# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wu Dayu' _publ_contact_author_email 'WUDAYU NJU@YAHOO.COM.CN' _publ_section_title ; An S = 3 Cyanide-Bridged Tetranuclear FeIII2NiII2 Square that Exhibits Slow Relaxation of the Magnetization: Synthesis, Structure and Magnetic Property ; loop_ _publ_author_name 'Wu Dayu' 'Wei Huang' 'Osamu Sato' # Attachment 'cif.txt.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 714488' #TrackingRef 'cif.txt.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 B Cl Fe N17 Ni O8' _chemical_formula_weight 989.59 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 12.812(3) _cell_length_b 14.131(3) _cell_length_c 14.936(3) _cell_angle_alpha 69.05(3) _cell_angle_beta 68.80(3) _cell_angle_gamma 85.95(3) _cell_volume 2349.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7272 _cell_measurement_theta_min 3.0957 _cell_measurement_theta_max 27.8764 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7749 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Molybdenum _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 15610 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8101 _reflns_number_gt 7270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1240P)^2^+7.4789P] 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 8101 _refine_ls_number_parameters 627 _refine_ls_number_restraints 158 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.2763 _refine_ls_wR_factor_gt 0.2673 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -1.15215(7) -0.96285(7) 0.82634(7) 0.0344(3) Uani 1 1 d . . . Ni1 Ni -0.79443(6) -0.80700(7) 0.80615(6) 0.0384(3) Uani 1 1 d . . . C1 C -0.5691(7) -0.7979(9) 0.8186(6) 0.072(3) Uani 1 1 d . . . H1A H -0.5773 -0.8675 0.8344 0.086 Uiso 1 1 calc R . . C2 C -0.4687(7) -0.7564(12) 0.8047(7) 0.100(5) Uani 1 1 d . . . H2A H -0.4102 -0.7982 0.8108 0.121 Uiso 1 1 calc R . . C3 C -0.4533(10) -0.6583(15) 0.7828(9) 0.130(7) Uani 1 1 d . . . H3A H -0.3841 -0.6301 0.7712 0.156 Uiso 1 1 calc R . . C4 C -0.5410(12) -0.5995(12) 0.7776(8) 0.119(6) Uani 1 1 d . . . H4A H -0.5323 -0.5302 0.7632 0.143 Uiso 1 1 calc R . . C5 C -0.6478(9) -0.6439(10) 0.7943(6) 0.079(3) Uani 1 1 d . . . C6 C -0.8518(9) -0.6137(7) 0.8473(6) 0.069(3) Uani 1 1 d . . . C7 C -0.9266(11) -0.5411(7) 0.8752(8) 0.085(3) Uani 1 1 d . . . H7A H -0.9007 -0.4738 0.8539 0.102 Uiso 1 1 calc R . . C8 C -1.0345(10) -0.5704(9) 0.9325(9) 0.088(3) Uani 1 1 d . . . H8A H -1.0839 -0.5241 0.9528 0.106 Uiso 1 1 calc R . . C9 C -1.0711(8) -0.6669(8) 0.9606(7) 0.069(2) Uani 1 1 d . . . H9A H -1.1460 -0.6881 1.0006 0.083 Uiso 1 1 calc R . . C10 C -0.9984(6) -0.7329(6) 0.9302(6) 0.0530(19) Uani 1 1 d . . . H10A H -1.0253 -0.7996 0.9508 0.064 Uiso 1 1 calc R . . C11 C -0.8405(6) -0.6339(6) 0.6398(6) 0.0500(18) Uani 1 1 d . . . H11A H -0.9141 -0.6490 0.6862 0.060 Uiso 1 1 calc R . . C12 C -0.8169(8) -0.5459(6) 0.5583(6) 0.063(2) Uani 1 1 d . . . H12A H -0.8725 -0.5021 0.5477 0.076 Uiso 1 1 calc R . . C13 C -0.7051(9) -0.5234(8) 0.4904(7) 0.075(3) Uani 1 1 d . . . H13A H -0.6847 -0.4616 0.4357 0.090 Uiso 1 1 calc R . . C14 C -0.6265(8) -0.5910(7) 0.5038(6) 0.062(2) Uani 1 1 d . . . H14A H -0.5523 -0.5769 0.4586 0.074 Uiso 1 1 calc R . . C15 C -0.6602(7) -0.6820(7) 0.5872(6) 0.0538(19) Uani 1 1 d . . . C16 C -0.6049(6) -0.8587(6) 0.6450(5) 0.0485(18) Uani 1 1 d . . . C17 C -0.5320(6) -0.9205(7) 0.6015(6) 0.060(2) Uani 1 1 d . . . H17A H -0.4693 -0.8923 0.5424 0.072 Uiso 1 1 calc R . . C18 C -0.5530(8) -1.0234(8) 0.6461(7) 0.067(2) Uani 1 1 d . . . H18A H -0.5045 -1.0659 0.6177 0.081 Uiso 1 1 calc R . . C19 C -0.6488(8) -1.0650(7) 0.7357(6) 0.062(2) Uani 1 1 d . . . H19A H -0.6664 -1.1347 0.7667 0.075 Uiso 1 1 calc R . . C20 C -0.7142(6) -0.9983(6) 0.7746(6) 0.0462(17) Uani 1 1 d . . . H20A H -0.7767 -1.0246 0.8344 0.055 Uiso 1 1 calc R . . C21 C -1.1660(5) -1.0418(5) 0.9648(5) 0.0379(15) Uani 1 1 d . . . C22 C -1.0143(5) -0.9031(5) 0.8094(5) 0.0352(14) Uani 1 1 d . . . C23 C -1.2232(5) -0.8606(6) 0.8785(5) 0.0456(18) Uani 1 1 d . . . C24 C -1.1833(8) -1.1241(7) 0.4644(7) 0.067(2) Uani 1 1 d . . . H24A H -1.1534 -1.1285 0.3994 0.081 Uiso 1 1 calc R . . C25 C -1.2693(9) -1.1859(8) 0.5513(7) 0.076(3) Uani 1 1 d . . . H25A H -1.3071 -1.2400 0.5518 0.091 Uiso 1 1 calc R . . C26 C -1.2914(6) -1.1601(6) 0.6320(5) 0.0471(18) Uani 1 1 d . . . H26A H -1.3447 -1.1912 0.6973 0.056 Uiso 1 1 calc R . . C27 C -1.1342(6) -0.7807(6) 0.6354(6) 0.0500(18) Uani 1 1 d . . . H27A H -1.1129 -0.7323 0.6555 0.060 Uiso 1 1 calc R . . C28 C -1.1591(8) -0.7596(7) 0.5484(7) 0.064(2) Uani 1 1 d . . . H28A H -1.1568 -0.6959 0.4993 0.077 Uiso 1 1 calc R . . C29 C -1.1879(6) -0.8507(6) 0.5486(5) 0.0498(18) Uani 1 1 d . . . H29A H -1.2112 -0.8603 0.5001 0.060 Uiso 1 1 calc R . . C30 C -0.9939(6) -1.1245(6) 0.7881(6) 0.0464(17) Uani 1 1 d . . . H30A H -0.9569 -1.1235 0.8310 0.056 Uiso 1 1 calc R . . C31 C -0.9712(7) -1.1869(6) 0.7319(6) 0.0547(19) Uani 1 1 d . . . H31A H -0.9176 -1.2347 0.7293 0.066 Uiso 1 1 calc R . . C32 C -1.0436(6) -1.1641(6) 0.6809(6) 0.0465(17) Uani 1 1 d . . . H32A H -1.0494 -1.1944 0.6367 0.056 Uiso 1 1 calc R . . C33 C -1.3921(5) -1.0508(6) 0.9273(5) 0.0456(18) Uani 1 1 d . . . H33A H -1.4073 -1.0370 0.9870 0.055 Uiso 1 1 calc R . . C34 C -1.4664(6) -1.1010(7) 0.9078(6) 0.057(2) Uani 1 1 d . . . H34A H -1.5392 -1.1268 0.9512 0.068 Uiso 1 1 calc R . . C35 C -1.4108(6) -1.1048(7) 0.8119(6) 0.055(2) Uani 1 1 d . . . H35A H -1.4398 -1.1327 0.7773 0.066 Uiso 1 1 calc R . . N1 N -0.7378(8) -0.5849(6) 0.7932(5) 0.075(2) Uani 1 1 d . . . H1B H -0.7216 -0.5221 0.7540 0.090 Uiso 1 1 calc R . . N2 N -0.6572(5) -0.7409(6) 0.8102(5) 0.0571(18) Uani 1 1 d . . . N3 N -0.8884(5) -0.7074(5) 0.8714(4) 0.0483(15) Uani 1 1 d . . . N4 N -0.5830(5) -0.7546(5) 0.5963(5) 0.0510(16) Uani 1 1 d . . . H4B H -0.5135 -0.7328 0.5687 0.061 Uiso 1 1 calc R . . N5 N -0.6940(4) -0.8966(5) 0.7319(4) 0.0418(14) Uani 1 1 d . . . N6 N -0.7642(4) -0.7013(5) 0.6579(4) 0.0406(13) Uani 1 1 d . . . N7 N -1.1789(4) -1.0891(5) 1.0486(4) 0.0450(14) Uani 1 1 d . . . N8 N -0.9329(4) -0.8675(4) 0.8027(4) 0.0343(12) Uani 1 1 d . . . N9 N -1.2652(5) -0.8011(6) 0.9135(6) 0.0625(19) Uani 1 1 d . . . N10 N -1.1766(4) -0.9239(4) 0.6307(4) 0.0390(13) Uani 1 1 d . . . N11 N -1.1448(4) -0.8802(4) 0.6864(4) 0.0394(13) Uani 1 1 d . . . N12 N -1.0746(4) -1.0666(4) 0.7728(4) 0.0367(12) Uani 1 1 d . . . N13 N -1.1057(4) -1.0901(4) 0.7056(4) 0.0383(12) Uani 1 1 d . . . N14 N -1.2954(4) -1.0258(5) 0.8468(4) 0.0398(13) Uani 1 1 d . . . N15 N -1.3070(4) -1.0608(4) 0.7765(4) 0.0396(13) Uani 1 1 d . . . N16 N -1.1540(8) -1.0565(8) 0.4977(6) 0.094(3) Uani 1 1 d . . . N17 N -1.2201(5) -1.0784(5) 0.6000(4) 0.0472(15) Uani 1 1 d . . . B2 B -1.2057(6) -1.0378(7) 0.6760(5) 0.0412(18) Uani 1 1 d . . . Cl1 Cl -1.6496(3) -1.2952(3) 0.6571(3) 0.0644(11) Uani 0.695(7) 1 d PDU A 1 O11 O -1.5452(6) -1.2775(9) 0.6624(8) 0.097(3) Uani 0.695(7) 1 d PDU A 1 O12 O -1.7238(9) -1.3579(8) 0.7541(6) 0.101(4) Uani 0.695(7) 1 d PDU A 1 O13 O -1.6361(7) -1.3407(7) 0.5793(7) 0.074(3) Uani 0.695(7) 1 d PDU A 1 O14 O -1.6938(7) -1.2008(5) 0.6216(6) 0.061(2) Uani 0.695(7) 1 d PDU A 1 Cl1A Cl -1.6996(6) -1.3244(5) 0.6555(6) 0.062(2) Uani 0.305(7) 1 d PDU A 2 O14A O -1.8029(11) -1.3581(12) 0.6619(13) 0.058(5) Uani 0.305(7) 1 d PDU A 2 O13A O -1.6277(13) -1.3989(11) 0.6898(17) 0.092(7) Uani 0.305(7) 1 d PDU A 2 O12A O -1.7346(19) -1.2854(19) 0.7416(15) 0.098(7) Uiso 0.305(7) 1 d PDU A 2 O11A O -1.6406(18) -1.2438(17) 0.5658(16) 0.158(12) Uani 0.305(7) 1 d PDU A 2 O3W O -1.1238(11) -0.5233(14) 0.6822(11) 0.239(9) Uani 1 1 d . . . C1W C -1.2444(15) -0.3118(16) 0.9367(11) 0.135(6) Uani 1 1 d . . . O2W O -1.3956(19) -0.6359(16) 1.053(2) 0.330(14) Uani 1 1 d . . . O1W O -1.3128(17) -0.419(4) 0.977(2) 0.49(4) Uani 1 1 d . . . O4W O -1.201(3) -0.4245(17) 0.786(5) 0.66(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 0.0187(5) 0.0559(6) 0.0330(5) -0.0195(4) -0.0093(4) -0.0046(4) Ni1 0.0225(4) 0.0630(6) 0.0314(5) -0.0186(4) -0.0070(3) -0.0117(4) C1 0.038(4) 0.134(8) 0.032(4) -0.014(5) -0.011(3) -0.026(5) C2 0.031(5) 0.203(14) 0.052(5) -0.022(7) -0.011(4) -0.050(7) C3 0.068(8) 0.240(18) 0.071(7) -0.020(9) -0.031(6) -0.096(10) C4 0.124(11) 0.162(12) 0.058(6) -0.011(7) -0.023(7) -0.115(10) C5 0.067(6) 0.122(9) 0.041(5) -0.030(5) -0.001(4) -0.061(6) C6 0.083(7) 0.080(6) 0.047(5) -0.026(4) -0.017(4) -0.025(5) C7 0.139(11) 0.053(5) 0.068(6) -0.033(5) -0.026(6) -0.021(6) C8 0.092(8) 0.085(7) 0.090(8) -0.051(6) -0.014(6) -0.004(6) C9 0.059(5) 0.087(7) 0.068(6) -0.046(5) -0.013(4) 0.011(5) C10 0.046(4) 0.067(5) 0.049(4) -0.028(4) -0.012(4) 0.002(4) C11 0.034(4) 0.064(5) 0.051(4) -0.026(4) -0.008(3) 0.004(3) C12 0.071(6) 0.056(5) 0.048(5) -0.013(4) -0.011(4) 0.005(4) C13 0.078(7) 0.070(6) 0.053(5) -0.005(4) -0.010(5) -0.012(5) C14 0.054(5) 0.068(5) 0.049(5) -0.016(4) -0.003(4) -0.019(4) C15 0.046(4) 0.076(5) 0.041(4) -0.021(4) -0.014(3) -0.016(4) C16 0.029(3) 0.079(5) 0.041(4) -0.020(4) -0.016(3) -0.001(3) C17 0.035(4) 0.091(7) 0.045(4) -0.022(4) -0.008(3) 0.011(4) C18 0.058(5) 0.102(7) 0.054(5) -0.047(5) -0.018(4) 0.029(5) C19 0.071(6) 0.069(5) 0.049(5) -0.019(4) -0.024(4) 0.001(4) C20 0.036(4) 0.064(5) 0.044(4) -0.023(4) -0.016(3) 0.003(3) C21 0.020(3) 0.059(4) 0.037(4) -0.020(3) -0.010(3) -0.006(3) C22 0.025(3) 0.053(4) 0.029(3) -0.018(3) -0.006(3) -0.001(3) C23 0.017(3) 0.085(5) 0.042(4) -0.030(4) -0.010(3) -0.008(3) C24 0.072(6) 0.098(7) 0.049(5) -0.044(5) -0.023(4) -0.002(5) C25 0.086(7) 0.084(6) 0.070(6) -0.032(5) -0.030(5) -0.027(5) C26 0.041(4) 0.064(5) 0.034(4) -0.022(3) -0.003(3) -0.023(3) C27 0.042(4) 0.061(5) 0.050(4) -0.022(4) -0.017(3) 0.000(3) C28 0.068(6) 0.069(6) 0.052(5) -0.013(4) -0.028(4) 0.014(4) C29 0.047(4) 0.068(5) 0.034(4) -0.016(3) -0.016(3) -0.001(4) C30 0.033(4) 0.059(4) 0.049(4) -0.018(3) -0.018(3) -0.001(3) C31 0.047(4) 0.052(4) 0.065(5) -0.031(4) -0.011(4) 0.005(3) C32 0.038(4) 0.055(4) 0.046(4) -0.026(3) -0.007(3) 0.002(3) C33 0.021(3) 0.087(5) 0.035(3) -0.034(4) -0.003(3) -0.009(3) C34 0.028(3) 0.102(6) 0.048(4) -0.040(4) -0.003(3) -0.023(4) C35 0.026(3) 0.099(6) 0.043(4) -0.034(4) -0.002(3) -0.021(4) N1 0.094(6) 0.076(5) 0.050(4) -0.020(4) -0.012(4) -0.045(5) N2 0.039(4) 0.094(5) 0.035(3) -0.019(3) -0.009(3) -0.025(4) N3 0.047(4) 0.062(4) 0.036(3) -0.024(3) -0.005(3) -0.018(3) N4 0.026(3) 0.073(4) 0.041(3) -0.013(3) -0.003(3) -0.012(3) N5 0.022(3) 0.071(4) 0.032(3) -0.017(3) -0.011(2) -0.003(3) N6 0.027(3) 0.063(4) 0.031(3) -0.020(3) -0.003(2) -0.013(3) N7 0.021(3) 0.075(4) 0.032(3) -0.014(3) -0.004(2) -0.013(3) N8 0.022(3) 0.052(3) 0.033(3) -0.018(2) -0.010(2) -0.001(2) N9 0.027(3) 0.099(5) 0.077(5) -0.060(5) -0.006(3) -0.003(3) N10 0.026(3) 0.061(4) 0.034(3) -0.021(3) -0.012(2) -0.001(2) N11 0.030(3) 0.055(4) 0.039(3) -0.020(3) -0.015(2) -0.002(2) N12 0.026(3) 0.054(3) 0.031(3) -0.013(2) -0.011(2) -0.008(2) N13 0.029(3) 0.053(3) 0.034(3) -0.019(3) -0.007(2) -0.009(2) N14 0.023(3) 0.068(4) 0.035(3) -0.024(3) -0.009(2) -0.008(2) N15 0.027(3) 0.065(4) 0.033(3) -0.022(3) -0.011(2) -0.008(2) N16 0.086(6) 0.131(8) 0.057(5) -0.034(5) -0.010(4) -0.017(6) N17 0.047(3) 0.065(4) 0.034(3) -0.027(3) -0.007(3) -0.013(3) B2 0.032(4) 0.063(5) 0.027(4) -0.015(3) -0.007(3) -0.016(3) Cl1 0.044(2) 0.062(2) 0.069(2) -0.0260(17) 0.0055(16) -0.0083(16) O11 0.055(6) 0.136(9) 0.101(8) -0.038(7) -0.035(5) 0.009(6) O12 0.124(9) 0.076(7) 0.062(6) -0.005(5) 0.001(6) -0.041(6) O13 0.046(5) 0.071(6) 0.099(7) -0.036(5) -0.011(5) -0.017(4) O14 0.060(5) 0.063(5) 0.056(5) -0.024(4) -0.013(4) 0.001(4) Cl1A 0.032(4) 0.037(4) 0.088(5) 0.000(3) -0.010(4) 0.000(3) O14A 0.062(11) 0.054(10) 0.069(11) -0.026(8) -0.033(9) 0.005(8) O13A 0.075(12) 0.029(8) 0.116(13) 0.011(9) -0.008(11) -0.002(8) O11A 0.095(15) 0.133(17) 0.127(17) 0.049(16) 0.000(14) 0.001(15) O3W 0.122(10) 0.32(2) 0.180(12) 0.062(13) -0.090(9) -0.014(11) C1W 0.106(12) 0.228(19) 0.076(8) -0.068(10) -0.019(8) -0.023(12) O2W 0.26(2) 0.27(2) 0.62(5) -0.22(3) -0.29(3) 0.079(18) O1W 0.134(17) 1.16(12) 0.28(3) -0.39(5) -0.064(17) 0.10(3) O4W 0.33(3) 0.20(2) 1.48(15) -0.27(5) -0.42(6) 0.16(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 Fe1 C22 1.905(6) . ? Fe1 C23 1.906(8) . ? Fe1 C21 1.915(7) . ? Fe1 N12 1.958(6) . ? Fe1 N11 1.967(6) . ? Fe1 N14 1.970(5) . ? Ni1 N8 2.047(5) . ? Ni1 N5 2.057(6) . ? Ni1 N7 2.058(6) 2_337 ? Ni1 N3 2.067(6) . ? Ni1 N2 2.078(6) . ? Ni1 N6 2.093(6) . ? C1 N2 1.357(12) . ? C1 C2 1.367(12) . ? C1 H1A 0.9300 . ? C2 C3 1.32(2) . ? C2 H2A 0.9300 . ? C3 C4 1.36(2) . ? C3 H3A 0.9300 . ? C4 C5 1.446(13) . ? C4 H4A 0.9300 . ? C5 N2 1.310(13) . ? C5 N1 1.376(14) . ? C6 N3 1.316(10) . ? C6 N1 1.396(12) . ? C6 C7 1.422(15) . ? C7 C8 1.337(15) . ? C7 H7A 0.9300 . ? C8 C9 1.339(14) . ? C8 H8A 0.9300 . ? C9 C10 1.349(11) . ? C9 H9A 0.9300 . ? C10 N3 1.355(9) . ? C10 H10A 0.9300 . ? C11 N6 1.345(9) . ? C11 C12 1.351(11) . ? C11 H11A 0.9300 . ? C12 C13 1.401(13) . ? C12 H12A 0.9300 . ? C13 C14 1.357(14) . ? C13 H13A 0.9300 . ? C14 C15 1.392(11) . ? C14 H14A 0.9300 . ? C15 N6 1.339(9) . ? C15 N4 1.380(10) . ? C16 N5 1.339(9) . ? C16 C17 1.381(11) . ? C16 N4 1.384(10) . ? C17 C18 1.365(13) . ? C17 H17A 0.9300 . ? C18 C19 1.412(13) . ? C18 H18A 0.9300 . ? C19 C20 1.362(11) . ? C19 H19A 0.9300 . ? C20 N5 1.349(9) . ? C20 H20A 0.9300 . ? C21 N7 1.144(9) . ? C22 N8 1.146(8) . ? C23 N9 1.147(10) . ? C24 N16 1.351(12) . ? C24 C25 1.396(13) . ? C24 H24A 0.9300 . ? C25 C26 1.312(11) . ? C25 H25A 0.9300 . ? C26 N17 1.353(9) . ? C26 H26A 0.9300 . ? C27 N11 1.328(9) . ? C27 C28 1.374(11) . ? C27 H27A 0.9300 . ? C28 C29 1.362(12) . ? C28 H28A 0.9300 . ? C29 N10 1.340(9) . ? C29 H29A 0.9300 . ? C30 N12 1.307(9) . ? C30 C31 1.373(10) . ? C30 H30A 0.9300 . ? C31 C32 1.355(11) . ? C31 H31A 0.9300 . ? C32 N13 1.345(9) . ? C32 H32A 0.9300 . ? C33 N14 1.336(8) . ? C33 C34 1.393(9) . ? C33 H33A 0.9300 . ? C34 C35 1.369(10) . ? C34 H34A 0.9300 . ? C35 N15 1.344(8) . ? C35 H35A 0.9300 . ? N1 H1B 0.8600 . ? N4 H4B 0.8600 . ? N7 Ni1 2.058(6) 2_337 ? N10 N11 1.374(7) . ? N10 B2 1.521(10) . ? N12 N13 1.350(7) . ? N13 B2 1.557(10) . ? N14 N15 1.366(7) . ? N15 B2 1.532(9) . ? N16 N17 1.383(9) . ? N17 B2 1.510(9) . ? Cl1 O14 1.409(7) . ? Cl1 O12 1.412(7) . ? Cl1 O11 1.413(7) . ? Cl1 O13 1.472(7) . ? Cl1A O14A 1.397(9) . ? Cl1A O11A 1.401(9) . ? Cl1A O13A 1.427(9) . ? Cl1A O12A 1.487(9) . ? C1W O1W 1.60(5) . ? 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 C22 Fe1 C23 86.4(3) . . ? C22 Fe1 C21 87.9(3) . . ? C23 Fe1 C21 86.2(3) . . ? C22 Fe1 N12 91.8(2) . . ? C23 Fe1 N12 178.2(2) . . ? C21 Fe1 N12 93.5(3) . . ? C22 Fe1 N11 93.8(2) . . ? C23 Fe1 N11 92.0(3) . . ? C21 Fe1 N11 177.5(2) . . ? N12 Fe1 N11 88.4(2) . . ? C22 Fe1 N14 178.9(2) . . ? C23 Fe1 N14 93.3(2) . . ? C21 Fe1 N14 91.0(2) . . ? N12 Fe1 N14 88.5(2) . . ? N11 Fe1 N14 87.3(2) . . ? N8 Ni1 N5 90.2(2) . . ? N8 Ni1 N7 90.9(2) . 2_337 ? N5 Ni1 N7 94.6(2) . 2_337 ? N8 Ni1 N3 92.0(2) . . ? N5 Ni1 N3 175.6(2) . . ? N7 Ni1 N3 89.1(2) 2_337 . ? N8 Ni1 N2 177.8(3) . . ? N5 Ni1 N2 91.8(3) . . ? N7 Ni1 N2 89.8(2) 2_337 . ? N3 Ni1 N2 86.0(3) . . ? N8 Ni1 N6 90.0(2) . . ? N5 Ni1 N6 84.8(2) . . ? N7 Ni1 N6 179.0(2) 2_337 . ? N3 Ni1 N6 91.4(2) . . ? N2 Ni1 N6 89.4(2) . . ? N2 C1 C2 122.2(11) . . ? N2 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C3 C2 C1 121.1(13) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C2 C3 C4 118.4(9) . . ? C2 C3 H3A 120.8 . . ? C4 C3 H3A 120.8 . . ? C3 C4 C5 120.4(13) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? N2 C5 N1 120.8(7) . . ? N2 C5 C4 119.0(13) . . ? N1 C5 C4 120.2(12) . . ? N3 C6 N1 119.5(9) . . ? N3 C6 C7 121.1(9) . . ? N1 C6 C7 119.5(9) . . ? C8 C7 C6 119.3(9) . . ? C8 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? C7 C8 C9 119.7(10) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C8 C9 C10 119.3(9) . . ? C8 C9 H9A 120.3 . . ? C10 C9 H9A 120.3 . . ? C9 C10 N3 123.7(8) . . ? C9 C10 H10A 118.1 . . ? N3 C10 H10A 118.1 . . ? N6 C11 C12 124.1(7) . . ? N6 C11 H11A 118.0 . . ? C12 C11 H11A 118.0 . . ? C11 C12 C13 117.2(9) . . ? C11 C12 H12A 121.4 . . ? C13 C12 H12A 121.4 . . ? C14 C13 C12 120.5(8) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 118.0(8) . . ? C13 C14 H14A 121.0 . . ? C15 C14 H14A 121.0 . . ? N6 C15 N4 119.4(7) . . ? N6 C15 C14 122.3(8) . . ? N4 C15 C14 118.3(7) . . ? N5 C16 C17 122.0(8) . . ? N5 C16 N4 120.0(7) . . ? C17 C16 N4 118.0(7) . . ? C18 C17 C16 119.4(7) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 119.6(8) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C20 C19 C18 116.9(8) . . ? C20 C19 H19A 121.5 . . ? C18 C19 H19A 121.5 . . ? N5 C20 C19 124.1(7) . . ? N5 C20 H20A 117.9 . . ? C19 C20 H20A 117.9 . . ? N7 C21 Fe1 177.3(6) . . ? N8 C22 Fe1 177.6(5) . . ? N9 C23 Fe1 177.2(7) . . ? N16 C24 C25 103.3(7) . . ? N16 C24 H24A 128.3 . . ? C25 C24 H24A 128.3 . . ? C26 C25 C24 113.4(8) . . ? C26 C25 H25A 123.3 . . ? C24 C25 H25A 123.3 . . ? C25 C26 N17 105.3(7) . . ? C25 C26 H26A 127.4 . . ? N17 C26 H26A 127.4 . . ? N11 C27 C28 110.1(7) . . ? N11 C27 H27A 125.0 . . ? C28 C27 H27A 125.0 . . ? C29 C28 C27 106.2(8) . . ? C29 C28 H28A 126.9 . . ? C27 C28 H28A 126.9 . . ? N10 C29 C28 108.1(7) . . ? N10 C29 H29A 125.9 . . ? C28 C29 H29A 125.9 . . ? N12 C30 C31 110.6(7) . . ? N12 C30 H30A 124.7 . . ? C31 C30 H30A 124.7 . . ? C32 C31 C30 105.5(7) . . ? C32 C31 H31A 127.3 . . ? C30 C31 H31A 127.3 . . ? N13 C32 C31 107.9(6) . . ? N13 C32 H32A 126.1 . . ? C31 C32 H32A 126.1 . . ? N14 C33 C34 109.3(6) . . ? N14 C33 H33A 125.4 . . ? C34 C33 H33A 125.4 . . ? C35 C34 C33 106.2(6) . . ? C35 C34 H34A 126.9 . . ? C33 C34 H34A 126.9 . . ? N15 C35 C34 107.9(6) . . ? N15 C35 H35A 126.1 . . ? C34 C35 H35A 126.1 . . ? C5 N1 C6 128.4(8) . . ? C5 N1 H1B 115.8 . . ? C6 N1 H1B 115.8 . . ? C5 N2 C1 118.8(8) . . ? C5 N2 Ni1 122.3(7) . . ? C1 N2 Ni1 118.4(6) . . ? C6 N3 C10 116.8(8) . . ? C6 N3 Ni1 123.1(6) . . ? C10 N3 Ni1 119.4(5) . . ? C15 N4 C16 127.3(6) . . ? C15 N4 H4B 116.4 . . ? C16 N4 H4B 116.4 . . ? C16 N5 C20 117.9(7) . . ? C16 N5 Ni1 122.8(5) . . ? C20 N5 Ni1 119.2(4) . . ? C15 N6 C11 117.5(7) . . ? C15 N6 Ni1 120.3(5) . . ? C11 N6 Ni1 120.1(4) . . ? C21 N7 Ni1 171.2(6) . 2_337 ? C22 N8 Ni1 174.4(5) . . ? C29 N10 N11 109.1(6) . . ? C29 N10 B2 132.1(6) . . ? N11 N10 B2 118.2(5) . . ? C27 N11 N10 106.4(5) . . ? C27 N11 Fe1 132.7(5) . . ? N10 N11 Fe1 119.6(4) . . ? C30 N12 N13 106.9(6) . . ? C30 N12 Fe1 133.9(5) . . ? N13 N12 Fe1 119.2(4) . . ? C32 N13 N12 109.1(6) . . ? C32 N13 B2 131.2(6) . . ? N12 N13 B2 119.5(5) . . ? C33 N14 N15 106.9(5) . . ? C33 N14 Fe1 130.9(4) . . ? N15 N14 Fe1 122.0(4) . . ? C35 N15 N14 109.7(5) . . ? C35 N15 B2 134.5(6) . . ? N14 N15 B2 115.7(5) . . ? C24 N16 N17 108.8(8) . . ? C26 N17 N16 109.2(6) . . ? C26 N17 B2 121.0(6) . . ? N16 N17 B2 128.6(6) . . ? N17 B2 N10 112.6(6) . . ? N17 B2 N15 114.7(5) . . ? N10 B2 N15 107.9(6) . . ? N17 B2 N13 107.4(6) . . ? N10 B2 N13 107.3(5) . . ? N15 B2 N13 106.6(5) . . ? O14 Cl1 O12 111.2(6) . . ? O14 Cl1 O11 108.6(6) . . ? O12 Cl1 O11 110.6(7) . . ? O14 Cl1 O13 104.7(5) . . ? O12 Cl1 O13 110.3(6) . . ? O11 Cl1 O13 111.4(6) . . ? O14A Cl1A O11A 116.3(12) . . ? O14A Cl1A O13A 118.1(10) . . ? O11A Cl1A O13A 112.4(11) . . ? O14A Cl1A O12A 101.5(10) . . ? O11A Cl1A O12A 107.1(13) . . ? O13A Cl1A O12A 98.2(11) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.210 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.106