 0.061(7) 0.075(7) -0.011(6) 0.020(5) -0.017(6) C14 0.054(6) 0.046(6) 0.098(8) 0.005(6) 0.021(6) -0.011(5) C15 0.063(7) 0.036(5) 0.085(7) 0.005(5) 0.032(5) 0.005(5) C16 0.066(7) 0.052(6) 0.085(8) -0.013(6) 0.018(6) -0.004(6) C17 0.124(11) 0.042(6) 0.084(8) -0.003(5) 0.034(8) 0.022(7) C18 0.051(7) 0.108(11) 0.121(11) -0.034(9) 0.035(7) 0.015(7) C19 0.080(9) 0.072(8) 0.087(8) -0.011(6) 0.043(7) -0.008(7) C20 0.076(8) 0.066(7) 0.060(6) -0.003(5) 0.004(5) 0.000(6) C21 0.045(6) 0.044(5) 0.061(6) 0.001(4) 0.014(4) -0.001(4) C22 0.054(6) 0.056(6) 0.052(5) 0.002(4) 0.013(4) -0.006(5) C23 0.044(6) 0.062(7) 0.074(7) -0.003(5) 0.011(5) -0.007(5) C24 0.053(7) 0.067(7) 0.108(9) 0.003(6) 0.024(6) -0.013(6) C25 0.052(6) 0.047(6) 0.075(6) 0.002(5) 0.015(5) -0.001(5) C26 0.22(2) 0.066(10) 0.155(17) -0.021(10) 0.120(18) 0.015(14) C27 0.076(9) 0.135(14) 0.096(10) -0.005(9) 0.039(8) 0.026(10) C28 0.083(10) 0.132(14) 0.097(10) 0.001(9) 0.051(8) -0.004(10) C29 0.092(12) 0.165(17) 0.072(9) -0.019(10) 0.018(8) 0.008(11) C30 0.110(14) 0.17(2) 0.150(17) -0.090(16) 0.077(13) -0.066(15) N 0.048(5) 0.048(5) 0.070(5) -0.009(4) 0.018(4) 0.003(4) C31 0.051(6) 0.041(5) 0.103(8) -0.017(5) 0.011(5) 0.003(5) C32 0.083(8) 0.046(6) 0.098(9) 0.005(5) 0.032(7) -0.008(6) C33 0.057(7) 0.050(7) 0.134(11) -0.004(7) 0.024(7) -0.001(5) C34 0.103(11) 0.070(9) 0.152(13) 0.008(8) 0.054(9) -0.032(8) C35 0.066(7) 0.041(5) 0.077(7) -0.005(5) 0.034(5) 0.014(5) C36 0.065(7) 0.041(6) 0.119(9) -0.005(6) 0.034(7) 0.004(5) C37 0.079(9) 0.081(9) 0.097(9) 0.005(7) 0.035(7) 0.021(7) C38 0.078(8) 0.077(8) 0.092(8) 0.014(6) 0.041(7) 0.015(7) C39 0.071(7) 0.071(7) 0.078(7) -0.011(6) 0.024(6) 0.020(6) C40 0.089(9) 0.078(8) 0.089(8) 0.015(6) 0.041(7) 0.025(7) C41 0.104(10) 0.109(11) 0.083(8) 0.026(7) 0.042(7) 0.058(9) C42 0.153(16) 0.142(16) 0.149(15) 0.051(12) 0.093(13) 0.044(13) C43 0.072(7) 0.046(6) 0.071(7) -0.007(5) 0.026(5) -0.007(5) C44 0.060(6) 0.044(5) 0.081(7) -0.012(5) 0.012(5) 0.002(5) C45 0.072(7) 0.055(6) 0.084(8) 0.009(5) 0.023(6) 0.004(6) C46 0.068(8) 0.092(10) 0.114(10) 0.013(8) 0.020(7) 0.020(7) O 0.18(3) 0.048(14) 0.56(7) -0.01(2) 0.11(4) -0.012(16) C50 0.17(3) 0.22(3) 0.26(4) 0.18(3) 0.13(3) 0.11(3) C51 0.59(9) 0.57(8) 0.71(9) 0.55(8) 0.52(8) 0.46(7) _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 Ni S1 2.147(3) . ? Ni S5 2.147(3) . ? Ni S2 2.155(2) . ? Ni S6 2.156(3) . ? Fe1 C11 2.030(9) . ? Fe1 C18 2.031(11) . ? Fe1 C15 2.028(9) . ? Fe1 C17 2.033(10) . ? Fe1 C20 2.046(10) . ? Fe1 C19 2.049(11) . ? Fe1 C13 2.050(10) . ? Fe1 C12 2.053(10) . ? Fe1 C16 2.062(11) . ? Fe1 C14 2.064(10) . ? Fe3 C26 2.000(14) . ? Fe3 C30 2.010(16) . ? Fe3 C27 2.015(12) . ? Fe3 C25 2.022(10) . ? Fe3 C28 2.025(12) . ? Fe3 C29 2.029(13) . ? Fe3 C24 2.031(12) . ? Fe3 C22 2.033(9) . ? Fe3 C23 2.040(10) . ? Fe3 C21 2.040(9) . ? S1 C1 1.722(9) . ? S2 C2 1.729(9) . ? S3 C3 1.750(9) . ? S3 C1 1.753(9) . ? S4 C2 1.749(9) . ? S4 C4 1.777(9) . ? S5 C5 1.721(10) . ? S6 C6 1.724(9) . ? S7 C5 1.753(8) . ? S7 C7 1.773(10) . ? S8 C8 1.744(10) . ? S8 C6 1.765(9) . ? C1 C2 1.367(12) . ? C3 C4 1.352(12) . ? C4 C11 1.475(12) . ? C5 C6 1.367(13) . ? C7 C8 1.337(13) . ? C7 C21 1.472(13) . ? C11 C15 1.430(13) . ? C11 C12 1.433(13) . ? C12 C13 1.421(13) . ? C13 C14 1.379(15) . ? C14 C15 1.405(14) . ? C16 C20 1.368(15) . ? C16 C17 1.417(16) . ? C17 C18 1.457(17) . ? C18 C19 1.390(18) . ? C19 C20 1.361(16) . ? C21 C22 1.405(13) . ? C21 C25 1.407(13) . ? C22 C23 1.410(13) . ? C23 C24 1.391(16) . ? C24 C25 1.425(14) . ? C26 C27 1.36(2) . ? C26 C30 1.38(3) . ? C27 C28 1.35(2) . ? C28 C29 1.36(2) . ? C29 C30 1.41(3) . ? N C39 1.497(13) . ? N C43 1.509(13) . ? N C31 1.532(12) . ? N C35 1.539(11) . ? C31 C32 1.524(15) . ? C32 C33 1.516(14) . ? C33 C34 1.484(17) . ? C35 C36 1.526(15) . ? C36 C37 1.531(14) . ? C37 C38 1.513(16) . ? C39 C40 1.529(16) . ? C40 C41 1.484(16) . ? C41 C42 1.52(2) . ? C43 C44 1.509(13) . ? C44 C45 1.543(15) . ? C45 C46 1.531(15) . ? C50 C51 1.86(4) . ? C50 C51 1.86(4) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni S5 88.31(10) . . ? S1 Ni S2 91.44(10) . . ? S5 Ni S2 174.63(13) . . ? S1 Ni S6 178.01(12) . . ? S5 Ni S6 91.45(10) . . ? S2 Ni S6 88.98(10) . . ? C11 Fe1 C18 154.9(5) . . ? C11 Fe1 C15 41.3(4) . . ? C18 Fe1 C15 163.1(5) . . ? C11 Fe1 C17 118.8(4) . . ? C18 Fe1 C17 42.0(5) . . ? C15 Fe1 C17 152.4(5) . . ? C11 Fe1 C20 126.9(4) . . ? C18 Fe1 C20 66.6(5) . . ? C15 Fe1 C20 107.7(5) . . ? C17 Fe1 C20 66.6(5) . . ? C11 Fe1 C19 163.2(5) . . ? C18 Fe1 C19 39.8(5) . . ? C15 Fe1 C19 125.9(5) . . ? C17 Fe1 C19 67.7(5) . . ? C20 Fe1 C19 38.8(5) . . ? C11 Fe1 C13 67.9(4) . . ? C18 Fe1 C13 110.1(5) . . ? C15 Fe1 C13 67.3(4) . . ? C17 Fe1 C13 130.2(5) . . ? C20 Fe1 C13 153.2(4) . . ? C19 Fe1 C13 121.2(5) . . ? C11 Fe1 C12 41.1(4) . . ? C18 Fe1 C12 120.6(5) . . ? C15 Fe1 C12 69.1(4) . . ? C17 Fe1 C12 109.0(4) . . ? C20 Fe1 C12 164.9(4) . . ? C19 Fe1 C12 154.8(5) . . ? C13 Fe1 C12 40.5(4) . . ? C11 Fe1 C16 107.7(4) . . ? C18 Fe1 C16 68.6(5) . . ? C15 Fe1 C16 117.8(4) . . ? C17 Fe1 C16 40.5(5) . . ? C20 Fe1 C16 38.9(4) . . ? C19 Fe1 C16 66.4(5) . . ? C13 Fe1 C16 167.3(5) . . ? C12 Fe1 C16 128.4(4) . . ? C11 Fe1 C14 68.0(4) . . ? C18 Fe1 C14 127.3(5) . . ? C15 Fe1 C14 40.2(4) . . ? C17 Fe1 C14 166.6(5) . . ? C20 Fe1 C14 119.9(5) . . ? C19 Fe1 C14 109.2(5) . . ? C13 Fe1 C14 39.2(4) . . ? C12 Fe1 C14 67.8(4) . . ? C16 Fe1 C14 151.7(5) . . ? C26 Fe3 C30 40.2(8) . . ? C26 Fe3 C27 39.7(7) . . ? C30 Fe3 C27 67.5(7) . . ? C26 Fe3 C25 156.7(9) . . ? C30 Fe3 C25 121.1(8) . . ? C27 Fe3 C25 161.6(6) . . ? C26 Fe3 C28 65.7(7) . . ? C30 Fe3 C28 66.5(7) . . ? C27 Fe3 C28 39.1(6) . . ? C25 Fe3 C28 126.0(6) . . ? C26 Fe3 C29 67.6(8) . . ? C30 Fe3 C29 41.0(8) . . ? C27 Fe3 C29 67.2(6) . . ? C25 Fe3 C29 107.6(6) . . ? C28 Fe3 C29 39.2(6) . . ? C26 Fe3 C24 161.5(10) . . ? C30 Fe3 C24 155.6(10) . . ? C27 Fe3 C24 124.5(6) . . ? C25 Fe3 C24 41.2(4) . . ? C28 Fe3 C24 108.2(6) . . ? C29 Fe3 C24 119.6(7) . . ? C26 Fe3 C22 110.1(7) . . ? C30 Fe3 C22 127.6(8) . . ? C27 Fe3 C22 121.3(5) . . ? C25 Fe3 C22 68.2(4) . . ? C28 Fe3 C22 154.9(6) . . ? C29 Fe3 C22 164.9(6) . . ? C24 Fe3 C22 67.5(4) . . ? C26 Fe3 C23 126.2(9) . . ? C30 Fe3 C23 163.8(10) . . ? C27 Fe3 C23 107.5(6) . . ? C25 Fe3 C23 68.6(4) . . ? C28 Fe3 C23 120.1(5) . . ? C29 Fe3 C23 153.1(7) . . ? C24 Fe3 C23 40.0(4) . . ? C22 Fe3 C23 40.5(4) . . ? C26 Fe3 C21 122.9(6) . . ? C30 Fe3 C21 109.8(5) . . ? C27 Fe3 C21 156.4(6) . . ? C25 Fe3 C21 40.5(4) . . ? C28 Fe3 C21 163.3(6) . . ? C29 Fe3 C21 127.2(6) . . ? C24 Fe3 C21 68.1(4) . . ? C22 Fe3 C21 40.4(4) . . ? C23 Fe3 C21 68.2(4) . . ? C1 S1 Ni 104.1(3) . . ? C2 S2 Ni 104.0(3) . . ? C3 S3 C1 103.2(4) . . ? C2 S4 C4 102.6(4) . . ? C5 S5 Ni 104.5(3) . . ? C6 S6 Ni 104.0(3) . . ? C5 S7 C7 103.0(4) . . ? C8 S8 C6 101.8(5) . . ? C2 C1 S1 120.3(7) . . ? C2 C1 S3 123.6(7) . . ? S1 C1 S3 116.1(5) . . ? C1 C2 S2 119.2(6) . . ? C1 C2 S4 124.1(7) . . ? S2 C2 S4 116.6(5) . . ? C4 C3 S3 125.2(7) . . ? C3 C4 C11 122.2(8) . . ? C3 C4 S4 122.6(7) . . ? C11 C4 S4 115.1(7) . . ? C6 C5 S5 119.6(7) . . ? C6 C5 S7 123.2(7) . . ? S5 C5 S7 117.2(5) . . ? C5 C6 S6 120.1(7) . . ? C5 C6 S8 122.7(7) . . ? S6 C6 S8 117.2(6) . . ? C8 C7 C21 123.4(9) . . ? C8 C7 S7 120.8(8) . . ? C21 C7 S7 115.8(7) . . ? C7 C8 S8 126.3(8) . . ? C15 C11 C12 107.8(8) . . ? C15 C11 C4 126.0(9) . . ? C12 C11 C4 126.1(8) . . ? C15 C11 Fe1 69.3(5) . . ? C12 C11 Fe1 70.3(5) . . ? C4 C11 Fe1 124.7(6) . . ? C13 C12 C11 105.8(9) . . ? C13 C12 Fe1 69.6(6) . . ? C11 C12 Fe1 68.6(5) . . ? C14 C13 C12 110.2(9) . . ? C14 C13 Fe1 70.9(6) . . ? C12 C13 Fe1 69.8(6) . . ? C13 C14 C15 108.4(9) . . ? C13 C14 Fe1 69.9(6) . . ? C15 C14 Fe1 68.5(5) . . ? C14 C15 C11 107.7(10) . . ? C14 C15 Fe1 71.3(6) . . ? C11 C15 Fe1 69.4(5) . . ? C20 C16 C17 107.0(10) . . ? C20 C16 Fe1 69.9(6) . . ? C17 C16 Fe1 68.7(6) . . ? C16 C17 C18 106.8(11) . . ? C16 C17 Fe1 70.9(6) . . ? C18 C17 Fe1 68.9(6) . . ? C19 C18 C17 106.1(11) . . ? C19 C18 Fe1 70.8(7) . . ? C17 C18 Fe1 69.1(6) . . ? C20 C19 C18 108.9(11) . . ? C20 C19 Fe1 70.5(6) . . ? C18 C19 Fe1 69.4(7) . . ? C19 C20 C16 111.2(11) . . ? C19 C20 Fe1 70.7(6) . . ? C16 C20 Fe1 71.2(6) . . ? C22 C21 C25 107.9(8) . . ? C22 C21 C7 127.0(8) . . ? C25 C21 C7 125.1(9) . . ? C22 C21 Fe3 69.5(5) . . ? C25 C21 Fe3 69.0(5) . . ? C7 C21 Fe3 124.9(6) . . ? C21 C22 C23 108.7(9) . . ? C21 C22 Fe3 70.1(5) . . ? C23 C22 Fe3 70.0(5) . . ? C24 C23 C22 107.5(9) . . ? C24 C23 Fe3 69.7(7) . . ? C22 C23 Fe3 69.5(5) . . ? C23 C24 C25 108.8(10) . . ? C23 C24 Fe3 70.4(7) . . ? C25 C24 Fe3 69.1(6) . . ? C21 C25 C24 107.2(9) . . ? C21 C25 Fe3 70.4(5) . . ? C24 C25 Fe3 69.7(6) . . ? C27 C26 C30 109.2(18) . . ? C27 C26 Fe3 70.7(8) . . ? C30 C26 Fe3 70.2(10) . . ? C28 C27 C26 107.0(17) . . ? C28 C27 Fe3 70.9(8) . . ? C26 C27 Fe3 69.6(8) . . ? C27 C28 C29 111.2(16) . . ? C27 C28 Fe3 70.1(8) . . ? C29 C28 Fe3 70.6(7) . . ? C28 C29 C30 105.8(17) . . ? C28 C29 Fe3 70.2(8) . . ? C30 C29 Fe3 68.8(9) . . ? C29 C30 C26 106.8(16) . . ? C29 C30 Fe3 70.2(10) . . ? C26 C30 Fe3 69.5(9) . . ? C39 N C43 110.7(8) . . ? C39 N C31 107.2(8) . . ? C43 N C31 110.1(8) . . ? C39 N C35 111.4(8) . . ? C43 N C35 106.8(7) . . ? C31 N C35 110.6(7) . . ? C32 C31 N 115.7(8) . . ? C33 C32 C31 110.9(10) . . ? C34 C33 C32 114.4(11) . . ? C36 C35 N 114.2(8) . . ? C35 C36 C37 110.3(9) . . ? C38 C37 C36 110.7(11) . . ? N C39 C40 116.1(9) . . ? C41 C40 C39 112.5(12) . . ? C40 C41 C42 112.3(14) . . ? C44 C43 N 116.1(8) . . ? C43 C44 C45 110.8(8) . . ? C46 C45 C44 111.4(9) . . ? C51 C50 C51 180.000(4) . 3 ? _diffrn_measured_fraction_theta_max 0.593 _diffrn_reflns_theta_full 23.47 _diffrn_measured_fraction_theta_full 0.593 _refine_diff_density_max 1.441 _refine_diff_density_min -1.289 _refine_diff_density_rms 0.146 #===END # Complex 2 data_ni-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'TBA[Ni(dfcvdt)2](COMe2)' _chemical_formula_moiety '(C16H36N)[Ni(C24H18S4Fe2)2](C3H6O)' _chemical_formula_sum 'C67 H78 Fe4 N Ni O S8' _chemical_formula_weight 1451.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 20.457(14) _cell_length_b 39.220(13) _cell_length_c 8.496(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6817(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 23.45 _exptl_crystal_description 'parallelipiped' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3020 _exptl_absorpt_coefficient_mu 1.388 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3052 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2180 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 23.45 _reflns_number_total 3052 _reflns_number_gt 1267 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1566P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3052 _refine_ls_number_parameters 335 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2474 _refine_ls_R_factor_gt 0.1093 _refine_ls_wR_factor_ref 0.3047 _refine_ls_wR_factor_gt 0.2571 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 4.605 _refine_ls_shift/su_mean 0.259 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.0501(2) 0.2500 0.1832(5) 0.0595(14) Uani 1 d S . . Fe1 Fe -0.11742(17) 0.10409(10) -0.0784(5) 0.0809(15) Uani 1 d . . . Fe2 Fe 0.19185(18) 0.05551(10) 0.0303(5) 0.0754(14) Uani 1 d . . . S1 S 0.1231(3) 0.21235(18) 0.1330(8) 0.071(2) Uani 1 d . . . S2 S -0.0217(3) 0.21188(18) 0.2335(9) 0.074(2) Uani 1 d . . . S3 S 0.1317(3) 0.13656(19) 0.1696(10) 0.078(2) Uani 1 d . . . S4 S -0.0177(3) 0.13556(18) 0.2667(9) 0.080(2) Uani 1 d . . . C1 C 0.0853(12) 0.1742(7) 0.171(3) 0.072(8) Uani 1 d . . . C2 C 0.0208(11) 0.1761(6) 0.220(3) 0.058(7) Uani 1 d . . . C3 C 0.0774(10) 0.1082(6) 0.080(3) 0.053(7) Uani 1 d . . . C4 C 0.0151(12) 0.1099(6) 0.123(3) 0.058(7) Uani 1 d . . . C5 C 0.1086(9) 0.0818(7) -0.015(3) 0.052(7) Uani 1 d . . . C6 C 0.1583(12) 0.0904(6) -0.125(3) 0.063(8) Uani 1 d . . . H6 H 0.1772 0.1116 -0.1430 0.076 Uiso 1 calc R . . C7 C 0.1732(13) 0.0575(9) -0.206(3) 0.090(10) Uani 1 d . . . H7 H 0.2026 0.0554 -0.2894 0.108 Uiso 1 calc R . . C8 C 0.1387(15) 0.0308(8) -0.145(4) 0.105(12) Uani 1 d . . . H8 H 0.1421 0.0078 -0.1709 0.126 Uiso 1 calc R . . C9 C 0.0957(12) 0.0463(6) -0.030(3) 0.069(8) Uani 1 d . . . H9 H 0.0637 0.0346 0.0258 0.083 Uiso 1 calc R . . C10 C 0.2170(14) 0.0592(12) 0.261(3) 0.093(10) Uani 1 d . . . H10 H 0.1929 0.0698 0.3398 0.112 Uiso 1 calc R . . C11 C 0.2619(19) 0.0746(9) 0.160(5) 0.105(11) Uani 1 d U . . H11 H 0.2707 0.0978 0.1563 0.126 Uiso 1 calc R . . C12 C 0.2905(15) 0.0512(13) 0.068(4) 0.117(12) Uani 1 d . . . H12 H 0.3244 0.0548 -0.0031 0.141 Uiso 1 calc R . . C13 C 0.259(2) 0.0205(11) 0.100(5) 0.112(13) Uani 1 d . . . H13 H 0.2669 0.0000 0.0479 0.134 Uiso 1 calc R . . C14 C 0.215(2) 0.0255(9) 0.222(5) 0.106(12) Uani 1 d . . . H14 H 0.1892 0.0089 0.2692 0.127 Uiso 1 calc R . . C15 C -0.0360(13) 0.0872(7) 0.031(4) 0.084(9) Uani 1 d . . . C16 C -0.0341(12) 0.0760(7) -0.129(4) 0.075(8) Uani 1 d . . . H16 H -0.0019 0.0806 -0.2037 0.090 Uiso 1 calc R . . C17 C -0.0897(17) 0.0570(9) -0.150(4) 0.106(11) Uani 1 d . . . H17 H -0.1015 0.0461 -0.2427 0.127 Uiso 1 calc R . . C18 C -0.1265(15) 0.0566(8) -0.010(6) 0.112(13) Uani 1 d . . . H18 H -0.1666 0.0459 0.0031 0.135 Uiso 1 calc R . . C19 C -0.0932(14) 0.0750(7) 0.108(4) 0.082(9) Uani 1 d . . . H19 H -0.1058 0.0784 0.2122 0.099 Uiso 1 calc R . . C20 C -0.108(2) 0.1576(9) -0.081(5) 0.112(13) Uani 1 d . . . H20 H -0.0744 0.1713 -0.0455 0.134 Uiso 1 calc R . . C21 C -0.1184(18) 0.1446(9) -0.229(6) 0.111(12) Uani 1 d . . . H21 H -0.0899 0.1483 -0.3122 0.133 Uiso 1 calc R . . C22 C -0.177(2) 0.1249(9) -0.241(6) 0.131(14) Uani 1 d . . . H22 H -0.1918 0.1130 -0.3292 0.157 Uiso 1 calc R . . C23 C -0.2070(14) 0.1271(9) -0.097(5) 0.109(12) Uani 1 d U . . H23 H -0.2480 0.1188 -0.0695 0.131 Uiso 1 calc R . . C24 C -0.162(2) 0.1450(8) 0.001(5) 0.117(12) Uani 1 d . . . H24 H -0.1675 0.1479 0.1084 0.141 Uiso 1 calc R . . N1 N 0.2363(16) 0.2500 0.571(4) 0.094(11) Uiso 1 d S . . C31 C 0.214(2) 0.2222(11) 0.650(5) 0.171(17) Uiso 1 d . . . C32 C 0.165(2) 0.2115(11) 0.579(5) 0.153(15) Uiso 1 d . . . C33 C 0.131(3) 0.1838(13) 0.686(6) 0.21(2) Uiso 1 d . . . C34 C 0.075(2) 0.1645(12) 0.657(6) 0.191(19) Uiso 1 d . . . C35 C 0.258(2) 0.2500 0.414(5) 0.089(13) Uiso 1 d S . . C36 C 0.288(2) 0.2223(13) 0.328(6) 0.073(16) Uiso 0.50 d P . . C37 C 0.3060(19) 0.2340(9) 0.143(5) 0.043(12) Uiso 0.50 d P . . C38 C 0.316(3) 0.2008(14) 0.062(6) 0.090(19) Uiso 0.50 d P . . C39 C 0.298(3) 0.2273(13) 0.673(6) 0.081(17) Uiso 0.50 d P . . C40 C 0.3586(18) 0.2500 0.660(5) 0.076(12) Uiso 1 d S . . C41 C 0.410(3) 0.2335(13) 0.784(7) 0.10(2) Uiso 0.50 d P . . C42 C 0.472(3) 0.2500 0.777(7) 0.17(2) Uiso 1 d S . . C51 C 0.0000 0.0000 0.5000 0.24(4) Uiso 1 d S . . C52 C 0.038(3) 0.0289(14) 0.451(6) 0.31(2) Uiso 1 d . . . O1 O 0.046(4) -0.009(2) 0.532(9) 0.38(3) Uiso 0.50 d P . . 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 Ni 0.046(3) 0.079(3) 0.053(3) 0.000 -0.002(3) 0.000 Fe1 0.046(2) 0.082(3) 0.115(4) 0.011(3) -0.017(2) -0.004(2) Fe2 0.058(2) 0.077(3) 0.092(3) 0.003(3) -0.010(2) 0.016(2) S1 0.049(4) 0.089(5) 0.074(5) -0.011(5) 0.007(4) -0.006(4) S2 0.055(4) 0.075(5) 0.093(6) 0.002(5) 0.021(4) 0.008(4) S3 0.043(4) 0.094(5) 0.096(6) -0.019(5) -0.017(4) 0.004(4) S4 0.063(4) 0.098(6) 0.078(6) -0.005(5) 0.018(4) 0.004(4) C1 0.051(16) 0.11(2) 0.049(18) 0.002(17) 0.022(14) -0.013(16) C2 0.066(16) 0.085(19) 0.024(17) 0.007(13) 0.014(13) -0.052(15) C3 0.037(13) 0.055(15) 0.066(18) -0.039(15) 0.005(14) 0.015(12) C4 0.060(17) 0.087(19) 0.027(16) 0.016(14) -0.005(14) 0.009(16) C5 0.014(11) 0.09(2) 0.052(17) 0.023(16) -0.003(12) -0.013(13) C6 0.084(19) 0.038(16) 0.07(2) -0.001(15) -0.009(17) 0.001(15) C7 0.09(2) 0.15(3) 0.029(18) -0.016(19) -0.015(14) 0.06(2) C8 0.08(2) 0.10(2) 0.13(3) 0.05(2) -0.01(2) -0.05(2) C9 0.047(17) 0.06(2) 0.10(2) 0.007(17) -0.002(16) -0.035(14) C10 0.06(2) 0.17(4) 0.05(2) 0.00(2) -0.019(17) 0.05(2) C11 0.087(19) 0.12(2) 0.11(2) 0.02(2) -0.054(18) 0.01(2) C12 0.08(2) 0.13(3) 0.14(3) -0.04(3) -0.03(2) 0.04(3) C13 0.14(3) 0.10(3) 0.09(4) -0.03(3) -0.04(3) 0.07(3) C14 0.17(4) 0.06(3) 0.09(3) -0.01(2) -0.07(3) 0.03(2) C15 0.07(2) 0.08(2) 0.10(3) 0.01(2) 0.04(2) 0.035(17) C16 0.042(16) 0.10(2) 0.08(3) 0.003(19) 0.006(17) -0.002(16) C17 0.07(2) 0.15(3) 0.10(3) -0.02(3) -0.01(2) -0.01(2) C18 0.06(2) 0.08(2) 0.20(4) 0.01(3) -0.01(3) -0.060(18) C19 0.067(19) 0.08(2) 0.10(3) 0.01(2) 0.04(2) 0.039(17) C20 0.14(4) 0.08(3) 0.11(4) 0.03(3) -0.02(3) -0.01(2) C21 0.11(3) 0.08(3) 0.13(4) 0.04(3) -0.01(3) -0.02(2) C22 0.13(4) 0.09(3) 0.17(4) 0.03(3) -0.05(4) 0.01(3) C23 0.044(17) 0.12(2) 0.16(3) 0.02(2) -0.02(2) 0.035(16) C24 0.13(3) 0.09(3) 0.13(3) 0.02(2) -0.05(3) -0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S1 2.143(8) 7_565 ? Ni S1 2.143(8) . ? Ni S2 2.140(7) . ? Ni S2 2.140(7) 7_565 ? Fe1 C18 1.96(3) . ? Fe1 C24 1.96(3) . ? Fe1 C15 2.02(3) . ? Fe1 C21 2.04(3) . ? Fe1 C16 2.08(2) . ? Fe1 C22 2.02(3) . ? Fe1 C23 2.05(3) . ? Fe1 C19 2.01(3) . ? Fe1 C17 2.02(3) . ? Fe1 C20 2.11(4) . ? Fe2 C11 1.95(3) . ? Fe2 C13 2.04(3) . ? Fe2 C10 2.03(3) . ? Fe2 C6 2.02(2) . ? Fe2 C5 2.03(2) . ? Fe2 C9 2.07(2) . ? Fe2 C12 2.05(3) . ? Fe2 C7 2.05(2) . ? Fe2 C8 2.08(3) . ? Fe2 C14 2.07(3) . ? S1 C1 1.72(2) . ? S2 C2 1.65(2) . ? S3 C1 1.75(3) . ? S3 C3 1.75(2) . ? S4 C4 1.72(2) . ? S4 C2 1.82(2) . ? C1 C2 1.39(3) . ? C3 C4 1.33(3) . ? C3 C5 1.46(3) . ? C4 C15 1.58(4) . ? C5 C6 1.43(3) . ? C5 C9 1.42(3) . ? C6 C7 1.49(3) . ? C7 C8 1.37(3) . ? C8 C9 1.45(4) . ? C10 C11 1.40(4) . ? C10 C14 1.36(4) . ? C11 C12 1.34(4) . ? C12 C13 1.39(4) . ? C13 C14 1.39(4) . ? C15 C16 1.43(4) . ? C15 C19 1.42(3) . ? C16 C17 1.37(4) . ? C17 C18 1.41(4) . ? C18 C19 1.41(4) . ? C20 C21 1.36(4) . ? C20 C24 1.39(4) . ? C21 C22 1.43(4) . ? C22 C23 1.37(4) . ? C23 C24 1.43(4) . ? N1 C31 1.36(4) 7_565 ? N1 C31 1.36(4) . ? N1 C35 1.40(4) . ? N1 C39 1.78(6) 7_565 ? N1 C39 1.78(6) . ? C31 C32 1.25(5) . ? C31 C39 1.74(7) . ? C32 C33 1.57(5) . ? C33 C34 1.40(6) . ? C35 C36 1.44(5) 7_565 ? C35 C36 1.44(5) . ? C36 C37 1.68(6) . ? C37 C37 1.25(7) 7_565 ? C37 C38 1.49(6) . ? C39 C40 1.52(5) . ? C39 C39 1.78(10) 7_565 ? C40 C39 1.52(5) 7_565 ? C40 C41 1.63(6) 7_565 ? C40 C41 1.63(6) . ? C41 C41 1.29(10) 7_565 ? C41 C42 1.43(6) . ? C42 C41 1.43(6) 7_565 ? C51 C52 1.44(6) . ? C51 C52 1.44(6) 5_556 ? C51 O1 1.04(8) 5_556 ? C51 O1 1.04(8) . ? C52 O1 1.89(8) 5_556 ? C52 O1 1.66(8) . ? O1 C52 1.89(8) 5_556 ? 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 S1 Ni S1 87.1(4) 7_565 . ? S1 Ni S2 179.2(3) 7_565 . ? S1 Ni S2 92.1(3) . . ? S1 Ni S2 92.1(3) 7_565 7_565 ? S1 Ni S2 179.2(3) . 7_565 ? S2 Ni S2 88.7(4) . 7_565 ? C18 Fe1 C24 129.2(19) . . ? C18 Fe1 C15 68.2(12) . . ? C24 Fe1 C15 119.4(14) . . ? C18 Fe1 C21 158(2) . . ? C24 Fe1 C21 64.6(15) . . ? C15 Fe1 C21 123.5(14) . . ? C18 Fe1 C16 68.6(12) . . ? C24 Fe1 C16 152.3(15) . . ? C15 Fe1 C16 41.0(10) . . ? C21 Fe1 C16 107.0(13) . . ? C18 Fe1 C22 122.1(15) . . ? C24 Fe1 C22 67.9(15) . . ? C15 Fe1 C22 161.4(17) . . ? C21 Fe1 C22 41.4(12) . . ? C16 Fe1 C22 124.7(17) . . ? C18 Fe1 C23 110.9(14) . . ? C24 Fe1 C23 41.7(12) . . ? C15 Fe1 C23 156.6(17) . . ? C21 Fe1 C23 66.3(14) . . ? C16 Fe1 C23 162.2(16) . . ? C22 Fe1 C23 39.4(12) . . ? C18 Fe1 C19 41.5(11) . . ? C24 Fe1 C19 107.9(14) . . ? C15 Fe1 C19 41.3(9) . . ? C21 Fe1 C19 159.4(17) . . ? C16 Fe1 C19 70.2(10) . . ? C22 Fe1 C19 156.5(17) . . ? C23 Fe1 C19 122.1(14) . . ? C18 Fe1 C17 41.4(12) . . ? C24 Fe1 C17 168.0(17) . . ? C15 Fe1 C17 66.9(12) . . ? C21 Fe1 C17 121.8(17) . . ? C16 Fe1 C17 39.1(10) . . ? C22 Fe1 C17 109.4(15) . . ? C23 Fe1 C17 129.0(15) . . ? C19 Fe1 C17 69.6(12) . . ? C18 Fe1 C20 163.3(19) . . ? C24 Fe1 C20 39.6(12) . . ? C15 Fe1 C20 105.1(14) . . ? C21 Fe1 C20 38.4(12) . . ? C16 Fe1 C20 117.0(14) . . ? C22 Fe1 C20 69.0(14) . . ? C23 Fe1 C20 68.8(15) . . ? C19 Fe1 C20 123.5(16) . . ? C17 Fe1 C20 151.7(17) . . ? C11 Fe2 C13 66.3(14) . . ? C11 Fe2 C10 41.0(11) . . ? C13 Fe2 C10 66.2(13) . . ? C11 Fe2 C6 110.9(12) . . ? C13 Fe2 C6 151.2(18) . . ? C10 Fe2 C6 132.0(14) . . ? C11 Fe2 C5 121.8(14) . . ? C13 Fe2 C5 165.5(17) . . ? C10 Fe2 C5 111.0(11) . . ? C6 Fe2 C5 41.2(9) . . ? C11 Fe2 C9 154.9(18) . . ? C13 Fe2 C9 126.9(16) . . ? C10 Fe2 C9 119.6(13) . . ? C6 Fe2 C9 68.4(10) . . ? C5 Fe2 C9 40.7(8) . . ? C11 Fe2 C12 38.9(12) . . ? C13 Fe2 C12 39.7(12) . . ? C10 Fe2 C12 66.8(13) . . ? C6 Fe2 C12 119.4(15) . . ? C5 Fe2 C12 153.9(16) . . ? C9 Fe2 C12 164.2(15) . . ? C11 Fe2 C7 132.4(16) . . ? C13 Fe2 C7 115.9(15) . . ? C10 Fe2 C7 172.6(17) . . ? C6 Fe2 C7 43.1(9) . . ? C5 Fe2 C7 68.9(10) . . ? C9 Fe2 C7 65.4(11) . . ? C12 Fe2 C7 109.8(13) . . ? C11 Fe2 C8 164.3(18) . . ? C13 Fe2 C8 104.3(15) . . ? C10 Fe2 C8 148.7(16) . . ? C6 Fe2 C8 70.8(11) . . ? C5 Fe2 C8 70.3(11) . . ? C9 Fe2 C8 40.8(10) . . ? C12 Fe2 C8 125.9(16) . . ? C7 Fe2 C8 38.6(9) . . ? C11 Fe2 C14 66.7(13) . . ? C13 Fe2 C14 39.7(11) . . ? C10 Fe2 C14 38.7(10) . . ? C6 Fe2 C14 168.3(16) . . ? C5 Fe2 C14 129.2(15) . . ? C9 Fe2 C14 108.5(13) . . ? C12 Fe2 C14 66.6(15) . . ? C7 Fe2 C14 147.1(15) . . ? C8 Fe2 C14 114.9(13) . . ? C1 S1 Ni 104.5(9) . . ? C2 S2 Ni 102.6(7) . . ? C1 S3 C3 101.2(11) . . ? C4 S4 C2 100.9(12) . . ? C2 C1 S1 116(2) . . ? C2 C1 S3 124(2) . . ? S1 C1 S3 119.2(14) . . ? C1 C2 S2 124.5(18) . . ? C1 C2 S4 116(2) . . ? S2 C2 S4 120.0(13) . . ? C4 C3 C5 128(2) . . ? C4 C3 S3 117.0(19) . . ? C5 C3 S3 114.5(16) . . ? C3 C4 C15 118(2) . . ? C3 C4 S4 127(2) . . ? C15 C4 S4 115.0(18) . . ? C6 C5 C9 108(2) . . ? C6 C5 C3 120(2) . . ? C9 C5 C3 132(2) . . ? C6 C5 Fe2 69.3(12) . . ? C9 C5 Fe2 71.1(13) . . ? C3 C5 Fe2 128.8(16) . . ? C5 C6 C7 104(2) . . ? C5 C6 Fe2 69.5(13) . . ? C7 C6 Fe2 69.4(13) . . ? C8 C7 C6 112(3) . . ? C8 C7 Fe2 72.0(17) . . ? C6 C7 Fe2 67.5(13) . . ? C7 C8 C9 104(3) . . ? C7 C8 Fe2 69.4(16) . . ? C9 C8 Fe2 69.0(17) . . ? C8 C9 C5 111(2) . . ? C8 C9 Fe2 70.2(15) . . ? C5 C9 Fe2 68.2(12) . . ? C11 C10 C14 107(3) . . ? C11 C10 Fe2 66.5(17) . . ? C14 C10 Fe2 72.0(18) . . ? C10 C11 C12 111(3) . . ? C10 C11 Fe2 72.5(18) . . ? C12 C11 Fe2 74(2) . . ? C13 C12 C11 106(4) . . ? C13 C12 Fe2 69.6(19) . . ? C11 C12 Fe2 66.6(18) . . ? C12 C13 C14 109(4) . . ? C12 C13 Fe2 70.7(19) . . ? C14 C13 Fe2 71.3(19) . . ? C13 C14 C10 108(4) . . ? C13 C14 Fe2 69(2) . . ? C10 C14 Fe2 69.2(18) . . ? C16 C15 C19 111(3) . . ? C16 C15 C4 129(2) . . ? C19 C15 C4 120(3) . . ? C16 C15 Fe1 71.6(18) . . ? C19 C15 Fe1 69.1(16) . . ? C4 C15 Fe1 126.1(17) . . ? C15 C16 C17 105(3) . . ? C15 C16 Fe1 67.4(16) . . ? C17 C16 Fe1 68.4(17) . . ? C18 C17 C16 110(3) . . ? C18 C17 Fe1 66.9(18) . . ? C16 C17 Fe1 72.5(18) . . ? C19 C18 C17 110(3) . . ? C19 C18 Fe1 71.4(16) . . ? C17 C18 Fe1 72(2) . . ? C18 C19 C15 104(3) . . ? C18 C19 Fe1 67.1(19) . . ? C15 C19 Fe1 69.5(17) . . ? C21 C20 C24 102(4) . . ? C21 C20 Fe1 68(2) . . ? C24 C20 Fe1 65(2) . . ? C20 C21 C22 113(4) . . ? C20 C21 Fe1 73(2) . . ? C22 C21 Fe1 68.6(19) . . ? C23 C22 C21 106(4) . . ? C23 C22 Fe1 72(2) . . ? C21 C22 Fe1 70.1(19) . . ? C22 C23 C24 105(3) . . ? C22 C23 Fe1 69.0(18) . . ? C24 C23 Fe1 65.8(17) . . ? C20 C24 C23 113(4) . . ? C20 C24 Fe1 76(2) . . ? C23 C24 Fe1 72.5(19) . . ? C31 N1 C31 107(5) 7_565 . ? C31 N1 C35 125(3) 7_565 . ? C31 N1 C35 125(3) . . ? C31 N1 C39 66(3) 7_565 7_565 ? C31 N1 C39 113(4) . 7_565 ? C35 N1 C39 104(3) . 7_565 ? C31 N1 C39 113(4) 7_565 . ? C31 N1 C39 66(3) . . ? C35 N1 C39 104(3) . . ? C39 N1 C39 60(3) 7_565 . ? C32 C31 N1 107(4) . . ? C32 C31 C39 153(5) . . ? N1 C31 C39 69(3) . . ? C31 C32 C33 108(4) . . ? C34 C33 C32 130(5) . . ? N1 C35 C36 128(3) . 7_565 ? N1 C35 C36 128(3) . . ? C36 C35 C36 98(5) 7_565 . ? C35 C36 C37 111(4) . . ? C37 C37 C38 151(3) 7_565 . ? C37 C37 C36 106(2) 7_565 . ? C38 C37 C36 103(3) . . ? C40 C39 C31 149(4) . . ? C40 C39 C39 54(2) . 7_565 ? C31 C39 C39 97(2) . 7_565 ? C40 C39 N1 105(3) . . ? C31 C39 N1 45.5(19) . . ? C39 C39 N1 60.0(17) 7_565 . ? C39 C40 C39 71(4) 7_565 . ? C39 C40 C41 104(3) 7_565 7_565 ? C39 C40 C41 135(4) . 7_565 ? C39 C40 C41 135(4) 7_565 . ? C39 C40 C41 104(3) . . ? C41 C40 C41 47(4) 7_565 . ? C41 C41 C42 63(2) 7_565 . ? C41 C41 C40 66.6(19) 7_565 . ? C42 C41 C40 112(5) . . ? C41 C42 C41 54(5) 7_565 . ? C52 C51 C52 180.000(16) . 5_556 ? C52 C51 O1 98(4) . 5_556 ? C52 C51 O1 82(4) 5_556 5_556 ? C52 C51 O1 82(4) . . ? C52 C51 O1 98(4) 5_556 . ? O1 C51 O1 180.00(3) 5_556 . ? C51 C52 O1 33(3) . 5_556 ? C51 C52 O1 38(3) . . ? O1 C52 O1 71(5) 5_556 . ? C51 O1 C52 49(3) . 5_556 ? C51 O1 C52 59(4) . . ? C52 O1 C52 109(5) 5_556 . ? _diffrn_measured_fraction_theta_max 0.541 _diffrn_reflns_theta_full 23.45 _diffrn_measured_fraction_theta_full 0.541 _refine_diff_density_max 1.058 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.143