# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xinfang Liu' _publ_contact_author_email liuxinfang6@126.com loop_ _publ_author_name 'Xinfang Liu' 'Songlin Zhang' 'Yuqiang Ding' data_lxf-28-5 _database_code_depnum_ccdc_archive 'CCDC 859530' #TrackingRef 'lxf-28-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H35 Cu F3 Fe N O P2' _chemical_formula_weight 820.05 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 9.5178(19) _cell_length_b 22.194(4) _cell_length_c 17.301(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.38(3) _cell_angle_gamma 90.00 _cell_volume 3651.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 223.15 _cell_measurement_reflns_used 14866 _cell_measurement_theta_min 3.0229 _cell_measurement_theta_max 27.4855 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7301 _exptl_absorpt_correction_T_max 0.8072 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223.15 _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 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 20958 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8306 _reflns_number_gt 6136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+1.9530P] 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 8306 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 Cu Cu 0.29777(5) 0.14000(2) 0.21655(3) 0.03558(14) Uani 1 1 d . . . Fe Fe 0.02650(6) 0.00767(2) 0.27261(3) 0.03763(16) Uani 1 1 d . . . P1 P 0.27992(11) 0.10359(4) 0.33779(6) 0.0363(2) Uani 1 1 d . . . P2 P 0.17994(11) 0.08406(5) 0.12777(6) 0.0368(3) Uani 1 1 d . . . C35 C 0.2609(4) 0.26449(16) 0.1993(2) 0.0351(9) Uani 1 1 d . . . C13 C 0.0271(4) 0.04868(18) 0.1667(2) 0.0384(9) Uani 1 1 d . . . N N 0.3752(3) 0.22175(13) 0.20192(18) 0.0372(8) Uani 1 1 d . . . C18 C 0.0232(5) -0.03818(19) 0.3757(2) 0.0519(12) Uani 1 1 d . . . H18 H -0.0547 -0.0567 0.3961 0.062 Uiso 1 1 calc R . . C19 C 0.1888(4) 0.03255(16) 0.3470(2) 0.0359(9) Uani 1 1 d . . . C1 C 0.1118(5) 0.12303(18) 0.0405(2) 0.0422(10) Uani 1 1 d . . . C23 C 0.1808(4) 0.15215(17) 0.4000(2) 0.0393(9) Uani 1 1 d . . . C7 C 0.4066(4) 0.00581(19) 0.1235(2) 0.0451(10) Uani 1 1 d . . . H7 H 0.4436 0.0283 0.1649 0.054 Uiso 1 1 calc R . . C14 C -0.0677(4) 0.0789(2) 0.2165(2) 0.0450(10) Uani 1 1 d . . . H14 H -0.0623 0.1190 0.2319 0.054 Uiso 1 1 calc R . . C36 C 0.0226(5) 0.33953(19) 0.1950(3) 0.0479(11) Uani 1 1 d . . . C8 C 0.4814(5) -0.0431(2) 0.0960(3) 0.0581(13) Uani 1 1 d . . . H8 H 0.5679 -0.0533 0.1194 0.070 Uiso 1 1 calc R . . C20 C 0.0648(4) 0.02172(18) 0.3889(2) 0.0440(10) Uani 1 1 d . . . H20 H 0.0197 0.0495 0.4196 0.053 Uiso 1 1 calc R . . C15 C -0.1408(5) -0.0188(2) 0.2032(3) 0.0584(13) Uani 1 1 d . . . H15 H -0.1921 -0.0542 0.2082 0.070 Uiso 1 1 calc R . . C21 C 0.2205(4) -0.02262(17) 0.3081(2) 0.0415(10) Uani 1 1 d . . . H21 H 0.2954 -0.0289 0.2762 0.050 Uiso 1 1 calc R . . C37 C 0.1140(5) 0.3379(2) 0.2569(3) 0.0555(12) Uani 1 1 d . . . H37 H 0.0969 0.3623 0.2993 0.067 Uiso 1 1 calc R . . C24 C 0.1905(5) 0.14773(19) 0.4806(2) 0.0545(12) Uani 1 1 d . . . H24 H 0.2542 0.1210 0.5042 0.065 Uiso 1 1 calc R . . C9 C 0.2779(4) 0.02111(17) 0.0896(2) 0.0391(9) Uani 1 1 d . . . C42 C 0.5037(4) 0.24412(18) 0.2071(2) 0.0384(9) Uani 1 1 d . . . C16 C -0.0201(5) -0.01193(19) 0.1593(2) 0.0469(11) Uani 1 1 d . . . H16 H 0.0215 -0.0419 0.1304 0.056 Uiso 1 1 calc R . . C17 C -0.1704(5) 0.0366(2) 0.2380(3) 0.0593(13) Uani 1 1 d . . . H17 H -0.2449 0.0443 0.2697 0.071 Uiso 1 1 calc R . . C25 C 0.0032(6) 0.2284(2) 0.4126(3) 0.0759(16) Uani 1 1 d . . . H25 H -0.0600 0.2557 0.3898 0.091 Uiso 1 1 calc R . . C10 C 0.2270(5) -0.0125(2) 0.0264(3) 0.0534(12) Uani 1 1 d . . . H10 H 0.1410 -0.0024 0.0023 0.064 Uiso 1 1 calc R . . C2 C 0.0266(7) 0.1904(3) -0.0878(3) 0.0792(18) Uani 1 1 d . . . H2 H -0.0029 0.2126 -0.1311 0.095 Uiso 1 1 calc R . . C26 C 0.0866(5) 0.1932(2) 0.3666(3) 0.0581(13) Uani 1 1 d . . . H26 H 0.0792 0.1971 0.3130 0.070 Uiso 1 1 calc R . . C3 C -0.0151(5) 0.1519(2) 0.0387(3) 0.0629(14) Uani 1 1 d . . . H3 H -0.0726 0.1489 0.0807 0.076 Uiso 1 1 calc R . . C29 C 0.4482(4) 0.0942(2) 0.3910(2) 0.0428(10) Uani 1 1 d . . . C22 C 0.1177(5) -0.06569(19) 0.3267(3) 0.0505(11) Uani 1 1 d . . . H22 H 0.1136 -0.1054 0.3095 0.061 Uiso 1 1 calc R . . C30 C 0.6431(7) 0.0379(3) 0.4435(4) 0.094(2) Uani 1 1 d . . . H30 H 0.6841 0.0006 0.4543 0.113 Uiso 1 1 calc R . . C27 C 0.0136(6) 0.2231(2) 0.4914(3) 0.0725(16) Uani 1 1 d . . . H27 H -0.0422 0.2469 0.5220 0.087 Uiso 1 1 calc R . . C4 C 0.1967(6) 0.1293(2) -0.0226(3) 0.0597(13) Uani 1 1 d . . . H4 H 0.2841 0.1105 -0.0218 0.072 Uiso 1 1 calc R . . C28 C 0.1057(6) 0.1830(2) 0.5253(3) 0.0654(14) Uani 1 1 d . . . H28 H 0.1115 0.1793 0.5788 0.078 Uiso 1 1 calc R . . C11 C 0.3020(6) -0.0604(2) -0.0009(3) 0.0632(14) Uani 1 1 d . . . H11 H 0.2672 -0.0821 -0.0435 0.076 Uiso 1 1 calc R . . C38 C 0.2320(5) 0.3014(2) 0.2598(3) 0.0572(13) Uani 1 1 d . . . H38 H 0.2925 0.3021 0.3034 0.069 Uiso 1 1 calc R . . C5 C -0.0588(6) 0.1860(3) -0.0258(4) 0.0814(18) Uani 1 1 d . . . H5 H -0.1453 0.2056 -0.0269 0.098 Uiso 1 1 calc R . . C12 C 0.4281(6) -0.0763(2) 0.0347(3) 0.0644(14) Uani 1 1 d . . . H12 H 0.4774 -0.1095 0.0173 0.077 Uiso 1 1 calc R . . C39 C 0.1705(5) 0.2657(2) 0.1364(3) 0.0625(14) Uani 1 1 d . . . H39 H 0.1884 0.2416 0.0939 0.075 Uiso 1 1 calc R . . C6 C 0.1536(7) 0.1628(2) -0.0860(3) 0.0713(16) Uani 1 1 d . . . H6 H 0.2116 0.1664 -0.1277 0.086 Uiso 1 1 calc R . . C31 C 0.5101(6) 0.0398(2) 0.4069(3) 0.0748(16) Uani 1 1 d . . . H31 H 0.4637 0.0043 0.3933 0.090 Uiso 1 1 calc R . . C32 C 0.7136(6) 0.0877(4) 0.4636(3) 0.085(2) Uani 1 1 d . . . H32 H 0.8023 0.0853 0.4881 0.103 Uiso 1 1 calc R . . C33 C 0.5233(6) 0.1446(3) 0.4104(4) 0.091(2) Uani 1 1 d . . . H33 H 0.4851 0.1821 0.3979 0.109 Uiso 1 1 calc R . . O O 0.5445(3) 0.29673(12) 0.21139(17) 0.0496(8) Uani 1 1 d . . . F1 F 0.5799(3) 0.13986(12) 0.2095(2) 0.0878(10) Uani 1 1 d . . . F2 F 0.7151(4) 0.20371(16) 0.2608(2) 0.1127(13) Uani 1 1 d . . . F3 F 0.6883(4) 0.20043(17) 0.1411(2) 0.1157(14) Uani 1 1 d . . . C43 C 0.6203(5) 0.1965(2) 0.2051(3) 0.0514(11) Uani 1 1 d . . . C41 C -0.1069(5) 0.3784(2) 0.1932(3) 0.0724(15) Uani 1 1 d . . . H41A H -0.1875 0.3539 0.2027 0.109 Uiso 1 1 calc R . . H41B H -0.1189 0.3971 0.1433 0.109 Uiso 1 1 calc R . . H41C H -0.0969 0.4089 0.2323 0.109 Uiso 1 1 calc R . . C40 C 0.0524(6) 0.3021(2) 0.1342(3) 0.0759(17) Uani 1 1 d . . . H40 H -0.0084 0.3013 0.0908 0.091 Uiso 1 1 calc R . . C34 C 0.6541(7) 0.1420(4) 0.4478(4) 0.106(2) Uani 1 1 d . . . H34 H 0.7010 0.1773 0.4622 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0357(3) 0.0306(2) 0.0402(3) 0.0032(2) -0.0008(2) -0.0003(2) Fe 0.0366(3) 0.0365(3) 0.0398(3) 0.0021(3) 0.0026(3) -0.0041(3) P1 0.0411(6) 0.0321(5) 0.0354(5) 0.0020(5) -0.0009(5) -0.0022(5) P2 0.0365(6) 0.0387(6) 0.0350(5) 0.0020(5) -0.0012(5) -0.0035(5) C35 0.032(2) 0.0290(19) 0.044(2) 0.0052(18) 0.0002(18) -0.0025(17) C13 0.034(2) 0.042(2) 0.038(2) 0.0014(19) -0.0011(18) -0.0052(18) N 0.0361(19) 0.0315(17) 0.0436(19) 0.0039(15) -0.0024(16) 0.0007(15) C18 0.058(3) 0.046(3) 0.051(3) 0.017(2) 0.005(2) -0.014(2) C19 0.042(2) 0.031(2) 0.034(2) 0.0030(17) -0.0014(18) -0.0014(18) C1 0.046(3) 0.041(2) 0.039(2) 0.0021(19) -0.004(2) -0.010(2) C23 0.046(2) 0.033(2) 0.039(2) 0.0007(18) 0.004(2) -0.0030(19) C7 0.043(3) 0.050(3) 0.043(2) 0.003(2) 0.008(2) -0.001(2) C14 0.039(2) 0.052(3) 0.043(2) 0.005(2) -0.007(2) 0.011(2) C36 0.044(3) 0.044(2) 0.055(3) -0.003(2) 0.001(2) 0.007(2) C8 0.052(3) 0.056(3) 0.067(3) 0.014(3) 0.017(3) 0.011(2) C20 0.047(3) 0.042(2) 0.044(2) 0.004(2) 0.008(2) -0.003(2) C15 0.042(3) 0.077(3) 0.056(3) 0.004(3) -0.003(2) -0.026(3) C21 0.044(3) 0.032(2) 0.048(2) 0.0002(19) -0.003(2) 0.0071(19) C37 0.061(3) 0.054(3) 0.052(3) -0.018(2) 0.007(3) 0.013(2) C24 0.077(3) 0.043(3) 0.043(2) -0.003(2) 0.009(2) 0.006(2) C9 0.038(2) 0.036(2) 0.043(2) 0.0016(19) 0.0041(19) -0.0036(18) C42 0.039(2) 0.042(2) 0.035(2) 0.0057(19) 0.0045(18) 0.0015(19) C16 0.050(3) 0.049(3) 0.042(2) -0.005(2) -0.001(2) -0.013(2) C17 0.029(2) 0.089(4) 0.059(3) 0.017(3) 0.004(2) 0.002(2) C25 0.078(4) 0.064(3) 0.086(4) -0.010(3) -0.002(3) 0.032(3) C10 0.049(3) 0.053(3) 0.058(3) -0.011(2) 0.004(2) -0.004(2) C2 0.096(5) 0.076(4) 0.063(4) 0.033(3) -0.031(3) -0.032(4) C26 0.066(3) 0.048(3) 0.061(3) -0.005(2) 0.005(3) 0.012(2) C3 0.046(3) 0.076(3) 0.065(3) 0.028(3) -0.005(2) -0.002(3) C29 0.039(2) 0.053(3) 0.036(2) 0.002(2) -0.0003(19) -0.003(2) C22 0.057(3) 0.034(2) 0.060(3) 0.007(2) -0.007(2) -0.001(2) C30 0.065(4) 0.098(5) 0.116(5) 0.022(4) -0.021(4) 0.022(4) C27 0.080(4) 0.062(3) 0.077(4) -0.026(3) 0.021(3) 0.004(3) C4 0.070(3) 0.063(3) 0.047(3) 0.006(2) 0.007(2) -0.004(3) C28 0.086(4) 0.058(3) 0.053(3) -0.010(3) 0.017(3) -0.005(3) C11 0.069(4) 0.052(3) 0.069(3) -0.017(3) 0.017(3) -0.014(3) C38 0.065(3) 0.063(3) 0.042(3) -0.016(2) -0.013(2) 0.014(3) C5 0.058(4) 0.084(4) 0.099(5) 0.037(4) -0.028(3) -0.004(3) C12 0.066(4) 0.048(3) 0.080(4) -0.002(3) 0.020(3) 0.002(3) C39 0.065(3) 0.070(3) 0.051(3) -0.022(3) -0.014(3) 0.031(3) C6 0.102(5) 0.069(3) 0.042(3) 0.013(3) -0.004(3) -0.016(3) C31 0.053(3) 0.068(3) 0.102(4) 0.003(3) -0.020(3) 0.007(3) C32 0.041(3) 0.151(7) 0.063(4) -0.014(4) -0.006(3) -0.003(4) C33 0.068(4) 0.073(4) 0.128(5) -0.005(4) -0.041(4) -0.016(3) O 0.0449(18) 0.0383(16) 0.066(2) -0.0006(15) 0.0101(16) -0.0106(14) F1 0.0521(18) 0.0465(16) 0.165(3) 0.0081(19) 0.0098(19) 0.0129(14) F2 0.075(2) 0.106(3) 0.152(3) -0.015(2) -0.058(2) 0.030(2) F3 0.110(3) 0.120(3) 0.123(3) 0.048(2) 0.071(2) 0.064(2) C43 0.041(3) 0.051(3) 0.062(3) 0.008(2) 0.000(2) 0.003(2) C41 0.056(3) 0.068(3) 0.092(4) -0.015(3) -0.002(3) 0.025(3) C40 0.069(4) 0.091(4) 0.065(3) -0.027(3) -0.029(3) 0.038(3) C34 0.071(5) 0.113(6) 0.131(6) -0.029(5) -0.030(4) -0.024(4) _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 Cu N 1.979(3) . ? Cu P2 2.2396(12) . ? Cu P1 2.2607(12) . ? Fe C21 2.035(4) . ? Fe C16 2.039(4) . ? Fe C15 2.041(4) . ? Fe C14 2.042(4) . ? Fe C19 2.045(4) . ? Fe C13 2.046(4) . ? Fe C17 2.048(4) . ? Fe C22 2.052(4) . ? Fe C18 2.054(4) . ? Fe C20 2.054(4) . ? P1 C19 1.810(4) . ? P1 C23 1.815(4) . ? P1 C29 1.826(4) . ? P2 C13 1.808(4) . ? P2 C9 1.819(4) . ? P2 C1 1.835(4) . ? C35 C39 1.360(6) . ? C35 C38 1.366(6) . ? C35 N 1.443(5) . ? C13 C16 1.422(5) . ? C13 C14 1.438(5) . ? N C42 1.319(5) . ? C18 C22 1.401(6) . ? C18 C20 1.403(6) . ? C18 H18 0.9300 . ? C19 C20 1.431(5) . ? C19 C21 1.435(5) . ? C1 C3 1.367(6) . ? C1 C4 1.392(6) . ? C23 C26 1.388(6) . ? C23 C24 1.396(5) . ? C7 C9 1.378(6) . ? C7 C8 1.393(6) . ? C7 H7 0.9300 . ? C14 C17 1.415(6) . ? C14 H14 0.9300 . ? C36 C37 1.353(6) . ? C36 C40 1.378(6) . ? C36 C41 1.503(6) . ? C8 C12 1.371(7) . ? C8 H8 0.9300 . ? C20 H20 0.9300 . ? C15 C17 1.404(7) . ? C15 C16 1.411(6) . ? C15 H15 0.9300 . ? C21 C22 1.414(6) . ? C21 H21 0.9300 . ? C37 C38 1.384(6) . ? C37 H37 0.9300 . ? C24 C28 1.384(6) . ? C24 H24 0.9300 . ? C9 C10 1.395(6) . ? C42 O 1.232(5) . ? C42 C43 1.534(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C25 C27 1.368(7) . ? C25 C26 1.389(6) . ? C25 H25 0.9300 . ? C10 C11 1.374(6) . ? C10 H10 0.9300 . ? C2 C6 1.355(8) . ? C2 C5 1.375(8) . ? C2 H2 0.9300 . ? C26 H26 0.9300 . ? C3 C5 1.398(6) . ? C3 H3 0.9300 . ? C29 C33 1.361(6) . ? C29 C31 1.367(6) . ? C22 H22 0.9300 . ? C30 C32 1.333(8) . ? C30 C31 1.393(7) . ? C30 H30 0.9300 . ? C27 C28 1.363(7) . ? C27 H27 0.9300 . ? C4 C6 1.374(6) . ? C4 H4 0.9300 . ? C28 H28 0.9300 . ? C11 C12 1.372(7) . ? C11 H11 0.9300 . ? C38 H38 0.9300 . ? C5 H5 0.9300 . ? C12 H12 0.9300 . ? C39 C40 1.383(6) . ? C39 H39 0.9300 . ? C6 H6 0.9300 . ? C31 H31 0.9300 . ? C32 C34 1.353(9) . ? C32 H32 0.9300 . ? C33 C34 1.381(8) . ? C33 H33 0.9300 . ? F1 C43 1.318(5) . ? F2 C43 1.304(5) . ? F3 C43 1.308(5) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C40 H40 0.9300 . ? C34 H34 0.9300 . ? 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 N Cu P2 126.81(10) . . ? N Cu P1 119.29(10) . . ? P2 Cu P1 112.55(4) . . ? C21 Fe C16 112.20(18) . . ? C21 Fe C15 139.30(19) . . ? C16 Fe C15 40.48(17) . . ? C21 Fe C14 140.67(17) . . ? C16 Fe C14 68.56(17) . . ? C15 Fe C14 68.09(19) . . ? C21 Fe C19 41.18(15) . . ? C16 Fe C19 142.29(17) . . ? C15 Fe C19 177.04(17) . . ? C14 Fe C19 113.28(16) . . ? C21 Fe C13 112.38(16) . . ? C16 Fe C13 40.75(15) . . ? C15 Fe C13 68.41(17) . . ? C14 Fe C13 41.20(15) . . ? C19 Fe C13 114.41(15) . . ? C21 Fe C17 178.84(18) . . ? C16 Fe C17 68.02(19) . . ? C15 Fe C17 40.17(19) . . ? C14 Fe C17 40.48(17) . . ? C19 Fe C17 139.27(19) . . ? C13 Fe C17 68.56(17) . . ? C21 Fe C22 40.49(16) . . ? C16 Fe C22 109.89(18) . . ? C15 Fe C22 110.17(19) . . ? C14 Fe C22 178.21(18) . . ? C19 Fe C22 68.48(16) . . ? C13 Fe C22 138.11(18) . . ? C17 Fe C22 138.36(19) . . ? C21 Fe C18 67.74(18) . . ? C16 Fe C18 135.92(17) . . ? C15 Fe C18 109.18(18) . . ? C14 Fe C18 140.67(18) . . ? C19 Fe C18 68.04(16) . . ? C13 Fe C18 176.65(17) . . ? C17 Fe C18 111.27(19) . . ? C22 Fe C18 39.89(17) . . ? C21 Fe C20 68.46(17) . . ? C16 Fe C20 175.65(16) . . ? C15 Fe C20 136.30(18) . . ? C14 Fe C20 113.87(17) . . ? C19 Fe C20 40.87(15) . . ? C13 Fe C20 143.40(16) . . ? C17 Fe C20 111.24(19) . . ? C22 Fe C20 67.61(17) . . ? C18 Fe C20 39.95(16) . . ? C19 P1 C23 101.68(18) . . ? C19 P1 C29 105.66(19) . . ? C23 P1 C29 103.58(19) . . ? C19 P1 Cu 116.61(13) . . ? C23 P1 Cu 113.53(13) . . ? C29 P1 Cu 114.23(13) . . ? C13 P2 C9 103.56(18) . . ? C13 P2 C1 104.43(19) . . ? C9 P2 C1 103.44(19) . . ? C13 P2 Cu 111.88(13) . . ? C9 P2 Cu 115.16(14) . . ? C1 P2 Cu 116.93(13) . . ? C39 C35 C38 117.4(4) . . ? C39 C35 N 119.3(4) . . ? C38 C35 N 123.1(4) . . ? C16 C13 C14 106.9(4) . . ? C16 C13 P2 129.3(3) . . ? C14 C13 P2 123.7(3) . . ? C16 C13 Fe 69.4(2) . . ? C14 C13 Fe 69.3(2) . . ? P2 C13 Fe 124.0(2) . . ? C42 N C35 116.8(3) . . ? C42 N Cu 133.3(3) . . ? C35 N Cu 108.8(2) . . ? C22 C18 C20 109.1(4) . . ? C22 C18 Fe 70.0(2) . . ? C20 C18 Fe 70.0(2) . . ? C22 C18 H18 125.4 . . ? C20 C18 H18 125.4 . . ? Fe C18 H18 126.1 . . ? C20 C19 C21 106.7(3) . . ? C20 C19 P1 126.8(3) . . ? C21 C19 P1 126.2(3) . . ? C20 C19 Fe 69.9(2) . . ? C21 C19 Fe 69.0(2) . . ? P1 C19 Fe 122.14(19) . . ? C3 C1 C4 118.5(4) . . ? C3 C1 P2 121.4(3) . . ? C4 C1 P2 119.7(4) . . ? C26 C23 C24 118.5(4) . . ? C26 C23 P1 119.0(3) . . ? C24 C23 P1 122.4(3) . . ? C9 C7 C8 120.3(4) . . ? C9 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C17 C14 C13 107.8(4) . . ? C17 C14 Fe 70.0(3) . . ? C13 C14 Fe 69.5(2) . . ? C17 C14 H14 126.1 . . ? C13 C14 H14 126.1 . . ? Fe C14 H14 126.0 . . ? C37 C36 C40 116.3(4) . . ? C37 C36 C41 122.1(4) . . ? C40 C36 C41 121.6(4) . . ? C12 C8 C7 120.3(5) . . ? C12 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C18 C20 C19 108.0(4) . . ? C18 C20 Fe 70.0(2) . . ? C19 C20 Fe 69.2(2) . . ? C18 C20 H20 126.0 . . ? C19 C20 H20 126.0 . . ? Fe C20 H20 126.3 . . ? C17 C15 C16 108.5(4) . . ? C17 C15 Fe 70.2(3) . . ? C16 C15 Fe 69.7(2) . . ? C17 C15 H15 125.7 . . ? C16 C15 H15 125.7 . . ? Fe C15 H15 126.0 . . ? C22 C21 C19 108.0(4) . . ? C22 C21 Fe 70.4(2) . . ? C19 C21 Fe 69.8(2) . . ? C22 C21 H21 126.0 . . ? C19 C21 H21 126.0 . . ? Fe C21 H21 125.4 . . ? C36 C37 C38 122.5(4) . . ? C36 C37 H37 118.8 . . ? C38 C37 H37 118.8 . . ? C28 C24 C23 120.1(5) . . ? C28 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C7 C9 C10 118.4(4) . . ? C7 C9 P2 119.7(3) . . ? C10 C9 P2 122.0(3) . . ? O C42 N 130.6(4) . . ? O C42 C43 115.3(4) . . ? N C42 C43 114.1(4) . . ? C15 C16 C13 108.3(4) . . ? C15 C16 Fe 69.8(3) . . ? C13 C16 Fe 69.9(2) . . ? C15 C16 H16 125.8 . . ? C13 C16 H16 125.8 . . ? Fe C16 H16 126.0 . . ? C15 C17 C14 108.3(4) . . ? C15 C17 Fe 69.7(3) . . ? C14 C17 Fe 69.5(2) . . ? C15 C17 H17 125.8 . . ? C14 C17 H17 125.8 . . ? Fe C17 H17 126.6 . . ? C27 C25 C26 120.3(5) . . ? C27 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C11 C10 C9 121.0(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C6 C2 C5 120.4(5) . . ? C6 C2 H2 119.8 . . ? C5 C2 H2 119.8 . . ? C23 C26 C25 120.3(5) . . ? C23 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C1 C3 C5 120.4(5) . . ? C1 C3 H3 119.8 . . ? C5 C3 H3 119.8 . . ? C33 C29 C31 117.3(5) . . ? C33 C29 P1 118.1(4) . . ? C31 C29 P1 124.3(4) . . ? C18 C22 C21 108.1(4) . . ? C18 C22 Fe 70.1(2) . . ? C21 C22 Fe 69.1(2) . . ? C18 C22 H22 125.9 . . ? C21 C22 H22 125.9 . . ? Fe C22 H22 126.4 . . ? C32 C30 C31 122.1(6) . . ? C32 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C28 C27 C25 120.2(5) . . ? C28 C27 H27 119.9 . . ? C25 C27 H27 119.9 . . ? C6 C4 C1 121.1(5) . . ? C6 C4 H4 119.4 . . ? C1 C4 H4 119.4 . . ? C27 C28 C24 120.6(5) . . ? C27 C28 H28 119.7 . . ? C24 C28 H28 119.7 . . ? C12 C11 C10 120.1(5) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C35 C38 C37 120.9(4) . . ? C35 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C2 C5 C3 119.7(5) . . ? C2 C5 H5 120.2 . . ? C3 C5 H5 120.2 . . ? C8 C12 C11 119.8(5) . . ? C8 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C35 C39 C40 121.3(4) . . ? C35 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C2 C6 C4 120.0(5) . . ? C2 C6 H6 120.0 . . ? C4 C6 H6 120.0 . . ? C29 C31 C30 119.7(5) . . ? C29 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C30 C32 C34 119.0(6) . . ? C30 C32 H32 120.5 . . ? C34 C32 H32 120.5 . . ? C29 C33 C34 122.4(6) . . ? C29 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? F2 C43 F3 105.5(4) . . ? F2 C43 F1 105.5(4) . . ? F3 C43 F1 105.6(4) . . ? F2 C43 C42 112.2(4) . . ? F3 C43 C42 111.0(4) . . ? F1 C43 C42 116.3(4) . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C40 C39 121.6(5) . . ? C36 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C32 C34 C33 119.6(6) . . ? C32 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.301 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.070 # Attachment 'lxf-29-1.cif' data_lxf-29-1 _database_code_depnum_ccdc_archive 'CCDC 859531' #TrackingRef 'lxf-29-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H32 Cl Cu F3 Fe N O P2' _chemical_formula_weight 840.47 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' 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' Cu Cu 0.3201 1.2651 '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 9.5154(19) _cell_length_b 22.267(5) _cell_length_c 17.178(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.80(3) _cell_angle_gamma 90.00 _cell_volume 3635.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 223.15 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 3.0179 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 1.197 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5932 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223.15 _diffrn_radiation_wavelength 0.710747 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% NONE _diffrn_reflns_number 20645 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8262 _reflns_number_gt 6927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+1.3449P] 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 8262 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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 Cu Cu 0.29419(4) 0.138001(17) 0.71772(2) 0.03382(12) Uani 1 1 d . . . Fe Fe 0.02521(5) 0.00590(2) 0.77286(3) 0.03474(13) Uani 1 1 d . . . P1 P 0.27915(9) 0.10159(4) 0.83943(5) 0.03393(19) Uani 1 1 d . . . P2 P 0.17787(9) 0.08229(4) 0.62773(5) 0.0344(2) Uani 1 1 d . . . N N 0.3689(3) 0.21998(12) 0.70254(16) 0.0366(6) Uani 1 1 d . . . C13 C 0.0251(3) 0.04710(15) 0.66643(18) 0.0359(7) Uani 1 1 d . . . C35 C 0.2569(3) 0.26278(14) 0.69916(19) 0.0345(7) Uani 1 1 d . . . C1 C 0.1104(4) 0.12187(15) 0.54011(19) 0.0393(8) Uani 1 1 d . . . C36 C 0.0288(4) 0.34019(17) 0.6937(2) 0.0478(9) Uani 1 1 d . . . C18 C 0.0201(4) -0.03947(16) 0.8764(2) 0.0472(9) Uani 1 1 d . . . H18 H -0.0587 -0.0576 0.8962 0.057 Uiso 1 1 calc R . . C19 C 0.1883(3) 0.03049(14) 0.84853(18) 0.0346(7) Uani 1 1 d . . . C23 C 0.4490(4) 0.09232(17) 0.89164(19) 0.0413(8) Uani 1 1 d . . . C29 C 0.1972(4) 0.14636(16) 0.9837(2) 0.0495(9) Uani 1 1 d . . . H29 H 0.2626 0.1199 1.0066 0.059 Uiso 1 1 calc R . . C7 C 0.4047(4) 0.00400(16) 0.6253(2) 0.0421(8) Uani 1 1 d . . . H7 H 0.4407 0.0260 0.6677 0.051 Uiso 1 1 calc R . . C30 C 0.1807(4) 0.14997(15) 0.90287(19) 0.0400(8) Uani 1 1 d . . . C20 C 0.2193(4) -0.02429(15) 0.8093(2) 0.0410(8) Uani 1 1 d . . . H20 H 0.2939 -0.0306 0.7772 0.049 Uiso 1 1 calc R . . C21 C 0.0636(4) 0.02040(16) 0.88995(19) 0.0401(8) Uani 1 1 d . . . H21 H 0.0190 0.0484 0.9205 0.048 Uiso 1 1 calc R . . C37 C 0.1158(5) 0.33807(18) 0.7580(2) 0.0562(10) Uani 1 1 d . . . H37 H 0.0994 0.3627 0.8003 0.067 Uiso 1 1 calc R . . C14 C -0.1730(4) 0.0343(2) 0.7371(2) 0.0533(10) Uani 1 1 d . . . H14 H -0.2477 0.0418 0.7686 0.064 Uiso 1 1 calc R . . C15 C -0.0208(4) -0.01403(17) 0.6583(2) 0.0445(8) Uani 1 1 d . . . H15 H 0.0215 -0.0438 0.6294 0.053 Uiso 1 1 calc R . . C16 C -0.1420(4) -0.0209(2) 0.7021(2) 0.0550(10) Uani 1 1 d . . . H16 H -0.1929 -0.0563 0.7069 0.066 Uiso 1 1 calc R . . C8 C 0.4796(4) -0.04482(17) 0.5980(2) 0.0523(10) Uani 1 1 d . . . H8 H 0.5646 -0.0560 0.6229 0.063 Uiso 1 1 calc R . . C22 C 0.1161(4) -0.06718(16) 0.8279(2) 0.0486(9) Uani 1 1 d . . . H22 H 0.1124 -0.1068 0.8110 0.058 Uiso 1 1 calc R . . C9 C 0.2766(3) 0.01973(15) 0.58913(19) 0.0369(7) Uani 1 1 d . . . C38 C 0.1685(4) 0.2665(2) 0.6346(2) 0.0601(11) Uani 1 1 d . . . H38 H 0.1864 0.2428 0.5915 0.072 Uiso 1 1 calc R . . C10 C 0.2260(4) -0.01258(17) 0.5244(2) 0.0473(9) Uani 1 1 d . . . H10 H 0.1404 -0.0022 0.4995 0.057 Uiso 1 1 calc R . . C2 C 0.0271(6) 0.1915(2) 0.4123(3) 0.0702(14) Uani 1 1 d . . . H2 H -0.0017 0.2145 0.3693 0.084 Uiso 1 1 calc R . . C24 C 0.6556(6) 0.1410(3) 0.9462(3) 0.0941(18) Uani 1 1 d . . . H24 H 0.7037 0.1762 0.9591 0.113 Uiso 1 1 calc R . . C11 C 0.3031(5) -0.06006(18) 0.4971(2) 0.0567(10) Uani 1 1 d . . . H11 H 0.2700 -0.0810 0.4531 0.068 Uiso 1 1 calc R . . C12 C 0.4274(4) -0.07651(18) 0.5342(3) 0.0578(11) Uani 1 1 d . . . H12 H 0.4770 -0.1093 0.5162 0.069 Uiso 1 1 calc R . . C17 C -0.0701(4) 0.07635(17) 0.7159(2) 0.0434(8) Uani 1 1 d . . . H17 H -0.0653 0.1163 0.7315 0.052 Uiso 1 1 calc R . . C3 C -0.0157(4) 0.15141(19) 0.5383(2) 0.0566(10) Uani 1 1 d . . . H3 H -0.0734 0.1481 0.5803 0.068 Uiso 1 1 calc R . . C25 C 0.5124(4) 0.0380(2) 0.9070(3) 0.0617(11) Uani 1 1 d . . . H25 H 0.4657 0.0025 0.8934 0.074 Uiso 1 1 calc R . . C31 C 0.0845(4) 0.19035(17) 0.8693(2) 0.0533(10) Uani 1 1 d . . . H31 H 0.0749 0.1938 0.8154 0.064 Uiso 1 1 calc R . . C4 C 0.1544(6) 0.1632(2) 0.4131(2) 0.0667(13) Uani 1 1 d . . . H4 H 0.2124 0.1672 0.3714 0.080 Uiso 1 1 calc R . . C5 C 0.1955(5) 0.12864(18) 0.4768(2) 0.0543(10) Uani 1 1 d . . . H5 H 0.2821 0.1093 0.4775 0.065 Uiso 1 1 calc R . . C26 C 0.6466(5) 0.0360(3) 0.9429(3) 0.0809(15) Uani 1 1 d . . . H26 H 0.6890 -0.0010 0.9532 0.097 Uiso 1 1 calc R . . C32 C 0.1164(5) 0.18210(18) 1.0301(3) 0.0602(11) Uani 1 1 d . . . H32 H 0.1273 0.1796 1.0841 0.072 Uiso 1 1 calc R . . C33 C 0.0027(5) 0.2256(2) 0.9158(3) 0.0688(13) Uani 1 1 d . . . H33 H -0.0633 0.2519 0.8932 0.083 Uiso 1 1 calc R . . C39 C 0.2292(4) 0.29932(18) 0.7610(2) 0.0549(10) Uani 1 1 d . . . H39 H 0.2881 0.2979 0.8058 0.066 Uiso 1 1 calc R . . C6 C -0.0591(5) 0.1867(2) 0.4737(3) 0.0732(14) Uani 1 1 d . . . H6 H -0.1452 0.2066 0.4726 0.088 Uiso 1 1 calc R . . C40 C 0.0530(5) 0.3043(2) 0.6311(3) 0.0778(16) Uani 1 1 d . . . H40 H -0.0073 0.3053 0.5869 0.093 Uiso 1 1 calc R . . C27 C 0.7166(5) 0.0872(3) 0.9630(3) 0.0818(17) Uani 1 1 d . . . H27 H 0.8054 0.0854 0.9880 0.098 Uiso 1 1 calc R . . C28 C 0.5236(5) 0.1439(2) 0.9103(3) 0.0761(14) Uani 1 1 d . . . H28 H 0.4840 0.1812 0.8985 0.091 Uiso 1 1 calc R . . C34 C 0.0200(5) 0.2213(2) 0.9961(3) 0.0683(13) Uani 1 1 d . . . H34 H -0.0341 0.2453 1.0274 0.082 Uiso 1 1 calc R . . Cl Cl -0.11392(13) 0.38978(6) 0.68953(8) 0.0805(4) Uani 1 1 d . . . O O 0.5388(3) 0.29423(11) 0.71240(16) 0.0510(6) Uani 1 1 d . . . F3 F 0.5739(3) 0.13755(10) 0.71145(19) 0.0806(8) Uani 1 1 d . . . F1 F 0.7114(3) 0.20167(15) 0.7617(2) 0.1043(11) Uani 1 1 d . . . F2 F 0.6815(3) 0.19790(15) 0.64097(19) 0.1081(12) Uani 1 1 d . . . C41 C 0.4976(4) 0.24103(15) 0.70777(19) 0.0372(7) Uani 1 1 d . . . C42 C 0.6145(4) 0.19457(17) 0.7057(2) 0.0505(9) 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 Cu 0.0329(2) 0.0299(2) 0.0385(2) 0.00246(17) -0.00024(16) -0.00062(16) Fe 0.0329(3) 0.0351(3) 0.0363(3) 0.0010(2) 0.00261(19) -0.00386(19) P1 0.0376(5) 0.0302(4) 0.0336(4) 0.0000(3) -0.0012(3) -0.0019(3) P2 0.0325(5) 0.0368(4) 0.0336(4) 0.0016(4) -0.0004(3) -0.0026(3) N 0.0343(15) 0.0313(14) 0.0440(15) 0.0028(12) -0.0002(12) 0.0005(11) C13 0.0299(17) 0.0444(19) 0.0329(16) 0.0031(15) -0.0023(13) -0.0009(14) C35 0.0345(17) 0.0284(15) 0.0405(17) 0.0035(14) 0.0016(13) -0.0019(13) C1 0.041(2) 0.0414(18) 0.0352(17) 0.0001(15) -0.0039(14) -0.0101(15) C36 0.041(2) 0.045(2) 0.058(2) -0.0028(19) 0.0047(17) 0.0079(16) C18 0.051(2) 0.045(2) 0.046(2) 0.0123(17) 0.0010(17) -0.0121(17) C19 0.0359(18) 0.0325(16) 0.0350(16) 0.0025(14) -0.0016(13) 0.0005(14) C23 0.0368(19) 0.053(2) 0.0336(17) -0.0041(16) -0.0019(14) -0.0036(16) C29 0.065(3) 0.0389(19) 0.045(2) -0.0029(17) 0.0090(18) -0.0005(17) C7 0.0372(19) 0.048(2) 0.0417(18) 0.0047(16) 0.0039(15) -0.0019(15) C30 0.046(2) 0.0343(17) 0.0398(18) -0.0025(15) 0.0014(15) -0.0052(15) C20 0.042(2) 0.0338(17) 0.0474(19) 0.0018(16) -0.0010(15) 0.0046(15) C21 0.043(2) 0.0423(18) 0.0352(17) 0.0031(15) 0.0038(14) -0.0045(15) C37 0.067(3) 0.052(2) 0.050(2) -0.0145(19) 0.0049(19) 0.013(2) C14 0.0276(18) 0.083(3) 0.049(2) 0.012(2) 0.0037(15) 0.0019(19) C15 0.047(2) 0.048(2) 0.0387(18) -0.0053(16) -0.0002(15) -0.0124(17) C16 0.046(2) 0.073(3) 0.045(2) 0.003(2) -0.0036(17) -0.023(2) C8 0.041(2) 0.052(2) 0.064(2) 0.011(2) 0.0080(18) 0.0049(17) C22 0.054(2) 0.0334(18) 0.058(2) 0.0052(17) -0.0035(18) -0.0034(16) C9 0.0332(18) 0.0375(17) 0.0404(17) 0.0009(15) 0.0058(14) -0.0029(14) C38 0.058(3) 0.069(3) 0.051(2) -0.017(2) -0.0126(19) 0.027(2) C10 0.041(2) 0.052(2) 0.049(2) -0.0074(18) -0.0008(16) -0.0067(17) C2 0.086(4) 0.069(3) 0.053(3) 0.027(2) -0.019(2) -0.025(3) C24 0.055(3) 0.118(5) 0.107(4) -0.032(4) -0.021(3) -0.024(3) C11 0.058(3) 0.053(2) 0.060(2) -0.019(2) 0.011(2) -0.007(2) C12 0.051(3) 0.042(2) 0.082(3) -0.005(2) 0.020(2) -0.0001(18) C17 0.0345(19) 0.048(2) 0.0471(19) 0.0082(17) -0.0015(15) 0.0084(16) C3 0.040(2) 0.066(3) 0.063(2) 0.020(2) -0.0026(18) -0.0020(19) C25 0.043(2) 0.063(3) 0.078(3) 0.009(2) -0.005(2) 0.006(2) C31 0.055(3) 0.051(2) 0.053(2) -0.0055(19) 0.0013(18) 0.0072(19) C4 0.091(4) 0.064(3) 0.044(2) 0.014(2) 0.002(2) -0.018(3) C5 0.061(3) 0.059(2) 0.043(2) 0.0063(19) 0.0056(18) -0.005(2) C26 0.049(3) 0.098(4) 0.095(4) 0.019(3) -0.009(3) 0.018(3) C32 0.078(3) 0.051(2) 0.053(2) -0.009(2) 0.016(2) -0.010(2) C33 0.062(3) 0.059(3) 0.085(3) -0.017(3) -0.001(2) 0.022(2) C39 0.059(3) 0.060(2) 0.044(2) -0.0076(19) -0.0127(18) 0.016(2) C6 0.055(3) 0.077(3) 0.086(3) 0.029(3) -0.021(2) -0.001(2) C40 0.071(3) 0.099(4) 0.061(3) -0.024(3) -0.026(2) 0.046(3) C27 0.036(2) 0.154(6) 0.055(3) -0.008(3) -0.007(2) 0.000(3) C28 0.059(3) 0.068(3) 0.099(4) -0.003(3) -0.025(3) -0.015(2) C34 0.072(3) 0.059(3) 0.076(3) -0.024(2) 0.025(2) 0.002(2) Cl 0.0625(7) 0.0827(8) 0.0957(9) -0.0162(7) -0.0017(6) 0.0375(6) O 0.0476(16) 0.0416(14) 0.0648(16) -0.0040(13) 0.0116(13) -0.0111(11) F3 0.0518(16) 0.0438(13) 0.147(3) 0.0094(15) 0.0116(16) 0.0114(11) F1 0.070(2) 0.103(2) 0.134(3) -0.012(2) -0.0507(19) 0.0236(17) F2 0.105(2) 0.111(2) 0.115(2) 0.045(2) 0.069(2) 0.0581(19) C41 0.0366(18) 0.0383(18) 0.0368(17) -0.0014(15) 0.0022(14) -0.0012(14) C42 0.038(2) 0.052(2) 0.061(2) 0.009(2) 0.0028(18) 0.0005(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 Cu N 1.981(3) . ? Cu P2 2.2330(10) . ? Cu P1 2.2535(10) . ? Fe C20 2.035(3) . ? Fe C17 2.038(3) . ? Fe C16 2.044(4) . ? Fe C15 2.044(3) . ? Fe C13 2.046(3) . ? Fe C18 2.048(3) . ? Fe C19 2.050(3) . ? Fe C22 2.052(4) . ? Fe C21 2.052(3) . ? Fe C14 2.054(4) . ? P1 C19 1.814(3) . ? P1 C23 1.821(4) . ? P1 C30 1.824(4) . ? P2 C13 1.807(3) . ? P2 C9 1.823(3) . ? P2 C1 1.833(3) . ? N C41 1.310(4) . ? N C35 1.429(4) . ? C13 C17 1.429(5) . ? C13 C15 1.434(5) . ? C35 C38 1.361(5) . ? C35 C39 1.374(5) . ? C1 C3 1.368(5) . ? C1 C5 1.396(5) . ? C36 C37 1.349(5) . ? C36 C40 1.368(6) . ? C36 Cl 1.749(4) . ? C18 C22 1.408(5) . ? C18 C21 1.412(5) . ? C18 H18 0.9300 . ? C19 C21 1.431(5) . ? C19 C20 1.431(4) . ? C23 C25 1.371(5) . ? C23 C28 1.381(5) . ? C29 C32 1.385(5) . ? C29 C30 1.392(5) . ? C29 H29 0.9300 . ? C7 C9 1.385(5) . ? C7 C8 1.393(5) . ? C7 H7 0.9300 . ? C30 C31 1.388(5) . ? C20 C22 1.418(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C37 C39 1.381(5) . ? C37 H37 0.9300 . ? C14 C16 1.406(6) . ? C14 C17 1.415(5) . ? C14 H14 0.9300 . ? C15 C16 1.415(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C8 C12 1.375(6) . ? C8 H8 0.9300 . ? C22 H22 0.9300 . ? C9 C10 1.391(5) . ? C38 C40 1.384(5) . ? C38 H38 0.9300 . ? C10 C11 1.382(5) . ? C10 H10 0.9300 . ? C2 C4 1.364(7) . ? C2 C6 1.372(7) . ? C2 H2 0.9300 . ? C24 C27 1.356(8) . ? C24 C28 1.373(7) . ? C24 H24 0.9300 . ? C11 C12 1.366(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C17 H17 0.9300 . ? C3 C6 1.405(6) . ? C3 H3 0.9300 . ? C25 C26 1.392(6) . ? C25 H25 0.9300 . ? C31 C33 1.385(6) . ? C31 H31 0.9300 . ? C4 C5 1.378(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C26 C27 1.356(8) . ? C26 H26 0.9300 . ? C32 C34 1.376(6) . ? C32 H32 0.9300 . ? C33 C34 1.385(6) . ? C33 H33 0.9300 . ? C39 H39 0.9300 . ? C6 H6 0.9300 . ? C40 H40 0.9300 . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C34 H34 0.9300 . ? O C41 1.249(4) . ? F3 C42 1.332(4) . ? F1 C42 1.309(5) . ? F2 C42 1.311(5) . ? C41 C42 1.521(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 N Cu P2 126.14(8) . . ? N Cu P1 119.55(8) . . ? P2 Cu P1 112.99(4) . . ? C20 Fe C17 141.05(14) . . ? C20 Fe C16 138.99(16) . . ? C17 Fe C16 67.93(17) . . ? C20 Fe C15 111.87(15) . . ? C17 Fe C15 68.62(15) . . ? C16 Fe C15 40.51(14) . . ? C20 Fe C13 112.57(14) . . ? C17 Fe C13 40.96(13) . . ? C16 Fe C13 68.45(14) . . ? C15 Fe C13 41.06(13) . . ? C20 Fe C18 68.27(15) . . ? C17 Fe C18 140.15(15) . . ? C16 Fe C18 108.78(15) . . ? C15 Fe C18 135.73(15) . . ? C13 Fe C18 176.77(14) . . ? C20 Fe C19 41.02(13) . . ? C17 Fe C19 113.85(14) . . ? C16 Fe C19 177.04(14) . . ? C15 Fe C19 142.04(14) . . ? C13 Fe C19 114.48(13) . . ? C18 Fe C19 68.30(14) . . ? C20 Fe C22 40.60(14) . . ? C17 Fe C22 177.84(15) . . ? C16 Fe C22 109.92(17) . . ? C15 Fe C22 109.71(16) . . ? C13 Fe C22 138.55(15) . . ? C18 Fe C22 40.16(15) . . ? C19 Fe C22 68.32(14) . . ? C20 Fe C21 68.62(14) . . ? C17 Fe C21 113.77(15) . . ? C16 Fe C21 136.50(15) . . ? C15 Fe C21 175.86(14) . . ? C13 Fe C21 142.92(14) . . ? C18 Fe C21 40.28(13) . . ? C19 Fe C21 40.84(13) . . ? C22 Fe C21 67.80(15) . . ? C20 Fe C14 178.48(15) . . ? C17 Fe C14 40.47(15) . . ? C16 Fe C14 40.14(17) . . ? C15 Fe C14 68.20(16) . . ? C13 Fe C14 68.55(14) . . ? C18 Fe C14 110.56(15) . . ? C19 Fe C14 139.74(16) . . ? C22 Fe C14 137.89(16) . . ? C21 Fe C14 111.19(15) . . ? C19 P1 C23 105.88(16) . . ? C19 P1 C30 101.73(16) . . ? C23 P1 C30 104.01(16) . . ? C19 P1 Cu 116.49(11) . . ? C23 P1 Cu 113.74(12) . . ? C30 P1 Cu 113.56(12) . . ? C13 P2 C9 103.93(15) . . ? C13 P2 C1 104.76(15) . . ? C9 P2 C1 103.59(16) . . ? C13 P2 Cu 111.52(11) . . ? C9 P2 Cu 115.43(11) . . ? C1 P2 Cu 116.31(11) . . ? C41 N C35 117.2(3) . . ? C41 N Cu 131.4(2) . . ? C35 N Cu 110.4(2) . . ? C17 C13 C15 107.0(3) . . ? C17 C13 P2 124.5(3) . . ? C15 C13 P2 128.5(3) . . ? C17 C13 Fe 69.24(19) . . ? C15 C13 Fe 69.42(19) . . ? P2 C13 Fe 123.92(17) . . ? C38 C35 C39 117.4(3) . . ? C38 C35 N 120.2(3) . . ? C39 C35 N 122.3(3) . . ? C3 C1 C5 118.2(3) . . ? C3 C1 P2 121.4(3) . . ? C5 C1 P2 119.9(3) . . ? C37 C36 C40 120.2(4) . . ? C37 C36 Cl 120.0(3) . . ? C40 C36 Cl 119.8(3) . . ? C22 C18 C21 108.6(3) . . ? C22 C18 Fe 70.1(2) . . ? C21 C18 Fe 70.02(19) . . ? C22 C18 H18 125.7 . . ? C21 C18 H18 125.7 . . ? Fe C18 H18 125.8 . . ? C21 C19 C20 107.2(3) . . ? C21 C19 P1 126.2(3) . . ? C20 C19 P1 126.4(3) . . ? C21 C19 Fe 69.67(19) . . ? C20 C19 Fe 68.94(19) . . ? P1 C19 Fe 121.85(16) . . ? C25 C23 C28 118.2(4) . . ? C25 C23 P1 124.5(3) . . ? C28 C23 P1 117.0(3) . . ? C32 C29 C30 120.1(4) . . ? C32 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C9 C7 C8 120.0(3) . . ? C9 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C31 C30 C29 119.4(3) . . ? C31 C30 P1 118.8(3) . . ? C29 C30 P1 121.7(3) . . ? C22 C20 C19 107.8(3) . . ? C22 C20 Fe 70.3(2) . . ? C19 C20 Fe 70.04(19) . . ? C22 C20 H20 126.1 . . ? C19 C20 H20 126.1 . . ? Fe C20 H20 125.1 . . ? C18 C21 C19 108.0(3) . . ? C18 C21 Fe 69.7(2) . . ? C19 C21 Fe 69.49(19) . . ? C18 C21 H21 126.0 . . ? C19 C21 H21 126.0 . . ? Fe C21 H21 126.4 . . ? C36 C37 C39 120.0(4) . . ? C36 C37 H37 120.0 . . ? C39 C37 H37 120.0 . . ? C16 C14 C17 107.8(3) . . ? C16 C14 Fe 69.5(2) . . ? C17 C14 Fe 69.2(2) . . ? C16 C14 H14 126.1 . . ? C17 C14 H14 126.1 . . ? Fe C14 H14 126.8 . . ? C16 C15 C13 107.6(3) . . ? C16 C15 Fe 69.7(2) . . ? C13 C15 Fe 69.52(18) . . ? C16 C15 H15 126.2 . . ? C13 C15 H15 126.2 . . ? Fe C15 H15 126.1 . . ? C14 C16 C15 109.0(3) . . ? C14 C16 Fe 70.3(2) . . ? C15 C16 Fe 69.8(2) . . ? C14 C16 H16 125.5 . . ? C15 C16 H16 125.5 . . ? Fe C16 H16 126.0 . . ? C12 C8 C7 119.8(4) . . ? C12 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C18 C22 C20 108.4(3) . . ? C18 C22 Fe 69.8(2) . . ? C20 C22 Fe 69.07(19) . . ? C18 C22 H22 125.8 . . ? C20 C22 H22 125.8 . . ? Fe C22 H22 126.9 . . ? C7 C9 C10 119.4(3) . . ? C7 C9 P2 119.2(3) . . ? C10 C9 P2 121.4(3) . . ? C35 C38 C40 122.0(4) . . ? C35 C38 H38 119.0 . . ? C40 C38 H38 119.0 . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C4 C2 C6 121.4(4) . . ? C4 C2 H2 119.3 . . ? C6 C2 H2 119.3 . . ? C27 C24 C28 120.7(5) . . ? C27 C24 H24 119.7 . . ? C28 C24 H24 119.7 . . ? C12 C11 C10 120.6(4) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C8 120.3(4) . . ? C11 C12 H12 119.8 . . ? C8 C12 H12 119.8 . . ? C14 C17 C13 108.5(3) . . ? C14 C17 Fe 70.4(2) . . ? C13 C17 Fe 69.80(19) . . ? C14 C17 H17 125.7 . . ? C13 C17 H17 125.7 . . ? Fe C17 H17 125.7 . . ? C1 C3 C6 120.7(4) . . ? C1 C3 H3 119.6 . . ? C6 C3 H3 119.6 . . ? C23 C25 C26 120.0(4) . . ? C23 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C33 C31 C30 120.3(4) . . ? C33 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C2 C4 C5 118.9(4) . . ? C2 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C1 121.7(4) . . ? C4 C5 H5 119.1 . . ? C1 C5 H5 119.1 . . ? C27 C26 C25 121.0(5) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C34 C32 C29 119.9(4) . . ? C34 C32 H32 120.0 . . ? C29 C32 H32 120.0 . . ? C34 C33 C31 119.6(4) . . ? C34 C33 H33 120.2 . . ? C31 C33 H33 120.2 . . ? C35 C39 C37 121.4(3) . . ? C35 C39 H39 119.3 . . ? C37 C39 H39 119.3 . . ? C2 C6 C3 119.1(4) . . ? C2 C6 H6 120.5 . . ? C3 C6 H6 120.5 . . ? C36 C40 C38 119.0(4) . . ? C36 C40 H40 120.5 . . ? C38 C40 H40 120.5 . . ? C26 C27 C24 119.2(4) . . ? C26 C27 H27 120.4 . . ? C24 C27 H27 120.4 . . ? C24 C28 C23 120.9(5) . . ? C24 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? C32 C34 C33 120.6(4) . . ? C32 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? O C41 N 129.3(3) . . ? O C41 C42 114.7(3) . . ? N C41 C42 115.9(3) . . ? F1 C42 F2 105.2(4) . . ? F1 C42 F3 104.9(3) . . ? F2 C42 F3 105.7(4) . . ? F1 C42 C41 113.0(3) . . ? F2 C42 C41 111.6(3) . . ? F3 C42 C41 115.6(3) . . ? 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 N Cu P1 C19 172.08(15) . . . . ? P2 Cu P1 C19 4.40(13) . . . . ? N Cu P1 C23 -64.33(16) . . . . ? P2 Cu P1 C23 127.98(13) . . . . ? N Cu P1 C30 54.37(16) . . . . ? P2 Cu P1 C30 -113.31(13) . . . . ? N Cu P2 C13 -135.12(15) . . . . ? P1 Cu P2 C13 31.60(13) . . . . ? N Cu P2 C9 106.59(15) . . . . ? P1 Cu P2 C9 -86.69(12) . . . . ? N Cu P2 C1 -15.09(17) . . . . ? P1 Cu P2 C1 151.63(13) . . . . ? P2 Cu N C41 -118.2(3) . . . . ? P1 Cu N C41 75.9(3) . . . . ? P2 Cu N C35 74.2(2) . . . . ? P1 Cu N C35 -91.8(2) . . . . ? C9 P2 C13 C17 167.5(3) . . . . ? C1 P2 C13 C17 -84.1(3) . . . . ? Cu P2 C13 C17 42.5(3) . . . . ? C9 P2 C13 C15 -8.9(3) . . . . ? C1 P2 C13 C15 99.5(3) . . . . ? Cu P2 C13 C15 -133.9(3) . . . . ? C9 P2 C13 Fe 80.7(2) . . . . ? C1 P2 C13 Fe -170.88(19) . . . . ? Cu P2 C13 Fe -44.3(2) . . . . ? C20 Fe C13 C17 -143.7(2) . . . . ? C16 Fe C13 C17 80.7(2) . . . . ? C15 Fe C13 C17 118.4(3) . . . . ? C18 Fe C13 C17 112(3) . . . . ? C19 Fe C13 C17 -98.8(2) . . . . ? C22 Fe C13 C17 176.8(2) . . . . ? C21 Fe C13 C17 -59.7(3) . . . . ? C14 Fe C13 C17 37.4(2) . . . . ? C20 Fe C13 C15 97.9(2) . . . . ? C17 Fe C13 C15 -118.4(3) . . . . ? C16 Fe C13 C15 -37.7(2) . . . . ? C18 Fe C13 C15 -6(3) . . . . ? C19 Fe C13 C15 142.8(2) . . . . ? C22 Fe C13 C15 58.4(3) . . . . ? C21 Fe C13 C15 -178.1(2) . . . . ? C14 Fe C13 C15 -81.0(2) . . . . ? C20 Fe C13 P2 -25.4(3) . . . . ? C17 Fe C13 P2 118.3(3) . . . . ? C16 Fe C13 P2 -161.0(3) . . . . ? C15 Fe C13 P2 -123.3(3) . . . . ? C18 Fe C13 P2 -130(3) . . . . ? C19 Fe C13 P2 19.5(3) . . . . ? C22 Fe C13 P2 -64.9(3) . . . . ? C21 Fe C13 P2 58.6(3) . . . . ? C14 Fe C13 P2 155.7(3) . . . . ? C41 N C35 C38 116.4(4) . . . . ? Cu N C35 C38 -74.0(4) . . . . ? C41 N C35 C39 -66.8(4) . . . . ? Cu N C35 C39 102.7(3) . . . . ? C13 P2 C1 C3 39.4(3) . . . . ? C9 P2 C1 C3 148.1(3) . . . . ? Cu P2 C1 C3 -84.2(3) . . . . ? C13 P2 C1 C5 -148.5(3) . . . . ? C9 P2 C1 C5 -39.8(3) . . . . ? Cu P2 C1 C5 87.9(3) . . . . ? C20 Fe C18 C22 -37.3(2) . . . . ? C17 Fe C18 C22 176.7(2) . . . . ? C16 Fe C18 C22 98.9(2) . . . . ? C15 Fe C18 C22 62.2(3) . . . . ? C13 Fe C18 C22 68(3) . . . . ? C19 Fe C18 C22 -81.7(2) . . . . ? C21 Fe C18 C22 -119.5(3) . . . . ? C14 Fe C18 C22 141.6(2) . . . . ? C20 Fe C18 C21 82.1(2) . . . . ? C17 Fe C18 C21 -63.8(3) . . . . ? C16 Fe C18 C21 -141.6(2) . . . . ? C15 Fe C18 C21 -178.3(2) . . . . ? C13 Fe C18 C21 -172(3) . . . . ? C19 Fe C18 C21 37.8(2) . . . . ? C22 Fe C18 C21 119.5(3) . . . . ? C14 Fe C18 C21 -98.9(2) . . . . ? C23 P1 C19 C21 113.8(3) . . . . ? C30 P1 C19 C21 5.4(3) . . . . ? Cu P1 C19 C21 -118.6(3) . . . . ? C23 P1 C19 C20 -73.1(3) . . . . ? C30 P1 C19 C20 178.5(3) . . . . ? Cu P1 C19 C20 54.4(3) . . . . ? C23 P1 C19 Fe -159.21(18) . . . . ? C30 P1 C19 Fe 92.4(2) . . . . ? Cu P1 C19 Fe -31.7(2) . . . . ? C20 Fe C19 C21 -118.7(3) . . . . ? C17 Fe C19 C21 99.4(2) . . . . ? C16 Fe C19 C21 -27(3) . . . . ? C15 Fe C19 C21 -175.3(2) . . . . ? C13 Fe C19 C21 144.5(2) . . . . ? C18 Fe C19 C21 -37.3(2) . . . . ? C22 Fe C19 C21 -80.7(2) . . . . ? C14 Fe C19 C21 59.3(3) . . . . ? C17 Fe C19 C20 -141.9(2) . . . . ? C16 Fe C19 C20 92(3) . . . . ? C15 Fe C19 C20 -56.6(3) . . . . ? C13 Fe C19 C20 -96.8(2) . . . . ? C18 Fe C19 C20 81.4(2) . . . . ? C22 Fe C19 C20 38.0(2) . . . . ? C21 Fe C19 C20 118.7(3) . . . . ? C14 Fe C19 C20 178.0(2) . . . . ? C20 Fe C19 P1 120.6(3) . . . . ? C17 Fe C19 P1 -21.3(2) . . . . ? C16 Fe C19 P1 -148(3) . . . . ? C15 Fe C19 P1 64.0(3) . . . . ? C13 Fe C19 P1 23.8(2) . . . . ? C18 Fe C19 P1 -158.0(2) . . . . ? C22 Fe C19 P1 158.6(2) . . . . ? C21 Fe C19 P1 -120.7(3) . . . . ? C14 Fe C19 P1 -61.4(3) . . . . ? C19 P1 C23 C25 22.2(4) . . . . ? C30 P1 C23 C25 129.0(3) . . . . ? Cu P1 C23 C25 -107.0(3) . . . . ? C19 P1 C23 C28 -164.1(3) . . . . ? C30 P1 C23 C28 -57.3(4) . . . . ? Cu P1 C23 C28 66.8(4) . . . . ? C32 C29 C30 C31 1.1(6) . . . . ? C32 C29 C30 P1 -177.3(3) . . . . ? C19 P1 C30 C31 -103.2(3) . . . . ? C23 P1 C30 C31 146.9(3) . . . . ? Cu P1 C30 C31 22.8(3) . . . . ? C19 P1 C30 C29 75.3(3) . . . . ? C23 P1 C30 C29 -34.6(3) . . . . ? Cu P1 C30 C29 -158.8(3) . . . . ? C21 C19 C20 C22 -1.0(4) . . . . ? P1 C19 C20 C22 -175.2(2) . . . . ? Fe C19 C20 C22 -60.5(2) . . . . ? C21 C19 C20 Fe 59.4(2) . . . . ? P1 C19 C20 Fe -114.7(3) . . . . ? C17 Fe C20 C22 -177.8(2) . . . . ? C16 Fe C20 C22 -57.1(3) . . . . ? C15 Fe C20 C22 -95.2(2) . . . . ? C13 Fe C20 C22 -139.7(2) . . . . ? C18 Fe C20 C22 37.0(2) . . . . ? C19 Fe C20 C22 118.4(3) . . . . ? C21 Fe C20 C22 80.4(2) . . . . ? C14 Fe C20 C22 -3(6) . . . . ? C17 Fe C20 C19 63.8(3) . . . . ? C16 Fe C20 C19 -175.5(2) . . . . ? C15 Fe C20 C19 146.40(19) . . . . ? C13 Fe C20 C19 101.9(2) . . . . ? C18 Fe C20 C19 -81.5(2) . . . . ? C22 Fe C20 C19 -118.4(3) . . . . ? C21 Fe C20 C19 -38.02(19) . . . . ? C14 Fe C20 C19 -121(6) . . . . ? C22 C18 C21 C19 0.6(4) . . . . ? Fe C18 C21 C19 -59.1(2) . . . . ? C22 C18 C21 Fe 59.7(3) . . . . ? C20 C19 C21 C18 0.3(4) . . . . ? P1 C19 C21 C18 174.5(2) . . . . ? Fe C19 C21 C18 59.2(2) . . . . ? C20 C19 C21 Fe -59.0(2) . . . . ? P1 C19 C21 Fe 115.2(3) . . . . ? C20 Fe C21 C18 -81.2(2) . . . . ? C17 Fe C21 C18 141.1(2) . . . . ? C16 Fe C21 C18 58.7(3) . . . . ? C15 Fe C21 C18 16(2) . . . . ? C13 Fe C21 C18 179.3(2) . . . . ? C19 Fe C21 C18 -119.4(3) . . . . ? C22 Fe C21 C18 -37.3(2) . . . . ? C14 Fe C21 C18 97.2(3) . . . . ? C20 Fe C21 C19 38.19(19) . . . . ? C17 Fe C21 C19 -99.6(2) . . . . ? C16 Fe C21 C19 178.1(2) . . . . ? C15 Fe C21 C19 136(2) . . . . ? C13 Fe C21 C19 -61.3(3) . . . . ? C18 Fe C21 C19 119.4(3) . . . . ? C22 Fe C21 C19 82.1(2) . . . . ? C14 Fe C21 C19 -143.4(2) . . . . ? C40 C36 C37 C39 -0.4(7) . . . . ? Cl C36 C37 C39 -179.4(3) . . . . ? C20 Fe C14 C16 -56(6) . . . . ? C17 Fe C14 C16 119.5(3) . . . . ? C15 Fe C14 C16 37.3(2) . . . . ? C13 Fe C14 C16 81.6(2) . . . . ? C18 Fe C14 C16 -95.1(2) . . . . ? C19 Fe C14 C16 -175.4(2) . . . . ? C22 Fe C14 C16 -58.4(3) . . . . ? C21 Fe C14 C16 -138.3(2) . . . . ? C20 Fe C14 C17 -175(49) . . . . ? C16 Fe C14 C17 -119.5(3) . . . . ? C15 Fe C14 C17 -82.2(2) . . . . ? C13 Fe C14 C17 -37.9(2) . . . . ? C18 Fe C14 C17 145.5(2) . . . . ? C19 Fe C14 C17 65.1(3) . . . . ? C22 Fe C14 C17 -177.9(2) . . . . ? C21 Fe C14 C17 102.2(2) . . . . ? C17 C13 C15 C16 0.2(4) . . . . ? P2 C13 C15 C16 177.1(3) . . . . ? Fe C13 C15 C16 59.6(2) . . . . ? C17 C13 C15 Fe -59.3(2) . . . . ? P2 C13 C15 Fe 117.6(3) . . . . ? C20 Fe C15 C16 141.4(2) . . . . ? C17 Fe C15 C16 -80.6(3) . . . . ? C13 Fe C15 C16 -118.9(3) . . . . ? C18 Fe C15 C16 60.6(3) . . . . ? C19 Fe C15 C16 177.6(2) . . . . ? C22 Fe C15 C16 97.9(3) . . . . ? C21 Fe C15 C16 45(2) . . . . ? C14 Fe C15 C16 -36.9(2) . . . . ? C20 Fe C15 C13 -99.7(2) . . . . ? C17 Fe C15 C13 38.3(2) . . . . ? C16 Fe C15 C13 118.9(3) . . . . ? C18 Fe C15 C13 179.5(2) . . . . ? C19 Fe C15 C13 -63.5(3) . . . . ? C22 Fe C15 C13 -143.2(2) . . . . ? C21 Fe C15 C13 164(2) . . . . ? C14 Fe C15 C13 81.9(2) . . . . ? C17 C14 C16 C15 -0.5(4) . . . . ? Fe C14 C16 C15 -59.2(3) . . . . ? C17 C14 C16 Fe 58.7(2) . . . . ? C13 C15 C16 C14 0.1(4) . . . . ? Fe C15 C16 C14 59.5(3) . . . . ? C13 C15 C16 Fe -59.4(2) . . . . ? C20 Fe C16 C14 178.1(2) . . . . ? C17 Fe C16 C14 -37.6(2) . . . . ? C15 Fe C16 C14 -120.1(3) . . . . ? C13 Fe C16 C14 -81.9(2) . . . . ? C18 Fe C16 C14 99.9(2) . . . . ? C19 Fe C16 C14 90(3) . . . . ? C22 Fe C16 C14 142.6(2) . . . . ? C21 Fe C16 C14 64.2(3) . . . . ? C20 Fe C16 C15 -61.9(3) . . . . ? C17 Fe C16 C15 82.5(2) . . . . ? C13 Fe C16 C15 38.2(2) . . . . ? C18 Fe C16 C15 -140.0(2) . . . . ? C19 Fe C16 C15 -150(3) . . . . ? C22 Fe C16 C15 -97.4(3) . . . . ? C21 Fe C16 C15 -175.7(2) . . . . ? C14 Fe C16 C15 120.1(3) . . . . ? C9 C7 C8 C12 1.4(5) . . . . ? C21 C18 C22 C20 -1.2(4) . . . . ? Fe C18 C22 C20 58.4(3) . . . . ? C21 C18 C22 Fe -59.7(2) . . . . ? C19 C20 C22 C18 1.4(4) . . . . ? Fe C20 C22 C18 -58.9(3) . . . . ? C19 C20 C22 Fe 60.3(2) . . . . ? C20 Fe C22 C18 120.0(3) . . . . ? C17 Fe C22 C18 -100(4) . . . . ? C16 Fe C22 C18 -95.8(2) . . . . ? C15 Fe C22 C18 -139.0(2) . . . . ? C13 Fe C22 C18 -175.5(2) . . . . ? C19 Fe C22 C18 81.6(2) . . . . ? C21 Fe C22 C18 37.4(2) . . . . ? C14 Fe C22 C18 -60.1(3) . . . . ? C17 Fe C22 C20 140(4) . . . . ? C16 Fe C22 C20 144.1(2) . . . . ? C15 Fe C22 C20 101.0(2) . . . . ? C13 Fe C22 C20 64.5(3) . . . . ? C18 Fe C22 C20 -120.0(3) . . . . ? C19 Fe C22 C20 -38.4(2) . . . . ? C21 Fe C22 C20 -82.6(2) . . . . ? C14 Fe C22 C20 179.9(2) . . . . ? C8 C7 C9 C10 -1.8(5) . . . . ? C8 C7 C9 P2 178.1(3) . . . . ? C13 P2 C9 C7 -111.8(3) . . . . ? C1 P2 C9 C7 139.0(3) . . . . ? Cu P2 C9 C7 10.7(3) . . . . ? C13 P2 C9 C10 68.1(3) . . . . ? C1 P2 C9 C10 -41.2(3) . . . . ? Cu P2 C9 C10 -169.5(2) . . . . ? C39 C35 C38 C40 -1.5(7) . . . . ? N C35 C38 C40 175.4(4) . . . . ? C7 C9 C10 C11 0.4(5) . . . . ? P2 C9 C10 C11 -179.4(3) . . . . ? C9 C10 C11 C12 1.4(6) . . . . ? C10 C11 C12 C8 -1.9(6) . . . . ? C7 C8 C12 C11 0.5(6) . . . . ? C16 C14 C17 C13 0.6(4) . . . . ? Fe C14 C17 C13 59.6(2) . . . . ? C16 C14 C17 Fe -59.0(3) . . . . ? C15 C13 C17 C14 -0.5(4) . . . . ? P2 C13 C17 C14 -177.6(2) . . . . ? Fe C13 C17 C14 -59.9(2) . . . . ? C15 C13 C17 Fe 59.4(2) . . . . ? P2 C13 C17 Fe -117.6(2) . . . . ? C20 Fe C17 C14 179.8(2) . . . . ? C16 Fe C17 C14 37.3(2) . . . . ? C15 Fe C17 C14 81.0(2) . . . . ? C13 Fe C17 C14 119.4(3) . . . . ? C18 Fe C17 C14 -55.9(3) . . . . ? C19 Fe C17 C14 -140.1(2) . . . . ? C22 Fe C17 C14 41(4) . . . . ? C21 Fe C17 C14 -95.3(2) . . . . ? C20 Fe C17 C13 60.4(3) . . . . ? C16 Fe C17 C13 -82.1(2) . . . . ? C15 Fe C17 C13 -38.3(2) . . . . ? C18 Fe C17 C13 -175.3(2) . . . . ? C19 Fe C17 C13 100.5(2) . . . . ? C22 Fe C17 C13 -78(4) . . . . ? C21 Fe C17 C13 145.3(2) . . . . ? C14 Fe C17 C13 -119.4(3) . . . . ? C5 C1 C3 C6 1.1(6) . . . . ? P2 C1 C3 C6 173.3(3) . . . . ? C28 C23 C25 C26 2.1(7) . . . . ? P1 C23 C25 C26 175.8(3) . . . . ? C29 C30 C31 C33 -1.8(6) . . . . ? P1 C30 C31 C33 176.7(3) . . . . ? C6 C2 C4 C5 0.8(7) . . . . ? C2 C4 C5 C1 0.0(6) . . . . ? C3 C1 C5 C4 -1.0(6) . . . . ? P2 C1 C5 C4 -173.3(3) . . . . ? C23 C25 C26 C27 -0.1(8) . . . . ? C30 C29 C32 C34 -0.2(6) . . . . ? C30 C31 C33 C34 1.6(7) . . . . ? C38 C35 C39 C37 0.3(6) . . . . ? N C35 C39 C37 -176.5(4) . . . . ? C36 C37 C39 C35 0.6(7) . . . . ? C4 C2 C6 C3 -0.7(7) . . . . ? C1 C3 C6 C2 -0.3(7) . . . . ? C37 C36 C40 C38 -0.7(8) . . . . ? Cl C36 C40 C38 178.3(4) . . . . ? C35 C38 C40 C36 1.7(8) . . . . ? C25 C26 C27 C24 -1.4(8) . . . . ? C28 C24 C27 C26 1.0(9) . . . . ? C27 C24 C28 C23 1.1(9) . . . . ? C25 C23 C28 C24 -2.6(7) . . . . ? P1 C23 C28 C24 -176.7(4) . . . . ? C29 C32 C34 C33 0.0(7) . . . . ? C31 C33 C34 C32 -0.7(7) . . . . ? C35 N C41 O 2.1(5) . . . . ? Cu N C41 O -164.8(3) . . . . ? C35 N C41 C42 -176.0(3) . . . . ? Cu N C41 C42 17.0(5) . . . . ? O C41 C42 F1 50.4(5) . . . . ? N C41 C42 F1 -131.2(4) . . . . ? O C41 C42 F2 -67.9(5) . . . . ? N C41 C42 F2 110.5(4) . . . . ? O C41 C42 F3 171.3(3) . . . . ? N C41 C42 F3 -10.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.396 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.067