# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Jean-Rene Hamon' _publ_contact_author_address ; UMR 6226 Sciences chimiques de Rennes CNRS - Universite de Rennes 1 Campus de Beaulieu, Bat. 10C, Case RENNES 35042 FRANCE ; _publ_contact_author_email JEAN-RENE.HAMON@UNIV-RENNES1.FR _publ_section_title ; Trinuclear ?-Conjugated Chromophores Formed by a Neutral Ferrocenyl Group and a Cationic Mixed Ruthenium Sandwich Linker Through an Unsymmetrical Schiff-Base Spacer. Synthesis, Characterization, Electrochemistry and X-ray Crystal Structures ; _publ_contact_author_fax 56-32-273422 _publ_contact_author_phone 56-32-273174 loop_ _publ_author_name 'Jean-Rene Hamon' 'D. Carrillo' 'M. Fuentealba' 'Carolina Manzur' # Attachment 'B707934F_Complex-3PF6.cif' data_l11niruab1 _database_code_depnum_ccdc_archive 'CCDC 640625' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36.50 H41 F6 Fe N2 Ni O2 P Ru' _chemical_formula_weight 900.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Ru Ru -1.2594 0.8363 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.118(4) _cell_length_b 11.668(3) _cell_length_c 18.793(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.925(6) _cell_angle_gamma 90.00 _cell_volume 3697.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 895 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.76 _exptl_crystal_description Needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.399 _exptl_crystal_size_mid 0.073 _exptl_crystal_size_min 0.064 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1828 _exptl_absorpt_coefficient_mu 1.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.566 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29157 _diffrn_reflns_av_R_equivalents 0.1736 _diffrn_reflns_av_sigmaI/netI 0.2936 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.76 _reflns_number_total 8104 _reflns_number_gt 2017 _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 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^)+(0.0973P)^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 8104 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2755 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.2538 _refine_ls_wR_factor_gt 0.1926 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all 0.801 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 1 0.500 0.000 0.000 199.7 48.3 2 0.000 0.500 0.500 199.7 48.2 _platon_squeeze_details ; ; 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 0.82030(12) 0.17757(16) 0.79547(11) 0.0757(7) Uani 1 1 d . . . Ni1 Ni 0.90927(9) 0.53248(12) 0.96457(9) 0.0582(5) Uani 1 1 d . . . Ru1 Ru 0.72041(7) 0.55166(9) 1.10972(7) 0.0708(4) Uani 1 1 d . . . N1 N 0.9511(6) 0.6129(9) 0.8961(6) 0.069(3) Uani 1 1 d . . . N2 N 0.9002(7) 0.6740(8) 1.0104(7) 0.071(3) Uani 1 1 d . . . O1 O 0.9136(5) 0.3939(6) 0.9204(5) 0.067(3) Uani 1 1 d . . . O2 O 0.8678(5) 0.4507(6) 1.0339(5) 0.076(3) Uani 1 1 d . . . C1 C 0.7343(10) 0.2936(17) 0.7923(15) 0.116(7) Uani 1 1 d . . . H1 H 0.7425 0.3738 0.8072 0.139 Uiso 1 1 calc R . . C2 C 0.7211(10) 0.203(2) 0.8383(12) 0.128(7) Uani 1 1 d . . . H2 H 0.7170 0.2086 0.8896 0.154 Uiso 1 1 calc R . . C3 C 0.7104(13) 0.1016(19) 0.7925(15) 0.132(10) Uani 1 1 d . . . H3 H 0.6998 0.0234 0.8071 0.158 Uiso 1 1 calc R . . C4 C 0.7198(12) 0.1360(18) 0.7282(18) 0.158(13) Uani 1 1 d . . . H4 H 0.7192 0.0827 0.6879 0.190 Uiso 1 1 calc R . . C5 C 0.7358(9) 0.252(3) 0.7223(11) 0.142(8) Uani 1 1 d . . . H5 H 0.7421 0.2953 0.6790 0.171 Uiso 1 1 calc R . . C6 C 0.9254(7) 0.2476(12) 0.8369(8) 0.066(4) Uani 1 1 d . . . C7 C 0.9060(9) 0.1635(11) 0.8822(9) 0.096(5) Uani 1 1 d . . . H7 H 0.9003 0.1724 0.9329 0.116 Uiso 1 1 calc R . . C8 C 0.9002(10) 0.0584(15) 0.8411(12) 0.119(6) Uani 1 1 d . . . H8 H 0.8875 -0.0174 0.8585 0.143 Uiso 1 1 calc R . . C9 C 0.9125(9) 0.0843(15) 0.7711(12) 0.109(6) Uani 1 1 d . . . H9 H 0.9106 0.0303 0.7309 0.131 Uiso 1 1 calc R . . C10 C 0.9295(9) 0.2061(12) 0.7695(10) 0.099(5) Uani 1 1 d . . . H10 H 0.9414 0.2501 0.7282 0.119 Uiso 1 1 calc R . . C11 C 0.9328(8) 0.3763(11) 0.8604(8) 0.065(4) Uani 1 1 d . . . C12 C 0.9573(8) 0.4567(13) 0.8155(8) 0.078(4) Uani 1 1 d . . . H12 H 0.9674 0.4329 0.7708 0.094 Uiso 1 1 calc R . . C13 C 0.9680(8) 0.5740(13) 0.8341(9) 0.079(4) Uani 1 1 d . . . C14 C 1.0003(9) 0.6489(13) 0.7817(8) 0.106(6) Uani 1 1 d . . . H14A H 0.9646 0.7117 0.7680 0.159 Uiso 1 1 calc R . . H14B H 1.0059 0.6052 0.7396 0.159 Uiso 1 1 calc R . . H14C H 1.0512 0.6781 0.8038 0.159 Uiso 1 1 calc R . . C15 C 0.9720(10) 0.7375(11) 0.9172(10) 0.112(6) Uani 1 1 d . . . H15A H 1.0273 0.7438 0.9395 0.134 Uiso 1 1 calc R . . H15B H 0.9626 0.7866 0.8750 0.134 Uiso 1 1 calc R . . C16 C 0.9222(11) 0.7686(10) 0.9665(9) 0.105(6) Uani 1 1 d . . . H16A H 0.8741 0.8021 0.9398 0.126 Uiso 1 1 calc R . . H16B H 0.9487 0.8271 0.9986 0.126 Uiso 1 1 calc R . . C17 C 0.8747(10) 0.6962(14) 1.0673(10) 0.102(5) Uani 1 1 d . . . H17 H 0.8736 0.7724 1.0817 0.122 Uiso 1 1 calc R . . C18 C 0.8456(9) 0.6061(12) 1.1137(8) 0.078(4) Uani 1 1 d . . . C19 C 0.8196(9) 0.6393(15) 1.1758(8) 0.089(5) Uani 1 1 d . . . H19 H 0.8154 0.7209 1.1869 0.107 Uiso 1 1 calc R . . C20 C 0.7906(11) 0.556(2) 1.2192(10) 0.121(6) Uani 1 1 d . . . H20 H 0.7649 0.5818 1.2591 0.145 Uiso 1 1 calc R . . C21 C 0.7842(11) 0.4434(16) 1.1997(10) 0.112(6) Uani 1 1 d . . . H21 H 0.7548 0.3898 1.2253 0.135 Uiso 1 1 calc R . . C22 C 0.8072(8) 0.4114(12) 1.1340(9) 0.081(4) Uani 1 1 d . . . H22 H 0.7926 0.3350 1.1145 0.097 Uiso 1 1 calc R . . C23 C 0.8437(8) 0.4878(13) 1.0922(8) 0.074(4) Uani 1 1 d . . . C24 C 0.6487(9) 0.627(2) 1.0185(10) 0.104(6) Uani 1 1 d . . . C25 C 0.6215(10) 0.6642(12) 1.0802(11) 0.096(5) Uani 1 1 d . . . C26 C 0.5973(10) 0.5658(19) 1.1114(10) 0.100(5) Uani 1 1 d . . . C27 C 0.6071(14) 0.4742(17) 1.0704(18) 0.139(9) Uani 1 1 d . . . C28 C 0.6393(16) 0.514(2) 1.0100(14) 0.142(11) Uani 1 1 d . . . C29 C 0.6780(11) 0.716(2) 0.9697(11) 0.205(13) Uani 1 1 d . . . H29A H 0.6392 0.7257 0.9267 0.308 Uiso 1 1 calc R . . H29B H 0.7271 0.6909 0.9570 0.308 Uiso 1 1 calc R . . H29C H 0.6861 0.7880 0.9948 0.308 Uiso 1 1 calc R . . C30 C 0.6101(13) 0.7947(16) 1.1146(12) 0.197(11) Uani 1 1 d . . . H30A H 0.6529 0.8435 1.1065 0.295 Uiso 1 1 calc R . . H30B H 0.6101 0.7884 1.1655 0.295 Uiso 1 1 calc R . . H30C H 0.5606 0.8270 1.0913 0.295 Uiso 1 1 calc R . . C31 C 0.5542(12) 0.572(2) 1.1770(13) 0.226(14) Uani 1 1 d . . . H31A H 0.5046 0.5318 1.1661 0.339 Uiso 1 1 calc R . . H31B H 0.5443 0.6509 1.1874 0.339 Uiso 1 1 calc R . . H31C H 0.5867 0.5377 1.2181 0.339 Uiso 1 1 calc R . . C32 C 0.5837(15) 0.3511(17) 1.0800(19) 0.35(3) Uani 1 1 d . . . H32A H 0.5957 0.3310 1.1302 0.526 Uiso 1 1 calc R . . H32B H 0.6125 0.3019 1.0528 0.526 Uiso 1 1 calc R . . H32C H 0.5278 0.3422 1.0630 0.526 Uiso 1 1 calc R . . C33 C 0.6624(16) 0.453(3) 0.9464(13) 0.30(2) Uani 1 1 d . . . H33A H 0.6198 0.4034 0.9250 0.450 Uiso 1 1 calc R . . H33B H 0.7091 0.4075 0.9622 0.450 Uiso 1 1 calc R . . H33C H 0.6730 0.5077 0.9114 0.450 Uiso 1 1 calc R . . P1 P 0.1776(3) 0.9544(4) 0.9044(3) 0.0980(15) Uani 1 1 d . . . F1 F 0.2604(9) 0.9268(16) 0.8954(10) 0.251(8) Uani 1 1 d . . . F2 F 0.1480(10) 0.8727(8) 0.8405(6) 0.210(7) Uani 1 1 d . . . F3 F 0.1798(11) 1.0532(8) 0.8510(7) 0.216(7) Uani 1 1 d . . . F4 F 0.2117(9) 1.0356(10) 0.9688(7) 0.199(6) Uani 1 1 d . . . F5 F 0.1854(12) 0.8549(10) 0.9581(7) 0.236(8) Uani 1 1 d . . . F6 F 0.1006(9) 0.9892(16) 0.9164(11) 0.282(10) 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 0.0774(15) 0.0618(12) 0.0893(16) -0.0241(11) 0.0184(13) 0.0002(11) Ni1 0.0628(11) 0.0422(9) 0.0690(12) 0.0025(8) 0.0098(9) -0.0036(8) Ru1 0.0751(9) 0.0641(7) 0.0756(9) -0.0050(6) 0.0202(7) 0.0065(6) N1 0.069(8) 0.068(7) 0.073(8) 0.015(6) 0.022(7) -0.006(6) N2 0.098(10) 0.040(6) 0.075(9) -0.019(6) 0.012(7) -0.011(6) O1 0.105(7) 0.051(5) 0.053(6) -0.001(4) 0.033(5) -0.022(5) O2 0.104(7) 0.049(5) 0.082(7) 0.017(5) 0.035(6) 0.012(5) C1 0.078(13) 0.100(14) 0.17(2) -0.050(15) 0.023(14) 0.006(11) C2 0.096(15) 0.162(19) 0.142(19) -0.056(17) 0.061(13) -0.015(14) C3 0.136(18) 0.082(14) 0.20(3) -0.021(16) 0.095(19) -0.035(12) C4 0.062(14) 0.075(14) 0.32(4) -0.05(2) -0.029(19) -0.021(10) C5 0.057(12) 0.24(3) 0.113(17) -0.041(19) -0.026(11) -0.016(15) C6 0.053(9) 0.076(10) 0.070(10) -0.011(8) 0.016(7) -0.006(7) C7 0.132(14) 0.037(8) 0.120(14) -0.013(9) 0.023(12) 0.017(8) C8 0.115(15) 0.095(13) 0.142(18) -0.020(14) 0.008(14) 0.039(11) C9 0.088(13) 0.107(15) 0.137(18) -0.050(13) 0.029(12) 0.015(10) C10 0.108(13) 0.072(11) 0.130(15) -0.046(10) 0.055(11) 0.002(9) C11 0.064(10) 0.059(8) 0.069(10) -0.006(8) 0.002(8) -0.001(7) C12 0.070(10) 0.092(11) 0.075(10) -0.013(10) 0.020(8) 0.007(9) C13 0.056(10) 0.090(12) 0.086(12) 0.014(10) 0.001(9) -0.015(8) C14 0.112(13) 0.124(13) 0.091(12) 0.027(10) 0.041(11) -0.041(11) C15 0.124(15) 0.052(9) 0.174(19) 0.004(10) 0.068(14) -0.025(9) C16 0.171(18) 0.034(8) 0.119(14) -0.001(9) 0.053(13) -0.025(9) C17 0.111(14) 0.074(11) 0.114(16) -0.019(11) 0.006(12) 0.000(10) C18 0.098(12) 0.057(9) 0.081(12) -0.024(9) 0.019(9) 0.004(8) C19 0.079(11) 0.121(13) 0.063(11) -0.027(10) 0.001(9) 0.019(10) C20 0.137(17) 0.147(18) 0.090(14) 0.015(14) 0.053(12) 0.006(15) C21 0.152(17) 0.093(13) 0.105(15) 0.039(12) 0.061(13) 0.011(12) C22 0.084(11) 0.072(9) 0.092(12) 0.028(9) 0.028(10) -0.001(8) C23 0.059(10) 0.107(12) 0.055(9) 0.015(9) 0.006(8) 0.024(8) C24 0.058(11) 0.19(2) 0.057(12) 0.045(14) 0.000(9) 0.007(12) C25 0.098(13) 0.057(10) 0.126(16) 0.007(11) 0.000(12) 0.009(9) C26 0.075(12) 0.120(15) 0.108(15) 0.009(13) 0.020(10) -0.013(11) C27 0.122(18) 0.075(14) 0.20(3) 0.000(16) -0.039(17) -0.035(12) C28 0.15(2) 0.114(18) 0.14(2) -0.075(17) -0.019(16) 0.079(16) C29 0.096(15) 0.32(3) 0.18(2) 0.17(2) -0.011(15) -0.005(18) C30 0.22(3) 0.117(16) 0.23(3) -0.007(16) -0.04(2) 0.017(17) C31 0.111(17) 0.41(4) 0.18(2) 0.07(3) 0.081(17) 0.05(2) C32 0.22(3) 0.093(15) 0.64(7) 0.09(2) -0.21(4) -0.108(17) C33 0.26(3) 0.42(4) 0.17(2) -0.21(3) -0.10(2) 0.18(3) P1 0.121(4) 0.059(3) 0.122(4) -0.004(3) 0.044(3) -0.014(3) F1 0.159(13) 0.33(2) 0.280(19) -0.038(17) 0.066(13) 0.067(14) F2 0.38(2) 0.082(7) 0.140(10) -0.026(7) -0.035(11) -0.031(9) F3 0.41(2) 0.074(7) 0.178(12) 0.000(7) 0.093(13) -0.057(10) F4 0.260(16) 0.133(9) 0.190(13) -0.077(9) 0.001(11) -0.031(10) F5 0.47(3) 0.104(8) 0.163(12) -0.009(8) 0.141(15) 0.010(12) F6 0.138(12) 0.31(2) 0.42(3) -0.10(2) 0.104(16) 0.028(13) _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 C1 1.994(16) . ? Fe1 C7 2.003(16) . ? Fe1 C6 2.007(13) . ? Fe1 C4 2.01(2) . ? Fe1 C5 2.01(2) . ? Fe1 C2 2.024(16) . ? Fe1 C8 2.033(17) . ? Fe1 C9 2.033(15) . ? Fe1 C10 2.040(15) . ? Fe1 C3 2.07(2) . ? Ni1 O1 1.825(8) . ? Ni1 N1 1.834(10) . ? Ni1 O2 1.852(8) . ? Ni1 N2 1.881(10) . ? Ru1 C26 2.120(16) . ? Ru1 C24 2.121(15) . ? Ru1 C25 2.138(15) . ? Ru1 C27 2.152(19) . ? Ru1 C28 2.18(2) . ? Ru1 C19 2.177(15) . ? Ru1 C20 2.197(18) . ? Ru1 C22 2.205(13) . ? Ru1 C18 2.225(15) . ? Ru1 C21 2.239(16) . ? Ru1 C23 2.315(14) . ? N1 C13 1.328(16) . ? N1 C15 1.532(16) . ? N2 C17 1.249(17) . ? N2 C16 1.466(15) . ? O1 C11 1.244(14) . ? O2 C23 1.309(14) . ? C1 C2 1.40(2) . ? C1 C5 1.41(2) . ? C2 C3 1.46(3) . ? C3 C4 1.31(3) . ? C4 C5 1.39(3) . ? C6 C10 1.370(17) . ? C6 C7 1.377(17) . ? C6 C11 1.564(17) . ? C7 C8 1.444(19) . ? C8 C9 1.40(2) . ? C9 C10 1.45(2) . ? C11 C12 1.374(17) . ? C12 C13 1.416(18) . ? C13 C14 1.493(17) . ? C15 C16 1.411(17) . ? C17 C18 1.50(2) . ? C18 C19 1.374(17) . ? C18 C23 1.438(18) . ? C19 C20 1.41(2) . ? C20 C21 1.36(2) . ? C21 C22 1.41(2) . ? C22 C23 1.404(17) . ? C24 C28 1.34(3) . ? C24 C25 1.39(2) . ? C24 C29 1.53(2) . ? C25 C26 1.39(2) . ? C25 C30 1.68(2) . ? C26 C27 1.34(3) . ? C26 C31 1.54(2) . ? C27 C28 1.42(3) . ? C27 C32 1.51(2) . ? C28 C33 1.50(3) . ? P1 F6 1.434(13) . ? P1 F1 1.491(13) . ? P1 F5 1.529(13) . ? P1 F3 1.533(12) . ? P1 F2 1.549(11) . ? P1 F4 1.567(11) . ? 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 C1 Fe1 C7 120.9(8) . . ? C1 Fe1 C6 110.1(7) . . ? C7 Fe1 C6 40.2(5) . . ? C1 Fe1 C4 66.3(8) . . ? C7 Fe1 C4 156.8(10) . . ? C6 Fe1 C4 162.7(10) . . ? C1 Fe1 C5 41.1(7) . . ? C7 Fe1 C5 158.5(9) . . ? C6 Fe1 C5 125.5(9) . . ? C4 Fe1 C5 40.4(8) . . ? C1 Fe1 C2 40.9(7) . . ? C7 Fe1 C2 103.6(8) . . ? C6 Fe1 C2 122.9(7) . . ? C4 Fe1 C2 66.4(10) . . ? C5 Fe1 C2 69.7(9) . . ? C1 Fe1 C8 156.4(10) . . ? C7 Fe1 C8 41.9(6) . . ? C6 Fe1 C8 67.8(7) . . ? C4 Fe1 C8 122.7(8) . . ? C5 Fe1 C8 159.2(10) . . ? C2 Fe1 C8 119.0(10) . . ? C1 Fe1 C9 162.7(10) . . ? C7 Fe1 C9 69.6(7) . . ? C6 Fe1 C9 68.1(6) . . ? C4 Fe1 C9 110.1(9) . . ? C5 Fe1 C9 124.9(9) . . ? C2 Fe1 C9 155.1(10) . . ? C8 Fe1 C9 40.3(6) . . ? C1 Fe1 C10 125.8(8) . . ? C7 Fe1 C10 68.6(7) . . ? C6 Fe1 C10 39.6(5) . . ? C4 Fe1 C10 127.5(11) . . ? C5 Fe1 C10 110.3(8) . . ? C2 Fe1 C10 159.7(8) . . ? C8 Fe1 C10 68.6(8) . . ? C9 Fe1 C10 41.8(6) . . ? C1 Fe1 C3 68.1(8) . . ? C7 Fe1 C3 121.4(9) . . ? C6 Fe1 C3 159.0(9) . . ? C4 Fe1 C3 37.4(9) . . ? C5 Fe1 C3 67.9(9) . . ? C2 Fe1 C3 41.8(7) . . ? C8 Fe1 C3 105.1(9) . . ? C9 Fe1 C3 120.1(8) . . ? C10 Fe1 C3 158.3(8) . . ? O1 Ni1 N1 94.7(4) . . ? O1 Ni1 O2 85.1(4) . . ? N1 Ni1 O2 179.6(4) . . ? O1 Ni1 N2 177.5(5) . . ? N1 Ni1 N2 86.9(5) . . ? O2 Ni1 N2 93.3(5) . . ? C26 Ru1 C24 62.7(6) . . ? C26 Ru1 C25 38.0(6) . . ? C24 Ru1 C25 38.1(6) . . ? C26 Ru1 C27 36.7(7) . . ? C24 Ru1 C27 62.3(8) . . ? C25 Ru1 C27 62.8(7) . . ? C26 Ru1 C28 62.6(8) . . ? C24 Ru1 C28 36.2(7) . . ? C25 Ru1 C28 62.7(6) . . ? C27 Ru1 C28 38.4(8) . . ? C26 Ru1 C19 129.4(7) . . ? C24 Ru1 C19 123.5(8) . . ? C25 Ru1 C19 111.3(6) . . ? C27 Ru1 C19 163.9(11) . . ? C28 Ru1 C19 154.8(12) . . ? C26 Ru1 C20 111.7(7) . . ? C24 Ru1 C20 153.5(10) . . ? C25 Ru1 C20 120.6(8) . . ? C27 Ru1 C20 130.2(10) . . ? C28 Ru1 C20 167.3(12) . . ? C19 Ru1 C20 37.7(6) . . ? C26 Ru1 C22 133.7(7) . . ? C24 Ru1 C22 138.7(8) . . ? C25 Ru1 C22 169.9(6) . . ? C27 Ru1 C22 107.1(7) . . ? C28 Ru1 C22 109.6(6) . . ? C19 Ru1 C22 78.4(6) . . ? C20 Ru1 C22 65.3(6) . . ? C26 Ru1 C18 158.8(7) . . ? C24 Ru1 C18 109.2(6) . . ? C25 Ru1 C18 123.2(6) . . ? C27 Ru1 C18 159.7(10) . . ? C28 Ru1 C18 123.7(10) . . ? C19 Ru1 C18 36.4(5) . . ? C20 Ru1 C18 66.0(6) . . ? C22 Ru1 C18 66.0(5) . . ? C26 Ru1 C21 113.0(7) . . ? C24 Ru1 C21 169.8(9) . . ? C25 Ru1 C21 143.5(8) . . ? C27 Ru1 C21 108.4(8) . . ? C28 Ru1 C21 133.8(10) . . ? C19 Ru1 C21 66.6(7) . . ? C20 Ru1 C21 35.8(6) . . ? C22 Ru1 C21 37.0(5) . . ? C18 Ru1 C21 78.1(6) . . ? C26 Ru1 C23 163.8(7) . . ? C24 Ru1 C23 115.7(6) . . ? C25 Ru1 C23 149.4(7) . . ? C27 Ru1 C23 127.3(9) . . ? C28 Ru1 C23 105.9(7) . . ? C19 Ru1 C23 65.9(5) . . ? C20 Ru1 C23 77.0(6) . . ? C22 Ru1 C23 36.1(4) . . ? C18 Ru1 C23 36.9(5) . . ? C21 Ru1 C23 65.6(6) . . ? C13 N1 C15 118.3(12) . . ? C13 N1 Ni1 127.6(9) . . ? C15 N1 Ni1 114.0(10) . . ? C17 N2 C16 119.1(13) . . ? C17 N2 Ni1 130.0(11) . . ? C16 N2 Ni1 110.7(9) . . ? C11 O1 Ni1 126.6(8) . . ? C23 O2 Ni1 129.2(9) . . ? C2 C1 C5 110.3(19) . . ? C2 C1 Fe1 70.7(11) . . ? C5 C1 Fe1 70.1(11) . . ? C1 C2 C3 105.3(18) . . ? C1 C2 Fe1 68.4(10) . . ? C3 C2 Fe1 70.8(10) . . ? C4 C3 C2 106(2) . . ? C4 C3 Fe1 68.8(12) . . ? C2 C3 Fe1 67.4(11) . . ? C3 C4 C5 115(3) . . ? C3 C4 Fe1 73.8(17) . . ? C5 C4 Fe1 69.9(11) . . ? C4 C5 C1 103(2) . . ? C4 C5 Fe1 69.8(14) . . ? C1 C5 Fe1 68.7(11) . . ? C10 C6 C7 112.1(13) . . ? C10 C6 C11 125.8(14) . . ? C7 C6 C11 121.8(13) . . ? C10 C6 Fe1 71.5(8) . . ? C7 C6 Fe1 69.8(9) . . ? C11 C6 Fe1 121.6(9) . . ? C6 C7 C8 106.0(15) . . ? C6 C7 Fe1 70.1(9) . . ? C8 C7 Fe1 70.2(10) . . ? C9 C8 C7 108.1(17) . . ? C9 C8 Fe1 69.9(10) . . ? C7 C8 Fe1 67.9(9) . . ? C8 C9 C10 107.1(16) . . ? C8 C9 Fe1 69.8(10) . . ? C10 C9 Fe1 69.4(8) . . ? C6 C10 C9 106.5(16) . . ? C6 C10 Fe1 68.9(8) . . ? C9 C10 Fe1 68.9(9) . . ? O1 C11 C12 126.8(12) . . ? O1 C11 C6 113.1(12) . . ? C12 C11 C6 120.1(14) . . ? C11 C12 C13 123.3(13) . . ? N1 C13 C12 120.6(13) . . ? N1 C13 C14 122.7(14) . . ? C12 C13 C14 116.7(15) . . ? C16 C15 N1 105.8(12) . . ? C15 C16 N2 114.8(12) . . ? N2 C17 C18 123.4(14) . . ? C19 C18 C23 120.9(15) . . ? C19 C18 C17 118.9(15) . . ? C23 C18 C17 120.1(13) . . ? C19 C18 Ru1 69.9(9) . . ? C23 C18 Ru1 75.0(9) . . ? C17 C18 Ru1 126.4(11) . . ? C18 C19 C20 119.6(16) . . ? C18 C19 Ru1 73.7(9) . . ? C20 C19 Ru1 71.9(10) . . ? C21 C20 C19 121.8(17) . . ? C21 C20 Ru1 73.8(12) . . ? C19 C20 Ru1 70.4(9) . . ? C20 C21 C22 118.1(15) . . ? C20 C21 Ru1 70.5(10) . . ? C22 C21 Ru1 70.2(9) . . ? C23 C22 C21 122.7(14) . . ? C23 C22 Ru1 76.2(8) . . ? C21 C22 Ru1 72.8(9) . . ? O2 C23 C22 119.5(14) . . ? O2 C23 C18 123.9(14) . . ? C22 C23 C18 116.3(14) . . ? O2 C23 Ru1 130.6(9) . . ? C22 C23 Ru1 67.7(8) . . ? C18 C23 Ru1 68.2(8) . . ? C28 C24 C25 110.9(19) . . ? C28 C24 C29 130(3) . . ? C25 C24 C29 119(2) . . ? C28 C24 Ru1 74.2(12) . . ? C25 C24 Ru1 71.6(9) . . ? C29 C24 Ru1 124.3(11) . . ? C26 C25 C24 105.2(15) . . ? C26 C25 C30 122(2) . . ? C24 C25 C30 133(2) . . ? C26 C25 Ru1 70.3(9) . . ? C24 C25 Ru1 70.3(9) . . ? C30 C25 Ru1 126.6(12) . . ? C27 C26 C25 109.9(18) . . ? C27 C26 C31 128(2) . . ? C25 C26 C31 121(2) . . ? C27 C26 Ru1 72.9(12) . . ? C25 C26 Ru1 71.7(9) . . ? C31 C26 Ru1 129.0(13) . . ? C26 C27 C28 107.6(18) . . ? C26 C27 C32 129(3) . . ? C28 C27 C32 124(3) . . ? C26 C27 Ru1 70.4(11) . . ? C28 C27 Ru1 71.8(13) . . ? C32 C27 Ru1 126.9(15) . . ? C24 C28 C27 106.3(18) . . ? C24 C28 C33 122(3) . . ? C27 C28 C33 132(3) . . ? C24 C28 Ru1 69.6(11) . . ? C27 C28 Ru1 69.9(13) . . ? C33 C28 Ru1 124.4(15) . . ? F6 P1 F1 175.2(11) . . ? F6 P1 F5 95.1(11) . . ? F1 P1 F5 86.3(10) . . ? F6 P1 F3 90.9(11) . . ? F1 P1 F3 87.6(10) . . ? F5 P1 F3 173.7(11) . . ? F6 P1 F2 96.3(10) . . ? F1 P1 F2 88.2(9) . . ? F5 P1 F2 91.3(7) . . ? F3 P1 F2 89.8(7) . . ? F6 P1 F4 86.4(9) . . ? F1 P1 F4 89.0(9) . . ? F5 P1 F4 88.4(8) . . ? F3 P1 F4 90.2(7) . . ? F2 P1 F4 177.3(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 N1 C13 6.0(12) . . . . ? O2 Ni1 N1 C13 68(72) . . . . ? N2 Ni1 N1 C13 -172.1(12) . . . . ? O1 Ni1 N1 C15 -170.4(10) . . . . ? O2 Ni1 N1 C15 -108(71) . . . . ? N2 Ni1 N1 C15 11.4(10) . . . . ? O1 Ni1 N2 C17 50(11) . . . . ? N1 Ni1 N2 C17 -179.5(15) . . . . ? O2 Ni1 N2 C17 0.1(15) . . . . ? O1 Ni1 N2 C16 -125(10) . . . . ? N1 Ni1 N2 C16 5.4(11) . . . . ? O2 Ni1 N2 C16 -175.0(10) . . . . ? N1 Ni1 O1 C11 -5.8(11) . . . . ? O2 Ni1 O1 C11 174.6(11) . . . . ? N2 Ni1 O1 C11 124(10) . . . . ? O1 Ni1 O2 C23 -178.9(11) . . . . ? N1 Ni1 O2 C23 119(71) . . . . ? N2 Ni1 O2 C23 -0.8(11) . . . . ? C7 Fe1 C1 C2 -74.3(14) . . . . ? C6 Fe1 C1 C2 -117.4(12) . . . . ? C4 Fe1 C1 C2 80.8(15) . . . . ? C5 Fe1 C1 C2 121.2(18) . . . . ? C8 Fe1 C1 C2 -37(2) . . . . ? C9 Fe1 C1 C2 162(2) . . . . ? C10 Fe1 C1 C2 -159.0(11) . . . . ? C3 Fe1 C1 C2 40.2(12) . . . . ? C7 Fe1 C1 C5 164.5(13) . . . . ? C6 Fe1 C1 C5 121.4(14) . . . . ? C4 Fe1 C1 C5 -40.4(14) . . . . ? C2 Fe1 C1 C5 -121.2(18) . . . . ? C8 Fe1 C1 C5 -158.3(19) . . . . ? C9 Fe1 C1 C5 41(3) . . . . ? C10 Fe1 C1 C5 79.8(15) . . . . ? C3 Fe1 C1 C5 -81.0(14) . . . . ? C5 C1 C2 C3 -3(2) . . . . ? Fe1 C1 C2 C3 -61.7(14) . . . . ? C5 C1 C2 Fe1 59.1(13) . . . . ? C7 Fe1 C2 C1 121.8(12) . . . . ? C6 Fe1 C2 C1 83.0(14) . . . . ? C4 Fe1 C2 C1 -80.4(13) . . . . ? C5 Fe1 C2 C1 -36.8(12) . . . . ? C8 Fe1 C2 C1 164.0(12) . . . . ? C9 Fe1 C2 C1 -167.4(17) . . . . ? C10 Fe1 C2 C1 57(3) . . . . ? C3 Fe1 C2 C1 -116.0(19) . . . . ? C1 Fe1 C2 C3 116.0(19) . . . . ? C7 Fe1 C2 C3 -122.2(15) . . . . ? C6 Fe1 C2 C3 -161.0(13) . . . . ? C4 Fe1 C2 C3 35.6(13) . . . . ? C5 Fe1 C2 C3 79.1(14) . . . . ? C8 Fe1 C2 C3 -80.0(16) . . . . ? C9 Fe1 C2 C3 -51(3) . . . . ? C10 Fe1 C2 C3 173(2) . . . . ? C1 C2 C3 C4 2(3) . . . . ? Fe1 C2 C3 C4 -58.4(18) . . . . ? C1 C2 C3 Fe1 60.1(13) . . . . ? C1 Fe1 C3 C4 79.1(16) . . . . ? C7 Fe1 C3 C4 -167.1(13) . . . . ? C6 Fe1 C3 C4 168.2(16) . . . . ? C5 Fe1 C3 C4 34.6(16) . . . . ? C2 Fe1 C3 C4 118(2) . . . . ? C8 Fe1 C3 C4 -124.7(16) . . . . ? C9 Fe1 C3 C4 -83.9(18) . . . . ? C10 Fe1 C3 C4 -55(3) . . . . ? C1 Fe1 C3 C2 -39.4(13) . . . . ? C7 Fe1 C3 C2 74.4(16) . . . . ? C6 Fe1 C3 C2 50(3) . . . . ? C4 Fe1 C3 C2 -118(2) . . . . ? C5 Fe1 C3 C2 -83.9(14) . . . . ? C8 Fe1 C3 C2 116.8(15) . . . . ? C9 Fe1 C3 C2 157.6(14) . . . . ? C10 Fe1 C3 C2 -173(2) . . . . ? C2 C3 C4 C5 0(3) . . . . ? Fe1 C3 C4 C5 -57.6(18) . . . . ? C2 C3 C4 Fe1 57.5(16) . . . . ? C1 Fe1 C4 C3 -84.5(18) . . . . ? C7 Fe1 C4 C3 29(3) . . . . ? C6 Fe1 C4 C3 -165.8(19) . . . . ? C5 Fe1 C4 C3 -126(3) . . . . ? C2 Fe1 C4 C3 -39.7(16) . . . . ? C8 Fe1 C4 C3 71(2) . . . . ? C9 Fe1 C4 C3 113.7(17) . . . . ? C10 Fe1 C4 C3 157.6(14) . . . . ? C1 Fe1 C4 C5 41.1(14) . . . . ? C7 Fe1 C4 C5 154.5(16) . . . . ? C6 Fe1 C4 C5 -40(4) . . . . ? C2 Fe1 C4 C5 86.0(15) . . . . ? C8 Fe1 C4 C5 -163.7(14) . . . . ? C9 Fe1 C4 C5 -120.6(16) . . . . ? C10 Fe1 C4 C5 -76.8(17) . . . . ? C3 Fe1 C4 C5 126(3) . . . . ? C3 C4 C5 C1 -1(3) . . . . ? Fe1 C4 C5 C1 -61.2(12) . . . . ? C3 C4 C5 Fe1 60(2) . . . . ? C2 C1 C5 C4 2(2) . . . . ? Fe1 C1 C5 C4 61.9(13) . . . . ? C2 C1 C5 Fe1 -59.4(14) . . . . ? C1 Fe1 C5 C4 -114(2) . . . . ? C7 Fe1 C5 C4 -152(2) . . . . ? C6 Fe1 C5 C4 166.4(16) . . . . ? C2 Fe1 C5 C4 -77.1(17) . . . . ? C8 Fe1 C5 C4 42(3) . . . . ? C9 Fe1 C5 C4 80.0(19) . . . . ? C10 Fe1 C5 C4 124.6(17) . . . . ? C3 Fe1 C5 C4 -32.1(17) . . . . ? C7 Fe1 C5 C1 -39(3) . . . . ? C6 Fe1 C5 C1 -79.9(15) . . . . ? C4 Fe1 C5 C1 114(2) . . . . ? C2 Fe1 C5 C1 36.6(11) . . . . ? C8 Fe1 C5 C1 155(2) . . . . ? C9 Fe1 C5 C1 -166.3(12) . . . . ? C10 Fe1 C5 C1 -121.7(13) . . . . ? C3 Fe1 C5 C1 81.6(13) . . . . ? C1 Fe1 C6 C10 -122.4(12) . . . . ? C7 Fe1 C6 C10 123.1(13) . . . . ? C4 Fe1 C6 C10 -48(3) . . . . ? C5 Fe1 C6 C10 -78.8(13) . . . . ? C2 Fe1 C6 C10 -166.1(12) . . . . ? C8 Fe1 C6 C10 82.8(11) . . . . ? C9 Fe1 C6 C10 39.2(10) . . . . ? C3 Fe1 C6 C10 157(2) . . . . ? C1 Fe1 C6 C7 114.5(11) . . . . ? C4 Fe1 C6 C7 -171(2) . . . . ? C5 Fe1 C6 C7 158.1(11) . . . . ? C2 Fe1 C6 C7 70.7(13) . . . . ? C8 Fe1 C6 C7 -40.3(9) . . . . ? C9 Fe1 C6 C7 -83.9(10) . . . . ? C10 Fe1 C6 C7 -123.1(13) . . . . ? C3 Fe1 C6 C7 33(2) . . . . ? C1 Fe1 C6 C11 -1.1(15) . . . . ? C7 Fe1 C6 C11 -115.6(15) . . . . ? C4 Fe1 C6 C11 73(3) . . . . ? C5 Fe1 C6 C11 42.5(16) . . . . ? C2 Fe1 C6 C11 -44.9(16) . . . . ? C8 Fe1 C6 C11 -155.9(14) . . . . ? C9 Fe1 C6 C11 160.5(14) . . . . ? C10 Fe1 C6 C11 121.3(16) . . . . ? C3 Fe1 C6 C11 -82(2) . . . . ? C10 C6 C7 C8 2.3(18) . . . . ? C11 C6 C7 C8 176.7(12) . . . . ? Fe1 C6 C7 C8 61.3(11) . . . . ? C10 C6 C7 Fe1 -59.0(11) . . . . ? C11 C6 C7 Fe1 115.4(12) . . . . ? C1 Fe1 C7 C6 -84.9(12) . . . . ? C4 Fe1 C7 C6 173(2) . . . . ? C5 Fe1 C7 C6 -56(2) . . . . ? C2 Fe1 C7 C6 -125.3(11) . . . . ? C8 Fe1 C7 C6 116.3(14) . . . . ? C9 Fe1 C7 C6 79.8(9) . . . . ? C10 Fe1 C7 C6 34.9(8) . . . . ? C3 Fe1 C7 C6 -166.6(10) . . . . ? C1 Fe1 C7 C8 158.8(13) . . . . ? C6 Fe1 C7 C8 -116.3(15) . . . . ? C4 Fe1 C7 C8 57(3) . . . . ? C5 Fe1 C7 C8 -173(2) . . . . ? C2 Fe1 C7 C8 118.4(13) . . . . ? C9 Fe1 C7 C8 -36.5(11) . . . . ? C10 Fe1 C7 C8 -81.4(11) . . . . ? C3 Fe1 C7 C8 77.1(14) . . . . ? C6 C7 C8 C9 -2.9(19) . . . . ? Fe1 C7 C8 C9 58.4(13) . . . . ? C6 C7 C8 Fe1 -61.3(11) . . . . ? C1 Fe1 C8 C9 -171.3(16) . . . . ? C7 Fe1 C8 C9 -120.4(17) . . . . ? C6 Fe1 C8 C9 -81.8(11) . . . . ? C4 Fe1 C8 C9 82.7(17) . . . . ? C5 Fe1 C8 C9 52(3) . . . . ? C2 Fe1 C8 C9 161.9(11) . . . . ? C10 Fe1 C8 C9 -39.0(11) . . . . ? C3 Fe1 C8 C9 119.0(13) . . . . ? C1 Fe1 C8 C7 -51(2) . . . . ? C6 Fe1 C8 C7 38.6(9) . . . . ? C4 Fe1 C8 C7 -156.9(14) . . . . ? C5 Fe1 C8 C7 172(2) . . . . ? C2 Fe1 C8 C7 -77.7(13) . . . . ? C9 Fe1 C8 C7 120.4(17) . . . . ? C10 Fe1 C8 C7 81.4(11) . . . . ? C3 Fe1 C8 C7 -120.5(12) . . . . ? C7 C8 C9 C10 2(2) . . . . ? Fe1 C8 C9 C10 59.6(12) . . . . ? C7 C8 C9 Fe1 -57.2(12) . . . . ? C1 Fe1 C9 C8 168(2) . . . . ? C7 Fe1 C9 C8 37.9(11) . . . . ? C6 Fe1 C9 C8 81.1(12) . . . . ? C4 Fe1 C9 C8 -117.3(14) . . . . ? C5 Fe1 C9 C8 -160.1(13) . . . . ? C2 Fe1 C9 C8 -40(2) . . . . ? C10 Fe1 C9 C8 118.3(16) . . . . ? C3 Fe1 C9 C8 -77.4(15) . . . . ? C1 Fe1 C9 C10 50(3) . . . . ? C7 Fe1 C9 C10 -80.4(11) . . . . ? C6 Fe1 C9 C10 -37.2(10) . . . . ? C4 Fe1 C9 C10 124.4(14) . . . . ? C5 Fe1 C9 C10 81.6(14) . . . . ? C2 Fe1 C9 C10 -158.6(17) . . . . ? C8 Fe1 C9 C10 -118.3(16) . . . . ? C3 Fe1 C9 C10 164.3(12) . . . . ? C7 C6 C10 C9 -0.9(18) . . . . ? C11 C6 C10 C9 -175.0(13) . . . . ? Fe1 C6 C10 C9 -58.9(11) . . . . ? C7 C6 C10 Fe1 58.0(11) . . . . ? C11 C6 C10 Fe1 -116.1(13) . . . . ? C8 C9 C10 C6 -1.0(19) . . . . ? Fe1 C9 C10 C6 58.9(10) . . . . ? C8 C9 C10 Fe1 -59.9(12) . . . . ? C1 Fe1 C10 C6 78.0(14) . . . . ? C7 Fe1 C10 C6 -35.4(8) . . . . ? C4 Fe1 C10 C6 163.8(11) . . . . ? C5 Fe1 C10 C6 121.6(12) . . . . ? C2 Fe1 C10 C6 35(3) . . . . ? C8 Fe1 C10 C6 -80.6(10) . . . . ? C9 Fe1 C10 C6 -118.3(15) . . . . ? C3 Fe1 C10 C6 -157(2) . . . . ? C1 Fe1 C10 C9 -163.7(13) . . . . ? C7 Fe1 C10 C9 82.9(11) . . . . ? C6 Fe1 C10 C9 118.3(15) . . . . ? C4 Fe1 C10 C9 -77.8(15) . . . . ? C5 Fe1 C10 C9 -120.1(14) . . . . ? C2 Fe1 C10 C9 154(2) . . . . ? C8 Fe1 C10 C9 37.7(11) . . . . ? C3 Fe1 C10 C9 -39(3) . . . . ? Ni1 O1 C11 C12 2(2) . . . . ? Ni1 O1 C11 C6 -176.7(8) . . . . ? C10 C6 C11 O1 168.4(13) . . . . ? C7 C6 C11 O1 -5.1(19) . . . . ? Fe1 C6 C11 O1 79.3(14) . . . . ? C10 C6 C11 C12 -11(2) . . . . ? C7 C6 C11 C12 175.8(13) . . . . ? Fe1 C6 C11 C12 -99.8(14) . . . . ? O1 C11 C12 C13 3(2) . . . . ? C6 C11 C12 C13 -177.8(12) . . . . ? C15 N1 C13 C12 173.6(13) . . . . ? Ni1 N1 C13 C12 -3(2) . . . . ? C15 N1 C13 C14 -5(2) . . . . ? Ni1 N1 C13 C14 178.5(10) . . . . ? C11 C12 C13 N1 -3(2) . . . . ? C11 C12 C13 C14 175.8(13) . . . . ? C13 N1 C15 C16 157.6(14) . . . . ? Ni1 N1 C15 C16 -25.6(17) . . . . ? N1 C15 C16 N2 30(2) . . . . ? C17 N2 C16 C15 161.3(16) . . . . ? Ni1 N2 C16 C15 -23.0(19) . . . . ? C16 N2 C17 C18 176.0(14) . . . . ? Ni1 N2 C17 C18 1(2) . . . . ? N2 C17 C18 C19 179.3(15) . . . . ? N2 C17 C18 C23 -2(2) . . . . ? N2 C17 C18 Ru1 -95.3(18) . . . . ? C26 Ru1 C18 C19 57(2) . . . . ? C24 Ru1 C18 C19 120.8(13) . . . . ? C25 Ru1 C18 C19 81.0(12) . . . . ? C27 Ru1 C18 C19 -177.8(18) . . . . ? C28 Ru1 C18 C19 158.2(11) . . . . ? C20 Ru1 C18 C19 -31.1(10) . . . . ? C22 Ru1 C18 C19 -103.5(11) . . . . ? C21 Ru1 C18 C19 -66.6(11) . . . . ? C23 Ru1 C18 C19 -131.6(14) . . . . ? C26 Ru1 C18 C23 -171.1(15) . . . . ? C24 Ru1 C18 C23 -107.5(11) . . . . ? C25 Ru1 C18 C23 -147.4(10) . . . . ? C27 Ru1 C18 C23 -46(2) . . . . ? C28 Ru1 C18 C23 -70.1(12) . . . . ? C19 Ru1 C18 C23 131.6(14) . . . . ? C20 Ru1 C18 C23 100.6(10) . . . . ? C22 Ru1 C18 C23 28.2(8) . . . . ? C21 Ru1 C18 C23 65.0(9) . . . . ? C26 Ru1 C18 C17 -54(2) . . . . ? C24 Ru1 C18 C17 9.0(16) . . . . ? C25 Ru1 C18 C17 -30.8(16) . . . . ? C27 Ru1 C18 C17 70(2) . . . . ? C28 Ru1 C18 C17 46.5(16) . . . . ? C19 Ru1 C18 C17 -111.8(17) . . . . ? C20 Ru1 C18 C17 -142.8(15) . . . . ? C22 Ru1 C18 C17 144.8(14) . . . . ? C21 Ru1 C18 C17 -178.4(14) . . . . ? C23 Ru1 C18 C17 116.6(16) . . . . ? C23 C18 C19 C20 0(2) . . . . ? C17 C18 C19 C20 178.7(15) . . . . ? Ru1 C18 C19 C20 57.4(14) . . . . ? C23 C18 C19 Ru1 -57.3(13) . . . . ? C17 C18 C19 Ru1 121.3(14) . . . . ? C26 Ru1 C19 C18 -156.8(10) . . . . ? C24 Ru1 C19 C18 -76.5(12) . . . . ? C25 Ru1 C19 C18 -117.5(11) . . . . ? C27 Ru1 C19 C18 177(2) . . . . ? C28 Ru1 C19 C18 -46.4(18) . . . . ? C20 Ru1 C19 C18 129.6(15) . . . . ? C22 Ru1 C19 C18 65.1(9) . . . . ? C21 Ru1 C19 C18 102.0(11) . . . . ? C23 Ru1 C19 C18 29.4(9) . . . . ? C26 Ru1 C19 C20 73.7(13) . . . . ? C24 Ru1 C19 C20 153.9(12) . . . . ? C25 Ru1 C19 C20 112.9(12) . . . . ? C27 Ru1 C19 C20 48(3) . . . . ? C28 Ru1 C19 C20 -176.0(14) . . . . ? C22 Ru1 C19 C20 -64.4(10) . . . . ? C18 Ru1 C19 C20 -129.6(15) . . . . ? C21 Ru1 C19 C20 -27.6(10) . . . . ? C23 Ru1 C19 C20 -100.2(11) . . . . ? C18 C19 C20 C21 -3(3) . . . . ? Ru1 C19 C20 C21 55.2(18) . . . . ? C18 C19 C20 Ru1 -58.3(13) . . . . ? C26 Ru1 C20 C21 99.6(12) . . . . ? C24 Ru1 C20 C21 171.5(13) . . . . ? C25 Ru1 C20 C21 140.9(11) . . . . ? C27 Ru1 C20 C21 62.2(16) . . . . ? C28 Ru1 C20 C21 39(4) . . . . ? C19 Ru1 C20 C21 -133.4(16) . . . . ? C22 Ru1 C20 C21 -29.9(10) . . . . ? C18 Ru1 C20 C21 -103.3(12) . . . . ? C23 Ru1 C20 C21 -66.1(11) . . . . ? C26 Ru1 C20 C19 -127.1(11) . . . . ? C24 Ru1 C20 C19 -55.2(18) . . . . ? C25 Ru1 C20 C19 -85.7(11) . . . . ? C27 Ru1 C20 C19 -164.5(12) . . . . ? C28 Ru1 C20 C19 172(3) . . . . ? C22 Ru1 C20 C19 103.5(10) . . . . ? C18 Ru1 C20 C19 30.0(9) . . . . ? C21 Ru1 C20 C19 133.4(16) . . . . ? C23 Ru1 C20 C19 67.2(10) . . . . ? C19 C20 C21 C22 0(3) . . . . ? Ru1 C20 C21 C22 53.5(16) . . . . ? C19 C20 C21 Ru1 -53.7(16) . . . . ? C26 Ru1 C21 C20 -95.6(13) . . . . ? C24 Ru1 C21 C20 -158(4) . . . . ? C25 Ru1 C21 C20 -65.8(16) . . . . ? C27 Ru1 C21 C20 -134.6(14) . . . . ? C28 Ru1 C21 C20 -169.0(14) . . . . ? C19 Ru1 C21 C20 29.0(10) . . . . ? C22 Ru1 C21 C20 131.1(16) . . . . ? C18 Ru1 C21 C20 65.3(11) . . . . ? C23 Ru1 C21 C20 102.0(12) . . . . ? C26 Ru1 C21 C22 133.3(10) . . . . ? C24 Ru1 C21 C22 71(4) . . . . ? C25 Ru1 C21 C22 163.1(10) . . . . ? C27 Ru1 C21 C22 94.2(14) . . . . ? C28 Ru1 C21 C22 59.9(16) . . . . ? C19 Ru1 C21 C22 -102.1(10) . . . . ? C20 Ru1 C21 C22 -131.1(16) . . . . ? C18 Ru1 C21 C22 -65.8(9) . . . . ? C23 Ru1 C21 C22 -29.1(9) . . . . ? C20 C21 C22 C23 7(3) . . . . ? Ru1 C21 C22 C23 60.3(13) . . . . ? C20 C21 C22 Ru1 -53.6(16) . . . . ? C26 Ru1 C22 C23 160.8(10) . . . . ? C24 Ru1 C22 C23 63.6(13) . . . . ? C25 Ru1 C22 C23 129(4) . . . . ? C27 Ru1 C22 C23 130.8(13) . . . . ? C28 Ru1 C22 C23 90.4(14) . . . . ? C19 Ru1 C22 C23 -64.8(10) . . . . ? C20 Ru1 C22 C23 -102.2(10) . . . . ? C18 Ru1 C22 C23 -28.7(9) . . . . ? C21 Ru1 C22 C23 -131.2(14) . . . . ? C26 Ru1 C22 C21 -68.1(13) . . . . ? C24 Ru1 C22 C21 -165.3(12) . . . . ? C25 Ru1 C22 C21 -99(4) . . . . ? C27 Ru1 C22 C21 -98.1(14) . . . . ? C28 Ru1 C22 C21 -138.5(14) . . . . ? C19 Ru1 C22 C21 66.4(10) . . . . ? C20 Ru1 C22 C21 29.0(10) . . . . ? C18 Ru1 C22 C21 102.4(11) . . . . ? C23 Ru1 C22 C21 131.2(14) . . . . ? Ni1 O2 C23 C22 174.1(9) . . . . ? Ni1 O2 C23 C18 0.0(19) . . . . ? Ni1 O2 C23 Ru1 89.2(15) . . . . ? C21 C22 C23 O2 176.1(14) . . . . ? Ru1 C22 C23 O2 -125.2(11) . . . . ? C21 C22 C23 C18 -9(2) . . . . ? Ru1 C22 C23 C18 49.3(12) . . . . ? C21 C22 C23 Ru1 -58.7(14) . . . . ? C19 C18 C23 O2 -179.9(13) . . . . ? C17 C18 C23 O2 2(2) . . . . ? Ru1 C18 C23 O2 125.1(13) . . . . ? C19 C18 C23 C22 6(2) . . . . ? C17 C18 C23 C22 -172.7(13) . . . . ? Ru1 C18 C23 C22 -49.1(11) . . . . ? C19 C18 C23 Ru1 54.9(13) . . . . ? C17 C18 C23 Ru1 -123.6(14) . . . . ? C26 Ru1 C23 O2 52(3) . . . . ? C24 Ru1 C23 O2 -28.6(17) . . . . ? C25 Ru1 C23 O2 -54(2) . . . . ? C27 Ru1 C23 O2 45.0(18) . . . . ? C28 Ru1 C23 O2 8.9(18) . . . . ? C19 Ru1 C23 O2 -145.7(15) . . . . ? C20 Ru1 C23 O2 176.2(15) . . . . ? C22 Ru1 C23 O2 110.5(18) . . . . ? C18 Ru1 C23 O2 -116.6(17) . . . . ? C21 Ru1 C23 O2 140.3(16) . . . . ? C26 Ru1 C23 C22 -59(2) . . . . ? C24 Ru1 C23 C22 -139.0(11) . . . . ? C25 Ru1 C23 C22 -164.6(12) . . . . ? C27 Ru1 C23 C22 -65.4(13) . . . . ? C28 Ru1 C23 C22 -101.6(13) . . . . ? C19 Ru1 C23 C22 103.9(10) . . . . ? C20 Ru1 C23 C22 65.7(10) . . . . ? C18 Ru1 C23 C22 132.9(13) . . . . ? C21 Ru1 C23 C22 29.8(9) . . . . ? C26 Ru1 C23 C18 168(2) . . . . ? C24 Ru1 C23 C18 88.1(12) . . . . ? C25 Ru1 C23 C18 62.5(15) . . . . ? C27 Ru1 C23 C18 161.7(12) . . . . ? C28 Ru1 C23 C18 125.5(13) . . . . ? C19 Ru1 C23 C18 -29.0(9) . . . . ? C20 Ru1 C23 C18 -67.2(10) . . . . ? C22 Ru1 C23 C18 -132.9(13) . . . . ? C21 Ru1 C23 C18 -103.1(10) . . . . ? C26 Ru1 C24 C28 -80.2(15) . . . . ? C25 Ru1 C24 C28 -119.0(19) . . . . ? C27 Ru1 C24 C28 -38.7(14) . . . . ? C19 Ru1 C24 C28 158.8(16) . . . . ? C20 Ru1 C24 C28 -164.2(19) . . . . ? C22 Ru1 C24 C28 46.0(19) . . . . ? C18 Ru1 C24 C28 121.2(16) . . . . ? C21 Ru1 C24 C28 -13(5) . . . . ? C23 Ru1 C24 C28 81.8(17) . . . . ? C26 Ru1 C24 C25 38.8(10) . . . . ? C27 Ru1 C24 C25 80.4(13) . . . . ? C28 Ru1 C24 C25 119.0(19) . . . . ? C19 Ru1 C24 C25 -82.1(12) . . . . ? C20 Ru1 C24 C25 -45.1(19) . . . . ? C22 Ru1 C24 C25 165.0(10) . . . . ? C18 Ru1 C24 C25 -119.8(11) . . . . ? C21 Ru1 C24 C25 106(5) . . . . ? C23 Ru1 C24 C25 -159.2(10) . . . . ? C26 Ru1 C24 C29 152(3) . . . . ? C25 Ru1 C24 C29 113(3) . . . . ? C27 Ru1 C24 C29 -167(3) . . . . ? C28 Ru1 C24 C29 -128(3) . . . . ? C19 Ru1 C24 C29 31(2) . . . . ? C20 Ru1 C24 C29 68(3) . . . . ? C22 Ru1 C24 C29 -82(3) . . . . ? C18 Ru1 C24 C29 -7(2) . . . . ? C21 Ru1 C24 C29 -142(3) . . . . ? C23 Ru1 C24 C29 -46(2) . . . . ? C28 C24 C25 C26 2(2) . . . . ? C29 C24 C25 C26 178.3(14) . . . . ? Ru1 C24 C25 C26 -62.0(11) . . . . ? C28 C24 C25 C30 -173.6(19) . . . . ? C29 C24 C25 C30 3(3) . . . . ? Ru1 C24 C25 C30 122.2(19) . . . . ? C28 C24 C25 Ru1 64.2(15) . . . . ? C29 C24 C25 Ru1 -119.7(14) . . . . ? C24 Ru1 C25 C26 115.1(15) . . . . ? C27 Ru1 C25 C26 36.2(12) . . . . ? C28 Ru1 C25 C26 79.6(13) . . . . ? C19 Ru1 C25 C26 -127.4(12) . . . . ? C20 Ru1 C25 C26 -86.4(13) . . . . ? C22 Ru1 C25 C26 38(5) . . . . ? C18 Ru1 C25 C26 -166.3(11) . . . . ? C21 Ru1 C25 C26 -48.2(17) . . . . ? C23 Ru1 C25 C26 154.2(13) . . . . ? C26 Ru1 C25 C24 -115.1(15) . . . . ? C27 Ru1 C25 C24 -78.9(14) . . . . ? C28 Ru1 C25 C24 -35.5(13) . . . . ? C19 Ru1 C25 C24 117.5(12) . . . . ? C20 Ru1 C25 C24 158.4(12) . . . . ? C22 Ru1 C25 C24 -77(5) . . . . ? C18 Ru1 C25 C24 78.6(13) . . . . ? C21 Ru1 C25 C24 -163.3(14) . . . . ? C23 Ru1 C25 C24 39.0(17) . . . . ? C26 Ru1 C25 C30 115(2) . . . . ? C24 Ru1 C25 C30 -129(3) . . . . ? C27 Ru1 C25 C30 152(2) . . . . ? C28 Ru1 C25 C30 -165(2) . . . . ? C19 Ru1 C25 C30 -12(2) . . . . ? C20 Ru1 C25 C30 29(2) . . . . ? C22 Ru1 C25 C30 153(3) . . . . ? C18 Ru1 C25 C30 -51(2) . . . . ? C21 Ru1 C25 C30 67(2) . . . . ? C23 Ru1 C25 C30 -90(2) . . . . ? C24 C25 C26 C27 -1(2) . . . . ? C30 C25 C26 C27 175.0(17) . . . . ? Ru1 C25 C26 C27 -63.4(14) . . . . ? C24 C25 C26 C31 -172.9(16) . . . . ? C30 C25 C26 C31 3(3) . . . . ? Ru1 C25 C26 C31 125.0(17) . . . . ? C24 C25 C26 Ru1 62.0(11) . . . . ? C30 C25 C26 Ru1 -121.6(15) . . . . ? C24 Ru1 C26 C27 79.5(14) . . . . ? C25 Ru1 C26 C27 118.4(18) . . . . ? C28 Ru1 C26 C27 38.5(12) . . . . ? C19 Ru1 C26 C27 -168.3(14) . . . . ? C20 Ru1 C26 C27 -129.1(15) . . . . ? C22 Ru1 C26 C27 -53.1(17) . . . . ? C18 Ru1 C26 C27 151.5(19) . . . . ? C21 Ru1 C26 C27 -90.4(15) . . . . ? C23 Ru1 C26 C27 -9(3) . . . . ? C24 Ru1 C26 C25 -39.0(11) . . . . ? C27 Ru1 C26 C25 -118.4(18) . . . . ? C28 Ru1 C26 C25 -79.9(12) . . . . ? C19 Ru1 C26 C25 73.3(14) . . . . ? C20 Ru1 C26 C25 112.5(13) . . . . ? C22 Ru1 C26 C25 -171.5(11) . . . . ? C18 Ru1 C26 C25 33(2) . . . . ? C21 Ru1 C26 C25 151.2(12) . . . . ? C23 Ru1 C26 C25 -127(2) . . . . ? C24 Ru1 C26 C31 -155(3) . . . . ? C25 Ru1 C26 C31 -116(3) . . . . ? C27 Ru1 C26 C31 126(3) . . . . ? C28 Ru1 C26 C31 164(3) . . . . ? C19 Ru1 C26 C31 -42(2) . . . . ? C20 Ru1 C26 C31 -3(2) . . . . ? C22 Ru1 C26 C31 73(2) . . . . ? C18 Ru1 C26 C31 -83(3) . . . . ? C21 Ru1 C26 C31 36(2) . . . . ? C23 Ru1 C26 C31 117(3) . . . . ? C25 C26 C27 C28 0(2) . . . . ? C31 C26 C27 C28 170.9(19) . . . . ? Ru1 C26 C27 C28 -62.5(16) . . . . ? C25 C26 C27 C32 -175(2) . . . . ? C31 C26 C27 C32 -4(4) . . . . ? Ru1 C26 C27 C32 122(2) . . . . ? C25 C26 C27 Ru1 62.6(13) . . . . ? C31 C26 C27 Ru1 -127(2) . . . . ? C24 Ru1 C27 C26 -80.6(13) . . . . ? C25 Ru1 C27 C26 -37.5(12) . . . . ? C28 Ru1 C27 C26 -117.1(18) . . . . ? C19 Ru1 C27 C26 35(3) . . . . ? C20 Ru1 C27 C26 70.9(15) . . . . ? C22 Ru1 C27 C26 142.8(13) . . . . ? C18 Ru1 C27 C26 -150.2(18) . . . . ? C21 Ru1 C27 C26 103.9(13) . . . . ? C23 Ru1 C27 C26 176.9(11) . . . . ? C26 Ru1 C27 C28 117.1(18) . . . . ? C24 Ru1 C27 C28 36.5(11) . . . . ? C25 Ru1 C27 C28 79.6(12) . . . . ? C19 Ru1 C27 C28 152(2) . . . . ? C20 Ru1 C27 C28 -172.0(12) . . . . ? C22 Ru1 C27 C28 -100.1(13) . . . . ? C18 Ru1 C27 C28 -33(3) . . . . ? C21 Ru1 C27 C28 -138.9(13) . . . . ? C23 Ru1 C27 C28 -66.0(14) . . . . ? C26 Ru1 C27 C32 -124(4) . . . . ? C24 Ru1 C27 C32 155(4) . . . . ? C25 Ru1 C27 C32 -162(4) . . . . ? C28 Ru1 C27 C32 119(4) . . . . ? C19 Ru1 C27 C32 -90(4) . . . . ? C20 Ru1 C27 C32 -53(4) . . . . ? C22 Ru1 C27 C32 19(3) . . . . ? C18 Ru1 C27 C32 86(4) . . . . ? C21 Ru1 C27 C32 -20(3) . . . . ? C23 Ru1 C27 C32 53(4) . . . . ? C25 C24 C28 C27 -2(2) . . . . ? C29 C24 C28 C27 -177.6(17) . . . . ? Ru1 C24 C28 C27 60.6(16) . . . . ? C25 C24 C28 C33 178.7(17) . . . . ? C29 C24 C28 C33 3(3) . . . . ? Ru1 C24 C28 C33 -119(2) . . . . ? C25 C24 C28 Ru1 -62.7(13) . . . . ? C29 C24 C28 Ru1 121.8(19) . . . . ? C26 C27 C28 C24 1(3) . . . . ? C32 C27 C28 C24 176.9(18) . . . . ? Ru1 C27 C28 C24 -60.4(15) . . . . ? C26 C27 C28 C33 -180(2) . . . . ? C32 C27 C28 C33 -4(4) . . . . ? Ru1 C27 C28 C33 119(3) . . . . ? C26 C27 C28 Ru1 61.6(15) . . . . ? C32 C27 C28 Ru1 -123(2) . . . . ? C26 Ru1 C28 C24 80.3(13) . . . . ? C25 Ru1 C28 C24 37.3(12) . . . . ? C27 Ru1 C28 C24 117.1(18) . . . . ? C19 Ru1 C28 C24 -45(2) . . . . ? C20 Ru1 C28 C24 146(3) . . . . ? C22 Ru1 C28 C24 -149.8(14) . . . . ? C18 Ru1 C28 C24 -76.1(15) . . . . ? C21 Ru1 C28 C24 176.7(12) . . . . ? C23 Ru1 C28 C24 -112.0(15) . . . . ? C26 Ru1 C28 C27 -36.8(12) . . . . ? C24 Ru1 C28 C27 -117.1(18) . . . . ? C25 Ru1 C28 C27 -79.7(13) . . . . ? C19 Ru1 C28 C27 -162.1(16) . . . . ? C20 Ru1 C28 C27 29(4) . . . . ? C22 Ru1 C28 C27 93.2(14) . . . . ? C18 Ru1 C28 C27 166.8(13) . . . . ? C21 Ru1 C28 C27 59.7(16) . . . . ? C23 Ru1 C28 C27 130.9(14) . . . . ? C26 Ru1 C28 C33 -165(4) . . . . ? C24 Ru1 C28 C33 115(4) . . . . ? C25 Ru1 C28 C33 152(4) . . . . ? C27 Ru1 C28 C33 -128(4) . . . . ? C19 Ru1 C28 C33 70(3) . . . . ? C20 Ru1 C28 C33 -99(5) . . . . ? C22 Ru1 C28 C33 -35(3) . . . . ? C18 Ru1 C28 C33 39(3) . . . . ? C21 Ru1 C28 C33 -68(4) . . . . ? C23 Ru1 C28 C33 3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.821 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.130 data_aimfl11ab1 _database_code_depnum_ccdc_archive 'CCDC 640626' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H22 Fe N2 Ni O2' _chemical_formula_sum 'C23 H22 Fe N2 Ni O2' _chemical_formula_weight 472.99 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' 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' _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+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0723(10) _cell_length_b 9.9509(9) _cell_length_c 18.5611(17) _cell_angle_alpha 90.00 _cell_angle_beta 106.6370(10) _cell_angle_gamma 90.00 _cell_volume 1959.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 998 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 28.11 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.685 _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 16092 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.11 _reflns_number_total 4434 _reflns_number_gt 3470 _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 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^)+(0.0730P)^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 4434 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Fe1 Fe 0.14069(3) 0.36882(3) 0.14483(2) 0.04283(14) Uani 1 1 d . . . Ni1 Ni 0.52727(3) 0.13937(3) 0.058009(17) 0.03727(12) Uani 1 1 d . . . N1 N 0.50070(19) 0.2612(2) -0.02042(11) 0.0432(5) Uani 1 1 d . . . N2 N 0.67513(19) 0.0945(2) 0.03689(11) 0.0411(5) Uani 1 1 d . . . O1 O 0.37636(15) 0.17459(17) 0.07812(9) 0.0443(4) Uani 1 1 d . . . O2 O 0.55582(14) 0.02445(17) 0.13942(9) 0.0423(4) Uani 1 1 d . . . C1 C 0.2984(3) 0.4811(3) 0.18370(17) 0.0592(7) Uani 1 1 d . . . H1 H 0.3729 0.4782 0.1652 0.071 Uiso 1 1 calc R . . C2 C 0.1929(3) 0.5651(3) 0.1563(2) 0.0696(9) Uani 1 1 d . . . H2 H 0.1807 0.6315 0.1159 0.083 Uiso 1 1 calc R . . C3 C 0.1088(3) 0.5364(4) 0.1986(2) 0.0815(11) Uani 1 1 d . . . H3 H 0.0267 0.5791 0.1921 0.098 Uiso 1 1 calc R . . C4 C 0.1613(3) 0.4357(5) 0.25063(19) 0.0805(11) Uani 1 1 d . . . H4 H 0.1235 0.3962 0.2875 0.097 Uiso 1 1 calc R . . C5 C 0.2787(3) 0.4030(4) 0.24104(18) 0.0683(9) Uani 1 1 d . . . H5 H 0.3371 0.3353 0.2699 0.082 Uiso 1 1 calc R . . C6 C 0.1713(2) 0.2496(3) 0.06298(14) 0.0452(6) Uani 1 1 d . . . C7 C 0.0597(3) 0.3289(3) 0.03411(16) 0.0546(7) Uani 1 1 d . . . H7 H 0.0450 0.3939 -0.0072 0.065 Uiso 1 1 calc R . . C8 C -0.0246(3) 0.2985(3) 0.07657(17) 0.0612(8) Uani 1 1 d . . . H8 H -0.1078 0.3391 0.0697 0.073 Uiso 1 1 calc R . . C9 C 0.0315(3) 0.2008(3) 0.13052(19) 0.0603(7) Uani 1 1 d . . . H9 H -0.0055 0.1613 0.1677 0.072 Uiso 1 1 calc R . . C10 C 0.1513(3) 0.1701(3) 0.12160(17) 0.0531(7) Uani 1 1 d . . . H10 H 0.2118 0.1061 0.1523 0.064 Uiso 1 1 calc R . . C11 C 0.2877(2) 0.2519(2) 0.03979(13) 0.0419(5) Uani 1 1 d . . . C12 C 0.2965(3) 0.3321(3) -0.01853(15) 0.0485(6) Uani 1 1 d . . . H12 H 0.2279 0.3866 -0.0412 0.058 Uiso 1 1 calc R . . C13 C 0.4018(3) 0.3379(2) -0.04656(14) 0.0467(6) Uani 1 1 d . . . C14 C 0.3957(3) 0.4393(3) -0.10784(18) 0.0665(8) Uani 1 1 d . . . H14A H 0.4636 0.5024 -0.0912 0.100 Uiso 1 1 calc R . . H14B H 0.3167 0.4862 -0.1192 0.100 Uiso 1 1 calc R . . H14C H 0.4028 0.3939 -0.1521 0.100 Uiso 1 1 calc R . . C15 C 0.6092(3) 0.2760(3) -0.05008(16) 0.0544(7) Uani 1 1 d . . . H15A H 0.6616 0.3504 -0.0255 0.065 Uiso 1 1 calc R . . H15B H 0.5809 0.2939 -0.1037 0.065 Uiso 1 1 calc R . . C16 C 0.6832(3) 0.1469(2) -0.03517(15) 0.0486(6) Uani 1 1 d . . . H16A H 0.6482 0.0825 -0.0749 0.058 Uiso 1 1 calc R . . H16B H 0.7705 0.1634 -0.0331 0.058 Uiso 1 1 calc R . . C17 C 0.7628(2) 0.0156(2) 0.07460(14) 0.0432(6) Uani 1 1 d . . . H17 H 0.8318 0.0021 0.0564 0.052 Uiso 1 1 calc R . . C18 C 0.7623(2) -0.0527(2) 0.14183(14) 0.0419(5) Uani 1 1 d . . . C19 C 0.8674(3) -0.1313(3) 0.17949(17) 0.0522(7) Uani 1 1 d . . . H19 H 0.9372 -0.1332 0.1611 0.063 Uiso 1 1 calc R . . C20 C 0.8701(3) -0.2042(3) 0.24156(16) 0.0580(7) Uani 1 1 d . . . H20 H 0.9402 -0.2557 0.2654 0.070 Uiso 1 1 calc R . . C21 C 0.7646(3) -0.2000(3) 0.26887(14) 0.0528(7) Uani 1 1 d . . . H21 H 0.7647 -0.2501 0.3112 0.063 Uiso 1 1 calc R . . C22 C 0.6624(3) -0.1242(2) 0.23484(15) 0.0481(6) Uani 1 1 d . . . H22 H 0.5942 -0.1230 0.2546 0.058 Uiso 1 1 calc R . . C23 C 0.6571(2) -0.0469(2) 0.17002(13) 0.0398(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 Fe1 0.0353(2) 0.0435(2) 0.0498(2) -0.00490(15) 0.01237(17) -0.00186(14) Ni1 0.0373(2) 0.0360(2) 0.03682(19) -0.00091(12) 0.00789(14) 0.00076(11) N1 0.0491(12) 0.0397(11) 0.0396(11) 0.0014(9) 0.0108(9) -0.0022(9) N2 0.0402(11) 0.0427(11) 0.0392(11) -0.0055(9) 0.0092(9) -0.0082(9) O1 0.0426(9) 0.0445(9) 0.0451(9) 0.0065(8) 0.0117(8) 0.0113(8) O2 0.0368(9) 0.0470(10) 0.0420(9) 0.0044(8) 0.0096(7) 0.0065(7) C1 0.0460(16) 0.0635(18) 0.074(2) -0.0160(16) 0.0257(14) -0.0182(14) C2 0.072(2) 0.0461(17) 0.093(2) -0.0107(16) 0.0282(19) -0.0111(15) C3 0.0552(19) 0.077(2) 0.120(3) -0.052(2) 0.037(2) -0.0113(17) C4 0.067(2) 0.123(3) 0.058(2) -0.031(2) 0.0280(17) -0.033(2) C5 0.0533(18) 0.087(2) 0.0548(18) -0.0104(16) 0.0004(15) -0.0184(16) C6 0.0436(14) 0.0400(13) 0.0477(14) -0.0057(11) 0.0063(11) 0.0060(11) C7 0.0472(16) 0.0524(15) 0.0545(16) -0.0057(13) -0.0007(13) 0.0120(12) C8 0.0361(14) 0.0631(19) 0.077(2) -0.0175(16) 0.0045(14) -0.0019(13) C9 0.0488(16) 0.0524(17) 0.080(2) -0.0056(16) 0.0193(15) -0.0117(13) C10 0.0488(15) 0.0397(13) 0.0697(19) 0.0012(13) 0.0154(14) -0.0003(12) C11 0.0436(13) 0.0360(12) 0.0407(13) -0.0075(10) 0.0038(11) 0.0048(10) C12 0.0525(15) 0.0415(13) 0.0456(14) 0.0042(11) 0.0047(12) 0.0103(12) C13 0.0607(17) 0.0381(13) 0.0372(13) -0.0024(10) 0.0076(12) 0.0012(12) C14 0.084(2) 0.0555(18) 0.0595(18) 0.0152(15) 0.0198(16) 0.0066(16) C15 0.0594(17) 0.0510(16) 0.0543(16) 0.0057(13) 0.0190(13) -0.0085(13) C16 0.0509(15) 0.0525(15) 0.0456(14) -0.0018(12) 0.0188(12) -0.0086(12) C17 0.0360(13) 0.0437(13) 0.0493(14) -0.0093(11) 0.0111(11) -0.0026(10) C18 0.0378(13) 0.0395(13) 0.0454(13) -0.0055(11) 0.0070(10) 0.0006(10) C19 0.0398(14) 0.0570(17) 0.0582(17) 0.0020(13) 0.0118(13) 0.0099(11) C20 0.0499(16) 0.0541(17) 0.0628(18) 0.0009(14) 0.0047(14) 0.0172(13) C21 0.0598(17) 0.0490(15) 0.0435(15) 0.0045(12) 0.0050(13) 0.0105(13) C22 0.0447(15) 0.0507(16) 0.0489(15) 0.0052(12) 0.0136(12) 0.0042(11) C23 0.0396(13) 0.0347(12) 0.0411(12) -0.0027(10) 0.0049(10) 0.0009(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 Fe1 C5 2.019(3) . ? Fe1 C4 2.023(3) . ? Fe1 C1 2.024(3) . ? Fe1 C3 2.026(3) . ? Fe1 C8 2.029(3) . ? Fe1 C2 2.031(3) . ? Fe1 C6 2.031(2) . ? Fe1 C7 2.032(3) . ? Fe1 C10 2.034(3) . ? Fe1 C9 2.035(3) . ? Ni1 N2 1.844(2) . ? Ni1 O1 1.8470(17) . ? Ni1 O2 1.8486(16) . ? Ni1 N1 1.8522(19) . ? N1 C13 1.308(3) . ? N1 C15 1.466(3) . ? N2 C17 1.288(3) . ? N2 C16 1.462(3) . ? O1 C11 1.290(3) . ? O2 C23 1.311(3) . ? C1 C5 1.385(4) . ? C1 C2 1.408(4) . ? C2 C3 1.407(5) . ? C3 C4 1.398(5) . ? C4 C5 1.400(5) . ? C6 C10 1.413(4) . ? C6 C7 1.434(3) . ? C6 C11 1.471(3) . ? C7 C8 1.416(4) . ? C8 C9 1.406(4) . ? C9 C10 1.416(4) . ? C11 C12 1.371(4) . ? C12 C13 1.408(4) . ? C13 C14 1.508(4) . ? C15 C16 1.506(4) . ? C17 C18 1.422(3) . ? C18 C23 1.409(3) . ? C18 C19 1.410(3) . ? C19 C20 1.354(4) . ? C20 C21 1.401(4) . ? C21 C22 1.356(4) . ? C22 C23 1.415(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 C5 Fe1 C4 40.52(13) . . ? C5 Fe1 C1 40.05(13) . . ? C4 Fe1 C1 68.07(13) . . ? C5 Fe1 C3 67.67(16) . . ? C4 Fe1 C3 40.40(16) . . ? C1 Fe1 C3 67.92(12) . . ? C5 Fe1 C8 158.32(14) . . ? C4 Fe1 C8 123.39(13) . . ? C1 Fe1 C8 160.90(14) . . ? C3 Fe1 C8 109.79(13) . . ? C5 Fe1 C2 67.94(15) . . ? C4 Fe1 C2 68.41(16) . . ? C1 Fe1 C2 40.63(12) . . ? C3 Fe1 C2 40.60(14) . . ? C8 Fe1 C2 125.19(13) . . ? C5 Fe1 C6 120.92(12) . . ? C4 Fe1 C6 157.12(15) . . ? C1 Fe1 C6 106.11(11) . . ? C3 Fe1 C6 159.94(16) . . ? C8 Fe1 C6 69.21(11) . . ? C2 Fe1 C6 122.50(13) . . ? C5 Fe1 C7 158.49(13) . . ? C4 Fe1 C7 160.08(14) . . ? C1 Fe1 C7 123.66(13) . . ? C3 Fe1 C7 124.78(15) . . ? C8 Fe1 C7 40.81(12) . . ? C2 Fe1 C7 108.93(14) . . ? C6 Fe1 C7 41.34(10) . . ? C5 Fe1 C10 106.02(14) . . ? C4 Fe1 C10 121.86(16) . . ? C1 Fe1 C10 121.04(12) . . ? C3 Fe1 C10 158.98(15) . . ? C8 Fe1 C10 68.21(12) . . ? C2 Fe1 C10 157.69(13) . . ? C6 Fe1 C10 40.67(11) . . ? C7 Fe1 C10 68.36(12) . . ? C5 Fe1 C9 121.64(14) . . ? C4 Fe1 C9 107.12(14) . . ? C1 Fe1 C9 156.84(13) . . ? C3 Fe1 C9 124.05(14) . . ? C8 Fe1 C9 40.47(12) . . ? C2 Fe1 C9 160.77(13) . . ? C6 Fe1 C9 69.05(12) . . ? C7 Fe1 C9 68.52(13) . . ? C10 Fe1 C9 40.73(11) . . ? N2 Ni1 O1 176.85(8) . . ? N2 Ni1 O2 94.00(8) . . ? O1 Ni1 O2 84.55(7) . . ? N2 Ni1 N1 86.69(9) . . ? O1 Ni1 N1 94.89(8) . . ? O2 Ni1 N1 177.30(8) . . ? C13 N1 C15 119.4(2) . . ? C13 N1 Ni1 126.94(18) . . ? C15 N1 Ni1 113.47(16) . . ? C17 N2 C16 118.7(2) . . ? C17 N2 Ni1 127.47(18) . . ? C16 N2 Ni1 113.51(17) . . ? C11 O1 Ni1 126.30(17) . . ? C23 O2 Ni1 127.87(16) . . ? C5 C1 C2 108.3(3) . . ? C5 C1 Fe1 69.79(16) . . ? C2 C1 Fe1 69.94(16) . . ? C3 C2 C1 107.0(3) . . ? C3 C2 Fe1 69.51(18) . . ? C1 C2 Fe1 69.43(16) . . ? C4 C3 C2 108.7(3) . . ? C4 C3 Fe1 69.71(19) . . ? C2 C3 Fe1 69.89(17) . . ? C3 C4 C5 107.2(3) . . ? C3 C4 Fe1 69.89(19) . . ? C5 C4 Fe1 69.58(18) . . ? C1 C5 C4 108.9(3) . . ? C1 C5 Fe1 70.16(17) . . ? C4 C5 Fe1 69.90(18) . . ? C10 C6 C7 106.7(2) . . ? C10 C6 C11 125.3(2) . . ? C7 C6 C11 128.0(2) . . ? C10 C6 Fe1 69.79(15) . . ? C7 C6 Fe1 69.37(15) . . ? C11 C6 Fe1 123.86(17) . . ? C8 C7 C6 108.0(3) . . ? C8 C7 Fe1 69.48(17) . . ? C6 C7 Fe1 69.29(15) . . ? C9 C8 C7 108.5(3) . . ? C9 C8 Fe1 69.99(15) . . ? C7 C8 Fe1 69.71(15) . . ? C8 C9 C10 107.7(3) . . ? C8 C9 Fe1 69.54(16) . . ? C10 C9 Fe1 69.60(16) . . ? C6 C10 C9 109.1(3) . . ? C6 C10 Fe1 69.54(15) . . ? C9 C10 Fe1 69.67(16) . . ? O1 C11 C12 124.6(2) . . ? O1 C11 C6 114.9(2) . . ? C12 C11 C6 120.5(2) . . ? C11 C12 C13 124.7(2) . . ? N1 C13 C12 122.2(2) . . ? N1 C13 C14 121.5(3) . . ? C12 C13 C14 116.3(2) . . ? N1 C15 C16 107.8(2) . . ? N2 C16 C15 107.4(2) . . ? N2 C17 C18 125.2(2) . . ? C23 C18 C19 119.4(2) . . ? C23 C18 C17 121.2(2) . . ? C19 C18 C17 119.4(2) . . ? C20 C19 C18 122.2(3) . . ? C19 C20 C21 118.3(2) . . ? C22 C21 C20 121.3(3) . . ? C21 C22 C23 121.6(3) . . ? O2 C23 C18 123.9(2) . . ? O2 C23 C22 119.0(2) . . ? C18 C23 C22 117.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C13 176.5(2) . . . . ? O1 Ni1 N1 C13 -0.7(2) . . . . ? O2 Ni1 N1 C13 -78.7(18) . . . . ? N2 Ni1 N1 C15 -8.41(17) . . . . ? O1 Ni1 N1 C15 174.32(17) . . . . ? O2 Ni1 N1 C15 96.3(17) . . . . ? O1 Ni1 N2 C17 -66.5(15) . . . . ? O2 Ni1 N2 C17 -4.1(2) . . . . ? N1 Ni1 N2 C17 173.3(2) . . . . ? O1 Ni1 N2 C16 107.1(15) . . . . ? O2 Ni1 N2 C16 169.56(16) . . . . ? N1 Ni1 N2 C16 -13.06(17) . . . . ? N2 Ni1 O1 C11 -114.5(15) . . . . ? O2 Ni1 O1 C11 -177.11(19) . . . . ? N1 Ni1 O1 C11 5.5(2) . . . . ? N2 Ni1 O2 C23 6.22(19) . . . . ? O1 Ni1 O2 C23 -176.58(19) . . . . ? N1 Ni1 O2 C23 -98.4(17) . . . . ? C4 Fe1 C1 C5 37.4(2) . . . . ? C3 Fe1 C1 C5 81.1(2) . . . . ? C8 Fe1 C1 C5 168.0(3) . . . . ? C2 Fe1 C1 C5 119.3(3) . . . . ? C6 Fe1 C1 C5 -119.2(2) . . . . ? C7 Fe1 C1 C5 -160.89(19) . . . . ? C10 Fe1 C1 C5 -77.6(2) . . . . ? C9 Fe1 C1 C5 -44.9(4) . . . . ? C5 Fe1 C1 C2 -119.3(3) . . . . ? C4 Fe1 C1 C2 -82.0(2) . . . . ? C3 Fe1 C1 C2 -38.2(2) . . . . ? C8 Fe1 C1 C2 48.6(4) . . . . ? C6 Fe1 C1 C2 121.5(2) . . . . ? C7 Fe1 C1 C2 79.8(2) . . . . ? C10 Fe1 C1 C2 163.1(2) . . . . ? C9 Fe1 C1 C2 -164.2(3) . . . . ? C5 C1 C2 C3 0.2(3) . . . . ? Fe1 C1 C2 C3 59.6(2) . . . . ? C5 C1 C2 Fe1 -59.5(2) . . . . ? C5 Fe1 C2 C3 -81.0(2) . . . . ? C4 Fe1 C2 C3 -37.2(2) . . . . ? C1 Fe1 C2 C3 -118.2(3) . . . . ? C8 Fe1 C2 C3 79.3(3) . . . . ? C6 Fe1 C2 C3 165.5(2) . . . . ? C7 Fe1 C2 C3 121.8(2) . . . . ? C10 Fe1 C2 C3 -159.2(3) . . . . ? C9 Fe1 C2 C3 42.9(5) . . . . ? C5 Fe1 C2 C1 37.25(19) . . . . ? C4 Fe1 C2 C1 81.1(2) . . . . ? C3 Fe1 C2 C1 118.2(3) . . . . ? C8 Fe1 C2 C1 -162.52(18) . . . . ? C6 Fe1 C2 C1 -76.3(2) . . . . ? C7 Fe1 C2 C1 -120.0(2) . . . . ? C10 Fe1 C2 C1 -41.0(4) . . . . ? C9 Fe1 C2 C1 161.1(4) . . . . ? C1 C2 C3 C4 -0.5(4) . . . . ? Fe1 C2 C3 C4 59.1(2) . . . . ? C1 C2 C3 Fe1 -59.6(2) . . . . ? C5 Fe1 C3 C4 -38.2(2) . . . . ? C1 Fe1 C3 C4 -81.7(2) . . . . ? C8 Fe1 C3 C4 118.7(2) . . . . ? C2 Fe1 C3 C4 -119.9(3) . . . . ? C6 Fe1 C3 C4 -157.9(3) . . . . ? C7 Fe1 C3 C4 161.82(19) . . . . ? C10 Fe1 C3 C4 38.1(4) . . . . ? C9 Fe1 C3 C4 75.8(2) . . . . ? C5 Fe1 C3 C2 81.7(2) . . . . ? C4 Fe1 C3 C2 119.9(3) . . . . ? C1 Fe1 C3 C2 38.3(2) . . . . ? C8 Fe1 C3 C2 -121.4(2) . . . . ? C6 Fe1 C3 C2 -38.0(5) . . . . ? C7 Fe1 C3 C2 -78.3(3) . . . . ? C10 Fe1 C3 C2 158.0(3) . . . . ? C9 Fe1 C3 C2 -164.3(2) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? Fe1 C3 C4 C5 59.8(2) . . . . ? C2 C3 C4 Fe1 -59.2(2) . . . . ? C5 Fe1 C4 C3 118.2(3) . . . . ? C1 Fe1 C4 C3 81.2(2) . . . . ? C8 Fe1 C4 C3 -81.4(2) . . . . ? C2 Fe1 C4 C3 37.3(2) . . . . ? C6 Fe1 C4 C3 160.6(3) . . . . ? C7 Fe1 C4 C3 -48.8(5) . . . . ? C10 Fe1 C4 C3 -164.91(18) . . . . ? C9 Fe1 C4 C3 -122.8(2) . . . . ? C1 Fe1 C4 C5 -37.0(2) . . . . ? C3 Fe1 C4 C5 -118.2(3) . . . . ? C8 Fe1 C4 C5 160.4(2) . . . . ? C2 Fe1 C4 C5 -80.9(2) . . . . ? C6 Fe1 C4 C5 42.4(4) . . . . ? C7 Fe1 C4 C5 -167.0(4) . . . . ? C10 Fe1 C4 C5 76.9(2) . . . . ? C9 Fe1 C4 C5 119.0(2) . . . . ? C2 C1 C5 C4 0.2(3) . . . . ? Fe1 C1 C5 C4 -59.4(2) . . . . ? C2 C1 C5 Fe1 59.6(2) . . . . ? C3 C4 C5 C1 -0.5(4) . . . . ? Fe1 C4 C5 C1 59.5(2) . . . . ? C3 C4 C5 Fe1 -60.0(2) . . . . ? C4 Fe1 C5 C1 -119.9(3) . . . . ? C3 Fe1 C5 C1 -81.8(2) . . . . ? C8 Fe1 C5 C1 -169.4(3) . . . . ? C2 Fe1 C5 C1 -37.77(19) . . . . ? C6 Fe1 C5 C1 77.9(2) . . . . ? C7 Fe1 C5 C1 48.0(5) . . . . ? C10 Fe1 C5 C1 119.48(19) . . . . ? C9 Fe1 C5 C1 160.97(18) . . . . ? C1 Fe1 C5 C4 119.9(3) . . . . ? C3 Fe1 C5 C4 38.1(2) . . . . ? C8 Fe1 C5 C4 -49.4(5) . . . . ? C2 Fe1 C5 C4 82.1(3) . . . . ? C6 Fe1 C5 C4 -162.2(2) . . . . ? C7 Fe1 C5 C4 167.9(3) . . . . ? C10 Fe1 C5 C4 -120.6(2) . . . . ? C9 Fe1 C5 C4 -79.1(3) . . . . ? C5 Fe1 C6 C10 78.3(2) . . . . ? C4 Fe1 C6 C10 47.5(4) . . . . ? C1 Fe1 C6 C10 119.17(17) . . . . ? C3 Fe1 C6 C10 -171.3(3) . . . . ? C8 Fe1 C6 C10 -80.37(18) . . . . ? C2 Fe1 C6 C10 160.35(18) . . . . ? C7 Fe1 C6 C10 -117.8(2) . . . . ? C9 Fe1 C6 C10 -36.92(16) . . . . ? C5 Fe1 C6 C7 -163.95(19) . . . . ? C4 Fe1 C6 C7 165.3(3) . . . . ? C1 Fe1 C6 C7 -123.04(19) . . . . ? C3 Fe1 C6 C7 -53.5(4) . . . . ? C8 Fe1 C6 C7 37.43(18) . . . . ? C2 Fe1 C6 C7 -81.9(2) . . . . ? C10 Fe1 C6 C7 117.8(2) . . . . ? C9 Fe1 C6 C7 80.88(19) . . . . ? C5 Fe1 C6 C11 -41.3(3) . . . . ? C4 Fe1 C6 C11 -72.1(4) . . . . ? C1 Fe1 C6 C11 -0.4(2) . . . . ? C3 Fe1 C6 C11 69.1(4) . . . . ? C8 Fe1 C6 C11 160.0(2) . . . . ? C2 Fe1 C6 C11 40.7(3) . . . . ? C7 Fe1 C6 C11 122.6(3) . . . . ? C10 Fe1 C6 C11 -119.6(3) . . . . ? C9 Fe1 C6 C11 -156.5(2) . . . . ? C10 C6 C7 C8 1.2(3) . . . . ? C11 C6 C7 C8 -176.3(2) . . . . ? Fe1 C6 C7 C8 -58.88(19) . . . . ? C10 C6 C7 Fe1 60.09(18) . . . . ? C11 C6 C7 Fe1 -117.5(3) . . . . ? C5 Fe1 C7 C8 159.9(4) . . . . ? C4 Fe1 C7 C8 -43.6(5) . . . . ? C1 Fe1 C7 C8 -164.99(18) . . . . ? C3 Fe1 C7 C8 -80.0(2) . . . . ? C2 Fe1 C7 C8 -122.35(19) . . . . ? C6 Fe1 C7 C8 119.6(2) . . . . ? C10 Fe1 C7 C8 81.29(19) . . . . ? C9 Fe1 C7 C8 37.33(17) . . . . ? C5 Fe1 C7 C6 40.3(4) . . . . ? C4 Fe1 C7 C6 -163.2(4) . . . . ? C1 Fe1 C7 C6 75.4(2) . . . . ? C3 Fe1 C7 C6 160.38(18) . . . . ? C8 Fe1 C7 C6 -119.6(2) . . . . ? C2 Fe1 C7 C6 118.04(18) . . . . ? C10 Fe1 C7 C6 -38.33(16) . . . . ? C9 Fe1 C7 C6 -82.28(18) . . . . ? C6 C7 C8 C9 -0.7(3) . . . . ? Fe1 C7 C8 C9 -59.47(19) . . . . ? C6 C7 C8 Fe1 58.76(18) . . . . ? C5 Fe1 C8 C9 -40.5(4) . . . . ? C4 Fe1 C8 C9 -76.7(3) . . . . ? C1 Fe1 C8 C9 160.8(3) . . . . ? C3 Fe1 C8 C9 -119.7(2) . . . . ? C2 Fe1 C8 C9 -162.47(19) . . . . ? C6 Fe1 C8 C9 81.71(19) . . . . ? C7 Fe1 C8 C9 119.6(2) . . . . ? C10 Fe1 C8 C9 37.93(18) . . . . ? C5 Fe1 C8 C7 -160.1(3) . . . . ? C4 Fe1 C8 C7 163.7(2) . . . . ? C1 Fe1 C8 C7 41.2(4) . . . . ? C3 Fe1 C8 C7 120.7(2) . . . . ? C2 Fe1 C8 C7 77.9(2) . . . . ? C6 Fe1 C8 C7 -37.90(16) . . . . ? C10 Fe1 C8 C7 -81.68(18) . . . . ? C9 Fe1 C8 C7 -119.6(2) . . . . ? C7 C8 C9 C10 -0.1(3) . . . . ? Fe1 C8 C9 C10 -59.37(19) . . . . ? C7 C8 C9 Fe1 59.29(19) . . . . ? C5 Fe1 C9 C8 163.63(19) . . . . ? C4 Fe1 C9 C8 121.7(2) . . . . ? C1 Fe1 C9 C8 -164.1(3) . . . . ? C3 Fe1 C9 C8 80.6(2) . . . . ? C2 Fe1 C9 C8 48.4(5) . . . . ? C6 Fe1 C9 C8 -82.14(19) . . . . ? C7 Fe1 C9 C8 -37.64(17) . . . . ? C10 Fe1 C9 C8 -119.0(3) . . . . ? C5 Fe1 C9 C10 -77.4(2) . . . . ? C4 Fe1 C9 C10 -119.3(2) . . . . ? C1 Fe1 C9 C10 -45.1(4) . . . . ? C3 Fe1 C9 C10 -160.4(2) . . . . ? C8 Fe1 C9 C10 119.0(3) . . . . ? C2 Fe1 C9 C10 167.4(4) . . . . ? C6 Fe1 C9 C10 36.86(17) . . . . ? C7 Fe1 C9 C10 81.36(19) . . . . ? C7 C6 C10 C9 -1.3(3) . . . . ? C11 C6 C10 C9 176.4(2) . . . . ? Fe1 C6 C10 C9 58.55(19) . . . . ? C7 C6 C10 Fe1 -59.82(17) . . . . ? C11 C6 C10 Fe1 117.8(2) . . . . ? C8 C9 C10 C6 0.9(3) . . . . ? Fe1 C9 C10 C6 -58.48(18) . . . . ? C8 C9 C10 Fe1 59.33(19) . . . . ? C5 Fe1 C10 C6 -119.09(17) . . . . ? C4 Fe1 C10 C6 -160.27(16) . . . . ? C1 Fe1 C10 C6 -78.26(19) . . . . ? C3 Fe1 C10 C6 171.7(3) . . . . ? C8 Fe1 C10 C6 83.03(17) . . . . ? C2 Fe1 C10 C6 -48.3(4) . . . . ? C7 Fe1 C10 C6 38.95(15) . . . . ? C9 Fe1 C10 C6 120.7(2) . . . . ? C5 Fe1 C10 C9 120.2(2) . . . . ? C4 Fe1 C10 C9 79.0(2) . . . . ? C1 Fe1 C10 C9 161.01(19) . . . . ? C3 Fe1 C10 C9 51.0(4) . . . . ? C8 Fe1 C10 C9 -37.69(18) . . . . ? C2 Fe1 C10 C9 -169.1(3) . . . . ? C6 Fe1 C10 C9 -120.7(2) . . . . ? C7 Fe1 C10 C9 -81.8(2) . . . . ? Ni1 O1 C11 C12 -7.0(3) . . . . ? Ni1 O1 C11 C6 173.06(15) . . . . ? C10 C6 C11 O1 -0.7(3) . . . . ? C7 C6 C11 O1 176.5(2) . . . . ? Fe1 C6 C11 O1 87.3(2) . . . . ? C10 C6 C11 C12 179.4(3) . . . . ? C7 C6 C11 C12 -3.5(4) . . . . ? Fe1 C6 C11 C12 -92.7(3) . . . . ? O1 C11 C12 C13 2.4(4) . . . . ? C6 C11 C12 C13 -177.7(2) . . . . ? C15 N1 C13 C12 -177.6(2) . . . . ? Ni1 N1 C13 C12 -2.8(4) . . . . ? C15 N1 C13 C14 1.4(4) . . . . ? Ni1 N1 C13 C14 176.14(19) . . . . ? C11 C12 C13 N1 2.8(4) . . . . ? C11 C12 C13 C14 -176.2(3) . . . . ? C13 N1 C15 C16 -157.9(2) . . . . ? Ni1 N1 C15 C16 26.6(3) . . . . ? C17 N2 C16 C15 -155.5(2) . . . . ? Ni1 N2 C16 C15 30.2(2) . . . . ? N1 C15 C16 N2 -35.1(3) . . . . ? C16 N2 C17 C18 -174.0(2) . . . . ? Ni1 N2 C17 C18 -0.7(3) . . . . ? N2 C17 C18 C23 5.3(4) . . . . ? N2 C17 C18 C19 -177.0(2) . . . . ? C23 C18 C19 C20 1.2(4) . . . . ? C17 C18 C19 C20 -176.6(2) . . . . ? C18 C19 C20 C21 -0.3(4) . . . . ? C19 C20 C21 C22 -0.6(4) . . . . ? C20 C21 C22 C23 0.5(4) . . . . ? Ni1 O2 C23 C18 -3.6(3) . . . . ? Ni1 O2 C23 C22 176.93(17) . . . . ? C19 C18 C23 O2 179.2(2) . . . . ? C17 C18 C23 O2 -3.0(4) . . . . ? C19 C18 C23 C22 -1.3(3) . . . . ? C17 C18 C23 C22 176.4(2) . . . . ? C21 C22 C23 O2 179.9(2) . . . . ? C21 C22 C23 C18 0.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.014 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.104