Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_990624c _database_code_CSD 158045 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cheng, Peng' 'Fu, Xue-Qi' 'Jiang, Zong-Hui' 'Li, Jing' 'Liao, Dai-Zheng' 'Yan, Shi-Ping' 'Yin, Li-Hua' _publ_contact_author_name 'Professor Peng Cheng' _publ_contact_author_address ; Professor Peng Cheng Department of Chemistry Nankai University Tianjin 300071, P. R. China ; _publ_contact_author_email 'pcheng@nankai.edu.cn' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H61 Cl2 Fe N10 Ni O20 P2' _chemical_formula_weight 1489.59 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' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.3028(15) _cell_length_b 20.5989(19) _cell_length_c 20.1296(19) _cell_angle_alpha 90.00 _cell_angle_beta 111.796(2) _cell_angle_gamma 90.00 _cell_volume 6661.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3076 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8712 _exptl_absorpt_correction_T_max 0.9325 _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 '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 27433 _diffrn_reflns_av_R_equivalents 0.0971 _diffrn_reflns_av_sigmaI/netI 0.1216 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11663 _reflns_number_gt 5111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1000P)^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 11663 _refine_ls_number_parameters 874 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1739 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.2145 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 2.296 _refine_ls_shift/su_mean 0.113 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 Ni1 Ni 0.30366(5) 0.33537(4) 0.85276(5) 0.0566(3) Uani 1 1 d . . . Fe1 Fe 0.26861(6) 0.18479(4) 0.93629(5) 0.0528(3) Uani 1 1 d . . . P1 P 0.15265(12) 0.14439(9) 0.76586(10) 0.0617(5) Uani 1 1 d . . . N1 N 0.4042(4) 0.3118(3) 0.8177(3) 0.0643(15) Uani 1 1 d . . . N2 N 0.3685(4) 0.1142(3) 0.9344(3) 0.0671(16) Uani 1 1 d . . . O1 O 0.1397(3) 0.0716(2) 0.7376(3) 0.0769(14) Uani 1 1 d . . . O2 O 0.0621(3) 0.1737(3) 0.7466(3) 0.0788(15) Uani 1 1 d . . . O3 O 0.1872(3) 0.1449(2) 0.8462(2) 0.0643(12) Uani 1 1 d . . . O4 O 0.1993(3) 0.1763(2) 0.7277(3) 0.0722(13) Uani 1 1 d . . . O5 O 0.2133(3) 0.3546(2) 0.8924(2) 0.0631(12) Uani 1 1 d . . . O6 O 0.0736(3) 0.3083(2) 0.8561(2) 0.0621(12) Uani 1 1 d . . . O7 O 0.1427(3) 0.3483(2) 0.9824(2) 0.0645(12) Uani 1 1 d . . . O8 O 0.1916(3) 0.24847(19) 0.9480(2) 0.0580(12) Uani 1 1 d . . . O9 O 0.3227(3) 0.23847(19) 0.8873(2) 0.0553(11) Uani 1 1 d . . . O10 O 0.2168(3) 0.2983(3) 0.7587(3) 0.0815(16) Uani 1 1 d . . . C1 C 0.3303(5) 0.0486(3) 0.9226(5) 0.081(2) Uani 1 1 d . . . H1A H 0.2989 0.0417 0.8720 0.097 Uiso 1 1 calc R . . H1B H 0.3733 0.0157 0.9391 0.097 Uiso 1 1 calc R . . Cl1 Cl 0.34454(15) -0.16952(12) 1.03799(16) 0.1048(8) Uani 1 1 d D . . P2 P 0.16044(11) 0.31425(8) 0.91901(10) 0.0532(5) Uani 1 1 d . . . C2 C 0.4391(4) 0.1179(4) 1.0017(5) 0.088(3) Uani 1 1 d . . . H2A H 0.4900 0.1193 0.9921 0.105 Uiso 1 1 calc R . . H2B H 0.4406 0.0791 1.0295 0.105 Uiso 1 1 calc R . . Cl2 Cl 0.6026(3) 0.0601(2) 1.2172(3) 0.207(2) Uani 1 1 d D . . C3 C 0.4853(5) 0.3352(4) 0.8709(4) 0.073(2) Uani 1 1 d . . . H3A H 0.5091 0.3673 0.8488 0.088 Uiso 1 1 calc R . . H3B H 0.5240 0.2992 0.8865 0.088 Uiso 1 1 calc R . . C4 C 0.3832(6) 0.3458(4) 0.7469(4) 0.088(3) Uani 1 1 d . . . H4B H 0.4333 0.3528 0.7369 0.106 Uiso 1 1 calc R . . H4C H 0.3451 0.3196 0.7087 0.106 Uiso 1 1 calc R . . C5 C 0.3874(5) 0.1392(4) 0.8736(4) 0.073(2) Uani 1 1 d . . . H5A H 0.3436 0.1269 0.8290 0.088 Uiso 1 1 calc R . . H5B H 0.4394 0.1207 0.8744 0.088 Uiso 1 1 calc R . . C6 C 0.3944(4) 0.2124(3) 0.8791(4) 0.0609(19) Uani 1 1 d . . . H6A H 0.4437 0.2241 0.9209 0.073 Uiso 1 1 calc R . . C7 C 0.4033(5) 0.2398(3) 0.8123(4) 0.068(2) Uani 1 1 d . . . H7A H 0.4546 0.2246 0.8086 0.081 Uiso 1 1 calc R . . H7B H 0.3571 0.2258 0.7701 0.081 Uiso 1 1 calc R . . C8 C 0.1473(10) 0.3300(6) 0.7194(7) 0.171(6) Uani 1 1 d . . . H8A H 0.1162 0.3042 0.6784 0.256 Uiso 1 1 calc R . . H8B H 0.1618 0.3707 0.7039 0.256 Uiso 1 1 calc R . . H8C H 0.1142 0.3377 0.7477 0.256 Uiso 1 1 calc R . . C10 C 0.2754(5) 0.0444(4) 0.9626(4) 0.073(2) Uani 1 1 d . . . N11 N 0.2437(4) 0.0987(3) 0.9808(3) 0.0657(16) Uani 1 1 d . . . C11 C 0.1896(5) 0.0778(4) 1.0133(4) 0.0654(19) Uani 1 1 d . . . C20 C 0.4352(5) 0.1756(5) 1.0438(5) 0.079(2) Uani 1 1 d . . . N21 N 0.3664(4) 0.2055(3) 1.0354(3) 0.0682(16) Uani 1 1 d . . . C21 C 0.3861(6) 0.2547(4) 1.0884(4) 0.078(2) Uani 1 1 d . . . C22 C 0.4725(7) 0.2515(6) 1.1254(5) 0.100(3) Uani 1 1 d . . . N22 N 0.5016(5) 0.2031(5) 1.0980(4) 0.104(3) Uani 1 1 d . . . H22A H 0.5527 0.1909 1.1116 0.125 Uiso 1 1 calc R . . C23 C 0.5092(9) 0.3013(8) 1.1802(6) 0.139(6) Uani 1 1 d . . . H23A H 0.5666 0.3050 1.2030 0.167 Uiso 1 1 calc R . . C24 C 0.4589(12) 0.3404(7) 1.1959(7) 0.141(6) Uani 1 1 d . . . H24A H 0.4816 0.3688 1.2342 0.169 Uiso 1 1 calc R . . C25 C 0.3767(10) 0.3419(5) 1.1601(6) 0.117(4) Uani 1 1 d . . . H25A H 0.3453 0.3729 1.1723 0.141 Uiso 1 1 calc R . . C26 C 0.3361(6) 0.2983(4) 1.1047(4) 0.088(3) Uani 1 1 d . . . H26A H 0.2787 0.2989 1.0806 0.105 Uiso 1 1 calc R . . C30 C 0.4724(5) 0.3647(3) 0.9343(4) 0.0613(18) Uani 1 1 d . . . N31 N 0.3986(3) 0.3746(2) 0.9357(3) 0.0529(13) Uani 1 1 d . . . C31 C 0.4124(5) 0.4117(3) 0.9974(4) 0.0565(18) Uani 1 1 d . . . N32 N 0.5347(4) 0.3893(3) 0.9907(3) 0.0709(17) Uani 1 1 d . . . H32A H 0.5872 0.3865 0.9993 0.085 Uiso 1 1 calc R . . C32 C 0.4979(5) 0.4199(3) 1.0318(4) 0.0640(19) Uani 1 1 d . . . C33 C 0.5323(6) 0.4562(4) 1.0949(4) 0.089(3) Uani 1 1 d . . . H33A H 0.5895 0.4604 1.1188 0.106 Uiso 1 1 calc R . . C34 C 0.4759(7) 0.4856(4) 1.1198(4) 0.090(3) Uani 1 1 d . . . H34A H 0.4956 0.5107 1.1611 0.108 Uiso 1 1 calc R . . C35 C 0.3909(6) 0.4779(4) 1.0841(4) 0.081(2) Uani 1 1 d . . . H35A H 0.3548 0.4982 1.1022 0.098 Uiso 1 1 calc R . . C36 C 0.3577(5) 0.4410(3) 1.0223(4) 0.0660(19) Uani 1 1 d . . . H36A H 0.3005 0.4365 0.9987 0.079 Uiso 1 1 calc R . . C40 C 0.3440(6) 0.4092(4) 0.7516(4) 0.075(2) Uani 1 1 d . . . N41 N 0.3018(4) 0.4166(3) 0.7931(3) 0.0707(17) Uani 1 1 d . . . C41 C 0.2756(5) 0.4816(4) 0.7853(4) 0.072(2) Uani 1 1 d . . . C42 C 0.3068(6) 0.5111(5) 0.7377(4) 0.087(3) Uani 1 1 d . . . N42 N 0.3475(5) 0.4648(4) 0.7169(3) 0.090(2) Uani 1 1 d . . . H42A H 0.3716 0.4696 0.6867 0.108 Uiso 1 1 calc R . . C43 C 0.2923(8) 0.5780(6) 0.7233(6) 0.127(4) Uani 1 1 d . . . H43A H 0.3096 0.5985 0.6901 0.152 Uiso 1 1 calc R . . C44 C 0.2528(9) 0.6112(6) 0.7587(8) 0.143(5) Uani 1 1 d . . . H44A H 0.2464 0.6559 0.7520 0.171 Uiso 1 1 calc R . . C45 C 0.2207(6) 0.5808(5) 0.8056(7) 0.118(4) Uani 1 1 d . . . H45A H 0.1924 0.6051 0.8283 0.142 Uiso 1 1 calc R . . C46 C 0.2312(5) 0.5148(4) 0.8180(5) 0.092(3) Uani 1 1 d . . . H46A H 0.2088 0.4937 0.8476 0.110 Uiso 1 1 calc R . . C51 C 0.1300(4) 0.4146(3) 0.9895(4) 0.0605(18) Uani 1 1 d . . . C52 C 0.1511(5) 0.4372(4) 1.0578(4) 0.082(2) Uani 1 1 d . . . H52A H 0.1733 0.4091 1.0964 0.099 Uiso 1 1 calc R . . C53 C 0.1392(7) 0.5012(5) 1.0691(6) 0.114(3) Uani 1 1 d . . . H53A H 0.1542 0.5167 1.1156 0.137 Uiso 1 1 calc R . . C54 C 0.1054(7) 0.5429(5) 1.0123(6) 0.111(3) Uani 1 1 d . . . H54A H 0.0977 0.5866 1.0201 0.134 Uiso 1 1 calc R . . C55 C 0.0835(6) 0.5197(4) 0.9451(6) 0.104(3) Uani 1 1 d . . . H55A H 0.0599 0.5479 0.9067 0.125 Uiso 1 1 calc R . . C56 C 0.0953(5) 0.4544(4) 0.9315(5) 0.082(2) Uani 1 1 d . . . H56A H 0.0802 0.4388 0.8850 0.099 Uiso 1 1 calc R . . C61 C 0.0007(4) 0.2811(4) 0.8644(4) 0.0578(18) Uani 1 1 d . . . C62 C -0.0037(5) 0.2186(4) 0.8789(4) 0.082(2) Uani 1 1 d . . . H62A H 0.0420 0.1917 0.8871 0.098 Uiso 1 1 calc R . . C63 C -0.0757(8) 0.1941(6) 0.8818(5) 0.108(3) Uani 1 1 d . . . H63A H -0.0784 0.1506 0.8931 0.129 Uiso 1 1 calc R . . C64 C -0.1420(8) 0.2318(8) 0.8688(5) 0.115(4) Uani 1 1 d . . . H64A H -0.1912 0.2143 0.8695 0.138 Uiso 1 1 calc R . . C65 C -0.1382(6) 0.2963(7) 0.8544(6) 0.116(4) Uani 1 1 d . . . H65A H -0.1838 0.3231 0.8472 0.139 Uiso 1 1 calc R . . C66 C -0.0656(5) 0.3212(4) 0.8507(4) 0.085(2) Uani 1 1 d . . . H66A H -0.0624 0.3646 0.8391 0.102 Uiso 1 1 calc R . . C71 C 0.0065(5) 0.1942(3) 0.6809(4) 0.0643(19) Uani 1 1 d . . . C72 C 0.0219(5) 0.1919(4) 0.6174(5) 0.088(2) Uani 1 1 d . . . H72A H 0.0712 0.1744 0.6168 0.106 Uiso 1 1 calc R . . C73 C -0.0366(7) 0.2157(5) 0.5566(5) 0.111(3) Uani 1 1 d . . . H73A H -0.0260 0.2159 0.5145 0.133 Uiso 1 1 calc R . . C74 C -0.1099(7) 0.2391(5) 0.5559(6) 0.113(3) Uani 1 1 d . . . H74A H -0.1491 0.2553 0.5137 0.135 Uiso 1 1 calc R . . C75 C -0.1261(6) 0.2390(5) 0.6166(6) 0.105(3) Uani 1 1 d . . . H75A H -0.1766 0.2553 0.6155 0.126 Uiso 1 1 calc R . . C76 C -0.0687(5) 0.2150(4) 0.6808(4) 0.077(2) Uani 1 1 d . . . H76A H -0.0811 0.2132 0.7219 0.093 Uiso 1 1 calc R . . C81 C 0.1093(6) 0.0200(4) 0.7671(4) 0.075(2) Uani 1 1 d . . . C82 C 0.0353(7) 0.0204(5) 0.7723(5) 0.106(3) Uani 1 1 d . . . H82A H 0.0025 0.0575 0.7583 0.127 Uiso 1 1 calc R . . C83 C 0.0048(8) -0.0321(6) 0.7976(7) 0.132(4) Uani 1 1 d . . . H83A H -0.0477 -0.0309 0.8003 0.158 Uiso 1 1 calc R . . C84 C 0.0545(10) -0.0860(6) 0.8185(6) 0.127(4) Uani 1 1 d . . . H84A H 0.0365 -0.1218 0.8370 0.153 Uiso 1 1 calc R . . C85 C 0.1299(8) -0.0869(5) 0.8122(6) 0.119(3) Uani 1 1 d . . . H85A H 0.1631 -0.1237 0.8263 0.142 Uiso 1 1 calc R . . C86 C 0.1587(6) -0.0335(5) 0.7848(5) 0.094(3) Uani 1 1 d . . . H88A H 0.2095 -0.0347 0.7790 0.113 Uiso 1 1 calc R . . O11 O 0.4044(6) -0.1577(8) 1.1084(5) 0.341(10) Uani 1 1 d D . . C12 C 0.1933(5) 0.0097(4) 1.0157(4) 0.077(2) Uani 1 1 d . . . N12 N 0.2474(4) -0.0083(3) 0.9849(4) 0.089(2) Uani 1 1 d . . . H12A H 0.2616 -0.0476 0.9805 0.106 Uiso 1 1 calc R . . O12 O 0.3609(7) -0.2276(4) 1.0103(6) 0.267(6) Uani 1 1 d D . . C13 C 0.1438(7) -0.0258(5) 1.0450(6) 0.115(3) Uani 1 1 d . . . H13A H 0.1457 -0.0709 1.0471 0.138 Uiso 1 1 calc R . . O13 O 0.3617(9) -0.1164(5) 0.9939(9) 0.400(12) Uani 1 1 d D . . C14 C 0.0940(8) 0.0083(6) 1.0696(6) 0.128(4) Uani 1 1 d . . . H14A H 0.0615 -0.0135 1.0902 0.154 Uiso 1 1 calc R . . O14 O 0.2646(4) -0.1562(5) 1.0342(7) 0.292(9) Uani 1 1 d D . . C15 C 0.0900(7) 0.0757(5) 1.0650(6) 0.124(4) Uani 1 1 d . . . H15A H 0.0534 0.0977 1.0811 0.149 Uiso 1 1 calc R . . O15 O 0.6679(10) 0.0235(10) 1.2657(8) 0.56(3) Uani 1 1 d D . . C16 C 0.1384(6) 0.1108(4) 1.0373(4) 0.089(3) Uani 1 1 d . . . H16A H 0.1359 0.1559 1.0353 0.107 Uiso 1 1 calc R . . O16 O 0.6253(6) 0.0895(5) 1.1642(5) 0.277(8) Uani 1 1 d D . . O17 O 0.5638(7) 0.0993(5) 1.2496(5) 0.231(5) Uani 1 1 d D . . O18 O 0.5360(12) 0.0111(7) 1.1789(8) 0.68(4) Uani 1 1 d D . . O22 O 0.6986(5) 0.3674(5) 0.9894(7) 0.209(5) Uani 1 1 d . . . O21 O 0.4222(8) -0.0042(7) 1.1238(7) 0.114(4) Uani 0.50 1 d P . . O23 O 0.6701(15) 0.2041(12) 1.1499(15) 0.240(10) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0617(6) 0.0521(5) 0.0553(6) -0.0033(4) 0.0210(4) -0.0065(4) Fe1 0.0537(6) 0.0442(5) 0.0581(6) 0.0029(4) 0.0180(5) 0.0005(4) P1 0.0649(12) 0.0608(12) 0.0589(13) -0.0066(9) 0.0222(10) -0.0065(9) N1 0.075(4) 0.061(4) 0.068(4) -0.001(3) 0.039(3) -0.010(3) N2 0.062(4) 0.053(4) 0.086(5) 0.004(3) 0.028(4) 0.012(3) O1 0.103(4) 0.062(3) 0.078(4) -0.018(3) 0.048(3) -0.020(3) O2 0.065(3) 0.112(4) 0.059(3) 0.007(3) 0.022(3) 0.012(3) O3 0.068(3) 0.064(3) 0.054(3) -0.002(2) 0.015(2) -0.010(2) O4 0.080(3) 0.074(3) 0.069(3) -0.012(3) 0.035(3) -0.017(3) O5 0.060(3) 0.055(3) 0.079(3) -0.002(2) 0.031(3) -0.005(2) O6 0.068(3) 0.062(3) 0.057(3) -0.003(2) 0.023(2) 0.000(2) O7 0.077(3) 0.058(3) 0.064(3) 0.000(2) 0.032(3) 0.000(2) O8 0.069(3) 0.047(3) 0.061(3) -0.001(2) 0.028(2) 0.003(2) O9 0.061(3) 0.044(2) 0.063(3) 0.000(2) 0.026(2) 0.003(2) O10 0.084(4) 0.074(4) 0.062(3) 0.007(3) -0.002(3) -0.001(3) C1 0.080(5) 0.047(5) 0.117(7) 0.009(4) 0.039(5) 0.008(4) Cl1 0.0785(16) 0.0882(17) 0.141(2) 0.0043(15) 0.0335(15) 0.0072(12) P2 0.0543(11) 0.0496(10) 0.0564(11) -0.0020(9) 0.0213(9) -0.0005(8) C2 0.048(5) 0.103(7) 0.103(7) 0.024(6) 0.018(5) 0.011(4) Cl2 0.294(6) 0.193(4) 0.224(5) 0.114(4) 0.200(5) 0.135(4) C3 0.074(5) 0.068(5) 0.094(6) -0.001(4) 0.050(5) -0.005(4) C4 0.117(7) 0.093(7) 0.076(6) -0.002(5) 0.061(5) -0.023(5) C5 0.068(5) 0.068(5) 0.091(6) -0.006(4) 0.040(5) 0.009(4) C6 0.059(4) 0.045(4) 0.089(6) -0.007(4) 0.039(4) -0.005(3) C7 0.074(5) 0.063(5) 0.077(5) -0.013(4) 0.041(4) -0.004(4) C8 0.253(18) 0.123(10) 0.127(11) 0.003(8) 0.059(12) -0.022(11) C10 0.077(5) 0.048(5) 0.087(6) 0.018(4) 0.023(5) 0.014(4) N11 0.074(4) 0.055(4) 0.063(4) 0.014(3) 0.020(3) 0.000(3) C11 0.073(5) 0.068(5) 0.057(5) 0.007(4) 0.026(4) -0.005(4) C20 0.056(5) 0.094(7) 0.074(6) 0.013(5) 0.008(5) -0.016(5) N21 0.067(4) 0.064(4) 0.059(4) 0.013(3) 0.006(3) -0.007(3) C21 0.099(7) 0.071(6) 0.050(5) 0.013(4) 0.013(5) -0.019(5) C22 0.105(9) 0.126(9) 0.061(6) 0.014(6) 0.022(6) -0.043(7) N22 0.067(5) 0.148(8) 0.083(6) 0.021(5) 0.012(4) -0.021(5) C23 0.144(12) 0.201(15) 0.059(7) -0.010(8) 0.022(7) -0.110(11) C24 0.228(19) 0.134(12) 0.057(8) -0.009(7) 0.049(10) -0.095(12) C25 0.204(13) 0.080(7) 0.057(7) 0.005(5) 0.037(7) -0.028(8) C26 0.127(8) 0.071(6) 0.048(5) 0.008(4) 0.014(5) -0.014(6) C30 0.066(5) 0.054(4) 0.065(5) 0.002(4) 0.026(4) -0.012(4) N31 0.056(4) 0.053(3) 0.052(4) -0.004(3) 0.023(3) -0.008(3) C31 0.068(5) 0.047(4) 0.056(5) -0.002(3) 0.025(4) -0.016(3) N32 0.057(4) 0.073(4) 0.073(5) 0.010(3) 0.013(4) -0.014(3) C32 0.071(5) 0.058(5) 0.061(5) 0.004(4) 0.022(4) -0.019(4) C33 0.097(7) 0.084(6) 0.058(6) 0.013(5) -0.002(5) -0.040(5) C34 0.124(8) 0.085(6) 0.052(5) -0.004(4) 0.021(6) -0.037(6) C35 0.125(8) 0.061(5) 0.070(6) -0.002(4) 0.051(6) -0.013(5) C36 0.080(5) 0.057(4) 0.063(5) 0.004(4) 0.029(4) -0.008(4) C40 0.106(7) 0.065(6) 0.057(5) -0.003(4) 0.033(5) -0.020(5) N41 0.075(4) 0.072(5) 0.058(4) 0.003(3) 0.016(3) -0.009(3) C41 0.073(5) 0.055(5) 0.071(6) 0.008(4) 0.006(4) -0.005(4) C42 0.104(7) 0.080(7) 0.055(5) 0.006(5) 0.005(5) -0.026(5) N42 0.131(6) 0.086(5) 0.049(4) 0.007(4) 0.028(4) -0.029(5) C43 0.161(11) 0.086(8) 0.087(8) 0.037(6) -0.009(7) -0.035(8) C44 0.164(12) 0.066(7) 0.140(12) 0.027(8) -0.012(9) 0.017(8) C45 0.116(8) 0.072(7) 0.135(10) 0.018(7) 0.011(7) 0.022(6) C46 0.074(6) 0.073(6) 0.112(7) 0.017(5) 0.017(5) 0.011(5) C51 0.071(5) 0.057(5) 0.060(5) -0.006(4) 0.032(4) 0.002(4) C52 0.094(6) 0.081(6) 0.071(6) -0.004(5) 0.029(5) -0.007(5) C53 0.176(10) 0.081(7) 0.113(9) -0.035(6) 0.084(8) -0.004(7) C54 0.168(10) 0.059(6) 0.116(9) -0.011(6) 0.063(8) 0.005(6) C55 0.147(9) 0.066(6) 0.106(8) 0.010(5) 0.053(7) 0.029(5) C56 0.099(6) 0.062(5) 0.088(6) -0.002(5) 0.038(5) 0.016(4) C61 0.057(5) 0.067(5) 0.056(4) -0.009(4) 0.029(4) -0.014(4) C62 0.085(6) 0.079(6) 0.076(6) -0.007(4) 0.024(5) -0.023(5) C63 0.099(8) 0.127(9) 0.097(8) -0.019(6) 0.037(7) -0.054(8) C64 0.083(8) 0.182(13) 0.085(7) -0.050(8) 0.038(6) -0.068(9) C65 0.058(6) 0.177(12) 0.114(8) -0.054(8) 0.032(5) -0.022(7) C66 0.063(5) 0.096(6) 0.088(6) -0.010(5) 0.018(5) -0.004(5) C71 0.072(5) 0.058(4) 0.060(5) -0.003(4) 0.020(4) -0.002(4) C72 0.080(6) 0.117(7) 0.068(6) 0.003(5) 0.027(5) 0.017(5) C73 0.115(8) 0.157(9) 0.049(6) 0.008(6) 0.016(6) 0.010(7) C74 0.100(8) 0.146(9) 0.076(7) 0.012(6) 0.013(6) 0.039(7) C75 0.077(6) 0.137(9) 0.091(8) -0.010(6) 0.019(6) 0.026(6) C76 0.063(5) 0.097(6) 0.069(6) -0.009(4) 0.020(5) -0.006(4) C81 0.088(6) 0.071(6) 0.073(6) -0.024(4) 0.039(5) -0.024(5) C82 0.117(8) 0.089(7) 0.138(9) -0.008(6) 0.079(7) -0.017(6) C83 0.164(11) 0.106(9) 0.164(11) -0.009(8) 0.106(10) -0.039(9) C84 0.164(12) 0.103(9) 0.148(11) 0.020(7) 0.095(10) -0.006(8) C85 0.130(9) 0.084(8) 0.131(10) 0.002(6) 0.036(8) -0.004(7) C86 0.093(6) 0.075(6) 0.106(7) -0.011(5) 0.028(6) -0.011(6) O11 0.217(12) 0.51(3) 0.218(14) -0.133(17) -0.003(11) 0.035(14) C12 0.086(6) 0.063(6) 0.077(6) 0.014(4) 0.025(5) 0.002(5) N12 0.100(5) 0.042(4) 0.116(6) 0.020(4) 0.031(5) 0.011(4) O12 0.368(16) 0.140(8) 0.276(14) 0.000(8) 0.100(12) 0.123(10) C13 0.159(10) 0.079(7) 0.123(9) 0.028(6) 0.070(8) -0.021(7) O13 0.44(2) 0.212(12) 0.67(4) 0.125(17) 0.35(3) 0.127(14) C14 0.174(11) 0.102(9) 0.153(11) 0.014(7) 0.113(9) -0.015(8) O14 0.090(6) 0.199(10) 0.53(3) -0.078(12) 0.050(10) -0.007(6) C15 0.164(10) 0.100(8) 0.156(10) 0.013(7) 0.117(9) -0.006(7) O15 0.57(4) 0.73(5) 0.57(4) 0.52(4) 0.42(3) 0.50(4) C16 0.125(7) 0.073(6) 0.085(6) 0.015(5) 0.059(6) -0.004(5) O16 0.250(12) 0.43(2) 0.229(12) 0.173(13) 0.179(11) 0.209(13) O17 0.261(12) 0.280(13) 0.222(11) 0.026(9) 0.174(10) 0.127(10) O18 1.60(10) 0.256(19) 0.64(5) -0.21(3) 0.94(7) -0.37(4) O22 0.122(6) 0.171(8) 0.342(15) 0.027(9) 0.094(8) 0.040(6) O21 0.116(10) 0.138(12) 0.091(9) 0.009(8) 0.043(8) -0.012(8) O23 0.23(2) 0.22(2) 0.29(3) 0.05(2) 0.12(2) 0.015(17) _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 Ni1 N31 2.025(5) . ? Ni1 O5 2.040(4) . ? Ni1 N41 2.052(6) . ? Ni1 O10 2.077(5) . ? Ni1 O9 2.099(4) . ? Ni1 N1 2.161(6) . ? Fe1 O9 1.938(4) . ? Fe1 O8 1.946(4) . ? Fe1 O3 2.013(4) . ? Fe1 N11 2.102(6) . ? Fe1 N21 2.126(6) . ? Fe1 N2 2.270(5) . ? P1 O4 1.461(5) . ? P1 O3 1.503(5) . ? P1 O2 1.586(5) . ? P1 O1 1.590(5) . ? N1 C7 1.486(8) . ? N1 C3 1.495(9) . ? N1 C4 1.507(9) . ? N2 C2 1.451(9) . ? N2 C5 1.472(9) . ? N2 C1 1.482(9) . ? O1 C81 1.410(9) . ? O2 C71 1.382(8) . ? O5 P2 1.476(5) . ? O6 C61 1.443(7) . ? O6 P2 1.570(5) . ? O7 C51 1.399(8) . ? O7 P2 1.582(5) . ? O8 P2 1.495(4) . ? O9 C6 1.417(7) . ? O10 C8 1.337(14) . ? C1 C10 1.458(10) . ? Cl1 O14 1.383(6) . ? Cl1 O12 1.392(6) . ? Cl1 O11 1.432(7) . ? Cl1 O13 1.505(7) . ? C2 C20 1.477(12) . ? Cl2 O17 1.362(6) . ? Cl2 O16 1.405(6) . ? Cl2 O15 1.407(7) . ? Cl2 O18 1.510(9) . ? C3 C30 1.502(10) . ? C4 C40 1.492(11) . ? C5 C6 1.514(9) . ? C6 C7 1.518(10) . ? C10 N12 1.333(9) . ? C10 N11 1.355(9) . ? N11 C11 1.395(9) . ? C11 C16 1.340(10) . ? C11 C12 1.403(10) . ? C20 N21 1.294(9) . ? C20 N22 1.378(10) . ? N21 C21 1.418(10) . ? C21 C26 1.369(11) . ? C21 C22 1.403(12) . ? C22 N22 1.326(12) . ? C22 C23 1.466(16) . ? C23 C24 1.309(18) . ? C24 C25 1.334(17) . ? C25 C26 1.400(13) . ? C30 N31 1.304(8) . ? C30 N32 1.341(8) . ? N31 C31 1.402(8) . ? C31 C36 1.365(9) . ? C31 C32 1.391(9) . ? N32 C32 1.372(9) . ? C32 C33 1.402(11) . ? C33 C34 1.389(12) . ? C34 C35 1.387(12) . ? C35 C36 1.387(10) . ? C40 N41 1.307(9) . ? C40 N42 1.354(9) . ? N41 C41 1.404(9) . ? C41 C46 1.367(11) . ? C41 C42 1.400(11) . ? C42 N42 1.343(11) . ? C42 C43 1.411(14) . ? C43 C44 1.344(16) . ? C44 C45 1.408(16) . ? C45 C46 1.382(12) . ? C51 C52 1.366(10) . ? C51 C56 1.369(10) . ? C52 C53 1.367(11) . ? C53 C54 1.376(13) . ? C54 C55 1.350(12) . ? C55 C56 1.404(11) . ? C61 C62 1.329(10) . ? C61 C66 1.358(10) . ? C62 C63 1.366(12) . ? C63 C64 1.328(14) . ? C64 C65 1.365(15) . ? C65 C66 1.384(12) . ? C71 C76 1.370(10) . ? C71 C72 1.400(10) . ? C72 C73 1.356(11) . ? C73 C74 1.352(12) . ? C74 C75 1.351(13) . ? C75 C76 1.395(12) . ? C81 C82 1.323(11) . ? C81 C86 1.359(11) . ? C82 C83 1.381(12) . ? C83 C84 1.371(15) . ? C84 C85 1.358(13) . ? C85 C86 1.403(13) . ? C12 N12 1.353(10) . ? C12 C13 1.411(12) . ? C13 C14 1.342(13) . ? C14 C15 1.392(13) . ? C15 C16 1.370(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 N31 Ni1 O5 96.0(2) . . ? N31 Ni1 N41 89.3(2) . . ? O5 Ni1 N41 102.9(2) . . ? N31 Ni1 O10 171.5(2) . . ? O5 Ni1 O10 91.6(2) . . ? N41 Ni1 O10 85.3(2) . . ? N31 Ni1 O9 97.30(19) . . ? O5 Ni1 O9 95.92(17) . . ? N41 Ni1 O9 159.3(2) . . ? O10 Ni1 O9 85.64(19) . . ? N31 Ni1 N1 81.6(2) . . ? O5 Ni1 N1 176.1(2) . . ? N41 Ni1 N1 80.3(2) . . ? O10 Ni1 N1 91.0(2) . . ? O9 Ni1 N1 81.28(19) . . ? O9 Fe1 O8 99.14(18) . . ? O9 Fe1 O3 94.81(18) . . ? O8 Fe1 O3 95.90(19) . . ? O9 Fe1 N11 155.8(2) . . ? O8 Fe1 N11 105.0(2) . . ? O3 Fe1 N11 81.6(2) . . ? O9 Fe1 N21 89.8(2) . . ? O8 Fe1 N21 95.3(2) . . ? O3 Fe1 N21 167.0(2) . . ? N11 Fe1 N21 89.2(2) . . ? O9 Fe1 N2 81.0(2) . . ? O8 Fe1 N2 173.7(2) . . ? O3 Fe1 N2 90.3(2) . . ? N11 Fe1 N2 75.2(2) . . ? N21 Fe1 N2 78.4(2) . . ? O4 P1 O3 119.1(3) . . ? O4 P1 O2 112.9(3) . . ? O3 P1 O2 102.8(3) . . ? O4 P1 O1 105.6(3) . . ? O3 P1 O1 109.8(3) . . ? O2 P1 O1 106.0(3) . . ? C7 N1 C3 110.9(6) . . ? C7 N1 C4 113.7(6) . . ? C3 N1 C4 111.1(6) . . ? C7 N1 Ni1 105.1(4) . . ? C3 N1 Ni1 110.4(4) . . ? C4 N1 Ni1 105.3(5) . . ? C2 N2 C5 112.8(6) . . ? C2 N2 C1 111.6(6) . . ? C5 N2 C1 114.2(6) . . ? C2 N2 Fe1 109.4(5) . . ? C5 N2 Fe1 101.3(4) . . ? C1 N2 Fe1 106.9(4) . . ? C81 O1 P1 125.8(4) . . ? C71 O2 P1 128.6(5) . . ? P1 O3 Fe1 146.9(3) . . ? P2 O5 Ni1 134.5(3) . . ? C61 O6 P2 123.6(4) . . ? C51 O7 P2 126.9(4) . . ? P2 O8 Fe1 136.7(3) . . ? C6 O9 Fe1 116.9(4) . . ? C6 O9 Ni1 111.0(3) . . ? Fe1 O9 Ni1 131.7(2) . . ? C8 O10 Ni1 123.2(7) . . ? C10 C1 N2 108.0(6) . . ? O14 Cl1 O12 119.7(6) . . ? O14 Cl1 O11 111.2(6) . . ? O12 Cl1 O11 111.2(6) . . ? O14 Cl1 O13 103.6(5) . . ? O12 Cl1 O13 105.9(6) . . ? O11 Cl1 O13 103.4(6) . . ? O5 P2 O8 118.0(3) . . ? O5 P2 O6 106.7(3) . . ? O8 P2 O6 110.1(3) . . ? O5 P2 O7 112.0(3) . . ? O8 P2 O7 103.7(3) . . ? O6 P2 O7 105.7(3) . . ? N2 C2 C20 112.1(6) . . ? O17 Cl2 O16 115.8(6) . . ? O17 Cl2 O15 113.4(7) . . ? O16 Cl2 O15 112.3(6) . . ? O17 Cl2 O18 102.8(7) . . ? O16 Cl2 O18 106.0(7) . . ? O15 Cl2 O18 105.1(7) . . ? N1 C3 C30 110.1(6) . . ? C40 C4 N1 107.6(6) . . ? N2 C5 C6 108.9(6) . . ? O9 C6 C5 109.7(5) . . ? O9 C6 C7 110.1(6) . . ? C5 C6 C7 109.7(6) . . ? N1 C7 C6 107.9(5) . . ? N12 C10 N11 110.3(7) . . ? N12 C10 C1 128.9(8) . . ? N11 C10 C1 120.8(7) . . ? C10 N11 C11 106.4(6) . . ? C10 N11 Fe1 114.4(5) . . ? C11 N11 Fe1 137.7(5) . . ? C16 C11 C12 121.5(8) . . ? C16 C11 N11 131.3(7) . . ? C12 C11 N11 107.1(7) . . ? N21 C20 N22 111.4(9) . . ? N21 C20 C2 123.0(7) . . ? N22 C20 C2 125.6(9) . . ? C20 N21 C21 106.8(7) . . ? C20 N21 Fe1 113.6(6) . . ? C21 N21 Fe1 137.3(6) . . ? C26 C21 C22 123.1(10) . . ? C26 C21 N21 130.8(8) . . ? C22 C21 N21 106.1(9) . . ? N22 C22 C21 107.9(9) . . ? N22 C22 C23 135.6(12) . . ? C21 C22 C23 116.4(13) . . ? C22 N22 C20 107.7(8) . . ? C24 C23 C22 118.2(14) . . ? C23 C24 C25 123.6(15) . . ? C24 C25 C26 122.4(13) . . ? C21 C26 C25 115.9(10) . . ? N31 C30 N32 114.1(7) . . ? N31 C30 C3 122.5(7) . . ? N32 C30 C3 123.0(7) . . ? C30 N31 C31 105.0(6) . . ? C30 N31 Ni1 114.9(5) . . ? C31 N31 Ni1 140.1(5) . . ? C36 C31 C32 121.2(7) . . ? C36 C31 N31 130.8(7) . . ? C32 C31 N31 107.9(6) . . ? C30 N32 C32 106.1(6) . . ? N32 C32 C31 106.8(7) . . ? N32 C32 C33 131.0(8) . . ? C31 C32 C33 122.1(8) . . ? C34 C33 C32 116.1(8) . . ? C35 C34 C33 121.0(8) . . ? C36 C35 C34 122.2(8) . . ? C31 C36 C35 117.3(7) . . ? N41 C40 N42 112.0(8) . . ? N41 C40 C4 121.1(7) . . ? N42 C40 C4 126.8(8) . . ? C40 N41 C41 105.8(7) . . ? C40 N41 Ni1 112.9(5) . . ? C41 N41 Ni1 141.1(6) . . ? C46 C41 C42 122.7(8) . . ? C46 C41 N41 129.7(8) . . ? C42 C41 N41 107.5(8) . . ? N42 C42 C41 106.6(8) . . ? N42 C42 C43 134.6(11) . . ? C41 C42 C43 118.7(11) . . ? C42 N42 C40 108.1(7) . . ? C44 C43 C42 118.3(12) . . ? C43 C44 C45 122.3(11) . . ? C46 C45 C44 120.0(11) . . ? C41 C46 C45 117.7(10) . . ? C52 C51 C56 121.6(7) . . ? C52 C51 O7 116.2(7) . . ? C56 C51 O7 122.2(7) . . ? C53 C52 C51 119.7(8) . . ? C52 C53 C54 120.6(9) . . ? C55 C54 C53 119.1(9) . . ? C54 C55 C56 121.9(9) . . ? C51 C56 C55 117.2(8) . . ? C62 C61 C66 121.3(7) . . ? C62 C61 O6 121.7(7) . . ? C66 C61 O6 116.7(7) . . ? C61 C62 C63 119.8(9) . . ? C64 C63 C62 120.6(11) . . ? C63 C64 C65 120.3(10) . . ? C66 C65 C64 119.3(10) . . ? C61 C66 C65 118.6(9) . . ? C76 C71 O2 114.9(7) . . ? C76 C71 C72 120.7(7) . . ? O2 C71 C72 124.3(7) . . ? C73 C72 C71 118.7(8) . . ? C74 C73 C72 121.4(9) . . ? C73 C74 C75 119.9(9) . . ? C74 C75 C76 121.5(9) . . ? C71 C76 C75 117.5(8) . . ? C82 C81 C86 121.1(9) . . ? C82 C81 O1 123.5(9) . . ? C86 C81 O1 115.2(8) . . ? C81 C82 C83 122.6(10) . . ? C84 C83 C82 117.7(11) . . ? C85 C84 C83 119.8(11) . . ? C84 C85 C86 121.3(10) . . ? C81 C86 C85 117.4(9) . . ? N12 C12 C11 106.8(7) . . ? N12 C12 C13 132.8(9) . . ? C11 C12 C13 120.4(9) . . ? C10 N12 C12 109.3(7) . . ? C14 C13 C12 117.1(9) . . ? C13 C14 C15 121.3(10) . . ? C16 C15 C14 122.1(10) . . ? C11 C16 C15 117.6(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.893 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.086