# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1673 #################################################### data_B003089I _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H114 Fe2 N30 Ni3 O12' _chemical_formula_weight 1591.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 10.018(2) _cell_length_b 13.861(3) _cell_length_c 15.162(3) _cell_angle_alpha 102.06(3) _cell_angle_beta 101.24(3) _cell_angle_gamma 92.67(3) _cell_volume 2011.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details ? _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 'NONIUS Kappa CCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.71 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26679 _diffrn_reflns_av_R_equivalents 0.2777 _diffrn_reflns_av_sigmaI/netI 0.3537 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7004 _reflns_number_gt 2227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS Kappa CCD' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'HKL Denzo & Maxus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXL (1990)' _computing_publication_material 'Siemens SHELXL-97' _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^)+(0.1011P)^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 7004 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2819 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2489 _refine_ls_wR_factor_gt 0.1742 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _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 Fe Fe 0.33443(15) 0.28106(10) 0.18608(10) 0.0443(5) Uani 1 1 d . . . Ni2 Ni 0.0000 0.0000 0.0000 0.0473(6) Uani 1 2 d S . . Ni3 Ni 0.5000 0.5000 0.0000 0.0436(6) Uani 1 2 d S . . Ni1 Ni 0.5000 0.5000 0.5000 0.0571(7) Uani 1 2 d S . . N5 N 0.1659(11) 0.2164(8) 0.3168(7) 0.085(4) Uani 1 1 d . . . C2 C 0.4680(12) 0.1946(8) 0.2118(9) 0.057(4) Uani 1 1 d . . . N1 N 0.1642(9) 0.1131(6) 0.0335(7) 0.060(3) Uani 1 1 d . . . N4 N 0.4781(9) 0.4392(7) 0.3557(7) 0.061(3) Uani 1 1 d . . . N3 N 0.4769(9) 0.3750(6) 0.0568(7) 0.054(3) Uani 1 1 d . . . C1 C 0.2336(10) 0.1771(7) 0.0893(8) 0.044(3) Uani 1 1 d . . . N2 N 0.5512(12) 0.1426(8) 0.2283(8) 0.081(3) Uani 1 1 d . . . C4 C 0.4275(11) 0.3806(9) 0.2877(9) 0.055(3) Uani 1 1 d . . . C5 C 0.2293(13) 0.2382(8) 0.2667(8) 0.061(4) Uani 1 1 d . . . C3 C 0.4302(11) 0.3325(8) 0.1043(8) 0.054(3) Uani 1 1 d . . . N10 N 0.1419(8) -0.1004(6) 0.0156(7) 0.056(3) Uani 1 1 d . . . H12 H 0.2243 -0.0647 0.0394 0.067 Uiso 1 1 calc R . . N13 N 0.3090(8) 0.5349(6) 0.0213(6) 0.042(2) Uani 1 1 d . . . N8 N 0.3376(9) 0.5850(7) 0.4760(6) 0.064(3) Uani 1 1 d . . . H8 H 0.3354 0.6267 0.5306 0.077 Uiso 1 1 calc R . . C6 C 0.2014(12) 0.3720(9) 0.1569(9) 0.055(4) Uani 1 1 d . . . N11 N -0.0136(9) 0.0309(7) 0.1363(6) 0.058(3) Uani 1 1 d . . . H11 H 0.0595 0.0738 0.1685 0.070 Uiso 1 1 calc R . . N9 N 0.4759(14) 0.7126(8) 0.4340(8) 0.078(3) Uani 1 1 d . . . N7 N 0.6461(10) 0.6110(7) 0.5001(7) 0.065(3) Uani 1 1 d . . . H10 H 0.6636 0.6537 0.5563 0.078 Uiso 1 1 calc R . . N14 N 0.5747(9) 0.5906(6) 0.1288(6) 0.050(3) Uani 1 1 d . . . H14 H 0.6080 0.6498 0.1211 0.061 Uiso 1 1 calc R . . C16 C 0.1188(13) -0.1594(9) 0.0819(12) 0.083(4) Uani 1 1 d . . . H9A H 0.0363 -0.2035 0.0547 0.100 Uiso 1 1 calc R . . H9B H 0.1940 -0.2005 0.0902 0.100 Uiso 1 1 calc R . . C20 C 0.3352(10) 0.6223(8) 0.0991(8) 0.055(3) Uani 1 1 d . . . H13A H 0.2540 0.6317 0.1247 0.066 Uiso 1 1 calc R . . H13B H 0.3568 0.6811 0.0775 0.066 Uiso 1 1 calc R . . C21 C 0.4540(10) 0.6074(8) 0.1733(8) 0.052(3) Uani 1 1 d . . . H14A H 0.4741 0.6655 0.2237 0.062 Uiso 1 1 calc R . . H14B H 0.4314 0.5507 0.1975 0.062 Uiso 1 1 calc R . . C9 C 0.3517(14) 0.6471(10) 0.4093(8) 0.075(4) Uani 1 1 d . . . H19A H 0.3482 0.6040 0.3495 0.090 Uiso 1 1 calc R . . H19B H 0.2743 0.6865 0.4035 0.090 Uiso 1 1 calc R . . N15 N 0.8039(8) 0.5264(7) 0.1420(6) 0.056(3) Uani 1 1 d . . . O4 O 0.2250(9) 0.7085(7) 0.6371(6) 0.106(3) Uani 1 1 d . . . O6 O -0.0737(9) 0.4025(7) 0.2741(7) 0.109(3) Uani 1 1 d . . . N12 N 0.1057(13) -0.1068(9) 0.1710(9) 0.082(4) Uani 1 1 d . . . N6 N 0.1242(11) 0.4283(9) 0.1370(9) 0.090(4) Uani 1 1 d . . . C23 C 0.8895(12) 0.6109(9) 0.1347(9) 0.075(4) Uani 1 1 d . . . H17A H 0.8317 0.6570 0.1094 0.090 Uiso 1 1 calc R . . H17B H 0.9484 0.5884 0.0922 0.090 Uiso 1 1 calc R . . C13 C -0.1356(14) 0.0816(10) 0.1422(9) 0.079(4) Uani 1 1 d . . . H7A H -0.1307 0.1177 0.2050 0.095 Uiso 1 1 calc R . . H7B H -0.2155 0.0341 0.1242 0.095 Uiso 1 1 calc R . . C10 C 0.5966(16) 0.6679(11) 0.4279(9) 0.083(5) Uani 1 1 d . . . H20A H 0.6680 0.7189 0.4309 0.099 Uiso 1 1 calc R . . H20B H 0.5835 0.6231 0.3678 0.099 Uiso 1 1 calc R . . C22 C 0.6876(12) 0.5483(9) 0.1852(8) 0.063(4) Uani 1 1 d . . . H16A H 0.7196 0.5949 0.2439 0.076 Uiso 1 1 calc R . . H16B H 0.6508 0.4878 0.1978 0.076 Uiso 1 1 calc R . . C19 C 0.2195(12) 0.5560(8) -0.0628(9) 0.064(4) Uani 1 1 d . . . H15A H 0.1321 0.5731 -0.0485 0.076 Uiso 1 1 calc R . . H15B H 0.2614 0.6129 -0.0784 0.076 Uiso 1 1 calc R . . C14 C 0.1458(13) -0.1525(10) -0.0784(11) 0.084(4) Uani 1 1 d . . . H8A H 0.0707 -0.2040 -0.1007 0.101 Uiso 1 1 calc R . . H8B H 0.2306 -0.1837 -0.0779 0.101 Uiso 1 1 calc R . . C8 C 0.7693(14) 0.5599(10) 0.4894(10) 0.083(4) Uani 1 1 d . . . H24A H 0.8486 0.6080 0.5069 0.099 Uiso 1 1 calc R . . H24B H 0.7612 0.5268 0.4253 0.099 Uiso 1 1 calc R . . C7 C 0.2116(12) 0.5164(10) 0.4500(9) 0.084(4) Uani 1 1 d . . . H23A H 0.1961 0.4835 0.3854 0.101 Uiso 1 1 calc R . . H23B H 0.1333 0.5527 0.4601 0.101 Uiso 1 1 calc R . . C17 C 0.2359(16) -0.0515(11) 0.2284(13) 0.112(6) Uani 1 1 d . . . H11A H 0.2810 -0.0182 0.1905 0.134 Uiso 1 1 calc R . . H11B H 0.2153 -0.0014 0.2777 0.134 Uiso 1 1 calc R . . C15 C -0.0137(14) -0.0533(10) 0.1772(9) 0.075(4) Uani 1 1 d . . . H10A H -0.0948 -0.0977 0.1467 0.090 Uiso 1 1 calc R . . H10B H -0.0180 -0.0314 0.2416 0.090 Uiso 1 1 calc R . . C11 C 0.4803(18) 0.7913(10) 0.5151(11) 0.115(6) Uani 1 1 d . . . H21A H 0.3908 0.8157 0.5130 0.138 Uiso 1 1 calc R . . H21B H 0.5036 0.7651 0.5702 0.138 Uiso 1 1 calc R . . O2 O 0.4642(10) -0.0451(10) 0.0659(10) 0.172(5) Uani 1 1 d . . . O3 O 0.6284(12) 0.8122(7) 0.1362(10) 0.169(6) Uani 1 1 d . . . O5 O -0.0089(16) 0.1754(15) 0.4337(12) 0.261(9) Uani 1 1 d . . . C24 C 0.9772(16) 0.6645(12) 0.2270(11) 0.141(7) Uani 1 1 d . . . H18A H 1.0305 0.7200 0.2188 0.211 Uiso 1 1 calc R . . H18B H 1.0371 0.6199 0.2514 0.211 Uiso 1 1 calc R . . H18C H 0.9194 0.6873 0.2692 0.211 Uiso 1 1 calc R . . O1 O 0.710(2) -0.063(3) 0.298(2) 0.47(2) Uani 1 1 d . . . C18 C 0.322(2) -0.1125(15) 0.2654(17) 0.208(11) Uani 1 1 d . . . H12A H 0.4030 -0.0742 0.3031 0.312 Uiso 1 1 calc R . . H12B H 0.3459 -0.1604 0.2168 0.312 Uiso 1 1 calc R . . H12C H 0.2772 -0.1462 0.3025 0.312 Uiso 1 1 calc R . . C12 C 0.577(3) 0.8697(14) 0.5197(14) 0.279(17) Uani 1 1 d . . . H22A H 0.5769 0.9209 0.5731 0.418 Uiso 1 1 calc R . . H22B H 0.5539 0.8957 0.4653 0.418 Uiso 1 1 calc R . . H22C H 0.6660 0.8461 0.5237 0.418 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0456(10) 0.0420(9) 0.0412(11) 0.0041(8) 0.0077(8) -0.0104(8) Ni2 0.0443(12) 0.0384(12) 0.0532(15) 0.0018(10) 0.0069(11) -0.0057(10) Ni3 0.0452(13) 0.0429(12) 0.0449(14) 0.0119(10) 0.0130(11) -0.0002(10) Ni1 0.0612(14) 0.0615(14) 0.0405(14) -0.0004(11) 0.0085(11) -0.0133(12) N5 0.106(9) 0.086(8) 0.060(8) 0.016(7) 0.019(7) -0.032(7) C2 0.052(8) 0.038(7) 0.079(10) 0.015(7) 0.005(8) 0.001(6) N1 0.060(6) 0.036(6) 0.081(8) 0.010(5) 0.011(6) -0.009(5) N4 0.053(6) 0.077(7) 0.055(7) 0.024(6) 0.006(6) -0.001(6) N3 0.054(6) 0.053(6) 0.059(7) 0.018(5) 0.016(5) 0.010(5) C1 0.047(7) 0.030(6) 0.063(9) 0.020(6) 0.015(6) 0.009(6) N2 0.086(9) 0.077(8) 0.073(9) 0.010(7) 0.011(7) 0.004(7) C4 0.041(7) 0.066(8) 0.057(9) 0.022(7) 0.001(7) -0.005(6) C5 0.087(10) 0.042(7) 0.045(9) 0.014(6) -0.007(7) -0.013(7) C3 0.052(8) 0.055(8) 0.037(8) -0.012(6) -0.004(6) 0.001(6) N10 0.046(6) 0.045(6) 0.069(8) 0.002(6) 0.006(5) 0.001(5) N13 0.049(6) 0.048(5) 0.024(5) 0.001(4) 0.002(5) 0.007(4) N8 0.062(7) 0.071(7) 0.051(7) 0.004(6) -0.001(5) -0.001(6) C6 0.047(8) 0.061(9) 0.060(9) 0.015(7) 0.016(7) -0.001(7) N11 0.046(6) 0.063(7) 0.064(7) 0.019(6) 0.004(5) 0.004(5) N9 0.103(10) 0.064(8) 0.066(9) 0.007(7) 0.024(8) -0.009(8) N7 0.060(7) 0.072(7) 0.051(7) -0.002(6) 0.006(6) -0.009(6) N14 0.048(6) 0.052(6) 0.056(7) 0.014(5) 0.017(5) 0.005(5) C16 0.074(10) 0.054(9) 0.124(14) 0.043(10) 0.005(10) 0.000(7) C20 0.042(7) 0.069(8) 0.062(9) 0.016(7) 0.026(7) 0.016(6) C21 0.045(7) 0.059(8) 0.056(8) 0.015(6) 0.014(7) 0.021(6) C9 0.101(11) 0.091(10) 0.035(8) 0.024(8) 0.011(8) 0.012(9) N15 0.038(5) 0.079(7) 0.049(7) 0.015(6) 0.006(5) -0.008(5) O4 0.104(7) 0.129(8) 0.078(7) -0.005(6) 0.035(6) 0.009(6) O6 0.098(7) 0.144(9) 0.097(8) 0.038(7) 0.034(6) 0.015(6) N12 0.081(9) 0.090(9) 0.068(9) 0.027(7) -0.008(8) -0.024(8) N6 0.058(8) 0.103(10) 0.114(11) 0.040(8) 0.017(7) 0.000(7) C23 0.066(8) 0.072(9) 0.087(11) 0.015(8) 0.023(8) -0.013(8) C13 0.073(10) 0.089(10) 0.069(10) -0.004(9) 0.026(8) -0.014(9) C10 0.100(12) 0.086(11) 0.053(10) 0.008(9) 0.011(10) -0.028(10) C22 0.059(8) 0.073(9) 0.058(9) 0.010(7) 0.016(7) 0.000(7) C19 0.061(8) 0.053(8) 0.070(10) 0.004(7) 0.011(8) -0.007(7) C14 0.065(9) 0.075(10) 0.097(13) -0.016(10) 0.013(9) 0.016(8) C8 0.075(10) 0.081(10) 0.081(11) -0.002(9) 0.016(9) -0.017(9) C7 0.060(9) 0.099(10) 0.074(10) 0.011(9) -0.015(8) -0.022(8) C17 0.082(12) 0.092(12) 0.165(18) 0.053(12) 0.008(12) 0.014(10) C15 0.075(11) 0.083(11) 0.062(10) 0.015(8) 0.004(8) 0.001(9) C11 0.186(17) 0.059(10) 0.087(13) -0.003(9) 0.028(12) -0.021(11) O2 0.096(8) 0.205(13) 0.222(15) 0.069(11) 0.032(9) -0.009(9) O3 0.164(11) 0.082(7) 0.262(17) 0.018(9) 0.076(11) -0.009(7) O5 0.200(15) 0.42(2) 0.235(18) 0.188(18) 0.094(13) 0.000(16) C24 0.141(15) 0.131(14) 0.130(16) 0.003(12) 0.027(13) -0.068(13) O1 0.33(3) 0.74(6) 0.44(4) 0.16(4) 0.28(3) -0.03(3) C18 0.19(2) 0.16(2) 0.25(3) 0.08(2) -0.06(2) -0.037(17) C12 0.53(5) 0.098(16) 0.14(2) 0.013(15) -0.06(3) -0.05(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 Fe C2 1.876(14) . ? Fe C4 1.892(12) . ? Fe C1 1.911(11) . ? Fe C5 1.924(13) . ? Fe C6 1.929(14) . ? Fe C3 1.934(13) . ? Ni2 N10 2.050(9) . ? Ni2 N10 2.050(9) 2 ? Ni2 N11 2.053(9) . ? Ni2 N11 2.053(9) 2 ? Ni2 N1 2.126(8) . ? Ni2 N1 2.126(8) 2 ? Ni3 N13 2.064(8) 2_665 ? Ni3 N13 2.064(8) . ? Ni3 N14 2.066(8) . ? Ni3 N14 2.066(8) 2_665 ? Ni3 N3 2.111(9) . ? Ni3 N3 2.111(9) 2_665 ? Ni1 N8 2.072(10) 2_666 ? Ni1 N8 2.072(10) . ? Ni1 N7 2.074(8) . ? Ni1 N7 2.074(8) 2_666 ? Ni1 N4 2.139(10) 2_666 ? Ni1 N4 2.139(10) . ? N5 C5 1.156(13) . ? C2 N2 1.152(13) . ? N1 C1 1.178(11) . ? N4 C4 1.177(12) . ? N3 C3 1.169(12) . ? N10 C14 1.466(14) . ? N10 C16 1.466(14) . ? N13 C20 1.477(12) . ? N13 C19 1.499(13) . ? N8 C9 1.479(13) . ? N8 C7 1.480(13) . ? C6 N6 1.167(13) . ? N11 C15 1.431(14) . ? N11 C13 1.447(14) . ? N9 C10 1.395(15) . ? N9 C9 1.444(14) . ? N9 C11 1.456(16) . ? N7 C8 1.470(15) . ? N7 C10 1.500(15) . ? N14 C22 1.499(13) . ? N14 C21 1.500(11) . ? C16 N12 1.428(16) . ? C20 C21 1.524(13) . ? N15 C19 1.447(13) 2_665 ? N15 C23 1.455(12) . ? N15 C22 1.459(13) . ? N12 C15 1.444(15) . ? N12 C17 1.494(16) . ? C23 C24 1.519(16) . ? C13 C14 1.509(17) 2 ? C19 N15 1.447(13) 2_665 ? C14 C13 1.509(17) 2 ? C8 C7 1.535(16) 2_666 ? C7 C8 1.535(16) 2_666 ? C17 C18 1.36(2) . ? C11 C12 1.40(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 C2 Fe C4 90.6(5) . . ? C2 Fe C1 89.3(5) . . ? C4 Fe C1 175.9(4) . . ? C2 Fe C5 92.0(5) . . ? C4 Fe C5 88.3(5) . . ? C1 Fe C5 87.6(4) . . ? C2 Fe C6 177.8(5) . . ? C4 Fe C6 89.2(5) . . ? C1 Fe C6 91.0(5) . . ? C5 Fe C6 90.2(5) . . ? C2 Fe C3 92.6(5) . . ? C4 Fe C3 90.9(4) . . ? C1 Fe C3 93.1(4) . . ? C5 Fe C3 175.3(5) . . ? C6 Fe C3 85.2(5) . . ? N10 Ni2 N10 180.0(7) . 2 ? N10 Ni2 N11 94.4(4) . . ? N10 Ni2 N11 85.6(4) 2 . ? N10 Ni2 N11 85.6(4) . 2 ? N10 Ni2 N11 94.4(4) 2 2 ? N11 Ni2 N11 180.0(5) . 2 ? N10 Ni2 N1 88.3(3) . . ? N10 Ni2 N1 91.7(3) 2 . ? N11 Ni2 N1 88.7(4) . . ? N11 Ni2 N1 91.3(4) 2 . ? N10 Ni2 N1 91.7(3) . 2 ? N10 Ni2 N1 88.3(3) 2 2 ? N11 Ni2 N1 91.3(4) . 2 ? N11 Ni2 N1 88.7(4) 2 2 ? N1 Ni2 N1 180.0(3) . 2 ? N13 Ni3 N13 180.0(4) 2_665 . ? N13 Ni3 N14 94.0(3) 2_665 . ? N13 Ni3 N14 86.0(3) . . ? N13 Ni3 N14 86.0(3) 2_665 2_665 ? N13 Ni3 N14 94.0(3) . 2_665 ? N14 Ni3 N14 180.000(1) . 2_665 ? N13 Ni3 N3 91.3(3) 2_665 . ? N13 Ni3 N3 88.7(3) . . ? N14 Ni3 N3 92.0(3) . . ? N14 Ni3 N3 88.0(3) 2_665 . ? N13 Ni3 N3 88.7(3) 2_665 2_665 ? N13 Ni3 N3 91.3(3) . 2_665 ? N14 Ni3 N3 88.0(3) . 2_665 ? N14 Ni3 N3 92.0(3) 2_665 2_665 ? N3 Ni3 N3 180.0(5) . 2_665 ? N8 Ni1 N8 180.000(2) 2_666 . ? N8 Ni1 N7 85.8(4) 2_666 . ? N8 Ni1 N7 94.2(4) . . ? N8 Ni1 N7 94.2(4) 2_666 2_666 ? N8 Ni1 N7 85.8(4) . 2_666 ? N7 Ni1 N7 180.000(1) . 2_666 ? N8 Ni1 N4 91.6(4) 2_666 2_666 ? N8 Ni1 N4 88.4(4) . 2_666 ? N7 Ni1 N4 87.2(4) . 2_666 ? N7 Ni1 N4 92.8(4) 2_666 2_666 ? N8 Ni1 N4 88.4(4) 2_666 . ? N8 Ni1 N4 91.6(4) . . ? N7 Ni1 N4 92.8(4) . . ? N7 Ni1 N4 87.2(4) 2_666 . ? N4 Ni1 N4 180.000(1) 2_666 . ? N2 C2 Fe 179.1(12) . . ? C1 N1 Ni2 148.5(9) . . ? C4 N4 Ni1 151.4(9) . . ? C3 N3 Ni3 152.1(9) . . ? N1 C1 Fe 175.0(9) . . ? N4 C4 Fe 173.9(10) . . ? N5 C5 Fe 177.3(11) . . ? N3 C3 Fe 170.2(11) . . ? C14 N10 C16 118.4(11) . . ? C14 N10 Ni2 105.2(7) . . ? C16 N10 Ni2 112.5(8) . . ? C20 N13 C19 111.6(8) . . ? C20 N13 Ni3 105.0(6) . . ? C19 N13 Ni3 112.5(6) . . ? C9 N8 C7 114.5(10) . . ? C9 N8 Ni1 113.3(8) . . ? C7 N8 Ni1 106.8(7) . . ? N6 C6 Fe 177.2(12) . . ? C15 N11 C13 111.3(10) . . ? C15 N11 Ni2 115.0(8) . . ? C13 N11 Ni2 106.9(8) . . ? C10 N9 C9 116.3(11) . . ? C10 N9 C11 116.5(13) . . ? C9 N9 C11 113.0(12) . . ? C8 N7 C10 115.3(11) . . ? C8 N7 Ni1 104.7(7) . . ? C10 N7 Ni1 111.3(7) . . ? C22 N14 C21 113.0(8) . . ? C22 N14 Ni3 112.7(7) . . ? C21 N14 Ni3 106.0(6) . . ? N12 C16 N10 117.2(10) . . ? N13 C20 C21 109.7(9) . . ? N14 C21 C20 107.1(9) . . ? N9 C9 N8 114.4(10) . . ? C19 N15 C23 114.8(9) 2_665 . ? C19 N15 C22 116.1(8) 2_665 . ? C23 N15 C22 116.6(9) . . ? C16 N12 C15 117.8(11) . . ? C16 N12 C17 113.5(13) . . ? C15 N12 C17 114.2(12) . . ? N15 C23 C24 112.6(10) . . ? N11 C13 C14 108.3(10) . 2 ? N9 C10 N7 116.2(12) . . ? N15 C22 N14 114.5(9) . . ? N15 C19 N13 113.5(9) 2_665 . ? N10 C14 C13 110.8(10) . 2 ? N7 C8 C7 110.5(11) . 2_666 ? N8 C7 C8 107.5(10) . 2_666 ? C18 C17 N12 111.9(14) . . ? N11 C15 N12 112.8(11) . . ? C12 C11 N9 111.1(16) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.741 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.102